# Electronic Supplementary Material (ESI) for ChemComm. # This journal is © The Royal Society of Chemistry 2022 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_lb1231 _database_code_depnum_ccdc_archive 'CCDC 2126561' loop_ _audit_author_name _audit_author_address 'Rosario Scopelliti' ;EPFL Switzerland ; _audit_update_record ; 2021-12-06 deposited with the CCDC. 2022-03-10 downloaded from the CCDC. ; _audit_creation_date 2021-03-02 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C66 H121 Mo N Na O12 P2 Si3 U, C6 H14' _chemical_formula_sum 'C72 H135 Mo N Na O12 P2 Si3 U' _chemical_formula_weight 1709.97 _chemical_melting_point ? _chemical_oxdiff_formula 'C72 H135 N1 O12 Na1 Si3 P2 Mo1 U1' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6525(2) _cell_length_b 16.4788(4) _cell_length_c 19.2469(4) _cell_angle_alpha 81.3024(19) _cell_angle_beta 79.5672(16) _cell_angle_gamma 82.5868(18) _cell_volume 4186.49(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 38652 _cell_measurement_temperature 140.00(10) _cell_measurement_theta_max 75.9200 _cell_measurement_theta_min 3.8110 _shelx_estimated_absorpt_T_max 0.319 _shelx_estimated_absorpt_T_min 0.147 _exptl_absorpt_coefficient_mu 7.873 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_correction_T_min 0.194 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'translucent dark black' _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description irregular _exptl_crystal_F_000 1774 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.1437 1 0 2 0.1480 2 -1 -2 0.1378 0 1 2 0.1294 1 1 2 0.1395 0 1 1 0.0969 -2 -1 0 0.1670 1 -1 -1 0.1208 0 1 0 0.1249 2 10 -1 0.1274 -8 0 4 0.1659 0 8 -7 0.1185 2 7 -8 0.1118 -2 8 -6 0.1290 4 -8 4 0.1207 0 5 -10 0.1097 3 3 -10 0.1065 -6 6 -6 0.1523 0 -5 -11 0.1066 -8 -4 -8 0.1438 4 -4 -9 0.0971 0 -10 -5 0.0851 -6 -9 -3 0.1106 2 -9 -5 0.0849 1 -10 3 0.0894 3 -10 2 0.0909 -4 -8 5 0.1250 0 -5 10 0.1230 4 -6 8 0.1232 0 9 7 0.0909 _exptl_crystal_size_max 0.395 _exptl_crystal_size_mid 0.233 _exptl_crystal_size_min 0.188 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0000 -0.0000 1.0000 0.0315 -0.0676 0.0343 1.0000 -0.0001 2.0000 0.0950 -0.1528 -0.0408 2.0000 -1.0000 -2.0000 -0.0704 0.0405 -0.3092 -0.0000 1.0000 2.0000 0.1342 -0.0758 0.0903 1.0000 0.9999 2.0000 0.1661 -0.0934 -0.0191 -0.0000 1.0000 1.0000 0.1026 -0.0082 0.0560 -2.0000 -1.0000 -0.0000 -0.1349 -0.0240 0.1973 1.0000 -1.0000 -1.0000 -0.0707 -0.0094 -0.1654 -0.0000 1.0000 -0.0000 0.0711 0.0593 0.0216 1.8943 10.3079 -1.0590 0.7598 0.6498 -0.0208 -7.8266 -0.0683 3.7355 -0.1366 -0.1183 0.9835 0.2266 7.7317 -7.1496 0.3314 0.9378 -0.1032 1.7324 7.0571 -7.5798 0.3179 0.9003 -0.2974 -1.8619 8.1607 -6.0948 0.3285 0.9289 0.1709 4.1630 -7.8680 4.2403 -0.2928 -0.8269 -0.4802 -0.0735 4.8602 -10.0986 0.0246 0.9720 -0.2337 2.7259 3.4575 -9.8981 0.0205 0.8258 -0.5636 -5.8393 5.5446 -5.8980 0.0219 0.8306 0.5565 0.0463 -5.3227 -11.3288 -0.7343 0.4487 -0.5093 -7.6765 -3.5081 -7.7872 -0.7399 0.4535 0.4969 4.2357 -4.2078 -8.7811 -0.4411 0.2688 -0.8563 0.0062 -10.1579 -5.0451 -0.8811 -0.2620 -0.3936 -5.6412 -9.0579 -2.5182 -0.9033 -0.2678 0.3351 2.4038 -9.0469 -5.3345 -0.7348 -0.2189 -0.6420 0.7363 -9.8755 2.6380 -0.5954 -0.7772 -0.2035 2.5374 -9.5470 1.5588 -0.5486 -0.7166 -0.4307 -3.9627 -8.0514 4.6287 -0.5528 -0.7205 0.4186 0.0171 -4.8438 10.1034 -0.0251 -0.9703 0.2404 4.0074 -5.7340 8.1026 -0.0242 -0.9584 -0.2843 0.0158 9.3544 7.1723 0.8918 0.0702 0.4469 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_unetI/netI 0.0252 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 49516 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.009 _diffrn_reflns_theta_min 3.310 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 140.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2817 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -52.00 25.00 1.00 2.00 -- -40.91 89.00 172.00 77 2 \w 10.00 35.00 1.00 2.00 -- 40.91 -89.00 57.00 25 3 \w 43.00 68.00 1.00 8.00 -- 112.00 -89.00 57.00 25 4 \w 104.00 135.00 1.00 8.00 -- 112.00 89.00 172.00 31 5 \w -115.00 -31.00 1.00 2.00 -- -40.91 -38.00 90.00 84 6 \w -77.00 -27.00 1.00 2.00 -- -40.91 125.00 60.00 50 7 \w 13.00 113.00 1.00 2.00 -- 40.91 57.00 -60.00 100 8 \w 31.00 97.00 1.00 2.00 -- 40.91-125.00 0.00 66 9 \w 16.00 111.00 1.00 2.00 -- 40.91 38.00 60.00 95 10 \w 55.00 109.00 1.00 8.00 -- 112.00-111.00-180.00 54 11 \w 86.00 172.00 1.00 8.00 -- 112.00 45.00-150.00 86 12 \w 36.00 140.00 1.00 8.00 -- 112.00 -30.00 30.00 104 13 \w 30.00 63.00 1.00 8.00 -- 112.00 -94.00 0.00 33 14 \w 47.00 74.00 1.00 8.00 -- 112.00 -77.00 120.00 27 15 \w 75.00 107.00 1.00 8.00 -- 112.00 -94.00 0.00 32 16 \w 113.00 144.00 1.00 8.00 -- 112.00 77.00 -60.00 31 17 \w 64.00 90.00 1.00 8.00 -- 112.00 178.00-150.00 26 18 \w 89.00 118.00 1.00 8.00 -- 112.00 -61.00 -60.00 29 19 \w 74.00 100.00 1.00 8.00 -- 112.00 178.00 0.00 26 20 \w 88.00 172.00 1.00 8.00 -- 112.00 45.00-120.00 84 21 \w 41.00 101.00 1.00 8.00 -- 112.00 -61.00-150.00 60 22 \w 50.00 109.00 1.00 8.00 -- 112.00-111.00 -30.00 59 23 \w 85.00 117.00 1.00 8.00 -- 112.00 -45.00 60.00 32 24 \w 92.00 119.00 1.00 8.00 -- 112.00 -77.00 120.00 27 25 \w 106.00 158.00 1.00 8.00 -- 112.00 111.00 -60.00 52 26 \w 39.00 97.00 1.00 8.00 -- 112.00-111.00 -60.00 58 27 \w 31.00 63.00 1.00 8.00 -- 112.00 -15.00 -30.00 32 28 \w 140.00 165.00 1.00 8.00 -- 112.00 -15.00 -30.00 25 29 \w 39.00 87.00 1.00 8.00 -- 112.00 -45.00 0.00 48 30 \w 75.00 108.00 1.00 8.00 -- 112.00-111.00-150.00 33 31 \w 68.00 109.00 1.00 8.00 -- 112.00-111.00 0.00 41 32 \w 41.00 67.00 1.00 8.00 -- 112.00 -61.00 -60.00 26 33 \w 55.00 109.00 1.00 8.00 -- 112.00-111.00 120.00 54 34 \w 77.00 109.00 1.00 8.00 -- 112.00-111.00 -90.00 32 35 \w 32.00 102.00 1.00 8.00 -- 112.00 -94.00 30.00 70 36 \w 61.00 115.00 1.00 8.00 -- 112.00 178.00 90.00 54 37 \w 34.00 75.00 1.00 8.00 -- 112.00 -94.00-150.00 41 38 \w 74.00 109.00 1.00 8.00 -- 112.00-111.00-120.00 35 39 \w 42.00 69.00 1.00 8.00 -- 112.00-111.00 90.00 27 40 \w 71.00 108.00 1.00 8.00 -- 112.00-111.00 90.00 37 41 \w 62.00 105.00 1.00 8.00 -- 112.00-111.00 150.00 43 42 \w 106.00 133.00 1.00 8.00 -- 112.00 111.00-120.00 27 43 \w 67.00 138.00 1.00 8.00 -- 112.00 -30.00-180.00 71 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0318941000 _diffrn_orient_matrix_UB_12 0.0710943000 _diffrn_orient_matrix_UB_13 0.0315469000 _diffrn_orient_matrix_UB_21 -0.0176515000 _diffrn_orient_matrix_UB_22 0.0593396000 _diffrn_orient_matrix_UB_23 -0.0675625000 _diffrn_orient_matrix_UB_31 -0.1094596000 _diffrn_orient_matrix_UB_32 0.0216254000 _diffrn_orient_matrix_UB_33 0.0343496000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 17102 _reflns_number_total 17241 _reflns_odcompleteness_completeness 99.47 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 1.724 _refine_diff_density_min -2.013 _refine_diff_density_rms 0.085 _refine_ls_extinction_coef 0.000193(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 876 _refine_ls_number_reflns 17241 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0268 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+3.4796P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.0717 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C92-C91 \\sim C93-C92 \\sim C94-C93 \\sim C95-C94 \\sim C96-C95 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 4.a Ternary CH refined with riding coordinates: C73(H73), C76(H76), C85(H85), C88(H88) 4.b Secondary CH2 refined with riding coordinates: C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B) 4.c Aromatic/amide H refined with riding coordinates: C62(H62), C63(H63), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C80(H80), C81(H81), C82(H82), C83(H83) 4.d Idealised Me refined as rotating group: C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A, H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A, H12B,H12C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B, H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C43(H43A, H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B, H52C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A, H78B,H78C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C96(H96A,H96B,H96C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.73448(2) 0.34333(2) 0.76633(2) 0.02020(4) Uani 1 1 d . . . . . Mo1 Mo 0.73992(2) 0.51601(2) 0.81041(2) 0.01987(5) Uani 1 1 d . . . . . P1 P 0.62701(5) 0.61826(4) 0.74331(3) 0.02334(12) Uani 1 1 d . . . . . P2 P 0.91743(5) 0.54586(4) 0.77922(4) 0.02570(13) Uani 1 1 d . . . . . Si1 Si 0.78912(6) 0.14369(5) 0.88856(4) 0.02676(14) Uani 1 1 d . . . . . Si2 Si 0.48629(5) 0.26291(5) 0.75974(4) 0.02683(14) Uani 1 1 d . . . . . Si3 Si 0.84740(6) 0.22276(5) 0.60986(4) 0.02677(14) Uani 1 1 d . . . . . Na08 Na 0.69788(8) 0.15101(7) 0.74223(6) 0.0275(2) Uani 1 1 d . . . . . O1 O 0.76940(16) 0.22880(12) 0.83835(11) 0.0319(4) Uani 1 1 d . . . . . O2 O 0.90369(16) 0.12306(13) 0.90262(11) 0.0328(4) Uani 1 1 d . . . . . O3 O 0.71842(16) 0.13422(14) 0.96602(11) 0.0347(4) Uani 1 1 d . . . . . O4 O 0.75721(16) 0.07310(12) 0.84655(11) 0.0304(4) Uani 1 1 d . . . . . O21 O 0.58908(14) 0.29206(13) 0.77019(11) 0.0310(4) Uani 1 1 d . . . . . O22 O 0.43969(15) 0.31289(13) 0.69218(11) 0.0321(4) Uani 1 1 d . . . . . O23 O 0.51689(14) 0.16702(13) 0.74100(11) 0.0309(4) Uani 1 1 d . . . . . O24 O 0.39668(14) 0.26698(13) 0.82762(11) 0.0317(4) Uani 1 1 d . . . . . O41 O 0.79675(15) 0.26436(12) 0.67905(10) 0.0291(4) Uani 1 1 d . . . . . O42 O 0.96834(15) 0.20389(14) 0.59898(12) 0.0342(4) Uani 1 1 d . . . . . O43 O 0.82366(17) 0.27332(14) 0.53436(11) 0.0365(5) Uani 1 1 d . . . . . O44 O 0.80183(15) 0.13169(13) 0.62579(11) 0.0297(4) Uani 1 1 d . . . . . N1 N 0.75766(17) 0.44897(14) 0.72076(12) 0.0254(4) Uani 1 1 d . . . . . C1 C 0.9987(2) 0.1373(2) 0.85854(18) 0.0371(6) Uani 1 1 d . . . . . C2 C 0.9962(3) 0.1274(3) 0.7818(2) 0.0599(12) Uani 1 1 d . . . . . H2A H 1.062917 0.132497 0.753493 0.090 Uiso 1 1 calc R U . . . H2B H 0.948051 0.170408 0.762555 0.090 Uiso 1 1 calc R U . . . H2C H 0.975967 0.072967 0.779905 0.090 Uiso 1 1 calc R U . . . C3 C 1.0751(3) 0.0730(3) 0.8887(2) 0.0489(8) Uani 1 1 d . . . . . H3A H 1.059536 0.017773 0.884413 0.073 Uiso 1 1 calc R U . . . H3B H 1.073153 0.077995 0.939088 0.073 Uiso 1 1 calc R U . . . H3C H 1.142162 0.081711 0.862256 0.073 Uiso 1 1 calc R U . . . C4 C 1.0210(3) 0.2231(3) 0.8663(3) 0.0665(13) Uani 1 1 d . . . . . H4A H 1.086675 0.233782 0.838418 0.100 Uiso 1 1 calc R U . . . H4B H 1.021343 0.226754 0.916598 0.100 Uiso 1 1 calc R U . . . H4C H 0.969405 0.264133 0.848863 0.100 Uiso 1 1 calc R U . . . C5 C 0.7106(3) 0.1648(2) 1.03318(16) 0.0378(7) Uani 1 1 d . . . . . C6 C 0.6303(3) 0.2384(2) 1.0349(2) 0.0474(8) Uani 1 1 d . . . . . H6A H 0.621344 0.259216 1.080951 0.071 Uiso 1 1 calc R U . . . H6B H 0.566909 0.221089 1.028273 0.071 Uiso 1 1 calc R U . . . H6C H 0.650975 0.282154 0.996552 0.071 Uiso 1 1 calc R U . . . C7 C 0.8092(3) 0.1900(3) 1.0436(2) 0.0564(10) Uani 1 1 d . . . . . H7A H 0.828774 0.235804 1.007007 0.085 Uiso 1 1 calc R U . . . H7B H 0.860862 0.142972 1.039552 0.085 Uiso 1 1 calc R U . . . H7C H 0.801832 0.207410 1.090879 0.085 Uiso 1 1 calc R U . . . C8 C 0.6757(4) 0.0944(3) 1.0895(2) 0.0625(11) Uani 1 1 d . . . . . H8A H 0.664101 0.112587 1.136744 0.094 Uiso 1 1 calc R U . . . H8B H 0.727163 0.047090 1.087978 0.094 Uiso 1 1 calc R U . . . H8C H 0.613283 0.078182 1.079954 0.094 Uiso 1 1 calc R U . . . C9 C 0.7507(2) -0.01392(18) 0.87222(18) 0.0355(6) Uani 1 1 d . . . . . C10 C 0.7657(3) -0.0576(2) 0.8067(2) 0.0533(9) Uani 1 1 d . . . . . H10A H 0.761589 -0.116796 0.821301 0.080 Uiso 1 1 calc R U . . . H10B H 0.831592 -0.048823 0.778373 0.080 Uiso 1 1 calc R U . . . H10C H 0.713469 -0.035294 0.778035 0.080 Uiso 1 1 calc R U . . . C11 C 0.6466(3) -0.0240(2) 0.9141(2) 0.0494(8) Uani 1 1 d . . . . . H11A H 0.596446 0.000321 0.884242 0.074 Uiso 1 1 calc R U . . . H11B H 0.636819 0.003935 0.956645 0.074 Uiso 1 1 calc R U . . . H11C H 0.639173 -0.082865 0.928347 0.074 Uiso 1 1 calc R U . . . C12 C 0.8304(3) -0.0490(2) 0.9179(2) 0.0522(9) Uani 1 1 d . . . . . H12A H 0.827689 -0.108656 0.930539 0.078 Uiso 1 1 calc R U . . . H12B H 0.818009 -0.022577 0.961423 0.078 Uiso 1 1 calc R U . . . H12C H 0.896652 -0.038368 0.891089 0.078 Uiso 1 1 calc R U . . . C21 C 0.3792(3) 0.3909(2) 0.6832(2) 0.0432(8) Uani 1 1 d . . . . . C22 C 0.2708(3) 0.3726(4) 0.6987(5) 0.097(2) Uani 1 1 d . . . . . H22A H 0.259861 0.336531 0.665371 0.146 Uiso 1 1 calc R U . . . H22B H 0.227087 0.424381 0.693111 0.146 Uiso 1 1 calc R U . . . H22C H 0.255469 0.345075 0.747633 0.146 Uiso 1 1 calc R U . . . C23 C 0.4121(5) 0.4284(3) 0.6072(2) 0.0804(18) Uani 1 1 d . . . . . H23A H 0.482984 0.437302 0.600304 0.121 Uiso 1 1 calc R U . . . H23B H 0.371941 0.481303 0.597503 0.121 Uiso 1 1 calc R U . . . H23C H 0.402628 0.390870 0.574611 0.121 Uiso 1 1 calc R U . . . C24 C 0.3964(4) 0.4475(2) 0.7340(2) 0.0573(10) Uani 1 1 d . . . . . H24A H 0.376822 0.422255 0.783275 0.086 Uiso 1 1 calc R U . . . H24B H 0.356139 0.500662 0.725759 0.086 Uiso 1 1 calc R U . . . H24C H 0.467496 0.456245 0.725944 0.086 Uiso 1 1 calc R U . . . C25 C 0.4545(2) 0.1159(2) 0.71576(18) 0.0346(6) Uani 1 1 d . . . . . C26 C 0.4645(3) 0.1364(2) 0.6355(2) 0.0460(8) Uani 1 1 d . . . . . H26A H 0.438196 0.194008 0.623333 0.069 Uiso 1 1 calc R U . . . H26B H 0.426413 0.100071 0.617292 0.069 Uiso 1 1 calc R U . . . H26C H 0.535189 0.128293 0.614012 0.069 Uiso 1 1 calc R U . . . C27 C 0.4954(3) 0.0269(2) 0.7370(2) 0.0428(7) Uani 1 1 d . . . . . H27A H 0.566627 0.018717 0.716607 0.064 Uiso 1 1 calc R U . . . H27B H 0.458603 -0.010471 0.718926 0.064 Uiso 1 1 calc R U . . . H27C H 0.487441 0.015136 0.789030 0.064 Uiso 1 1 calc R U . . . C28 C 0.3445(2) 0.1289(2) 0.7507(2) 0.0481(9) Uani 1 1 d . . . . . H28A H 0.339187 0.114752 0.802479 0.072 Uiso 1 1 calc R U . . . H28B H 0.305321 0.093390 0.732529 0.072 Uiso 1 1 calc R U . . . H28C H 0.318538 0.186775 0.739468 0.072 Uiso 1 1 calc R U . . . C29 C 0.3902(2) 0.2383(2) 0.90252(16) 0.0330(6) Uani 1 1 d . . . . . C30 C 0.2837(2) 0.2146(2) 0.9288(2) 0.0436(8) Uani 1 1 d . . . . . H30A H 0.235494 0.259715 0.912789 0.065 Uiso 1 1 calc R U . . . H30B H 0.271819 0.204232 0.980997 0.065 Uiso 1 1 calc R U . . . H30C H 0.275724 0.164531 0.909503 0.065 Uiso 1 1 calc R U . . . C31 C 0.4669(3) 0.1639(2) 0.91524(19) 0.0441(8) Uani 1 1 d . . . . . H31A H 0.455065 0.119562 0.890131 0.066 Uiso 1 1 calc R U . . . H31B H 0.460401 0.144593 0.966420 0.066 Uiso 1 1 calc R U . . . H31C H 0.534509 0.179954 0.897353 0.066 Uiso 1 1 calc R U . . . C32 C 0.4059(3) 0.3089(2) 0.9398(2) 0.0453(8) Uani 1 1 d . . . . . H32A H 0.474627 0.323326 0.924192 0.068 Uiso 1 1 calc R U . . . H32B H 0.394596 0.292312 0.991413 0.068 Uiso 1 1 calc R U . . . H32C H 0.358714 0.356881 0.927774 0.068 Uiso 1 1 calc R U . . . C41 C 1.0509(3) 0.2428(3) 0.5553(2) 0.0460(8) Uani 1 1 d . . . . . C42 C 1.1391(3) 0.2174(4) 0.5949(3) 0.0752(15) Uani 1 1 d . . . . . H42A H 1.123149 0.237129 0.641623 0.113 Uiso 1 1 calc R U . . . H42B H 1.198408 0.241531 0.567337 0.113 Uiso 1 1 calc R U . . . H42C H 1.152432 0.157072 0.601379 0.113 Uiso 1 1 calc R U . . . C43 C 1.0292(4) 0.3357(3) 0.5447(2) 0.0575(10) Uani 1 1 d . . . . . H43A H 0.977512 0.351581 0.514394 0.086 Uiso 1 1 calc R U . . . H43B H 1.090422 0.360460 0.521741 0.086 Uiso 1 1 calc R U . . . H43C H 1.005454 0.355351 0.591003 0.086 Uiso 1 1 calc R U . . . C44 C 1.0711(4) 0.2116(4) 0.4827(3) 0.0805(18) Uani 1 1 d . . . . . H44A H 1.084650 0.151341 0.489184 0.121 Uiso 1 1 calc R U . . . H44B H 1.129176 0.235810 0.453198 0.121 Uiso 1 1 calc R U . . . H44C H 1.012304 0.227731 0.459111 0.121 Uiso 1 1 calc R U . . . C45 C 0.7364(3) 0.3217(2) 0.51263(17) 0.0409(7) Uani 1 1 d . . . . . C46 C 0.6430(3) 0.2783(3) 0.5433(2) 0.0526(9) Uani 1 1 d . . . . . H46A H 0.652619 0.222435 0.529807 0.079 Uiso 1 1 calc R U . . . H46B H 0.585212 0.309413 0.524517 0.079 Uiso 1 1 calc R U . . . H46C H 0.631233 0.275018 0.595383 0.079 Uiso 1 1 calc R U . . . C47 C 0.7558(3) 0.3289(3) 0.43148(19) 0.0534(9) Uani 1 1 d . . . . . H47A H 0.818623 0.353347 0.412916 0.080 Uiso 1 1 calc R U . . . H47B H 0.700526 0.364006 0.412558 0.080 Uiso 1 1 calc R U . . . H47C H 0.760740 0.273874 0.416820 0.080 Uiso 1 1 calc R U . . . C48 C 0.7292(4) 0.4064(3) 0.5359(2) 0.0569(10) Uani 1 1 d . . . . . H48A H 0.722733 0.400843 0.587939 0.085 Uiso 1 1 calc R U . . . H48B H 0.670489 0.440392 0.520827 0.085 Uiso 1 1 calc R U . . . H48C H 0.789788 0.432751 0.514105 0.085 Uiso 1 1 calc R U . . . C49 C 0.8335(2) 0.06091(19) 0.58700(18) 0.0361(7) Uani 1 1 d . . . . . C50 C 0.9270(3) 0.0148(2) 0.6131(2) 0.0497(9) Uani 1 1 d . . . . . H50A H 0.946311 -0.035630 0.590522 0.075 Uiso 1 1 calc R U . . . H50B H 0.912988 0.000352 0.664935 0.075 Uiso 1 1 calc R U . . . H50C H 0.981762 0.050131 0.600522 0.075 Uiso 1 1 calc R U . . . C51 C 0.8529(3) 0.0877(2) 0.5071(2) 0.0488(9) Uani 1 1 d . . . . . H51A H 0.909207 0.121412 0.495125 0.073 Uiso 1 1 calc R U . . . H51B H 0.792958 0.120119 0.492418 0.073 Uiso 1 1 calc R U . . . H51C H 0.869057 0.038781 0.482192 0.073 Uiso 1 1 calc R U . . . C52 C 0.7483(3) 0.0068(2) 0.6054(2) 0.0439(8) Uani 1 1 d . . . . . H52A H 0.765366 -0.041250 0.579532 0.066 Uiso 1 1 calc R U . . . H52B H 0.687216 0.038454 0.591899 0.066 Uiso 1 1 calc R U . . . H52C H 0.737200 -0.011709 0.656817 0.066 Uiso 1 1 calc R U . . . C61 C 0.59656(18) 0.51662(16) 0.88629(13) 0.0236(5) Uani 1 1 d . . . . . C62 C 0.6383(2) 0.43303(17) 0.88638(13) 0.0242(5) Uani 1 1 d . . . . . H62 H 0.599788 0.392506 0.878025 0.029 Uiso 1 1 calc R U . . . C63 C 0.7407(2) 0.40998(16) 0.89939(14) 0.0246(5) Uani 1 1 d . . . . . H63 H 0.769573 0.354382 0.899162 0.030 Uiso 1 1 calc R U . . . C64 C 0.79740(19) 0.47155(17) 0.91249(13) 0.0240(5) Uani 1 1 d . . . . . C65 C 0.7514(2) 0.55399(17) 0.91770(14) 0.0255(5) Uani 1 1 d . . . . . H65 H 0.787291 0.593792 0.930285 0.031 Uiso 1 1 calc R U . . . C66 C 0.6526(2) 0.57598(17) 0.90410(14) 0.0245(5) Uani 1 1 d . . . . . H66 H 0.622833 0.631040 0.906794 0.029 Uiso 1 1 calc R U . . . C67 C 0.49953(19) 0.55117(16) 0.86271(14) 0.0251(5) Uani 1 1 d . . . . . C68 C 0.4079(2) 0.53657(18) 0.90636(16) 0.0300(6) Uani 1 1 d . . . . . H68 H 0.406806 0.499288 0.949214 0.036 Uiso 1 1 calc R U . . . C69 C 0.3191(2) 0.5762(2) 0.88734(18) 0.0349(6) Uani 1 1 d . . . . . H69 H 0.257005 0.564543 0.916111 0.042 Uiso 1 1 calc R U . . . C70 C 0.3208(2) 0.6331(2) 0.82620(18) 0.0347(6) Uani 1 1 d . . . . . H70 H 0.259958 0.661569 0.813974 0.042 Uiso 1 1 calc R U . . . C71 C 0.4113(2) 0.64859(18) 0.78278(17) 0.0309(6) Uani 1 1 d . . . . . H71 H 0.411882 0.688577 0.741643 0.037 Uiso 1 1 calc R U . . . C72 C 0.50199(19) 0.60585(17) 0.79896(15) 0.0254(5) Uani 1 1 d . . . . . C73 C 0.6143(2) 0.59138(18) 0.65448(15) 0.0298(6) Uani 1 1 d . . . . . H73 H 0.611643 0.530264 0.661682 0.036 Uiso 1 1 calc R U . . . C74 C 0.5221(3) 0.6278(2) 0.62183(18) 0.0404(7) Uani 1 1 d . . . . . H74A H 0.461804 0.610775 0.653904 0.061 Uiso 1 1 calc R U . . . H74B H 0.525952 0.607896 0.575839 0.061 Uiso 1 1 calc R U . . . H74C H 0.519174 0.688158 0.614733 0.061 Uiso 1 1 calc R U . . . C75 C 0.7094(2) 0.6065(2) 0.60018(17) 0.0384(7) Uani 1 1 d . . . . . H75A H 0.708345 0.665432 0.582184 0.058 Uiso 1 1 calc R U . . . H75B H 0.712326 0.574946 0.560441 0.058 Uiso 1 1 calc R U . . . H75C H 0.768426 0.588690 0.623229 0.058 Uiso 1 1 calc R U . . . C76 C 0.6215(2) 0.73374(18) 0.72861(17) 0.0316(6) Uani 1 1 d . . . . . H76 H 0.569380 0.754786 0.698037 0.038 Uiso 1 1 calc R U . . . C77 C 0.5911(3) 0.7721(2) 0.7977(2) 0.0436(8) Uani 1 1 d . . . . . H77A H 0.527875 0.752675 0.823360 0.065 Uiso 1 1 calc R U . . . H77B H 0.582438 0.832382 0.786614 0.065 Uiso 1 1 calc R U . . . H77C H 0.643321 0.755955 0.827421 0.065 Uiso 1 1 calc R U . . . C78 C 0.7206(3) 0.7645(2) 0.6893(2) 0.0443(8) Uani 1 1 d . . . . . H78A H 0.775291 0.738207 0.714298 0.066 Uiso 1 1 calc R U . . . H78B H 0.716500 0.824532 0.687866 0.066 Uiso 1 1 calc R U . . . H78C H 0.733405 0.750450 0.640533 0.066 Uiso 1 1 calc R U . . . C79 C 0.9071(2) 0.45627(17) 0.91423(15) 0.0267(5) Uani 1 1 d . . . . . C80 C 0.9444(2) 0.40572(19) 0.97061(16) 0.0333(6) Uani 1 1 d . . . . . H80 H 0.899809 0.379500 1.008568 0.040 Uiso 1 1 calc R U . . . C81 C 1.0470(3) 0.3938(2) 0.97106(18) 0.0378(7) Uani 1 1 d . . . . . H81 H 1.072424 0.358433 1.008928 0.045 Uiso 1 1 calc R U . . . C82 C 1.1121(2) 0.4330(2) 0.91705(19) 0.0394(7) Uani 1 1 d . . . . . H82 H 1.181886 0.425707 0.918486 0.047 Uiso 1 1 calc R U . . . C83 C 1.0760(2) 0.4828(2) 0.86075(18) 0.0356(6) Uani 1 1 d . . . . . H83 H 1.121438 0.509143 0.823464 0.043 Uiso 1 1 calc R U . . . C84 C 0.9729(2) 0.49482(18) 0.85806(16) 0.0297(6) Uani 1 1 d . . . . . C85 C 1.0067(2) 0.4963(2) 0.70874(17) 0.0351(6) Uani 1 1 d . . . . . H85 H 1.075523 0.509501 0.710803 0.042 Uiso 1 1 calc R U . . . C86 C 1.0060(3) 0.4030(2) 0.72295(19) 0.0443(8) Uani 1 1 d . . . . . H86A H 1.015136 0.383531 0.772294 0.066 Uiso 1 1 calc R U . . . H86B H 1.060620 0.377045 0.690396 0.066 Uiso 1 1 calc R U . . . H86C H 0.941856 0.388208 0.715324 0.066 Uiso 1 1 calc R U . . . C87 C 0.9826(3) 0.5303(2) 0.63457(18) 0.0440(8) Uani 1 1 d . . . . . H87A H 0.918405 0.513068 0.629607 0.066 Uiso 1 1 calc R U . . . H87B H 1.035552 0.508957 0.598294 0.066 Uiso 1 1 calc R U . . . H87C H 0.978308 0.590750 0.628296 0.066 Uiso 1 1 calc R U . . . C88 C 0.9548(2) 0.6537(2) 0.76284(18) 0.0356(6) Uani 1 1 d . . . . . H88 H 0.932500 0.679765 0.717141 0.043 Uiso 1 1 calc R U . . . C89 C 0.8979(3) 0.7048(2) 0.8201(2) 0.0452(8) Uani 1 1 d . . . . . H89A H 0.826075 0.700023 0.825304 0.068 Uiso 1 1 calc R U . . . H89B H 0.910143 0.762797 0.806128 0.068 Uiso 1 1 calc R U . . . H89C H 0.921017 0.684415 0.865480 0.068 Uiso 1 1 calc R U . . . C90 C 1.0668(3) 0.6635(3) 0.7535(3) 0.0586(11) Uani 1 1 d . . . . . H90A H 1.091056 0.644000 0.798628 0.088 Uiso 1 1 calc R U . . . H90B H 1.077208 0.721836 0.739205 0.088 Uiso 1 1 calc R U . . . H90C H 1.103712 0.630990 0.716622 0.088 Uiso 1 1 calc R U . . . C91 C 0.8714(6) 0.0972(5) 0.2565(5) 0.124(3) Uani 1 1 d D U . . . H91A H 0.904359 0.131293 0.214766 0.186 Uiso 1 1 calc R U . . . H91B H 0.863148 0.043651 0.243207 0.186 Uiso 1 1 calc R U . . . H91C H 0.912473 0.088763 0.294253 0.186 Uiso 1 1 calc R U . . . C92 C 0.7691(4) 0.1405(4) 0.2831(4) 0.0850(16) Uani 1 1 d D U . . . H92A H 0.778893 0.193619 0.297682 0.102 Uiso 1 1 calc R U . . . H92B H 0.730990 0.153433 0.242948 0.102 Uiso 1 1 calc R U . . . C93 C 0.7060(4) 0.0924(3) 0.3452(3) 0.0730(14) Uani 1 1 d D U . . . H93A H 0.696749 0.038970 0.330899 0.088 Uiso 1 1 calc R U . . . H93B H 0.743547 0.080126 0.385650 0.088 Uiso 1 1 calc R U . . . C94 C 0.6049(4) 0.1353(2) 0.3703(3) 0.0631(11) Uani 1 1 d D U . . . H94A H 0.567477 0.147236 0.329800 0.076 Uiso 1 1 calc R U . . . H94B H 0.614394 0.188878 0.384113 0.076 Uiso 1 1 calc R U . . . C95 C 0.5412(5) 0.0888(3) 0.4323(3) 0.0744(14) Uani 1 1 d D U . . . H95A H 0.536077 0.033385 0.420107 0.089 Uiso 1 1 calc R U . . . H95B H 0.575937 0.080861 0.474119 0.089 Uiso 1 1 calc R U . . . C96 C 0.4388(5) 0.1290(4) 0.4528(3) 0.0862(18) Uani 1 1 d D U . . . H96A H 0.404054 0.138776 0.411508 0.129 Uiso 1 1 calc R U . . . H96B H 0.442589 0.181791 0.469260 0.129 Uiso 1 1 calc R U . . . H96C H 0.401855 0.093114 0.491223 0.129 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01678(5) 0.02153(5) 0.02206(5) -0.00429(3) -0.00206(3) -0.00105(3) Mo1 0.01691(9) 0.02166(9) 0.02080(9) -0.00370(7) -0.00204(7) -0.00161(7) P1 0.0192(3) 0.0246(3) 0.0251(3) -0.0014(2) -0.0029(2) -0.0017(2) P2 0.0180(3) 0.0294(3) 0.0286(3) -0.0038(3) -0.0020(2) -0.0009(2) Si1 0.0283(3) 0.0255(3) 0.0262(3) -0.0009(3) -0.0070(3) -0.0016(3) Si2 0.0183(3) 0.0319(4) 0.0316(4) -0.0099(3) -0.0016(3) -0.0045(3) Si3 0.0266(3) 0.0279(3) 0.0244(3) -0.0078(3) 0.0010(3) 0.0002(3) Na08 0.0242(5) 0.0287(5) 0.0284(5) -0.0034(4) -0.0032(4) -0.0007(4) O1 0.0376(11) 0.0258(9) 0.0307(10) 0.0009(8) -0.0075(8) 0.0004(8) O2 0.0294(10) 0.0351(11) 0.0337(10) -0.0006(8) -0.0082(8) -0.0025(8) O3 0.0338(11) 0.0411(11) 0.0295(10) -0.0044(9) -0.0039(8) -0.0068(9) O4 0.0339(10) 0.0253(9) 0.0319(10) 0.0001(8) -0.0085(8) -0.0036(8) O21 0.0184(9) 0.0404(11) 0.0373(10) -0.0101(9) -0.0028(7) -0.0114(8) O22 0.0276(10) 0.0339(10) 0.0353(10) -0.0092(8) -0.0063(8) 0.0017(8) O23 0.0224(9) 0.0342(10) 0.0375(11) -0.0111(8) -0.0042(8) -0.0021(8) O24 0.0207(9) 0.0384(11) 0.0350(11) -0.0084(8) 0.0012(8) -0.0031(8) O41 0.0318(10) 0.0280(9) 0.0256(9) -0.0117(7) 0.0032(7) 0.0021(8) O42 0.0256(10) 0.0368(11) 0.0372(11) -0.0085(9) 0.0042(8) -0.0012(8) O43 0.0390(11) 0.0400(12) 0.0278(10) -0.0042(8) -0.0031(8) 0.0025(9) O44 0.0276(10) 0.0292(10) 0.0321(10) -0.0120(8) 0.0013(8) -0.0017(8) N1 0.0270(11) 0.0258(11) 0.0220(10) -0.0015(8) -0.0020(8) -0.0026(8) C1 0.0294(14) 0.0401(16) 0.0411(16) -0.0023(13) -0.0067(12) -0.0033(12) C2 0.0384(19) 0.095(3) 0.0388(19) -0.005(2) -0.0031(15) 0.012(2) C3 0.0316(16) 0.053(2) 0.062(2) -0.0024(17) -0.0161(15) 0.0027(15) C4 0.042(2) 0.042(2) 0.113(4) -0.003(2) -0.009(2) -0.0109(16) C5 0.0406(17) 0.0476(18) 0.0254(14) -0.0031(12) -0.0046(12) -0.0079(14) C6 0.048(2) 0.052(2) 0.0410(18) -0.0109(15) -0.0007(15) -0.0058(16) C7 0.046(2) 0.085(3) 0.045(2) -0.023(2) -0.0098(16) -0.012(2) C8 0.087(3) 0.061(3) 0.0349(18) 0.0088(17) -0.0046(19) -0.017(2) C9 0.0372(16) 0.0247(13) 0.0454(17) -0.0003(12) -0.0108(13) -0.0052(11) C10 0.066(2) 0.0341(17) 0.062(2) -0.0126(16) -0.0093(19) -0.0086(16) C11 0.0455(19) 0.0403(18) 0.060(2) 0.0034(16) -0.0056(16) -0.0120(15) C12 0.053(2) 0.0328(17) 0.071(3) 0.0125(16) -0.0262(19) -0.0073(15) C21 0.0362(17) 0.0397(17) 0.054(2) -0.0148(15) -0.0114(14) 0.0109(13) C22 0.036(2) 0.072(3) 0.191(8) -0.045(4) -0.028(3) 0.016(2) C23 0.121(5) 0.062(3) 0.048(2) -0.006(2) -0.027(3) 0.045(3) C24 0.085(3) 0.0347(18) 0.051(2) -0.0125(16) -0.004(2) -0.0051(18) C25 0.0282(14) 0.0346(15) 0.0439(17) -0.0142(13) -0.0050(12) -0.0052(11) C26 0.053(2) 0.0455(19) 0.0453(19) -0.0156(15) -0.0145(15) -0.0077(16) C27 0.0414(17) 0.0361(16) 0.0519(19) -0.0103(14) -0.0039(14) -0.0073(13) C28 0.0285(16) 0.052(2) 0.070(2) -0.0273(18) -0.0044(15) -0.0112(14) C29 0.0253(13) 0.0400(16) 0.0329(14) -0.0086(12) 0.0028(11) -0.0064(11) C30 0.0287(15) 0.053(2) 0.0467(18) -0.0068(15) 0.0052(13) -0.0119(14) C31 0.0372(17) 0.053(2) 0.0387(17) -0.0054(15) -0.0034(13) 0.0034(15) C32 0.0379(17) 0.055(2) 0.0463(19) -0.0211(16) 0.0003(14) -0.0103(15) C41 0.0372(17) 0.057(2) 0.0441(18) -0.0167(16) 0.0100(14) -0.0198(15) C42 0.033(2) 0.089(4) 0.100(4) -0.002(3) -0.003(2) -0.020(2) C43 0.080(3) 0.053(2) 0.043(2) -0.0045(16) -0.0029(19) -0.032(2) C44 0.073(3) 0.107(4) 0.065(3) -0.049(3) 0.038(2) -0.047(3) C45 0.0483(19) 0.0412(17) 0.0311(15) -0.0020(13) -0.0096(13) 0.0042(14) C46 0.0381(18) 0.061(2) 0.053(2) -0.0012(18) -0.0060(15) 0.0062(16) C47 0.062(2) 0.065(2) 0.0329(17) -0.0039(16) -0.0143(16) -0.0025(19) C48 0.078(3) 0.043(2) 0.050(2) -0.0070(16) -0.024(2) 0.0111(19) C49 0.0310(15) 0.0324(15) 0.0451(17) -0.0173(13) 0.0023(12) -0.0018(12) C50 0.0338(17) 0.0400(18) 0.075(3) -0.0211(17) -0.0039(16) 0.0056(14) C51 0.052(2) 0.052(2) 0.0440(19) -0.0276(16) 0.0087(15) -0.0117(16) C52 0.0388(17) 0.0363(16) 0.058(2) -0.0181(15) 0.0013(15) -0.0090(13) C61 0.0181(11) 0.0274(12) 0.0227(11) -0.0057(9) 0.0036(9) -0.0006(9) C62 0.0247(12) 0.0280(13) 0.0188(11) -0.0045(9) 0.0011(9) -0.0041(10) C63 0.0260(12) 0.0246(12) 0.0226(12) -0.0029(9) -0.0031(9) -0.0018(10) C64 0.0235(12) 0.0289(13) 0.0197(11) -0.0039(9) -0.0061(9) 0.0009(10) C65 0.0252(12) 0.0280(13) 0.0242(12) -0.0085(10) -0.0034(9) -0.0016(10) C66 0.0243(12) 0.0265(12) 0.0224(12) -0.0092(10) 0.0002(9) -0.0002(10) C67 0.0210(12) 0.0262(12) 0.0280(12) -0.0074(10) -0.0002(10) -0.0032(9) C68 0.0245(13) 0.0318(14) 0.0320(14) -0.0069(11) 0.0026(11) -0.0040(11) C69 0.0205(13) 0.0405(16) 0.0439(16) -0.0136(13) 0.0035(11) -0.0068(11) C70 0.0181(12) 0.0397(16) 0.0474(17) -0.0118(13) -0.0063(11) 0.0015(11) C71 0.0232(13) 0.0313(14) 0.0378(15) -0.0055(11) -0.0061(11) 0.0010(11) C72 0.0195(12) 0.0265(12) 0.0307(13) -0.0060(10) -0.0025(10) -0.0036(10) C73 0.0302(14) 0.0312(14) 0.0278(13) -0.0011(11) -0.0073(11) -0.0019(11) C74 0.0374(16) 0.0510(19) 0.0342(15) -0.0045(13) -0.0140(13) 0.0005(14) C75 0.0389(16) 0.0448(17) 0.0286(14) -0.0037(12) -0.0004(12) -0.0023(13) C76 0.0267(13) 0.0261(13) 0.0412(16) 0.0016(11) -0.0093(11) -0.0023(10) C77 0.0401(17) 0.0298(15) 0.057(2) -0.0122(14) 0.0076(15) -0.0050(13) C78 0.0438(18) 0.0363(16) 0.0500(19) -0.0053(14) 0.0035(15) -0.0102(14) C79 0.0254(13) 0.0270(12) 0.0292(13) -0.0078(10) -0.0080(10) 0.0016(10) C80 0.0352(15) 0.0346(15) 0.0321(14) -0.0089(12) -0.0117(12) 0.0028(12) C81 0.0379(16) 0.0355(15) 0.0439(17) -0.0082(13) -0.0217(13) 0.0067(12) C82 0.0262(14) 0.0426(17) 0.0533(19) -0.0132(14) -0.0180(13) 0.0063(12) C83 0.0235(13) 0.0407(16) 0.0439(17) -0.0094(13) -0.0080(12) 0.0001(12) C84 0.0238(13) 0.0316(14) 0.0344(14) -0.0079(11) -0.0067(11) 0.0007(10) C85 0.0227(13) 0.0454(17) 0.0340(15) -0.0068(12) 0.0010(11) 0.0025(12) C86 0.0452(19) 0.0444(18) 0.0416(17) -0.0154(14) -0.0062(14) 0.0113(15) C87 0.0398(17) 0.054(2) 0.0330(16) -0.0055(14) 0.0023(13) 0.0012(15) C88 0.0244(14) 0.0351(15) 0.0459(17) -0.0011(13) -0.0025(12) -0.0077(11) C89 0.0461(19) 0.0339(16) 0.057(2) -0.0092(15) -0.0048(16) -0.0110(14) C90 0.0265(16) 0.048(2) 0.100(3) -0.001(2) -0.0066(18) -0.0127(15) C91 0.116(6) 0.122(6) 0.151(7) -0.077(5) -0.054(5) 0.040(5) C92 0.082(3) 0.072(3) 0.114(4) -0.043(3) -0.035(3) 0.008(3) C93 0.102(3) 0.049(2) 0.081(3) -0.025(2) -0.055(3) 0.018(2) C94 0.091(3) 0.0365(18) 0.070(3) -0.0022(17) -0.043(2) -0.0026(19) C95 0.130(4) 0.044(2) 0.057(2) -0.0013(18) -0.036(3) -0.015(3) C96 0.114(5) 0.077(3) 0.074(3) 0.023(3) -0.039(3) -0.036(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 Mo1 3.1032(2) . ? U1 Na08 3.3833(11) . ? U1 O1 2.220(2) . ? U1 O21 2.2406(18) . ? U1 O41 2.2576(18) . ? U1 N1 1.865(2) . ? U1 C62 2.946(3) . ? U1 C63 2.954(3) . ? Mo1 P1 2.5053(7) . ? Mo1 P2 2.4832(7) . ? Mo1 N1 2.148(2) . ? Mo1 C61 2.220(2) . ? Mo1 C62 2.254(3) . ? Mo1 C63 2.254(3) . ? Mo1 C64 2.233(2) . ? Mo1 C65 2.283(3) . ? Mo1 C66 2.260(2) . ? P1 C72 1.861(3) . ? P1 C73 1.872(3) . ? P1 C76 1.875(3) . ? P2 C84 1.857(3) . ? P2 C85 1.863(3) . ? P2 C88 1.878(3) . ? Si1 Na08 3.2599(13) . ? Si1 O1 1.600(2) . ? Si1 O2 1.620(2) . ? Si1 O3 1.621(2) . ? Si1 O4 1.655(2) . ? Si2 Na08 3.2123(13) . ? Si2 O21 1.5956(19) . ? Si2 O22 1.617(2) . ? Si2 O23 1.658(2) . ? Si2 O24 1.623(2) . ? Si3 Na08 3.1439(13) . ? Si3 O41 1.5944(19) . ? Si3 O42 1.621(2) . ? Si3 O43 1.626(2) . ? Si3 O44 1.663(2) . ? Na08 O1 2.777(2) . ? Na08 O4 2.424(2) . ? Na08 O21 2.664(2) . ? Na08 O23 2.455(2) . ? Na08 O41 2.482(2) . ? Na08 O44 2.467(2) . ? O2 C1 1.442(4) . ? O3 C5 1.438(4) . ? O4 C9 1.453(3) . ? O22 C21 1.440(4) . ? O23 C25 1.459(3) . ? O24 C29 1.438(4) . ? O42 C41 1.439(4) . ? O43 C45 1.437(4) . ? O44 C49 1.456(3) . ? C1 C2 1.516(5) . ? C1 C3 1.515(5) . ? C1 C4 1.519(5) . ? C5 C6 1.527(5) . ? C5 C7 1.514(5) . ? C5 C8 1.525(5) . ? C9 C10 1.514(5) . ? C9 C11 1.518(5) . ? C9 C12 1.523(5) . ? C21 C22 1.516(6) . ? C21 C23 1.511(6) . ? C21 C24 1.516(5) . ? C25 C26 1.515(5) . ? C25 C27 1.524(5) . ? C25 C28 1.533(4) . ? C29 C30 1.530(4) . ? C29 C31 1.526(5) . ? C29 C32 1.512(5) . ? C41 C42 1.521(6) . ? C41 C43 1.511(6) . ? C41 C44 1.527(5) . ? C45 C46 1.524(5) . ? C45 C47 1.525(5) . ? C45 C48 1.515(5) . ? C49 C50 1.525(5) . ? C49 C51 1.519(5) . ? C49 C52 1.515(4) . ? C61 C62 1.421(4) . ? C61 C66 1.431(4) . ? C61 C67 1.493(4) . ? C62 C63 1.456(4) . ? C63 C64 1.430(4) . ? C64 C65 1.431(4) . ? C64 C79 1.493(4) . ? C65 C66 1.412(4) . ? C67 C68 1.401(4) . ? C67 C72 1.406(4) . ? C68 C69 1.384(4) . ? C69 C70 1.388(5) . ? C70 C71 1.391(4) . ? C71 C72 1.405(4) . ? C73 C74 1.522(4) . ? C73 C75 1.535(4) . ? C76 C77 1.525(5) . ? C76 C78 1.533(4) . ? C79 C80 1.396(4) . ? C79 C84 1.402(4) . ? C80 C81 1.391(5) . ? C81 C82 1.377(5) . ? C82 C83 1.382(5) . ? C83 C84 1.405(4) . ? C85 C86 1.522(5) . ? C85 C87 1.530(5) . ? C88 C89 1.525(5) . ? C88 C90 1.533(4) . ? C91 C92 1.522(8) . ? C92 C93 1.522(8) . ? C93 C94 1.500(6) . ? C94 C95 1.512(6) . ? C95 C96 1.480(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mo1 U1 Na08 170.405(19) . . ? O1 U1 Mo1 121.08(6) . . ? O1 U1 Na08 54.79(6) . . ? O1 U1 O21 84.32(8) . . ? O1 U1 O41 84.03(8) . . ? O1 U1 C62 92.47(7) . . ? O1 U1 C63 78.51(8) . . ? O21 U1 Mo1 121.24(5) . . ? O21 U1 Na08 51.82(6) . . ? O21 U1 O41 86.11(8) . . ? O21 U1 C62 88.56(7) . . ? O21 U1 C63 111.55(7) . . ? O41 U1 Mo1 142.35(5) . . ? O41 U1 Na08 47.17(6) . . ? O41 U1 C62 173.89(7) . . ? O41 U1 C63 153.50(8) . . ? N1 U1 Mo1 42.78(7) . . ? N1 U1 Na08 144.83(7) . . ? N1 U1 O1 153.38(9) . . ? N1 U1 O21 121.65(9) . . ? N1 U1 O41 102.14(9) . . ? N1 U1 C62 83.21(9) . . ? N1 U1 C63 85.65(9) . . ? C62 U1 Mo1 43.66(5) . . ? C62 U1 Na08 126.78(5) . . ? C62 U1 C63 28.58(7) . . ? C63 U1 Mo1 43.61(5) . . ? C63 U1 Na08 129.53(5) . . ? P1 Mo1 U1 108.297(17) . . ? P2 Mo1 U1 106.077(17) . . ? P2 Mo1 P1 112.20(2) . . ? N1 Mo1 U1 36.15(6) . . ? N1 Mo1 P1 85.02(6) . . ? N1 Mo1 P2 90.67(6) . . ? N1 Mo1 C61 118.80(9) . . ? N1 Mo1 C62 96.92(9) . . ? N1 Mo1 C63 99.95(9) . . ? N1 Mo1 C64 126.04(9) . . ? N1 Mo1 C65 162.85(9) . . ? N1 Mo1 C66 155.01(9) . . ? C61 Mo1 U1 96.27(7) . . ? C61 Mo1 P1 78.16(7) . . ? C61 Mo1 P2 150.01(7) . . ? C61 Mo1 C62 37.03(9) . . ? C61 Mo1 C63 67.48(10) . . ? C61 Mo1 C64 79.96(10) . . ? C61 Mo1 C65 66.67(10) . . ? C61 Mo1 C66 37.26(10) . . ? C62 Mo1 U1 64.46(7) . . ? C62 Mo1 P1 105.70(7) . . ? C62 Mo1 P2 141.85(7) . . ? C62 Mo1 C63 37.68(10) . . ? C62 Mo1 C65 78.34(10) . . ? C62 Mo1 C66 66.28(10) . . ? C63 Mo1 U1 64.66(7) . . ? C63 Mo1 P1 143.24(7) . . ? C63 Mo1 P2 104.19(7) . . ? C63 Mo1 C65 66.18(10) . . ? C63 Mo1 C66 78.31(10) . . ? C64 Mo1 U1 96.80(7) . . ? C64 Mo1 P1 148.17(7) . . ? C64 Mo1 P2 77.80(7) . . ? C64 Mo1 C62 67.52(10) . . ? C64 Mo1 C63 37.15(10) . . ? C64 Mo1 C65 36.92(9) . . ? C64 Mo1 C66 66.38(10) . . ? C65 Mo1 U1 130.79(7) . . ? C65 Mo1 P1 112.12(7) . . ? C65 Mo1 P2 83.52(7) . . ? C66 Mo1 U1 130.66(7) . . ? C66 Mo1 P1 82.28(7) . . ? C66 Mo1 P2 114.05(7) . . ? C66 Mo1 C65 36.21(10) . . ? C72 P1 Mo1 102.21(9) . . ? C72 P1 C73 104.38(13) . . ? C72 P1 C76 99.77(13) . . ? C73 P1 Mo1 114.55(9) . . ? C73 P1 C76 103.61(13) . . ? C76 P1 Mo1 128.83(10) . . ? C84 P2 Mo1 103.40(10) . . ? C84 P2 C85 98.75(13) . . ? C84 P2 C88 105.35(14) . . ? C85 P2 Mo1 121.75(11) . . ? C85 P2 C88 101.47(15) . . ? C88 P2 Mo1 122.57(10) . . ? O1 Si1 Na08 58.35(8) . . ? O1 Si1 O2 113.76(12) . . ? O1 Si1 O3 115.93(12) . . ? O1 Si1 O4 104.37(11) . . ? O2 Si1 Na08 129.82(9) . . ? O2 Si1 O3 106.61(12) . . ? O2 Si1 O4 111.36(11) . . ? O3 Si1 Na08 121.45(9) . . ? O3 Si1 O4 104.45(12) . . ? O4 Si1 Na08 46.05(7) . . ? O21 Si2 Na08 55.76(8) . . ? O21 Si2 O22 114.55(12) . . ? O21 Si2 O23 104.36(11) . . ? O21 Si2 O24 115.16(11) . . ? O22 Si2 Na08 122.37(8) . . ? O22 Si2 O23 105.48(11) . . ? O22 Si2 O24 105.78(11) . . ? O23 Si2 Na08 48.62(7) . . ? O24 Si2 Na08 130.58(9) . . ? O24 Si2 O23 111.18(11) . . ? O41 Si3 Na08 51.31(8) . . ? O41 Si3 O42 115.67(12) . . ? O41 Si3 O43 115.64(12) . . ? O41 Si3 O44 102.42(11) . . ? O42 Si3 Na08 125.35(9) . . ? O42 Si3 O43 104.94(12) . . ? O42 Si3 O44 106.61(11) . . ? O43 Si3 Na08 129.13(9) . . ? O43 Si3 O44 111.34(12) . . ? O44 Si3 Na08 51.11(7) . . ? Si1 Na08 U1 70.13(3) . . ? Si2 Na08 U1 70.80(3) . . ? Si2 Na08 Si1 107.49(4) . . ? Si3 Na08 U1 71.93(3) . . ? Si3 Na08 Si1 110.57(4) . . ? Si3 Na08 Si2 111.63(4) . . ? O1 Na08 U1 40.76(4) . . ? O1 Na08 Si1 29.37(4) . . ? O1 Na08 Si2 92.61(5) . . ? O1 Na08 Si3 94.25(6) . . ? O4 Na08 U1 99.56(6) . . ? O4 Na08 Si1 29.44(5) . . ? O4 Na08 Si2 119.76(6) . . ? O4 Na08 Si3 121.41(6) . . ? O4 Na08 O1 58.80(7) . . ? O4 Na08 O21 112.56(8) . . ? O4 Na08 O23 117.72(8) . . ? O4 Na08 O41 116.23(8) . . ? O4 Na08 O44 116.67(8) . . ? O21 Na08 U1 41.39(4) . . ? O21 Na08 Si1 89.17(6) . . ? O21 Na08 Si2 29.68(4) . . ? O21 Na08 Si3 98.13(6) . . ? O21 Na08 O1 66.72(6) . . ? O23 Na08 U1 101.15(6) . . ? O23 Na08 Si1 122.06(6) . . ? O23 Na08 Si2 30.45(5) . . ? O23 Na08 Si3 120.82(7) . . ? O23 Na08 O1 118.53(8) . . ? O23 Na08 O21 60.12(7) . . ? O23 Na08 O41 118.21(8) . . ? O23 Na08 O44 114.17(8) . . ? O41 Na08 U1 41.85(5) . . ? O41 Na08 Si1 93.24(6) . . ? O41 Na08 Si2 95.51(6) . . ? O41 Na08 Si3 30.09(4) . . ? O41 Na08 O1 69.21(7) . . ? O41 Na08 O21 73.18(7) . . ? O44 Na08 U1 103.58(6) . . ? O44 Na08 Si1 123.64(6) . . ? O44 Na08 Si2 123.45(6) . . ? O44 Na08 Si3 31.65(5) . . ? O44 Na08 O1 119.92(8) . . ? O44 Na08 O21 123.63(8) . . ? O44 Na08 O41 61.75(7) . . ? U1 O1 Na08 84.45(7) . . ? Si1 O1 U1 176.33(14) . . ? Si1 O1 Na08 92.28(10) . . ? C1 O2 Si1 132.8(2) . . ? C5 O3 Si1 137.5(2) . . ? Si1 O4 Na08 104.51(10) . . ? C9 O4 Si1 127.49(19) . . ? C9 O4 Na08 127.31(18) . . ? U1 O21 Na08 86.78(7) . . ? Si2 O21 U1 170.53(14) . . ? Si2 O21 Na08 94.57(10) . . ? C21 O22 Si2 131.9(2) . . ? Si2 O23 Na08 100.93(10) . . ? C25 O23 Si2 127.08(18) . . ? C25 O23 Na08 130.76(17) . . ? C29 O24 Si2 133.78(19) . . ? U1 O41 Na08 90.98(7) . . ? Si3 O41 U1 170.19(13) . . ? Si3 O41 Na08 98.60(10) . . ? C41 O42 Si3 135.2(2) . . ? C45 O43 Si3 133.5(2) . . ? Si3 O44 Na08 97.24(9) . . ? C49 O44 Si3 127.84(19) . . ? C49 O44 Na08 133.88(18) . . ? U1 N1 Mo1 101.06(10) . . ? O2 C1 C2 110.6(3) . . ? O2 C1 C3 105.9(3) . . ? O2 C1 C4 107.5(3) . . ? C2 C1 C4 112.3(4) . . ? C3 C1 C2 110.4(3) . . ? C3 C1 C4 109.9(3) . . ? O3 C5 C6 107.6(3) . . ? O3 C5 C7 111.9(3) . . ? O3 C5 C8 105.2(3) . . ? C7 C5 C6 110.5(3) . . ? C7 C5 C8 111.7(3) . . ? C8 C5 C6 109.7(3) . . ? O4 C9 C10 106.3(3) . . ? O4 C9 C11 108.5(3) . . ? O4 C9 C12 111.8(3) . . ? C10 C9 C11 109.3(3) . . ? C10 C9 C12 110.0(3) . . ? C11 C9 C12 110.8(3) . . ? O22 C21 C22 107.0(3) . . ? O22 C21 C23 105.7(3) . . ? O22 C21 C24 111.2(3) . . ? C22 C21 C24 109.8(4) . . ? C23 C21 C22 113.4(5) . . ? C23 C21 C24 109.7(4) . . ? O23 C25 C26 108.4(3) . . ? O23 C25 C27 105.8(3) . . ? O23 C25 C28 112.1(2) . . ? C26 C25 C27 111.1(3) . . ? C26 C25 C28 110.5(3) . . ? C27 C25 C28 108.9(3) . . ? O24 C29 C30 106.6(3) . . ? O24 C29 C31 110.7(2) . . ? O24 C29 C32 108.3(3) . . ? C31 C29 C30 110.5(3) . . ? C32 C29 C30 109.1(3) . . ? C32 C29 C31 111.5(3) . . ? O42 C41 C42 105.5(3) . . ? O42 C41 C43 111.8(3) . . ? O42 C41 C44 108.8(3) . . ? C42 C41 C44 111.5(4) . . ? C43 C41 C42 110.3(4) . . ? C43 C41 C44 109.0(4) . . ? O43 C45 C46 110.4(3) . . ? O43 C45 C47 104.9(3) . . ? O43 C45 C48 108.6(3) . . ? C46 C45 C47 110.7(3) . . ? C48 C45 C46 112.1(3) . . ? C48 C45 C47 109.9(3) . . ? O44 C49 C50 108.2(3) . . ? O44 C49 C51 111.2(3) . . ? O44 C49 C52 106.3(2) . . ? C51 C49 C50 111.3(3) . . ? C52 C49 C50 110.1(3) . . ? C52 C49 C51 109.6(3) . . ? C62 C61 Mo1 72.80(14) . . ? C62 C61 C66 119.8(2) . . ? C62 C61 C67 125.0(2) . . ? C66 C61 Mo1 72.87(14) . . ? C66 C61 C67 115.1(2) . . ? C67 C61 Mo1 121.37(18) . . ? Mo1 C62 U1 71.88(7) . . ? C61 C62 U1 129.82(17) . . ? C61 C62 Mo1 70.17(14) . . ? C61 C62 C63 119.5(2) . . ? C63 C62 U1 76.00(14) . . ? C63 C62 Mo1 71.16(15) . . ? Mo1 C63 U1 71.72(7) . . ? C62 C63 U1 75.43(14) . . ? C62 C63 Mo1 71.16(15) . . ? C64 C63 U1 130.54(17) . . ? C64 C63 Mo1 70.62(15) . . ? C64 C63 C62 119.6(2) . . ? C63 C64 Mo1 72.23(15) . . ? C63 C64 C65 120.0(2) . . ? C63 C64 C79 122.7(2) . . ? C65 C64 Mo1 73.45(15) . . ? C65 C64 C79 117.0(2) . . ? C79 C64 Mo1 121.03(18) . . ? C64 C65 Mo1 69.63(14) . . ? C66 C65 Mo1 70.97(15) . . ? C66 C65 C64 119.8(2) . . ? C61 C66 Mo1 69.87(14) . . ? C65 C66 Mo1 72.82(15) . . ? C65 C66 C61 121.0(2) . . ? C68 C67 C61 121.0(3) . . ? C68 C67 C72 120.3(3) . . ? C72 C67 C61 118.4(2) . . ? C69 C68 C67 120.3(3) . . ? C68 C69 C70 120.0(3) . . ? C69 C70 C71 120.2(3) . . ? C70 C71 C72 120.8(3) . . ? C67 C72 P1 116.9(2) . . ? C71 C72 P1 124.8(2) . . ? C71 C72 C67 118.2(2) . . ? C74 C73 P1 119.0(2) . . ? C74 C73 C75 109.9(3) . . ? C75 C73 P1 110.5(2) . . ? C77 C76 P1 112.8(2) . . ? C77 C76 C78 108.8(3) . . ? C78 C76 P1 112.6(2) . . ? C80 C79 C64 121.3(3) . . ? C80 C79 C84 120.2(3) . . ? C84 C79 C64 118.5(2) . . ? C81 C80 C79 119.8(3) . . ? C82 C81 C80 120.5(3) . . ? C81 C82 C83 120.1(3) . . ? C82 C83 C84 120.7(3) . . ? C79 C84 P2 116.2(2) . . ? C79 C84 C83 118.6(3) . . ? C83 C84 P2 124.6(2) . . ? C86 C85 P2 110.1(2) . . ? C86 C85 C87 111.2(3) . . ? C87 C85 P2 111.1(2) . . ? C89 C88 P2 111.1(2) . . ? C89 C88 C90 109.1(3) . . ? C90 C88 P2 117.4(2) . . ? C93 C92 C91 115.5(6) . . ? C94 C93 C92 115.0(4) . . ? C93 C94 C95 115.9(4) . . ? C96 C95 C94 115.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U1 C62 C63 Mo1 75.30(5) . . . . ? U1 C62 C63 C64 128.7(2) . . . . ? U1 C63 C64 Mo1 42.42(18) . . . . ? U1 C63 C64 C65 100.4(3) . . . . ? U1 C63 C64 C79 -73.5(3) . . . . ? Mo1 P1 C72 C67 3.8(2) . . . . ? Mo1 P1 C72 C71 -178.1(2) . . . . ? Mo1 P1 C73 C74 157.1(2) . . . . ? Mo1 P1 C73 C75 -74.3(2) . . . . ? Mo1 P1 C76 C77 -63.7(3) . . . . ? Mo1 P1 C76 C78 59.9(3) . . . . ? Mo1 P2 C84 C79 -1.9(2) . . . . ? Mo1 P2 C84 C83 168.9(2) . . . . ? Mo1 P2 C85 C86 -52.7(3) . . . . ? Mo1 P2 C85 C87 71.0(3) . . . . ? Mo1 P2 C88 C89 45.8(3) . . . . ? Mo1 P2 C88 C90 172.3(3) . . . . ? Mo1 C61 C62 U1 -43.01(18) . . . . ? Mo1 C61 C62 C63 53.3(2) . . . . ? Mo1 C61 C66 C65 -54.0(2) . . . . ? Mo1 C61 C67 C68 166.9(2) . . . . ? Mo1 C61 C67 C72 -19.7(3) . . . . ? Mo1 C62 C63 U1 -75.30(5) . . . . ? Mo1 C62 C63 C64 53.4(2) . . . . ? Mo1 C63 C64 C65 57.9(2) . . . . ? Mo1 C63 C64 C79 -115.9(2) . . . . ? Mo1 C64 C65 C66 52.2(2) . . . . ? Mo1 C64 C79 C80 -159.8(2) . . . . ? Mo1 C64 C79 C84 21.0(3) . . . . ? Mo1 C65 C66 C61 52.7(2) . . . . ? Si1 O2 C1 C2 -35.8(4) . . . . ? Si1 O2 C1 C3 -155.4(3) . . . . ? Si1 O2 C1 C4 87.1(4) . . . . ? Si1 O3 C5 C6 97.5(3) . . . . ? Si1 O3 C5 C7 -24.1(5) . . . . ? Si1 O3 C5 C8 -145.6(3) . . . . ? Si1 O4 C9 C10 -154.9(2) . . . . ? Si1 O4 C9 C11 87.6(3) . . . . ? Si1 O4 C9 C12 -34.8(4) . . . . ? Si2 O22 C21 C22 -93.5(4) . . . . ? Si2 O22 C21 C23 145.3(3) . . . . ? Si2 O22 C21 C24 26.3(5) . . . . ? Si2 O23 C25 C26 84.5(3) . . . . ? Si2 O23 C25 C27 -156.2(2) . . . . ? Si2 O23 C25 C28 -37.6(4) . . . . ? Si2 O24 C29 C30 -147.1(2) . . . . ? Si2 O24 C29 C31 -26.9(4) . . . . ? Si2 O24 C29 C32 95.6(3) . . . . ? Si3 O42 C41 C42 154.6(3) . . . . ? Si3 O42 C41 C43 34.7(5) . . . . ? Si3 O42 C41 C44 -85.7(5) . . . . ? Si3 O43 C45 C46 -44.1(4) . . . . ? Si3 O43 C45 C47 -163.3(3) . . . . ? Si3 O43 C45 C48 79.2(4) . . . . ? Si3 O44 C49 C50 80.7(3) . . . . ? Si3 O44 C49 C51 -41.8(4) . . . . ? Si3 O44 C49 C52 -161.0(2) . . . . ? Na08 U1 N1 Mo1 170.67(4) . . . . ? Na08 Si1 O2 C1 32.0(3) . . . . ? Na08 Si1 O3 C5 -142.8(3) . . . . ? Na08 Si1 O4 C9 -171.0(3) . . . . ? Na08 Si2 O22 C21 -146.5(3) . . . . ? Na08 Si2 O23 C25 -168.3(3) . . . . ? Na08 Si2 O24 C29 16.0(3) . . . . ? Na08 Si3 O42 C41 -161.0(3) . . . . ? Na08 Si3 O43 C45 23.0(4) . . . . ? Na08 Si3 O44 C49 -169.6(3) . . . . ? Na08 O4 C9 C10 36.2(4) . . . . ? Na08 O4 C9 C11 -81.4(3) . . . . ? Na08 O4 C9 C12 156.2(2) . . . . ? Na08 O23 C25 C26 -80.3(3) . . . . ? Na08 O23 C25 C27 39.0(3) . . . . ? Na08 O23 C25 C28 157.6(2) . . . . ? Na08 O44 C49 C50 -84.9(3) . . . . ? Na08 O44 C49 C51 152.6(2) . . . . ? Na08 O44 C49 C52 33.4(4) . . . . ? O1 U1 N1 Mo1 -62.7(2) . . . . ? O1 Si1 O2 C1 -35.7(3) . . . . ? O1 Si1 O3 C5 -75.6(3) . . . . ? O1 Si1 O4 Na08 -2.16(13) . . . . ? O1 Si1 O4 C9 -173.1(2) . . . . ? O2 Si1 O1 Na08 123.41(11) . . . . ? O2 Si1 O3 C5 52.2(3) . . . . ? O2 Si1 O4 Na08 -125.31(11) . . . . ? O2 Si1 O4 C9 63.7(3) . . . . ? O3 Si1 O1 Na08 -112.44(11) . . . . ? O3 Si1 O2 C1 -164.7(3) . . . . ? O3 Si1 O4 Na08 119.99(11) . . . . ? O3 Si1 O4 C9 -51.0(3) . . . . ? O4 Si1 O1 Na08 1.83(11) . . . . ? O4 Si1 O2 C1 81.9(3) . . . . ? O4 Si1 O3 C5 170.2(3) . . . . ? O21 U1 N1 Mo1 103.35(10) . . . . ? O21 Si2 O22 C21 -82.8(3) . . . . ? O21 Si2 O23 Na08 -1.30(13) . . . . ? O21 Si2 O23 C25 -169.6(2) . . . . ? O21 Si2 O24 C29 -49.4(3) . . . . ? O22 Si2 O21 Na08 -113.64(11) . . . . ? O22 Si2 O23 Na08 119.77(11) . . . . ? O22 Si2 O23 C25 -48.6(3) . . . . ? O22 Si2 O24 C29 -177.0(3) . . . . ? O23 Si2 O21 Na08 1.18(11) . . . . ? O23 Si2 O22 C21 163.1(3) . . . . ? O23 Si2 O24 C29 69.0(3) . . . . ? O24 Si2 O21 Na08 123.34(11) . . . . ? O24 Si2 O22 C21 45.2(3) . . . . ? O24 Si2 O23 Na08 -126.04(11) . . . . ? O24 Si2 O23 C25 65.6(3) . . . . ? O41 U1 N1 Mo1 -163.72(8) . . . . ? O41 Si3 O42 C41 -101.6(3) . . . . ? O41 Si3 O43 C45 -36.8(3) . . . . ? O41 Si3 O44 Na08 0.44(12) . . . . ? O41 Si3 O44 C49 -169.1(2) . . . . ? O42 Si3 O41 Na08 -115.95(11) . . . . ? O42 Si3 O43 C45 -165.5(3) . . . . ? O42 Si3 O44 Na08 122.35(10) . . . . ? O42 Si3 O44 C49 -47.2(3) . . . . ? O43 Si3 O41 Na08 120.83(12) . . . . ? O43 Si3 O42 C41 27.1(3) . . . . ? O43 Si3 O44 Na08 -123.74(10) . . . . ? O43 Si3 O44 C49 66.7(3) . . . . ? O44 Si3 O41 Na08 -0.44(12) . . . . ? O44 Si3 O42 C41 145.3(3) . . . . ? O44 Si3 O43 C45 79.6(3) . . . . ? C61 C62 C63 U1 -128.1(2) . . . . ? C61 C62 C63 Mo1 -52.8(2) . . . . ? C61 C62 C63 C64 0.5(4) . . . . ? C61 C67 C68 C69 172.9(3) . . . . ? C61 C67 C72 P1 8.5(3) . . . . ? C61 C67 C72 C71 -169.8(2) . . . . ? C62 U1 N1 Mo1 19.27(9) . . . . ? C62 C61 C66 Mo1 57.8(2) . . . . ? C62 C61 C66 C65 3.8(4) . . . . ? C62 C61 C67 C68 76.7(3) . . . . ? C62 C61 C67 C72 -109.9(3) . . . . ? C62 C63 C64 Mo1 -53.6(2) . . . . ? C62 C63 C64 C65 4.3(4) . . . . ? C62 C63 C64 C79 -169.5(2) . . . . ? C63 U1 N1 Mo1 -9.34(9) . . . . ? C63 C64 C65 Mo1 -57.4(2) . . . . ? C63 C64 C65 C66 -5.2(4) . . . . ? C63 C64 C79 C80 -72.0(4) . . . . ? C63 C64 C79 C84 108.8(3) . . . . ? C64 C65 C66 Mo1 -51.5(2) . . . . ? C64 C65 C66 C61 1.1(4) . . . . ? C64 C79 C80 C81 -179.0(3) . . . . ? C64 C79 C84 P2 -10.7(3) . . . . ? C64 C79 C84 C83 177.9(3) . . . . ? C65 C64 C79 C80 114.0(3) . . . . ? C65 C64 C79 C84 -65.2(3) . . . . ? C66 C61 C62 U1 -100.9(3) . . . . ? C66 C61 C62 Mo1 -57.8(2) . . . . ? C66 C61 C62 C63 -4.6(4) . . . . ? C66 C61 C67 C68 -108.6(3) . . . . ? C66 C61 C67 C72 64.8(3) . . . . ? C67 C61 C62 U1 73.6(3) . . . . ? C67 C61 C62 Mo1 116.6(2) . . . . ? C67 C61 C62 C63 169.9(2) . . . . ? C67 C61 C66 Mo1 -117.2(2) . . . . ? C67 C61 C66 C65 -171.2(2) . . . . ? C67 C68 C69 C70 -2.5(5) . . . . ? C68 C67 C72 P1 -178.0(2) . . . . ? C68 C67 C72 C71 3.7(4) . . . . ? C68 C69 C70 C71 1.9(5) . . . . ? C69 C70 C71 C72 1.5(5) . . . . ? C70 C71 C72 P1 177.6(2) . . . . ? C70 C71 C72 C67 -4.3(4) . . . . ? C72 P1 C73 C74 46.2(3) . . . . ? C72 P1 C73 C75 174.8(2) . . . . ? C72 P1 C76 C77 50.7(2) . . . . ? C72 P1 C76 C78 174.4(2) . . . . ? C72 C67 C68 C69 -0.4(4) . . . . ? C73 P1 C72 C67 123.4(2) . . . . ? C73 P1 C72 C71 -58.4(3) . . . . ? C73 P1 C76 C77 158.2(2) . . . . ? C73 P1 C76 C78 -78.1(3) . . . . ? C76 P1 C72 C67 -129.7(2) . . . . ? C76 P1 C72 C71 48.5(3) . . . . ? C76 P1 C73 C74 -57.8(3) . . . . ? C76 P1 C73 C75 70.8(2) . . . . ? C79 C64 C65 Mo1 116.9(2) . . . . ? C79 C64 C65 C66 169.0(2) . . . . ? C79 C80 C81 C82 1.4(5) . . . . ? C80 C79 C84 P2 170.1(2) . . . . ? C80 C79 C84 C83 -1.3(4) . . . . ? C80 C81 C82 C83 -1.8(5) . . . . ? C81 C82 C83 C84 0.6(5) . . . . ? C82 C83 C84 P2 -169.7(3) . . . . ? C82 C83 C84 C79 1.0(5) . . . . ? C84 P2 C85 C86 59.1(2) . . . . ? C84 P2 C85 C87 -177.2(2) . . . . ? C84 P2 C88 C89 -71.7(3) . . . . ? C84 P2 C88 C90 54.9(3) . . . . ? C84 C79 C80 C81 0.2(4) . . . . ? C85 P2 C84 C79 -127.7(2) . . . . ? C85 P2 C84 C83 43.2(3) . . . . ? C85 P2 C88 C89 -174.2(2) . . . . ? C85 P2 C88 C90 -47.6(3) . . . . ? C88 P2 C84 C79 127.8(2) . . . . ? C88 P2 C84 C83 -61.4(3) . . . . ? C88 P2 C85 C86 166.8(2) . . . . ? C88 P2 C85 C87 -69.5(3) . . . . ? C91 C92 C93 C94 -179.3(5) . . . . ? C92 C93 C94 C95 -179.6(4) . . . . ? C93 C94 C95 C96 -175.4(4) . . . . ? _shelx_res_file ; TITL LB1231 in P-1 lb1231.res created by SHELXL-2018/3 at 17:01:44 on 02-Mar-2021 CELL 1.54184 13.652528 16.47884 19.246882 81.3024 79.5672 82.5868 ZERR 2 0.000248 0.00043 0.000402 0.0019 0.0016 0.0018 LATT 1 SFAC C H Mo N Na O P Si U UNIT 144 270 2 2 2 24 4 6 2 SADI C92 C91 C93 C92 C94 C93 C95 C94 C96 C95 SIMU 0.01 0.02 2 C91 C92 C93 C94 C95 C96 L.S. 10 PLAN 10 SIZE 0.395 0.233 0.188 TEMP -133 CONF BOND WPDB -2 LIST 4 MORE -1 fmap 2 53 acta REM REM REM WGHT 0.043300 3.479600 EXTI 0.000193 FVAR 2.30670 U1 9 0.734480 0.343333 0.766334 11.00000 0.01678 0.02153 = 0.02206 -0.00429 -0.00206 -0.00105 MO1 3 0.739924 0.516009 0.810415 11.00000 0.01691 0.02166 = 0.02080 -0.00370 -0.00204 -0.00161 P1 7 0.627011 0.618262 0.743310 11.00000 0.01923 0.02458 = 0.02515 -0.00135 -0.00288 -0.00166 P2 7 0.917426 0.545863 0.779220 11.00000 0.01803 0.02940 = 0.02855 -0.00379 -0.00201 -0.00090 SI1 8 0.789116 0.143692 0.888557 11.00000 0.02835 0.02551 = 0.02625 -0.00087 -0.00702 -0.00160 SI2 8 0.486295 0.262909 0.759738 11.00000 0.01829 0.03194 = 0.03163 -0.00993 -0.00160 -0.00447 SI3 8 0.847396 0.222764 0.609857 11.00000 0.02663 0.02787 = 0.02438 -0.00776 0.00102 0.00020 NA08 5 0.697879 0.151007 0.742227 11.00000 0.02422 0.02872 = 0.02841 -0.00335 -0.00324 -0.00068 O1 6 0.769403 0.228804 0.838346 11.00000 0.03761 0.02579 = 0.03068 0.00087 -0.00750 0.00040 O2 6 0.903688 0.123056 0.902619 11.00000 0.02939 0.03509 = 0.03374 -0.00062 -0.00820 -0.00251 O3 6 0.718422 0.134219 0.966020 11.00000 0.03376 0.04108 = 0.02951 -0.00445 -0.00392 -0.00683 O4 6 0.757209 0.073100 0.846545 11.00000 0.03391 0.02535 = 0.03188 0.00007 -0.00846 -0.00356 O21 6 0.589082 0.292058 0.770186 11.00000 0.01841 0.04037 = 0.03729 -0.01013 -0.00284 -0.01139 O22 6 0.439693 0.312890 0.692180 11.00000 0.02764 0.03386 = 0.03529 -0.00920 -0.00631 0.00174 O23 6 0.516891 0.167016 0.741002 11.00000 0.02239 0.03419 = 0.03750 -0.01109 -0.00418 -0.00212 O24 6 0.396681 0.266984 0.827619 11.00000 0.02073 0.03842 = 0.03502 -0.00839 0.00118 -0.00306 O41 6 0.796750 0.264364 0.679053 11.00000 0.03180 0.02803 = 0.02563 -0.01171 0.00322 0.00208 O42 6 0.968338 0.203894 0.598980 11.00000 0.02560 0.03679 = 0.03722 -0.00849 0.00416 -0.00121 O43 6 0.823656 0.273317 0.534364 11.00000 0.03905 0.03995 = 0.02776 -0.00421 -0.00311 0.00247 O44 6 0.801834 0.131691 0.625794 11.00000 0.02762 0.02920 = 0.03213 -0.01202 0.00131 -0.00167 N1 4 0.757665 0.448970 0.720762 11.00000 0.02697 0.02583 = 0.02201 -0.00151 -0.00197 -0.00260 C1 1 0.998739 0.137266 0.858545 11.00000 0.02942 0.04007 = 0.04109 -0.00232 -0.00672 -0.00333 C2 1 0.996193 0.127413 0.781841 11.00000 0.03837 0.09507 = 0.03885 -0.00502 -0.00310 0.01194 AFIX 137 H2A 2 1.062917 0.132497 0.753493 11.00000 -1.50000 H2B 2 0.948051 0.170408 0.762555 11.00000 -1.50000 H2C 2 0.975967 0.072967 0.779905 11.00000 -1.50000 AFIX 0 C3 1 1.075143 0.073014 0.888741 11.00000 0.03163 0.05319 = 0.06165 -0.00242 -0.01611 0.00274 AFIX 137 H3A 2 1.059536 0.017773 0.884413 11.00000 -1.50000 H3B 2 1.073153 0.077995 0.939088 11.00000 -1.50000 H3C 2 1.142162 0.081711 0.862256 11.00000 -1.50000 AFIX 0 C4 1 1.021016 0.223095 0.866293 11.00000 0.04228 0.04212 = 0.11312 -0.00335 -0.00890 -0.01093 AFIX 137 H4A 2 1.086675 0.233782 0.838418 11.00000 -1.50000 H4B 2 1.021343 0.226754 0.916598 11.00000 -1.50000 H4C 2 0.969405 0.264133 0.848863 11.00000 -1.50000 AFIX 0 C5 1 0.710598 0.164800 1.033178 11.00000 0.04057 0.04763 = 0.02536 -0.00305 -0.00460 -0.00793 C6 1 0.630265 0.238404 1.034892 11.00000 0.04803 0.05238 = 0.04097 -0.01094 -0.00066 -0.00581 AFIX 137 H6A 2 0.621344 0.259216 1.080951 11.00000 -1.50000 H6B 2 0.566909 0.221089 1.028273 11.00000 -1.50000 H6C 2 0.650975 0.282154 0.996552 11.00000 -1.50000 AFIX 0 C7 1 0.809208 0.189964 1.043570 11.00000 0.04641 0.08525 = 0.04460 -0.02348 -0.00978 -0.01202 AFIX 137 H7A 2 0.828774 0.235804 1.007007 11.00000 -1.50000 H7B 2 0.860862 0.142972 1.039552 11.00000 -1.50000 H7C 2 0.801832 0.207410 1.090879 11.00000 -1.50000 AFIX 0 C8 1 0.675667 0.094376 1.089492 11.00000 0.08705 0.06122 = 0.03487 0.00875 -0.00460 -0.01716 AFIX 137 H8A 2 0.664101 0.112587 1.136744 11.00000 -1.50000 H8B 2 0.727163 0.047090 1.087978 11.00000 -1.50000 H8C 2 0.613283 0.078182 1.079954 11.00000 -1.50000 AFIX 0 C9 1 0.750682 -0.013916 0.872222 11.00000 0.03723 0.02467 = 0.04544 -0.00029 -0.01084 -0.00522 C10 1 0.765653 -0.057555 0.806706 11.00000 0.06581 0.03406 = 0.06243 -0.01257 -0.00926 -0.00860 AFIX 137 H10A 2 0.761589 -0.116796 0.821301 11.00000 -1.50000 H10B 2 0.831592 -0.048823 0.778373 11.00000 -1.50000 H10C 2 0.713469 -0.035294 0.778035 11.00000 -1.50000 AFIX 0 C11 1 0.646559 -0.024027 0.914070 11.00000 0.04553 0.04035 = 0.05994 0.00337 -0.00558 -0.01201 AFIX 137 H11A 2 0.596446 0.000321 0.884242 11.00000 -1.50000 H11B 2 0.636819 0.003935 0.956645 11.00000 -1.50000 H11C 2 0.639173 -0.082865 0.928347 11.00000 -1.50000 AFIX 0 C12 1 0.830363 -0.049008 0.917890 11.00000 0.05348 0.03279 = 0.07099 0.01249 -0.02624 -0.00730 AFIX 137 H12A 2 0.827689 -0.108656 0.930539 11.00000 -1.50000 H12B 2 0.818009 -0.022577 0.961423 11.00000 -1.50000 H12C 2 0.896652 -0.038368 0.891089 11.00000 -1.50000 AFIX 0 C21 1 0.379235 0.390869 0.683232 11.00000 0.03624 0.03967 = 0.05405 -0.01478 -0.01138 0.01086 C22 1 0.270833 0.372600 0.698704 11.00000 0.03612 0.07153 = 0.19108 -0.04457 -0.02834 0.01615 AFIX 137 H22A 2 0.259861 0.336531 0.665371 11.00000 -1.50000 H22B 2 0.227087 0.424381 0.693111 11.00000 -1.50000 H22C 2 0.255469 0.345075 0.747633 11.00000 -1.50000 AFIX 0 C23 1 0.412083 0.428382 0.607235 11.00000 0.12055 0.06230 = 0.04831 -0.00597 -0.02682 0.04510 AFIX 137 H23A 2 0.482984 0.437302 0.600304 11.00000 -1.50000 H23B 2 0.371941 0.481303 0.597503 11.00000 -1.50000 H23C 2 0.402628 0.390870 0.574611 11.00000 -1.50000 AFIX 0 C24 1 0.396445 0.447517 0.734045 11.00000 0.08517 0.03467 = 0.05102 -0.01247 -0.00364 -0.00512 AFIX 137 H24A 2 0.376822 0.422255 0.783275 11.00000 -1.50000 H24B 2 0.356139 0.500662 0.725759 11.00000 -1.50000 H24C 2 0.467496 0.456245 0.725944 11.00000 -1.50000 AFIX 0 C25 1 0.454492 0.115949 0.715757 11.00000 0.02824 0.03461 = 0.04389 -0.01425 -0.00497 -0.00520 C26 1 0.464452 0.136385 0.635513 11.00000 0.05335 0.04550 = 0.04529 -0.01559 -0.01453 -0.00766 AFIX 137 H26A 2 0.438196 0.194008 0.623333 11.00000 -1.50000 H26B 2 0.426413 0.100071 0.617292 11.00000 -1.50000 H26C 2 0.535189 0.128293 0.614012 11.00000 -1.50000 AFIX 0 C27 1 0.495446 0.026882 0.736974 11.00000 0.04135 0.03613 = 0.05187 -0.01031 -0.00392 -0.00733 AFIX 137 H27A 2 0.566627 0.018717 0.716607 11.00000 -1.50000 H27B 2 0.458603 -0.010471 0.718926 11.00000 -1.50000 H27C 2 0.487441 0.015136 0.789030 11.00000 -1.50000 AFIX 0 C28 1 0.344465 0.128882 0.750709 11.00000 0.02854 0.05206 = 0.07012 -0.02735 -0.00437 -0.01125 AFIX 137 H28A 2 0.339187 0.114752 0.802479 11.00000 -1.50000 H28B 2 0.305321 0.093390 0.732529 11.00000 -1.50000 H28C 2 0.318538 0.186775 0.739468 11.00000 -1.50000 AFIX 0 C29 1 0.390169 0.238275 0.902520 11.00000 0.02535 0.04000 = 0.03290 -0.00856 0.00284 -0.00642 C30 1 0.283737 0.214557 0.928815 11.00000 0.02869 0.05317 = 0.04672 -0.00676 0.00522 -0.01187 AFIX 137 H30A 2 0.235494 0.259715 0.912789 11.00000 -1.50000 H30B 2 0.271819 0.204232 0.980997 11.00000 -1.50000 H30C 2 0.275724 0.164531 0.909503 11.00000 -1.50000 AFIX 0 C31 1 0.466899 0.163947 0.915244 11.00000 0.03715 0.05305 = 0.03872 -0.00540 -0.00336 0.00337 AFIX 137 H31A 2 0.455065 0.119562 0.890131 11.00000 -1.50000 H31B 2 0.460401 0.144593 0.966420 11.00000 -1.50000 H31C 2 0.534509 0.179954 0.897353 11.00000 -1.50000 AFIX 0 C32 1 0.405912 0.308915 0.939751 11.00000 0.03786 0.05494 = 0.04627 -0.02113 0.00034 -0.01031 AFIX 137 H32A 2 0.474627 0.323326 0.924192 11.00000 -1.50000 H32B 2 0.394596 0.292312 0.991413 11.00000 -1.50000 H32C 2 0.358714 0.356881 0.927774 11.00000 -1.50000 AFIX 0 C41 1 1.050908 0.242826 0.555272 11.00000 0.03719 0.05742 = 0.04411 -0.01666 0.01000 -0.01978 C42 1 1.139060 0.217377 0.594928 11.00000 0.03338 0.08933 = 0.10030 -0.00220 -0.00280 -0.02009 AFIX 137 H42A 2 1.123149 0.237129 0.641623 11.00000 -1.50000 H42B 2 1.198408 0.241531 0.567337 11.00000 -1.50000 H42C 2 1.152432 0.157072 0.601379 11.00000 -1.50000 AFIX 0 C43 1 1.029163 0.335715 0.544671 11.00000 0.07995 0.05280 = 0.04330 -0.00449 -0.00285 -0.03210 AFIX 137 H43A 2 0.977512 0.351581 0.514394 11.00000 -1.50000 H43B 2 1.090422 0.360460 0.521741 11.00000 -1.50000 H43C 2 1.005454 0.355351 0.591003 11.00000 -1.50000 AFIX 0 C44 1 1.071065 0.211632 0.482688 11.00000 0.07302 0.10671 = 0.06488 -0.04890 0.03841 -0.04744 AFIX 137 H44A 2 1.084650 0.151341 0.489184 11.00000 -1.50000 H44B 2 1.129176 0.235810 0.453198 11.00000 -1.50000 H44C 2 1.012304 0.227731 0.459111 11.00000 -1.50000 AFIX 0 C45 1 0.736409 0.321726 0.512626 11.00000 0.04828 0.04123 = 0.03113 -0.00198 -0.00956 0.00416 C46 1 0.643039 0.278272 0.543322 11.00000 0.03810 0.06141 = 0.05258 -0.00123 -0.00600 0.00619 AFIX 137 H46A 2 0.652619 0.222435 0.529807 11.00000 -1.50000 H46B 2 0.585212 0.309413 0.524517 11.00000 -1.50000 H46C 2 0.631233 0.275018 0.595383 11.00000 -1.50000 AFIX 0 C47 1 0.755808 0.328877 0.431479 11.00000 0.06244 0.06535 = 0.03285 -0.00395 -0.01429 -0.00248 AFIX 137 H47A 2 0.818623 0.353347 0.412916 11.00000 -1.50000 H47B 2 0.700526 0.364006 0.412558 11.00000 -1.50000 H47C 2 0.760740 0.273874 0.416820 11.00000 -1.50000 AFIX 0 C48 1 0.729220 0.406407 0.535933 11.00000 0.07797 0.04336 = 0.04993 -0.00698 -0.02359 0.01111 AFIX 137 H48A 2 0.722733 0.400843 0.587939 11.00000 -1.50000 H48B 2 0.670489 0.440392 0.520827 11.00000 -1.50000 H48C 2 0.789788 0.432751 0.514105 11.00000 -1.50000 AFIX 0 C49 1 0.833483 0.060915 0.587004 11.00000 0.03097 0.03241 = 0.04508 -0.01733 0.00228 -0.00184 C50 1 0.926987 0.014826 0.613074 11.00000 0.03382 0.03996 = 0.07523 -0.02112 -0.00386 0.00563 AFIX 137 H50A 2 0.946311 -0.035630 0.590522 11.00000 -1.50000 H50B 2 0.912988 0.000352 0.664935 11.00000 -1.50000 H50C 2 0.981762 0.050131 0.600522 11.00000 -1.50000 AFIX 0 C51 1 0.852899 0.087681 0.507095 11.00000 0.05224 0.05234 = 0.04398 -0.02762 0.00873 -0.01171 AFIX 137 H51A 2 0.909207 0.121412 0.495125 11.00000 -1.50000 H51B 2 0.792958 0.120119 0.492418 11.00000 -1.50000 H51C 2 0.869057 0.038781 0.482192 11.00000 -1.50000 AFIX 0 C52 1 0.748295 0.006827 0.605441 11.00000 0.03881 0.03630 = 0.05810 -0.01808 0.00129 -0.00899 AFIX 137 H52A 2 0.765366 -0.041250 0.579532 11.00000 -1.50000 H52B 2 0.687216 0.038454 0.591899 11.00000 -1.50000 H52C 2 0.737200 -0.011709 0.656817 11.00000 -1.50000 AFIX 0 C61 1 0.596560 0.516620 0.886294 11.00000 0.01815 0.02745 = 0.02274 -0.00573 0.00360 -0.00061 C62 1 0.638331 0.433028 0.886383 11.00000 0.02472 0.02804 = 0.01885 -0.00448 0.00107 -0.00411 AFIX 43 H62 2 0.599788 0.392506 0.878025 11.00000 -1.20000 AFIX 0 C63 1 0.740676 0.409985 0.899386 11.00000 0.02602 0.02460 = 0.02262 -0.00292 -0.00312 -0.00179 AFIX 43 H63 2 0.769573 0.354382 0.899162 11.00000 -1.20000 AFIX 0 C64 1 0.797404 0.471552 0.912491 11.00000 0.02354 0.02893 = 0.01965 -0.00394 -0.00610 0.00093 C65 1 0.751427 0.553986 0.917705 11.00000 0.02517 0.02803 = 0.02420 -0.00852 -0.00335 -0.00161 AFIX 43 H65 2 0.787291 0.593792 0.930285 11.00000 -1.20000 AFIX 0 C66 1 0.652602 0.575982 0.904095 11.00000 0.02429 0.02649 = 0.02241 -0.00916 0.00022 -0.00021 AFIX 43 H66 2 0.622833 0.631040 0.906794 11.00000 -1.20000 AFIX 0 C67 1 0.499534 0.551168 0.862710 11.00000 0.02099 0.02622 = 0.02797 -0.00743 -0.00024 -0.00320 C68 1 0.407943 0.536575 0.906364 11.00000 0.02447 0.03184 = 0.03198 -0.00694 0.00262 -0.00398 AFIX 43 H68 2 0.406806 0.499288 0.949214 11.00000 -1.20000 AFIX 0 C69 1 0.319101 0.576246 0.887335 11.00000 0.02051 0.04045 = 0.04392 -0.01355 0.00349 -0.00679 AFIX 43 H69 2 0.257005 0.564543 0.916111 11.00000 -1.20000 AFIX 0 C70 1 0.320816 0.633116 0.826201 11.00000 0.01812 0.03968 = 0.04737 -0.01179 -0.00630 0.00148 AFIX 43 H70 2 0.259958 0.661569 0.813974 11.00000 -1.20000 AFIX 0 C71 1 0.411341 0.648588 0.782779 11.00000 0.02316 0.03130 = 0.03783 -0.00554 -0.00609 0.00100 AFIX 43 H71 2 0.411882 0.688577 0.741643 11.00000 -1.20000 AFIX 0 C72 1 0.501994 0.605848 0.798958 11.00000 0.01947 0.02654 = 0.03065 -0.00595 -0.00252 -0.00363 C73 1 0.614270 0.591377 0.654483 11.00000 0.03019 0.03118 = 0.02785 -0.00108 -0.00731 -0.00194 AFIX 13 H73 2 0.611643 0.530264 0.661682 11.00000 -1.20000 AFIX 0 C74 1 0.522095 0.627793 0.621833 11.00000 0.03739 0.05095 = 0.03416 -0.00454 -0.01400 0.00047 AFIX 137 H74A 2 0.461804 0.610775 0.653904 11.00000 -1.50000 H74B 2 0.525952 0.607896 0.575839 11.00000 -1.50000 H74C 2 0.519174 0.688158 0.614733 11.00000 -1.50000 AFIX 0 C75 1 0.709443 0.606476 0.600177 11.00000 0.03890 0.04481 = 0.02859 -0.00371 -0.00037 -0.00231 AFIX 137 H75A 2 0.708345 0.665432 0.582184 11.00000 -1.50000 H75B 2 0.712326 0.574946 0.560441 11.00000 -1.50000 H75C 2 0.768426 0.588690 0.623229 11.00000 -1.50000 AFIX 0 C76 1 0.621540 0.733738 0.728611 11.00000 0.02675 0.02607 = 0.04123 0.00161 -0.00925 -0.00231 AFIX 13 H76 2 0.569380 0.754786 0.698037 11.00000 -1.20000 AFIX 0 C77 1 0.591071 0.772117 0.797673 11.00000 0.04013 0.02982 = 0.05724 -0.01218 0.00759 -0.00504 AFIX 137 H77A 2 0.527875 0.752675 0.823360 11.00000 -1.50000 H77B 2 0.582438 0.832382 0.786614 11.00000 -1.50000 H77C 2 0.643321 0.755955 0.827421 11.00000 -1.50000 AFIX 0 C78 1 0.720618 0.764506 0.689280 11.00000 0.04382 0.03628 = 0.04996 -0.00530 0.00352 -0.01020 AFIX 137 H78A 2 0.775291 0.738207 0.714298 11.00000 -1.50000 H78B 2 0.716500 0.824532 0.687866 11.00000 -1.50000 H78C 2 0.733405 0.750450 0.640533 11.00000 -1.50000 AFIX 0 C79 1 0.907150 0.456268 0.914226 11.00000 0.02539 0.02697 = 0.02916 -0.00783 -0.00803 0.00159 C80 1 0.944408 0.405716 0.970607 11.00000 0.03518 0.03465 = 0.03207 -0.00893 -0.01174 0.00284 AFIX 43 H80 2 0.899809 0.379500 1.008568 11.00000 -1.20000 AFIX 0 C81 1 1.047017 0.393828 0.971060 11.00000 0.03786 0.03549 = 0.04388 -0.00821 -0.02170 0.00667 AFIX 43 H81 2 1.072424 0.358433 1.008928 11.00000 -1.20000 AFIX 0 C82 1 1.112080 0.432960 0.917048 11.00000 0.02618 0.04264 = 0.05333 -0.01317 -0.01796 0.00629 AFIX 43 H82 2 1.181886 0.425707 0.918486 11.00000 -1.20000 AFIX 0 C83 1 1.076023 0.482764 0.860752 11.00000 0.02353 0.04065 = 0.04388 -0.00943 -0.00800 0.00006 AFIX 43 H83 2 1.121438 0.509143 0.823464 11.00000 -1.20000 AFIX 0 C84 1 0.972912 0.494817 0.858060 11.00000 0.02385 0.03162 = 0.03440 -0.00789 -0.00670 0.00068 C85 1 1.006708 0.496336 0.708740 11.00000 0.02269 0.04544 = 0.03396 -0.00676 0.00101 0.00255 AFIX 13 H85 2 1.075523 0.509501 0.710803 11.00000 -1.20000 AFIX 0 C86 1 1.006019 0.402962 0.722955 11.00000 0.04523 0.04442 = 0.04159 -0.01541 -0.00624 0.01134 AFIX 137 H86A 2 1.015136 0.383531 0.772294 11.00000 -1.50000 H86B 2 1.060620 0.377045 0.690396 11.00000 -1.50000 H86C 2 0.941856 0.388208 0.715324 11.00000 -1.50000 AFIX 0 C87 1 0.982574 0.530334 0.634567 11.00000 0.03978 0.05424 = 0.03299 -0.00551 0.00230 0.00117 AFIX 137 H87A 2 0.918405 0.513068 0.629607 11.00000 -1.50000 H87B 2 1.035552 0.508957 0.598294 11.00000 -1.50000 H87C 2 0.978308 0.590750 0.628296 11.00000 -1.50000 AFIX 0 C88 1 0.954820 0.653717 0.762844 11.00000 0.02437 0.03508 = 0.04592 -0.00110 -0.00253 -0.00771 AFIX 13 H88 2 0.932500 0.679765 0.717141 11.00000 -1.20000 AFIX 0 C89 1 0.897930 0.704803 0.820051 11.00000 0.04613 0.03394 = 0.05703 -0.00921 -0.00476 -0.01103 AFIX 137 H89A 2 0.826075 0.700023 0.825304 11.00000 -1.50000 H89B 2 0.910143 0.762797 0.806128 11.00000 -1.50000 H89C 2 0.921017 0.684415 0.865480 11.00000 -1.50000 AFIX 0 C90 1 1.066801 0.663520 0.753480 11.00000 0.02655 0.04755 = 0.09992 -0.00075 -0.00660 -0.01274 AFIX 137 H90A 2 1.091056 0.644000 0.798628 11.00000 -1.50000 H90B 2 1.077208 0.721836 0.739205 11.00000 -1.50000 H90C 2 1.103712 0.630990 0.716622 11.00000 -1.50000 AFIX 0 C91 1 0.871375 0.097201 0.256458 11.00000 0.11613 0.12249 = 0.15059 -0.07709 -0.05387 0.03964 AFIX 137 H91A 2 0.904359 0.131293 0.214766 11.00000 -1.50000 H91B 2 0.863148 0.043651 0.243207 11.00000 -1.50000 H91C 2 0.912473 0.088763 0.294253 11.00000 -1.50000 AFIX 0 C92 1 0.769079 0.140534 0.283099 11.00000 0.08161 0.07239 = 0.11361 -0.04291 -0.03516 0.00766 AFIX 23 H92A 2 0.778893 0.193619 0.297682 11.00000 -1.20000 H92B 2 0.730990 0.153433 0.242948 11.00000 -1.20000 AFIX 0 C93 1 0.706008 0.092357 0.345191 11.00000 0.10210 0.04867 = 0.08146 -0.02497 -0.05456 0.01801 AFIX 23 H93A 2 0.696749 0.038970 0.330899 11.00000 -1.20000 H93B 2 0.743547 0.080126 0.385650 11.00000 -1.20000 AFIX 0 C94 1 0.604896 0.135283 0.370328 11.00000 0.09111 0.03647 = 0.07026 -0.00223 -0.04274 -0.00259 AFIX 23 H94A 2 0.567477 0.147236 0.329800 11.00000 -1.20000 H94B 2 0.614394 0.188878 0.384113 11.00000 -1.20000 AFIX 0 C95 1 0.541220 0.088766 0.432297 11.00000 0.13044 0.04386 = 0.05669 -0.00130 -0.03587 -0.01484 AFIX 23 H95A 2 0.536077 0.033385 0.420107 11.00000 -1.20000 H95B 2 0.575937 0.080861 0.474119 11.00000 -1.20000 AFIX 0 C96 1 0.438771 0.129013 0.452805 11.00000 0.11382 0.07668 = 0.07358 0.02314 -0.03935 -0.03565 AFIX 137 H96A 2 0.404054 0.138776 0.411508 11.00000 -1.50000 H96B 2 0.442589 0.181791 0.469260 11.00000 -1.50000 H96C 2 0.401855 0.093114 0.491223 11.00000 -1.50000 AFIX 0 HKLF 4 REM LB1231 in P-1 REM wR2 = 0.0717, GooF = S = 1.070, Restrained GooF = 1.072 for all data REM R1 = 0.0268 for 17102 Fo > 4sig(Fo) and 0.0270 for all 17241 data REM 876 parameters refined using 40 restraints END WGHT 0.0434 3.4714 REM Highest difference peak 1.724, deepest hole -2.013, 1-sigma level 0.085 Q1 1 0.7638 0.3968 0.7419 11.00000 0.05 1.72 Q2 1 0.6761 0.3801 0.7579 11.00000 0.05 1.18 Q3 1 0.6985 0.2867 0.7866 11.00000 0.05 1.02 Q4 1 0.7113 0.2999 0.7961 11.00000 0.05 1.00 Q5 1 0.8189 0.3363 0.7195 11.00000 0.05 0.95 Q6 1 0.7893 0.3194 0.7638 11.00000 0.05 0.95 Q7 1 0.7937 0.3003 0.7800 11.00000 0.05 0.93 Q8 1 0.6775 0.3826 0.7218 11.00000 0.05 0.93 Q9 1 0.6600 0.2924 0.7956 11.00000 0.05 0.82 Q10 1 0.6502 0.3510 0.8126 11.00000 0.05 0.80 ; _shelx_res_checksum 42601 _olex2_date_sample_data_collection 2021-03-01 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 2.288 _oxdiff_exptl_absorpt_empirical_full_min 0.629