data_v19009 # start Validation Reply Form _vrf_PLAT340_v19009 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.011 Ang. RESPONSE: The only carbon atoms are in a disordered cation in a cavity. The C-C bond precision is not bad for this situation. ; # end Validation Reply Form _audit_creation_date 2019-02-11 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506), SHELXL-2017/1, and manual edit ; _database_code_depnum_ccdc_archive ? _publ_contact_author_name 'Xray Staff' _publ_contact_author_address ; Beckman Institute Caltech 139-74 Pasadena CA 91125 USA ; _publ_contact_author_email xray@caltech.edu _shelx_SHELXL_version_number '2017/1' _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '10(O2 Si1), 0.89(F), C8 H15 N2' _chemical_formula_sum 'C8 H15 F0.89 N2 O20 Si10' _chemical_formula_weight 757.09 _chemical_absolute_configuration ad _chemical_melting_point ? 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' 'F' 'F' 0.0727 0.0534 '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' 'O' 'O' 0.0492 0.0322 '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' _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 'hexagonal' _space_group_IT_number 179 _space_group_name_H-M_alt 'P 65 2 2' _space_group_name_Hall 'P 65 2 (0 0 1)' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z+5/6' '-y, x-y, z+2/3' '-x, -y, z+1/2' '-x+y, -x, z+1/3' 'y, -x+y, z+1/6' 'x-y, -y, -z' '-x, -x+y, -z+1/3' 'y, x, -z+2/3' '-y, -x, -z+1/6' '-x+y, y, -z+1/2' 'x, x-y, -z+5/6' _cell_length_a 11.9347(18) _cell_length_b 11.9347(18) _cell_length_c 29.530(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3642.6(12) _cell_formula_units_Z 6 _cell_measurement_reflns_used 9820 _cell_measurement_temperature 298 _cell_measurement_theta_max 77.35 _cell_measurement_theta_min 4.28 _shelx_estimated_absorpt_T_max 0.887 _shelx_estimated_absorpt_T_min 0.791 _exptl_absorpt_coefficient_mu 6.144 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0992 before and 0.0803 after correction. The Ratio of minimum to maximum transmission is 0.7296. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'prism' _exptl_crystal_F_000 2310 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_unetI/netI 0.0365 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.949 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 16240 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.942 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 77.613 _diffrn_reflns_theta_min 4.277 _diffrn_ambient_temperature 298 _diffrn_detector 'CPAD Area Detector' _diffrn_detector_area_resol_mean 7.69 _diffrn_detector_type 'Bruker PHOTON II' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.949 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer mirrors' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'microfocus sealed tube' _diffrn_source_current 1 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatec I\mS HB' _diffrn_source_voltage 50 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.598 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.931 _reflns_number_gt 2262 _reflns_number_total 2443 _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_data_collection 'BIS V6.2.9/2018-03-16 & APEX3 v2018.7-2 (Bruker-AXS, 2018)' _computing_cell_refinement 'SAINT V8.38A (Bruker-AXS, 2016)' _computing_data_reduction 'SAINT V8.38A (Bruker-AXS, 2016)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2015)' _computing_molecular_graphics 'DIAMOND 3 (Crystal Impact, 1999)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _refine_diff_density_max 0.284 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.071 _refine_ls_abs_structure_details ; Flack x determined using 810 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_abs_structure_Hooft 0.05(2) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 2443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0347 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+6.5765P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.0807 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 2. Shared sites {C1, N1} 3. Uiso/Uaniso restraints and constraints Uanis(C1) = Uanis(N1) 4. Others Fixed Sof: C1(0.5) N1(0.5) H3A(0.5) H3B(0.5) H3C(0.5) H3D(0.5) H3E(0.5) H3F(0.5) H5A(0.5) H5B(0.5) H5C(0.5) 5.a Me refined with riding coordinates: C5(H5A,H5B,H5C) 5.b Idealised Me refined as rotating group: C3(H3A,H3B,H3C), C3(H3D,H3E,H3F), C4(H4A,H4B,H4C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 Si1 Si -0.02952(12) 0.12291(11) 0.53282(4) 0.0119(3) Uani 1 1 d . . . . . Si2 Si 0.25133(12) 0.33850(12) 0.54814(4) 0.0142(3) Uani 1 1 d . . . . . Si3 Si 0.52977(13) 0.41379(13) 0.53274(4) 0.0158(3) Uani 1 1 d . . . . . Si4 Si 0.70163(13) 0.37760(12) 0.46703(4) 0.0157(3) Uani 1 1 d . . . . . Si5 Si 0.90544(13) 0.30338(12) 0.48172(4) 0.0145(3) Uani 1 1 d . . . . . O1 O -0.0776(4) 0.000000 0.500000 0.0187(10) Uani 1 2 d S T P . . O2 O -0.0954(3) 0.2084(3) 0.52122(10) 0.0174(7) Uani 1 1 d . . . . . O3 O -0.0692(2) 0.0692(2) 0.583333 0.0177(10) Uani 1 2 d S T P . . O4 O 0.1249(3) 0.2134(3) 0.52767(10) 0.0174(7) Uani 1 1 d . . . . . O5 O 0.2347(3) 0.3236(3) 0.60197(10) 0.0210(8) Uani 1 1 d . . . . . O6 O 0.3739(3) 0.3281(3) 0.53069(11) 0.0206(7) Uani 1 1 d . . . . . O7 O 0.5845(3) 0.5558(3) 0.51095(11) 0.0232(8) Uani 1 1 d . . . . . O8 O 0.5843(2) 0.4157(2) 0.583333 0.0226(11) Uani 1 2 d S T P . . O9 O 0.5779(3) 0.3388(3) 0.49960(11) 0.0196(7) Uani 1 1 d . . . . . O10 O 0.6463(5) 0.3232(2) 0.416667 0.0217(11) Uani 1 2 d S T P . . O11 O 0.7874(3) 0.5329(3) 0.47020(12) 0.0227(8) Uani 1 1 d . . . . . O12 O 0.7723(3) 0.3046(4) 0.48829(11) 0.0209(7) Uani 1 1 d . . . . . F1 F 0.9082(5) 0.4541(3) 0.416667 0.0354(19) Uani 0.893(16) 2 d S T P . . C1 C 0.4953(6) 0.0087(6) 0.5225(2) 0.0408(14) Uani 0.5 1 d . . . A 1 N1 N 0.4953(6) 0.0087(6) 0.5225(2) 0.0408(14) Uani 0.5 1 d . . . A 2 C2 C 0.3926(6) 0.0151(6) 0.5369(2) 0.0365(14) Uani 1 1 d . . . . . N2 N 0.3175(7) 0.000000 0.500000 0.059(2) Uani 1 2 d S T P A . C3 C 0.6012(8) 0.0221(8) 0.5524(3) 0.067(2) Uani 1 1 d . . . . . H3A H 0.568711 -0.003804 0.582587 0.101 Uiso 0.5 1 calc GR . . A 1 H3B H 0.669715 0.110627 0.552572 0.101 Uiso 0.5 1 calc GR . . A 1 H3C H 0.633580 -0.031933 0.541312 0.101 Uiso 0.5 1 calc GR . . A 1 H3D H 0.644538 0.107100 0.565465 0.101 Uiso 0.5 1 calc GR . . A 2 H3E H 0.661724 0.009229 0.534957 0.101 Uiso 0.5 1 calc GR . . A 2 H3F H 0.565745 -0.041438 0.576050 0.101 Uiso 0.5 1 calc GR . . A 2 C4 C 0.3638(11) 0.0346(10) 0.5837(3) 0.099(4) Uani 1 1 d . . . . . H4A H 0.299462 0.060409 0.583542 0.148 Uiso 1 1 calc GR . . . . H4B H 0.441221 0.100752 0.597830 0.148 Uiso 1 1 calc GR . . . . H4C H 0.331917 -0.044756 0.600342 0.148 Uiso 1 1 calc GR . . . . C5 C 0.1965(9) 0.000000 0.500000 0.100(6) Uani 1 2 d S T P . . H5A H 0.163480 -0.012378 0.469658 0.150 Uiso 0.5 1 calc R . . A -1 H5B H 0.135225 -0.068887 0.518923 0.150 Uiso 0.5 1 calc R . . A -1 H5C H 0.210301 0.081265 0.511419 0.150 Uiso 0.5 1 calc R . . A -1 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 Si1 0.0127(6) 0.0119(6) 0.0109(5) 0.0001(5) 0.0001(5) 0.0060(5) Si2 0.0124(6) 0.0133(6) 0.0155(6) -0.0001(5) 0.0005(5) 0.0053(5) Si3 0.0144(6) 0.0161(6) 0.0168(6) 0.0008(5) 0.0014(5) 0.0074(5) Si4 0.0153(6) 0.0157(7) 0.0168(6) -0.0009(5) -0.0001(5) 0.0083(5) Si5 0.0143(6) 0.0135(6) 0.0161(6) 0.0008(5) 0.0001(5) 0.0074(6) O1 0.0211(19) 0.019(3) 0.015(2) -0.0029(19) -0.0015(9) 0.0096(13) O2 0.0190(17) 0.0179(17) 0.0169(15) 0.0021(13) 0.0041(14) 0.0104(15) O3 0.0219(19) 0.0219(19) 0.011(2) 0.0024(16) 0.0024(16) 0.012(2) O4 0.0146(17) 0.0163(17) 0.0182(16) -0.0025(13) -0.0001(13) 0.0053(14) O5 0.0199(19) 0.0192(18) 0.0175(16) -0.0007(13) 0.0006(14) 0.0049(15) O6 0.0162(18) 0.0202(18) 0.0253(18) -0.0032(15) 0.0013(14) 0.0090(15) O7 0.029(2) 0.0151(18) 0.0265(18) -0.0015(14) 0.0023(15) 0.0120(16) O8 0.026(2) 0.026(2) 0.019(2) -0.0036(17) -0.0036(17) 0.016(2) O9 0.0180(18) 0.0170(17) 0.0240(16) 0.0006(13) 0.0050(14) 0.0089(15) O10 0.021(3) 0.027(2) 0.016(2) -0.0015(17) 0.000 0.0104(13) O11 0.0203(18) 0.0182(18) 0.0278(19) 0.0012(15) 0.0045(15) 0.0083(15) O12 0.0173(18) 0.0232(19) 0.0255(18) 0.0052(15) 0.0045(14) 0.0126(15) F1 0.040(3) 0.033(3) 0.035(3) -0.0037(19) 0.000 0.0198(17) C1 0.037(3) 0.034(3) 0.044(3) 0.012(3) -0.002(3) 0.012(3) N1 0.037(3) 0.034(3) 0.044(3) 0.012(3) -0.002(3) 0.012(3) C2 0.032(3) 0.033(3) 0.035(3) -0.004(3) 0.000(3) 0.009(3) N2 0.038(4) 0.045(5) 0.096(7) 0.001(5) 0.000(2) 0.023(3) C3 0.053(5) 0.061(5) 0.079(6) 0.021(4) -0.017(4) 0.022(4) C4 0.125(10) 0.088(8) 0.058(6) 0.001(5) 0.033(6) 0.034(7) C5 0.038(4) 0.071(9) 0.203(17) -0.060(10) -0.030(5) 0.036(5) _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 Si1 O1 1.6059(13) . ? Si1 O2 1.606(3) . ? Si1 O3 1.5990(12) . ? Si1 O4 1.611(3) . ? Si2 O4 1.618(3) . ? Si2 O5 1.601(3) . ? Si2 O6 1.614(3) . ? Si2 O11 1.610(4) 7_566 ? Si3 O6 1.615(3) . ? Si3 O7 1.614(4) . ? Si3 O8 1.625(2) . ? Si3 O9 1.614(4) . ? Si4 O9 1.623(3) . ? Si4 O10 1.625(2) . ? Si4 O11 1.611(4) . ? Si4 O12 1.612(3) . ? Si5 O2 1.623(3) 1_655 ? Si5 O5 1.616(3) 2_654 ? Si5 O7 1.601(4) 7_666 ? Si5 O12 1.608(3) . ? C1 C1 1.341(12) 7_556 ? C1 C2 1.335(9) . ? C1 C3 1.483(9) . ? N1 C2 1.335(9) . ? N1 C3 1.483(9) . ? C2 N2 1.365(8) . ? C2 C4 1.471(9) . ? N2 C5 1.444(13) . ? 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 O1 Si1 O2 112.8(2) . . ? O1 Si1 O4 108.8(2) . . ? O2 Si1 O4 108.26(18) . . ? O3 Si1 O1 107.32(11) . . ? O3 Si1 O2 108.2(2) . . ? O3 Si1 O4 111.52(15) . . ? O5 Si2 O4 105.17(17) . . ? O5 Si2 O6 112.05(19) . . ? O5 Si2 O11 112.48(19) . 7_566 ? O6 Si2 O4 105.85(18) . . ? O11 Si2 O4 108.68(19) 7_566 . ? O11 Si2 O6 112.09(19) 7_566 . ? O6 Si3 O8 111.70(15) . . ? O7 Si3 O6 112.56(19) . . ? O7 Si3 O8 113.74(16) . . ? O9 Si3 O6 104.06(18) . . ? O9 Si3 O7 105.72(18) . . ? O9 Si3 O8 108.3(2) . . ? O9 Si4 O10 107.4(2) . . ? O11 Si4 O9 104.94(19) . . ? O11 Si4 O10 114.24(16) . . ? O11 Si4 O12 113.34(19) . . ? O12 Si4 O9 105.17(18) . . ? O12 Si4 O10 110.98(15) . . ? O5 Si5 O2 104.03(17) 2_654 1_655 ? O7 Si5 O2 108.51(18) 7_666 1_655 ? O7 Si5 O5 113.43(19) 7_666 2_654 ? O7 Si5 O12 111.58(19) 7_666 . ? O12 Si5 O2 104.98(18) . 1_655 ? O12 Si5 O5 113.53(19) . 2_654 ? Si1 O1 Si1 168.6(4) . 7_556 ? Si1 O2 Si5 139.7(2) . 1_455 ? Si1 O3 Si1 169.5(3) . 10_556 ? Si1 O4 Si2 144.1(2) . . ? Si2 O5 Si5 141.3(2) . 6_565 ? Si2 O6 Si3 137.8(2) . . ? Si5 O7 Si3 145.1(2) 7_566 . ? Si3 O8 Si3 140.9(3) . 10_666 ? Si3 O9 Si4 136.6(2) . . ? Si4 O10 Si4 138.8(3) . 12 ? Si2 O11 Si4 146.1(2) 7_666 . ? Si5 O12 Si4 138.1(2) . . ? C1 C1 C3 127.0(4) 7_556 . ? C2 C1 C1 108.8(4) . 7_556 ? C2 C1 C3 124.2(6) . . ? C2 N1 C3 124.2(6) . . ? C1 C2 N2 107.4(6) . . ? C1 C2 C4 127.0(7) . . ? N1 C2 N2 107.4(6) . . ? N1 C2 C4 127.0(7) . . ? N2 C2 C4 125.5(7) . . ? C2 N2 C2 107.5(8) . 7_556 ? C2 N2 C5 126.2(4) 7_556 . ? C2 N2 C5 126.2(4) . . ? _shelx_res_file ; TITL v19009 in P6(5)22 v19009.res created by SHELXL-2017/1 at 03:50:20 on 11-Feb-2019 CELL 1.54178 11.9347 11.9347 29.53 90 90 120 ZERR 6 0.0018 0.0018 0.0036 0 0 0 LATT -1 SYMM -Y+X,+X,0.833+Z SYMM -Y,+X-Y,0.667+Z SYMM -X,-Y,0.5+Z SYMM +Y-X,-X,0.333+Z SYMM +Y,-X+Y,0.167+Z SYMM -Y+X,-Y,-Z SYMM -X,-X+Y,0.333-Z SYMM +Y,+X,0.667-Z SYMM -Y,-X,0.167-Z SYMM +Y-X,+Y,0.5-Z SYMM +X,+X-Y,0.833-Z SFAC C H F N O Si UNIT 48 90 5.36 12 120 60 EADP C1 N1 EXYZ C1 N1 L.S. 55 PLAN 20 SIZE 0.02 0.03 0.04 TEMP 25 FREE Si5 O5 fmap -2 acta REM REM REM WGHT 0.025200 6.576500 FVAR 0.08343 SI1 6 -0.029524 0.122913 0.532820 11.00000 0.01273 0.01190 = 0.01092 0.00008 0.00014 0.00597 SI2 6 0.251327 0.338497 0.548140 11.00000 0.01236 0.01330 = 0.01555 -0.00011 0.00045 0.00534 SI3 6 0.529769 0.413787 0.532742 11.00000 0.01440 0.01608 = 0.01679 0.00081 0.00137 0.00742 SI4 6 0.701627 0.377598 0.467027 11.00000 0.01531 0.01568 = 0.01677 -0.00092 -0.00011 0.00833 SI5 6 0.905440 0.303382 0.481718 11.00000 0.01433 0.01352 = 0.01608 0.00075 0.00010 0.00736 O1 5 -0.077585 0.000000 0.500000 10.50000 0.02109 0.01917 = 0.01516 -0.00294 -0.00147 0.00958 O2 5 -0.095429 0.208391 0.521219 11.00000 0.01898 0.01791 = 0.01689 0.00212 0.00413 0.01040 O3 5 -0.069168 0.069168 0.583333 10.50000 0.02188 0.02188 = 0.01060 0.00242 0.00242 0.01183 O4 5 0.124877 0.213419 0.527673 11.00000 0.01461 0.01627 = 0.01817 -0.00254 -0.00009 0.00535 O5 5 0.234676 0.323569 0.601974 11.00000 0.01988 0.01920 = 0.01752 -0.00074 0.00060 0.00494 O6 5 0.373929 0.328094 0.530691 11.00000 0.01617 0.02024 = 0.02532 -0.00317 0.00126 0.00903 O7 5 0.584547 0.555785 0.510945 11.00000 0.02934 0.01512 = 0.02645 -0.00151 0.00226 0.01204 O8 5 0.584290 0.415710 0.583333 10.50000 0.02648 0.02648 = 0.01887 -0.00363 -0.00363 0.01636 O9 5 0.577941 0.338770 0.499601 11.00000 0.01801 0.01697 = 0.02404 0.00059 0.00502 0.00886 O10 5 0.646348 0.323174 0.416667 10.50000 0.02083 0.02661 = 0.01574 -0.00151 0.00000 0.01042 O11 5 0.787353 0.532884 0.470198 11.00000 0.02034 0.01817 = 0.02782 0.00118 0.00453 0.00831 O12 5 0.772277 0.304621 0.488290 11.00000 0.01728 0.02318 = 0.02546 0.00522 0.00451 0.01256 F1 3 0.908176 0.454088 0.416667 0.44672 0.03958 0.03341 = 0.03522 -0.00368 0.00000 0.01979 PART 1 C1 1 0.495296 0.008736 0.522509 10.50000 0.03670 0.03446 = 0.04404 0.01230 -0.00191 0.01248 PART 0 PART 2 N1 4 0.495296 0.008736 0.522509 10.50000 0.03670 0.03446 = 0.04404 0.01230 -0.00191 0.01248 PART 0 C2 1 0.392579 0.015053 0.536900 11.00000 0.03203 0.03342 = 0.03483 -0.00408 -0.00003 0.00941 N2 4 0.317474 0.000000 0.500000 10.50000 0.03790 0.04522 = 0.09628 0.00076 0.00038 0.02261 C3 1 0.601155 0.022083 0.552377 11.00000 0.05304 0.06104 = 0.07918 0.02114 -0.01672 0.02167 PART 1 AFIX 137 H3A 2 0.568711 -0.003804 0.582587 10.50000 -1.50000 H3B 2 0.669715 0.110627 0.552572 10.50000 -1.50000 H3C 2 0.633580 -0.031933 0.541312 10.50000 -1.50000 AFIX 137 PART 0 PART 2 H3D 2 0.644538 0.107100 0.565465 10.50000 -1.50000 H3E 2 0.661724 0.009229 0.534957 10.50000 -1.50000 H3F 2 0.565745 -0.041438 0.576050 10.50000 -1.50000 AFIX 0 PART 0 C4 1 0.363795 0.034559 0.583719 11.00000 0.12544 0.08777 = 0.05763 0.00110 0.03327 0.03439 AFIX 137 H4A 2 0.299462 0.060409 0.583542 11.00000 -1.50000 H4B 2 0.441221 0.100752 0.597830 11.00000 -1.50000 H4C 2 0.331917 -0.044756 0.600342 11.00000 -1.50000 AFIX 0 C5 1 0.196481 0.000000 0.500000 10.50000 0.03786 0.07105 = 0.20296 -0.06042 -0.03021 0.03553 PART -1 AFIX 33 H5A 2 0.163480 -0.012378 0.469658 10.50000 -1.50000 H5B 2 0.135225 -0.068887 0.518923 10.50000 -1.50000 H5C 2 0.210301 0.081265 0.511419 10.50000 -1.50000 AFIX 0 HKLF 4 REM v19009 in P6(5)22 REM R1 = 0.0347 for 2262 Fo > 4sig(Fo) and 0.0382 for all 2443 data REM 192 parameters refined using 0 restraints END WGHT 0.0252 6.5765 REM Highest difference peak 0.284, deepest hole -0.319, 1-sigma level 0.071 Q1 1 0.5013 0.3632 0.5528 11.00000 0.05 -0.32 Q2 1 0.1386 0.1371 0.5283 11.00000 0.05 0.28 Q3 1 0.7230 0.4153 0.4486 11.00000 0.05 -0.28 Q4 1 0.6492 0.6356 0.5176 11.00000 0.05 0.27 Q5 1 0.3982 -0.0348 0.5300 11.00000 0.05 0.27 Q6 1 0.0151 0.2280 0.5178 11.00000 0.05 0.26 Q7 1 0.2365 -0.0567 0.5901 11.00000 0.05 0.26 Q8 1 0.4284 0.0530 0.5488 11.00000 0.05 0.26 Q9 1 0.4623 0.1822 0.6308 11.00000 0.05 -0.25 Q10 1 0.5139 0.5638 0.5234 11.00000 0.05 0.25 Q11 1 0.4029 0.3795 0.5200 11.00000 0.05 0.24 Q12 1 0.0812 0.2179 0.5113 11.00000 0.05 0.24 Q13 1 0.9812 0.5556 0.4139 11.00000 0.05 0.23 Q14 1 0.7623 0.2427 0.4836 11.00000 0.05 0.23 Q15 1 0.9496 0.3150 0.4683 11.00000 0.05 -0.23 Q16 1 0.2944 0.0033 0.5184 11.00000 0.05 -0.23 Q17 1 0.6775 0.2576 0.4139 11.00000 0.05 0.23 Q18 1 0.4811 0.3816 0.5784 11.00000 0.05 0.22 Q19 1 0.8096 0.5835 0.4947 11.00000 0.05 -0.22 Q20 1 0.1945 0.2234 0.5416 11.00000 0.05 0.22 ; _shelx_res_checksum 83200 _shelx_hkl_file ; 1 -1 0 27.09 1.37 -1 1 0 25.26 1.36 0 -1 0 24.78 1.39 0 1 0 24.82 1.40 0 1 0 24.48 1.45 1 1 0 6.19 0.46 1 -2 0 6.13 0.79 -1 -1 0 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0 0.00 0.00 ; _shelx_hkl_checksum 10287 _olex2_submission_special_instructions 'No special instructions were received'