data_wl-s2cl5br-ligand
_audit_creation_date 2018-05-10
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2018.04.26 svn.r3501 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number '2018/3'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Bruker (2013). SAINT-Plus V8.34A Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2016). APEX2 Version 2016.5-1. Bruker AXS Inc., Madison, Wisconsin, USA.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., and Stalke, D., J. Appl. Cryst. (2015). 48, 1907-1913.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790
Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984
Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580
Petricek,V., Dusek,M. & Palatinus,L.(2006). Jana2006. The crystallographic computing system. Institute of Physics, Praha, Czech Republic.
Rigaku Oxford Diffraction, (2015), CrysAlisPro Software system, version 1.171.39.20a, Rigaku Corporation, Oxford, UK.
Sheldrick, G.M. (2015). Acta Cryst. (2015). A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. (2015). C71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
Spek, A. L. (2015). Acta Cryst. C71, 9-18.
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. A71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic
;
(1S)-1-(5-bromo-2-chlorophenyl)-2,2-diphenylcyclopropanecarboxylic acid
;
_chemical_formula_moiety 'C22 H16 Br Cl O2'
_chemical_formula_sum 'C22 H16 Br Cl O2'
_chemical_formula_weight 427.71
_chemical_absolute_configuration ad
_chemical_melting_point ?
_chemical_oxdiff_formula 'C176 H124 Br8 Cl8 O16 '
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'
'Br' 'Br' -0.6763 1.2805
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.3639 0.7018 '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'
_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 'orthorhombic'
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 8.91980(10)
_cell_length_b 14.41860(10)
_cell_length_c 29.7333(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3824.03(6)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 20231
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 77.9240
_cell_measurement_theta_min 2.9750
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 4.317
_exptl_absorpt_correction_T_max 0.873
_exptl_absorpt_correction_T_min 0.519
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
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 colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.486
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 1728
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 9 4 0.0470
0 -9 -4 0.0470
-5 0 -7 0.0913
5 0 7 0.0913
0 -1 0 0.0520
0 1 0 0.0520
5 0 1 0.0920
-5 0 -1 0.0920
0 0 -1 0.0971
0 0 1 0.0971
0 4 -5 0.0580
0 -4 5 0.0580
3 0 -5 0.0948
-4 0 5 0.1056
-1 1 -5 0.0810
1 -1 5 0.0810
2 -5 -2 0.0695
-1 -1 -5 0.0686
0 3 5 0.0556
-2 5 -3 0.0699
2 -5 3 0.0699
1 3 -5 0.0675
_exptl_crystal_recrystallization_method
'slow evaporation of 2% EtOAc in hexane'
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.168
_exptl_crystal_size_min 0.094
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
-0.0043 8.9966 4.0175 0.2425 -0.4357 -0.8476
0.0043 -8.9966 -4.0175 -0.2425 0.4357 0.8476
-5.0019 0.0048 -6.9572 -0.4493 0.7137 -0.4067
5.0019 -0.0048 6.9572 0.4493 -0.7137 0.4067
0.0007 -1.0001 -0.0024 -0.0041 0.0509 0.0938
-0.0007 1.0001 0.0024 0.0041 -0.0509 -0.0938
4.9994 0.0014 0.9638 0.1405 -0.7476 0.4118
-4.9994 -0.0014 -0.9638 -0.1405 0.7476 -0.4118
-0.0004 0.0010 -0.9989 -0.0515 -0.0057 0.0009
0.0004 -0.0010 0.9989 0.0515 0.0057 -0.0009
-0.0048 4.0055 -4.9848 -0.2410 -0.2319 -0.3710
0.0048 -4.0055 4.9848 0.2410 0.2319 0.3710
2.9973 0.0066 -5.0156 -0.2038 -0.4802 0.2518
-3.9971 -0.0071 5.0226 0.1860 0.6308 -0.3344
-1.0026 1.0048 -4.9851 -0.2710 0.0715 -0.1721
1.0026 -1.0048 4.9851 0.2710 -0.0715 0.1721
2.0021 -4.9974 -2.0240 -0.0877 -0.0580 0.6358
-1.0012 -0.9954 -4.9899 -0.2792 0.1733 0.0155
0.0001 2.9951 5.0018 0.2695 -0.1245 -0.2857
-2.0042 5.0025 -2.9705 -0.1696 0.0297 -0.6315
2.0042 -5.0025 2.9705 0.1696 -0.0297 0.6315
0.9957 3.0059 -4.9942 -0.2272 -0.3317 -0.1946
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0333
_diffrn_reflns_av_unetI/netI 0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 23741
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.913
_diffrn_reflns_theta_min 3.407
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100(2)
_diffrn_detector HyPix
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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 93.00 170.00 0.50 3.00 -- 110.00 125.00 0.00 154
2 \w 105.00 177.00 0.50 3.00 -- 110.00 84.00 156.00 144
3 \w 94.00 177.00 0.50 3.00 -- 110.00 61.00 120.00 166
4 \w -62.00 26.00 0.50 0.50 -- -47.12 57.00 0.00 176
5 \w 36.00 121.00 0.50 0.50 -- 47.12 38.00 -8.00 170
6 \w -67.00 -42.00 0.50 3.00 -- -88.50 38.00 -8.00 50
7 \w 92.00 173.00 0.50 3.00 -- 110.00 15.00 90.00 162
8 \w -119.00 -52.00 0.50 0.50 -- -47.12 -19.00 90.00 134
9 \w 4.00 35.00 0.50 0.50 -- 47.12 -57.00 120.00 62
10 \w 43.00 89.00 0.50 3.00 -- 110.00 -61.00 90.00 92
11 \w 39.00 88.00 0.50 3.00 -- 110.00 -61.00 30.00 98
12 \w 51.00 88.00 0.50 3.00 -- 110.00 -61.00-120.00 74
13 \w 38.00 106.00 0.50 3.00 -- 110.00 -77.00 90.00 136
14 \w 60.00 86.00 0.50 3.00 -- 110.00 -95.00 -30.00 52
15 \w 51.00 79.00 0.50 0.50 -- 47.12-125.00 -60.00 56
16 \w -137.00-112.00 0.50 3.00 -- -88.50-132.00 -28.00 50
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0181794000
_diffrn_orient_matrix_UB_12 0.0039626000
_diffrn_orient_matrix_UB_13 0.0515107000
_diffrn_orient_matrix_UB_21 -0.1506114000
_diffrn_orient_matrix_UB_22 -0.0510278000
_diffrn_orient_matrix_UB_23 0.0056679000
_diffrn_orient_matrix_UB_31 0.0825835000
_diffrn_orient_matrix_UB_32 -0.0937374000
_diffrn_orient_matrix_UB_33 -0.0009836000
_diffrn_radiation_monochromator 'multilayer mirror'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_current 1.0
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage 50
_reflns_Friedel_coverage 0.756
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.947
_reflns_number_gt 7700
_reflns_number_total 7890
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 68.13
_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 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max 0.475
_refine_diff_density_min -0.390
_refine_diff_density_rms 0.049
_refine_ls_abs_structure_details
;
Flack x determined using 3254 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.010(5)
_refine_ls_extinction_coef 0.00019(5)
_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 1.057
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 528
_refine_ls_number_reflns 7890
_refine_ls_number_restraints 308
_refine_ls_R_factor_all 0.0253
_refine_ls_R_factor_gt 0.0242
_refine_ls_restrained_S_all 1.071
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+1.1253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0618
_refine_ls_wR_factor_ref 0.0621
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All O(H) groups
At 1.5 times of:
All H(H) groups
2. Restrained distances
O1-H1
0.955 with sigma of 0.002
H1-O1'
1.655 with sigma of 0.001
C3'-H3'B \\sim C3'-H3'A
with sigma of 0.002
C3-H3A \\sim C3'-H3'B
with sigma of 0.002
C4_2-C1' \\sim C4_3-C1'
with sigma of 0.001
C3-H3A \\sim C3-H3B
with sigma of 0.001
C2'-C11_5 \\sim C2'-C11_4
with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C4_3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C5_3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C11_4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.002
Uiso(H3'B) = Uiso(H3'A)
Uanis(C11_4) = Uanis(C11_5)
Uanis(C16_4) = Uanis(C16_5)
Uanis(C15_4) = Uanis(C15_5)
Uanis(C14_4) = Uanis(C14_5)
Uanis(C13_4) = Uanis(C13_5)
Uanis(C12_4) = Uanis(C12_5)
Uanis(C5_2) = Uanis(C5_3)
Uanis(C4_2) = Uanis(C4_3)
Uanis(C9_2) = Uanis(C9_3)
Uanis(C8_2) = Uanis(C8_3)
Uanis(C7_2) = Uanis(C7_3)
Uanis(C6_2) = Uanis(C6_3)
Uiso(H3A) = Uiso(H3B)
Uiso(H3B) = Uiso(H3'B)
Uanis(Br1_2) = Uanis(Br1_3)
Uanis(Cl1_3) = Uanis(Cl1_2)
4. Rigid body (RIGU) restrains
Br1_1, Cl1_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1
Br1_2, Cl1_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2
Br1_3, Cl1_3, C4_3, C5_3, C6_3, C7_3, C8_3, C9_3
with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0004
C11_4, C12_4, C13_4, C14_4, C15_4, C16_4
C11_5, C12_5, C13_5, C14_5, C15_5, C16_5
with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0004
5. Same fragment restrains
{Br1_2, Cl1_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2}
{Br1_3, Cl1_3, C4_3, C5_3, C6_3, C7_3, C8_3, C9_3}
as
{Br1_1, Cl1_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1} sigma for 1-2: 0.002 1-3:
0.004
{C11_5, C12_5, C13_5, C14_5, C15_5, C16_5}
as
{C11_4, C12_4, C13_4, C14_4, C15_4, C16_4} sigma for 1-2: 0.002 1-3: 0.004
6. Others
Sof(Br1)=Sof(Cl1)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C8)=
Sof(C9)=Sof(H9)=1-FVAR(1)
Sof(Br1)=Sof(Cl1)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C8)=
Sof(C9)=Sof(H9)=FVAR(1)
Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=
Sof(H15)=Sof(C16)=Sof(H16)=1-FVAR(2)
Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=
Sof(H15)=Sof(C16)=Sof(H16)=FVAR(2)
Fixed X: H1(0.49172)
Fixed Y: H1(0.25486)
Fixed Z: H1(0.59948)
7.a Aromatic/amide H refined with riding coordinates:
C16(H16), C15(H15), C14(H14), C13(H13), C12(H12), C18(H18), C19(H19),
C20(H20), C21(H21), C22(H22), C18'(H18'), C19'(H19'), C20'(H20'), C21'(H21'),
C22'(H22'), C6(H6), C7(H7), C9(H9), C6(H6), C7(H7), C9(H9), C6(H6), C7(H7),
C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C12(H12), C13(H13),
C14(H14), C15(H15), C16(H16)
7.b Idealised tetrahedral OH refined as rotating group:
O2'(H2')
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_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
C11 C 0.3547(3) 0.54966(16) 0.70034(8) 0.0170(4) Uani 1 1 d . . . . .
C1 C 0.5253(2) 0.45853(16) 0.64236(8) 0.0160(4) Uani 1 1 d . . . . .
C16 C 0.2915(3) 0.53053(17) 0.74227(9) 0.0215(5) Uani 1 1 d . . . . .
H16 H 0.265653 0.469817 0.749443 0.026 Uiso 1 1 calc R . . . .
C2 C 0.3707(3) 0.47238(16) 0.66615(8) 0.0162(4) Uani 1 1 d . . . . .
C15 C 0.2664(3) 0.60072(18) 0.77355(9) 0.0240(5) Uani 1 1 d . . . . .
H15 H 0.223663 0.586644 0.801250 0.029 Uiso 1 1 calc R . . . .
C3 C 0.3913(3) 0.49966(17) 0.61768(8) 0.0182(5) Uani 1 1 d D . . . .
H3A H 0.396(4) 0.5668(11) 0.6098(11) 0.021(4) Uiso 1 1 d D . . . .
H3B H 0.346(3) 0.4586(18) 0.5944(8) 0.021(4) Uiso 1 1 d D . . . .
H1 H 0.491720 0.254860 0.599480 0.032 Uiso 1 1 d DR . . . .
C14 C 0.3048(3) 0.69129(19) 0.76351(10) 0.0251(5) Uani 1 1 d . . . . .
H14 H 0.286902 0.738493 0.784135 0.030 Uiso 1 1 calc R . . . .
C13 C 0.3703(3) 0.71083(19) 0.72243(11) 0.0297(6) Uani 1 1 d . . . . .
H13 H 0.398450 0.771373 0.715718 0.036 Uiso 1 1 calc R . . . .
C12 C 0.3946(3) 0.64081(18) 0.69101(10) 0.0244(5) Uani 1 1 d . . . . .
H12 H 0.438031 0.655233 0.663447 0.029 Uiso 1 1 calc R . . . .
C10 C 0.5648(3) 0.36204(16) 0.62805(8) 0.0161(4) Uani 1 1 d . . . . .
C17 C 0.2796(3) 0.38784(16) 0.67746(8) 0.0163(4) Uani 1 1 d . . . . .
C18 C 0.3404(3) 0.31293(17) 0.70092(9) 0.0206(5) Uani 1 1 d . . . . .
H18 H 0.441920 0.312903 0.708033 0.025 Uiso 1 1 calc R . . . .
C19 C 0.2517(3) 0.23855(18) 0.71381(10) 0.0257(5) Uani 1 1 d . . . . .
H19 H 0.294162 0.188530 0.728897 0.031 Uiso 1 1 calc R . . . .
C20 C 0.0997(3) 0.2389(2) 0.70415(11) 0.0291(6) Uani 1 1 d . . . . .
H20 H 0.039729 0.189378 0.712977 0.035 Uiso 1 1 calc R . . . .
C21 C 0.0374(3) 0.3133(2) 0.68126(10) 0.0284(6) Uani 1 1 d . . . . .
H21 H -0.064702 0.314027 0.675006 0.034 Uiso 1 1 calc R . . . .
C22 C 0.1274(3) 0.38695(18) 0.66765(9) 0.0214(5) Uani 1 1 d . . . . .
H22 H 0.085133 0.436080 0.651833 0.026 Uiso 1 1 calc R . . . .
O1 O 0.4665(2) 0.31879(11) 0.60431(7) 0.0238(4) Uani 1 1 d D . . . .
O2 O 0.6888(2) 0.32844(11) 0.63838(7) 0.0209(4) Uani 1 1 d . . . . .
C1' C 0.6977(3) 0.01755(16) 0.58158(8) 0.0170(4) Uani 1 1 d D . . . .
C2' C 0.7088(3) 0.00711(16) 0.52903(8) 0.0173(4) Uani 1 1 d D . . . .
C3' C 0.5828(3) -0.03607(16) 0.55502(9) 0.0197(5) Uani 1 1 d D . . . .
H3'A H 0.587(4) -0.1040(11) 0.5611(11) 0.021(4) Uiso 1 1 d D . . . .
H3'B H 0.480(2) -0.009(2) 0.5528(11) 0.021(4) Uiso 1 1 d D . . . .
C10' C 0.6529(3) 0.11346(16) 0.59615(8) 0.0166(5) Uani 1 1 d . . . . .
C17' C 0.6741(3) 0.09010(17) 0.49982(8) 0.0195(5) Uani 1 1 d . . . . .
C18' C 0.7633(3) 0.16947(18) 0.50071(9) 0.0239(5) Uani 1 1 d . . . . .
H18' H 0.843053 0.173411 0.520757 0.029 Uiso 1 1 calc R . . . .
C19' C 0.7331(4) 0.24292(19) 0.47163(10) 0.0316(6) Uani 1 1 d . . . . .
H19' H 0.792144 0.296050 0.472488 0.038 Uiso 1 1 calc R . . . .
C20' C 0.6155(4) 0.2369(2) 0.44150(11) 0.0353(7) Uani 1 1 d . . . . .
H20' H 0.596755 0.285513 0.421759 0.042 Uiso 1 1 calc R . . . .
C21' C 0.5261(4) 0.1590(2) 0.44062(10) 0.0345(7) Uani 1 1 d . . . . .
H21' H 0.446103 0.155488 0.420617 0.041 Uiso 1 1 calc R . . . .
C22' C 0.5556(3) 0.08556(19) 0.46973(9) 0.0257(5) Uani 1 1 d . . . . .
H22' H 0.495217 0.032985 0.468978 0.031 Uiso 1 1 calc R . . . .
O1' O 0.52585(19) 0.14426(8) 0.58846(7) 0.0228(4) Uani 1 1 d D . . . .
O2' O 0.7577(2) 0.16007(12) 0.61615(6) 0.0222(4) Uani 1 1 d . . . . .
H2' H 0.722353 0.221163 0.622642 0.027 Uiso 1 1 calc GR . . . .
Br1_1 Br 0.93608(4) 0.69649(2) 0.58355(2) 0.03685(10) Uani 1 1 d D U . . .
Cl1_1 Cl 0.66340(7) 0.44281(4) 0.73904(2) 0.02308(13) Uani 1 1 d D U . . .
C4_1 C 0.6605(2) 0.51591(15) 0.65444(7) 0.0168(4) Uani 1 1 d D U . . .
C5_1 C 0.7331(2) 0.51161(15) 0.69588(7) 0.0181(4) Uani 1 1 d D U . . .
C6_1 C 0.8642(3) 0.56043(16) 0.70450(8) 0.0222(4) Uani 1 1 d D U . . .
H6_1 H 0.910213 0.555690 0.732470 0.027 Uiso 1 1 calc R . . . .
C7_1 C 0.9268(3) 0.61639(17) 0.67136(8) 0.0250(4) Uani 1 1 d D U . . .
H7_1 H 1.014249 0.649652 0.676768 0.030 Uiso 1 1 calc R . . . .
C8_1 C 0.8553(3) 0.62123(16) 0.63012(8) 0.0238(4) Uani 1 1 d D U . . .
C9_1 C 0.7246(3) 0.57265(16) 0.62158(8) 0.0205(4) Uani 1 1 d D U . . .
H9_1 H 0.678821 0.577838 0.593595 0.025 Uiso 1 1 calc R . . . .
Br1_2 Br 1.25971(5) 0.01467(10) 0.63827(2) 0.0372(2) Uani 0.867(4) 1 d D U P A 1
Cl1_2 Cl 0.58927(16) -0.13478(19) 0.65062(7) 0.0348(3) Uani 0.867(4) 1 d D U P A
1
C4_2 C 0.8084(3) -0.0276(3) 0.61280(16) 0.0177(5) Uani 0.867(4) 1 d D U P A 1
C5_2 C 0.7722(3) -0.0949(3) 0.64467(15) 0.0214(5) Uani 0.867(4) 1 d D U P A 1
C6_2 C 0.8779(3) -0.1314(4) 0.67408(15) 0.0261(5) Uani 0.867(4) 1 d D U P A 1
H6_2 H 0.850081 -0.177043 0.694559 0.031 Uiso 0.867(4) 1 calc R . P A 1
C7_2 C 1.0252(3) -0.1000(3) 0.67297(14) 0.0273(5) Uani 0.867(4) 1 d D U P A 1
H7_2 H 1.097100 -0.123986 0.692416 0.033 Uiso 0.867(4) 1 calc R . P A 1
C8_2 C 1.0614(3) -0.0320(2) 0.64206(10) 0.0233(6) Uani 0.867(4) 1 d D U P A 1
C9_2 C 0.9564(3) 0.0042(2) 0.61267(11) 0.0189(8) Uani 0.867(4) 1 d D U P A 1
H9_2 H 0.984673 0.050300 0.592524 0.023 Uiso 0.867(4) 1 calc R . P A 1
Br1_3 Br 1.2597(4) -0.0240(5) 0.63697(13) 0.0372(2) Uani 0.133(4) 1 d D U P A 2
Cl1_3 Cl 0.5701(9) -0.1381(14) 0.6441(6) 0.0348(3) Uani 0.133(4) 1 d D U P A 2
C4_3 C 0.8037(9) -0.0365(19) 0.6109(10) 0.0177(5) Uani 0.133(4) 1 d D U P A 2
C5_3 C 0.7556(12) -0.101(2) 0.6425(9) 0.0214(5) Uani 0.133(4) 1 d D U P A 2
C6_3 C 0.8509(12) -0.136(2) 0.6754(9) 0.0261(5) Uani 0.133(4) 1 d D U P A 2
H6_3 H 0.813358 -0.174412 0.697871 0.031 Uiso 0.133(4) 1 calc R . P A 2
C7_3 C 1.0025(10) -0.113(2) 0.6749(8) 0.0273(5) Uani 0.133(4) 1 d D U P A 2
H7_3 H 1.067272 -0.135492 0.696879 0.033 Uiso 0.133(4) 1 calc R . P A 2
C8_3 C 1.0540(7) -0.0569(16) 0.6406(6) 0.0233(6) Uani 0.133(4) 1 d D U P A 2
C9_3 C 0.9565(9) -0.015(2) 0.6104(8) 0.0189(8) Uani 0.133(4) 1 d D U P A 2
H9_3 H 0.993325 0.026912 0.589555 0.023 Uiso 0.133(4) 1 calc R . P A 2
C11_4 C 0.8325(8) -0.0514(7) 0.5096(7) 0.0195(6) Uani 0.410(11) 1 d D U P B 1
C12_4 C 0.8028(8) -0.1413(7) 0.4943(4) 0.0201(9) Uani 0.410(11) 1 d D U P B 1
H12_4 H 0.705807 -0.164650 0.496305 0.024 Uiso 0.410(11) 1 calc R . P B 1
C13_4 C 0.9157(10) -0.1964(5) 0.4762(3) 0.0232(9) Uani 0.410(11) 1 d D U P B 1
H13_4 H 0.893364 -0.254380 0.464202 0.028 Uiso 0.410(11) 1 calc R . P B 1
C14_4 C 1.0622(9) -0.1639(6) 0.4762(3) 0.0226(8) Uani 0.410(11) 1 d D U P B 1
H14_4 H 1.139558 -0.202354 0.466645 0.027 Uiso 0.410(11) 1 calc R . P B 1
C15_4 C 1.0936(7) -0.0748(7) 0.4902(3) 0.0219(8) Uani 0.410(11) 1 d D U P B 1
H15_4 H 1.191656 -0.052881 0.489346 0.026 Uiso 0.410(11) 1 calc R . P B 1
C16_4 C 0.9790(8) -0.0175(6) 0.5058(4) 0.0201(8) Uani 0.410(11) 1 d D U P B 1
H16_4 H 0.999876 0.043531 0.513653 0.024 Uiso 0.410(11) 1 calc R . P B 1
C11_5 C 0.8222(6) -0.0592(5) 0.5098(5) 0.0195(6) Uani 0.590(11) 1 d D U P B 2
C12_5 C 0.7720(6) -0.1403(5) 0.4888(3) 0.0201(9) Uani 0.590(11) 1 d D U P B 2
H12_5 H 0.669854 -0.153114 0.488168 0.024 Uiso 0.590(11) 1 calc R . P B 2
C13_5 C 0.8716(8) -0.2022(4) 0.4689(2) 0.0232(9) Uani 0.590(11) 1 d D U P B 2
H13_5 H 0.836287 -0.255982 0.455335 0.028 Uiso 0.590(11) 1 calc R . P B 2
C14_5 C 1.0240(8) -0.1830(4) 0.4696(2) 0.0226(8) Uani 0.590(11) 1 d D U P B 2
H14_5 H 1.091183 -0.224417 0.456616 0.027 Uiso 0.590(11) 1 calc R . P B 2
C15_5 C 1.0762(6) -0.1027(5) 0.4894(2) 0.0219(8) Uani 0.590(11) 1 d D U P B 2
H15_5 H 1.178480 -0.090273 0.489752 0.026 Uiso 0.590(11) 1 calc R . P B 2
C16_5 C 0.9762(6) -0.0400(4) 0.5088(3) 0.0201(8) Uani 0.590(11) 1 d D U P B 2
H16_5 H 1.011972 0.014932 0.521114 0.024 Uiso 0.590(11) 1 calc R . P B 2
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
C11 0.0142(10) 0.0169(10) 0.0197(12) -0.0015(9) -0.0004(9) 0.0018(9)
C1 0.0145(10) 0.0182(11) 0.0153(10) -0.0009(8) -0.0014(8) 0.0005(8)
C16 0.0270(13) 0.0176(11) 0.0199(12) 0.0008(9) 0.0009(10) -0.0004(9)
C2 0.0147(10) 0.0158(10) 0.0180(11) 0.0003(9) -0.0007(8) 0.0012(8)
C15 0.0270(13) 0.0255(12) 0.0195(12) -0.0013(10) 0.0034(10) -0.0011(11)
C3 0.0184(10) 0.0189(11) 0.0174(11) 0.0017(9) -0.0016(9) 0.0029(9)
C14 0.0238(12) 0.0231(12) 0.0285(13) -0.0099(11) 0.0060(10) -0.0017(10)
C13 0.0326(14) 0.0177(11) 0.0387(16) -0.0056(11) 0.0122(12) -0.0053(11)
C12 0.0267(13) 0.0197(11) 0.0268(14) -0.0017(10) 0.0111(11) -0.0021(10)
C10 0.0141(10) 0.0185(10) 0.0157(10) -0.0005(8) 0.0014(9) 0.0005(9)
C17 0.0168(11) 0.0166(10) 0.0157(10) -0.0031(8) 0.0006(9) -0.0006(9)
C18 0.0162(11) 0.0203(11) 0.0251(12) 0.0018(10) -0.0018(10) -0.0003(9)
C19 0.0269(13) 0.0200(11) 0.0302(14) 0.0040(10) -0.0019(12) -0.0013(10)
C20 0.0238(14) 0.0290(13) 0.0345(15) 0.0050(11) -0.0017(11) -0.0096(11)
C21 0.0172(12) 0.0346(14) 0.0333(15) 0.0017(12) -0.0048(11) -0.0045(11)
C22 0.0179(12) 0.0232(12) 0.0232(13) -0.0002(10) -0.0025(10) 0.0015(10)
O1 0.0208(9) 0.0224(9) 0.0282(10) -0.0106(7) -0.0070(7) 0.0011(7)
O2 0.0171(8) 0.0193(8) 0.0264(9) -0.0039(7) -0.0033(7) 0.0033(6)
C1' 0.0170(10) 0.0169(10) 0.0170(11) -0.0007(9) 0.0019(9) -0.0014(8)
C2' 0.0175(11) 0.0178(10) 0.0165(11) -0.0025(9) -0.0015(9) 0.0001(9)
C3' 0.0188(11) 0.0185(11) 0.0218(12) -0.0021(9) 0.0018(10) -0.0020(9)
C10' 0.0182(11) 0.0179(11) 0.0137(10) 0.0006(8) 0.0027(9) -0.0026(9)
C17' 0.0211(12) 0.0221(11) 0.0154(11) -0.0037(9) 0.0021(10) 0.0033(9)
C18' 0.0252(13) 0.0253(12) 0.0213(12) 0.0005(10) 0.0045(11) -0.0018(10)
C19' 0.0418(17) 0.0233(13) 0.0298(14) 0.0031(11) 0.0125(13) 0.0022(12)
C20' 0.0458(18) 0.0336(15) 0.0267(15) 0.0083(12) 0.0108(13) 0.0200(13)
C21' 0.0350(16) 0.0434(16) 0.0251(14) 0.0002(12) -0.0035(12) 0.0168(13)
C22' 0.0241(12) 0.0298(13) 0.0231(13) -0.0042(10) -0.0013(11) 0.0054(11)
O1' 0.0181(8) 0.0218(8) 0.0287(10) -0.0043(7) 0.0014(7) 0.0029(7)
O2' 0.0229(9) 0.0177(8) 0.0259(9) -0.0041(7) -0.0033(8) 0.0000(7)
Br1_1 0.03892(17) 0.03489(16) 0.03675(17) 0.00310(13) 0.01412(14) -0.01405(13)
Cl1_1 0.0255(3) 0.0240(3) 0.0197(3) 0.0053(2) -0.0059(2) -0.0033(2)
C4_1 0.0148(8) 0.0163(9) 0.0193(8) -0.0014(6) 0.0009(6) 0.0011(7)
C5_1 0.0193(8) 0.0143(8) 0.0208(8) -0.0013(7) -0.0019(6) 0.0017(7)
C6_1 0.0199(8) 0.0191(9) 0.0275(10) -0.0054(7) -0.0014(7) -0.0002(7)
C7_1 0.0232(10) 0.0200(10) 0.0317(9) -0.0045(7) 0.0019(7) -0.0012(8)
C8_1 0.0202(8) 0.0221(10) 0.0292(9) -0.0019(8) 0.0055(7) -0.0018(7)
C9_1 0.0202(8) 0.0188(9) 0.0224(9) 0.0003(7) 0.0036(7) -0.0002(7)
Br1_2 0.01910(14) 0.0566(6) 0.03583(18) -0.0040(2) -0.00460(12) -0.0018(2)
Cl1_2 0.0274(5) 0.0415(4) 0.0354(9) 0.0167(6) 0.0015(4) -0.0095(5)
C4_2 0.0193(6) 0.0163(10) 0.0175(9) -0.0029(8) 0.0014(5) 0.0017(6)
C5_2 0.0236(7) 0.0190(9) 0.0217(8) 0.0005(7) 0.0028(6) 0.0012(6)
C6_2 0.0279(8) 0.0259(12) 0.0245(10) 0.0013(8) 0.0006(9) 0.0058(9)
C7_2 0.0276(8) 0.0303(14) 0.0241(10) -0.0004(9) -0.0002(8) 0.0054(9)
C8_2 0.0228(8) 0.0263(15) 0.0207(9) -0.0043(10) -0.0007(7) 0.0059(7)
C9_2 0.0193(6) 0.0179(17) 0.0194(11) -0.0041(12) 0.0010(6) 0.0013(7)
Br1_3 0.01910(14) 0.0566(6) 0.03583(18) -0.0040(2) -0.00460(12) -0.0018(2)
Cl1_3 0.0274(5) 0.0415(4) 0.0354(9) 0.0167(6) 0.0015(4) -0.0095(5)
C4_3 0.0193(6) 0.0163(10) 0.0175(9) -0.0029(8) 0.0014(5) 0.0017(6)
C5_3 0.0236(7) 0.0190(9) 0.0217(8) 0.0005(7) 0.0028(6) 0.0012(6)
C6_3 0.0279(8) 0.0259(12) 0.0245(10) 0.0013(8) 0.0006(9) 0.0058(9)
C7_3 0.0276(8) 0.0303(14) 0.0241(10) -0.0004(9) -0.0002(8) 0.0054(9)
C8_3 0.0228(8) 0.0263(15) 0.0207(9) -0.0043(10) -0.0007(7) 0.0059(7)
C9_3 0.0193(6) 0.0179(17) 0.0194(11) -0.0041(12) 0.0010(6) 0.0013(7)
C11_4 0.0215(8) 0.0196(9) 0.0174(9) 0.0020(8) 0.0007(7) 0.0012(8)
C12_4 0.0218(12) 0.0185(8) 0.020(2) 0.0027(11) -0.0032(15) 0.0029(11)
C13_4 0.0224(15) 0.0187(10) 0.029(2) -0.0003(11) -0.0007(16) 0.0016(13)
C14_4 0.0224(14) 0.0206(15) 0.0248(18) 0.0022(11) -0.0014(15) 0.0013(12)
C15_4 0.0214(11) 0.0217(18) 0.0226(13) 0.0016(16) 0.0022(11) -0.0002(12)
C16_4 0.0216(8) 0.0217(16) 0.0170(16) 0.0024(18) 0.0005(7) 0.0006(10)
C11_5 0.0215(8) 0.0196(9) 0.0174(9) 0.0020(8) 0.0007(7) 0.0012(8)
C12_5 0.0218(12) 0.0185(8) 0.020(2) 0.0027(11) -0.0032(15) 0.0029(11)
C13_5 0.0224(15) 0.0187(10) 0.029(2) -0.0003(11) -0.0007(16) 0.0016(13)
C14_5 0.0224(14) 0.0206(15) 0.0248(18) 0.0022(11) -0.0014(15) 0.0013(12)
C15_5 0.0214(11) 0.0217(18) 0.0226(13) 0.0016(16) 0.0022(11) -0.0002(12)
C16_5 0.0216(8) 0.0217(16) 0.0170(16) 0.0024(18) 0.0005(7) 0.0006(10)
_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
C11 C16 1.396(4) . ?
C11 C2 1.515(3) . ?
C11 C12 1.390(3) . ?
C1 C2 1.563(3) . ?
C1 C3 1.523(3) . ?
C1 C10 1.497(3) . ?
C1 C4_1 1.506(3) . ?
C16 C15 1.393(4) . ?
C2 C3 1.505(3) . ?
C2 C17 1.503(3) . ?
C15 C14 1.383(4) . ?
C14 C13 1.383(4) . ?
C13 C12 1.392(4) . ?
C10 O1 1.287(3) . ?
C10 O2 1.247(3) . ?
C17 C18 1.396(3) . ?
C17 C22 1.389(4) . ?
C18 C19 1.387(4) . ?
C19 C20 1.386(4) . ?
C20 C21 1.387(4) . ?
C21 C22 1.390(4) . ?
C1' C2' 1.573(3) . ?
C1' C3' 1.507(3) . ?
C1' C10' 1.504(3) . ?
C1' C4_2 1.503(3) . ?
C1' C4_3 1.503(3) . ?
C2' C3' 1.499(3) . ?
C2' C17' 1.511(3) . ?
C2' C11_4 1.505(4) . ?
C2' C11_5 1.505(3) . ?
C10' O1' 1.238(3) . ?
C10' O2' 1.296(3) . ?
C17' C18' 1.394(4) . ?
C17' C22' 1.387(4) . ?
C18' C19' 1.394(4) . ?
C19' C20' 1.382(5) . ?
C20' C21' 1.378(5) . ?
C21' C22' 1.393(4) . ?
Br1_1 C8_1 1.901(2) . ?
Cl1_1 C5_1 1.737(2) . ?
C4_1 C5_1 1.393(3) . ?
C4_1 C9_1 1.397(3) . ?
C5_1 C6_1 1.388(3) . ?
C6_1 C7_1 1.390(3) . ?
C7_1 C8_1 1.384(3) . ?
C8_1 C9_1 1.383(3) . ?
Br1_2 C8_2 1.895(2) . ?
Cl1_2 C5_2 1.739(2) . ?
C4_2 C5_2 1.394(3) . ?
C4_2 C9_2 1.397(3) . ?
C5_2 C6_2 1.390(3) . ?
C6_2 C7_2 1.390(3) . ?
C7_2 C8_2 1.382(3) . ?
C8_2 C9_2 1.384(3) . ?
Br1_3 C8_3 1.898(3) . ?
Cl1_3 C5_3 1.738(3) . ?
C4_3 C5_3 1.394(3) . ?
C4_3 C9_3 1.397(3) . ?
C5_3 C6_3 1.390(3) . ?
C6_3 C7_3 1.391(4) . ?
C7_3 C8_3 1.383(4) . ?
C8_3 C9_3 1.385(3) . ?
C11_4 C12_4 1.398(4) . ?
C11_4 C16_4 1.400(4) . ?
C12_4 C13_4 1.392(5) . ?
C13_4 C14_4 1.388(6) . ?
C14_4 C15_4 1.380(6) . ?
C15_4 C16_4 1.393(5) . ?
C11_5 C12_5 1.399(4) . ?
C11_5 C16_5 1.401(4) . ?
C12_5 C13_5 1.391(4) . ?
C13_5 C14_5 1.387(6) . ?
C14_5 C15_5 1.380(6) . ?
C15_5 C16_5 1.394(5) . ?
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
C16 C11 C2 119.5(2) . . ?
C12 C11 C16 117.9(2) . . ?
C12 C11 C2 122.5(2) . . ?
C3 C1 C2 58.37(15) . . ?
C10 C1 C2 117.0(2) . . ?
C10 C1 C3 114.2(2) . . ?
C10 C1 C4_1 112.99(19) . . ?
C4_1 C1 C2 121.91(19) . . ?
C4_1 C1 C3 122.0(2) . . ?
C15 C16 C11 121.2(2) . . ?
C11 C2 C1 118.7(2) . . ?
C3 C2 C11 117.5(2) . . ?
C3 C2 C1 59.49(15) . . ?
C17 C2 C11 113.3(2) . . ?
C17 C2 C1 118.34(19) . . ?
C17 C2 C3 119.5(2) . . ?
C14 C15 C16 120.2(2) . . ?
C2 C3 C1 62.14(16) . . ?
C15 C14 C13 119.2(2) . . ?
C14 C13 C12 120.7(3) . . ?
C11 C12 C13 120.8(3) . . ?
O1 C10 C1 116.5(2) . . ?
O2 C10 C1 120.0(2) . . ?
O2 C10 O1 123.5(2) . . ?
C18 C17 C2 122.0(2) . . ?
C22 C17 C2 119.3(2) . . ?
C22 C17 C18 118.5(2) . . ?
C19 C18 C17 121.0(2) . . ?
C20 C19 C18 119.9(3) . . ?
C19 C20 C21 119.7(3) . . ?
C20 C21 C22 120.2(3) . . ?
C17 C22 C21 120.7(2) . . ?
C3' C1' C2' 58.21(16) . . ?
C10' C1' C2' 113.0(2) . . ?
C10' C1' C3' 116.2(2) . . ?
C10' C1' C4_2 113.2(3) . . ?
C4_2 C1' C2' 122.1(3) . . ?
C4_2 C1' C3' 123.3(2) . . ?
C4_3 C1' C2' 119.1(15) . . ?
C4_3 C1' C3' 117.8(11) . . ?
C4_3 C1' C10' 118.5(15) . . ?
C3' C2' C1' 58.72(15) . . ?
C3' C2' C17' 118.2(2) . . ?
C3' C2' C11_4 121.0(6) . . ?
C3' C2' C11_5 115.9(4) . . ?
C17' C2' C1' 118.9(2) . . ?
C11_4 C2' C1' 118.8(8) . . ?
C11_4 C2' C17' 111.9(8) . . ?
C11_5 C2' C1' 118.7(6) . . ?
C11_5 C2' C17' 115.0(6) . . ?
C2' C3' C1' 63.07(16) . . ?
O1' C10' C1' 121.3(2) . . ?
O1' C10' O2' 124.0(2) . . ?
O2' C10' C1' 114.7(2) . . ?
C18' C17' C2' 121.5(2) . . ?
C22' C17' C2' 119.3(2) . . ?
C22' C17' C18' 119.1(3) . . ?
C19' C18' C17' 120.1(3) . . ?
C20' C19' C18' 120.0(3) . . ?
C21' C20' C19' 120.2(3) . . ?
C20' C21' C22' 119.9(3) . . ?
C17' C22' C21' 120.6(3) . . ?
C5_1 C4_1 C1 123.97(19) . . ?
C5_1 C4_1 C9_1 117.01(19) . . ?
C9_1 C4_1 C1 118.87(19) . . ?
C4_1 C5_1 Cl1_1 120.80(16) . . ?
C6_1 C5_1 Cl1_1 117.05(16) . . ?
C6_1 C5_1 C4_1 122.15(19) . . ?
C5_1 C6_1 C7_1 120.1(2) . . ?
C8_1 C7_1 C6_1 118.2(2) . . ?
C7_1 C8_1 Br1_1 119.97(17) . . ?
C9_1 C8_1 Br1_1 118.35(18) . . ?
C9_1 C8_1 C7_1 121.7(2) . . ?
C8_1 C9_1 C4_1 120.9(2) . . ?
C5_2 C4_2 C1' 124.6(2) . . ?
C5_2 C4_2 C9_2 116.7(2) . . ?
C9_2 C4_2 C1' 118.5(2) . . ?
C4_2 C5_2 Cl1_2 121.13(18) . . ?
C6_2 C5_2 Cl1_2 116.56(18) . . ?
C6_2 C5_2 C4_2 122.3(2) . . ?
C7_2 C6_2 C5_2 120.2(2) . . ?
C8_2 C7_2 C6_2 117.9(2) . . ?
C7_2 C8_2 Br1_2 120.64(18) . . ?
C7_2 C8_2 C9_2 121.9(2) . . ?
C9_2 C8_2 Br1_2 117.43(19) . . ?
C8_2 C9_2 C4_2 121.0(2) . . ?
C5_3 C4_3 C1' 123.0(7) . . ?
C5_3 C4_3 C9_3 116.9(3) . . ?
C9_3 C4_3 C1' 119.7(5) . . ?
C4_3 C5_3 Cl1_3 121.0(3) . . ?
C6_3 C5_3 Cl1_3 117.0(3) . . ?
C6_3 C5_3 C4_3 121.9(4) . . ?
C5_3 C6_3 C7_3 120.1(4) . . ?
C8_3 C7_3 C6_3 118.0(3) . . ?
C7_3 C8_3 Br1_3 120.6(3) . . ?
C7_3 C8_3 C9_3 121.5(4) . . ?
C9_3 C8_3 Br1_3 117.6(3) . . ?
C8_3 C9_3 C4_3 120.9(3) . . ?
C12_4 C11_4 C2' 120.4(5) . . ?
C12_4 C11_4 C16_4 118.3(3) . . ?
C16_4 C11_4 C2' 121.3(5) . . ?
C13_4 C12_4 C11_4 121.2(4) . . ?
C14_4 C13_4 C12_4 119.2(4) . . ?
C15_4 C14_4 C13_4 120.4(4) . . ?
C14_4 C15_4 C16_4 120.2(4) . . ?
C15_4 C16_4 C11_4 120.4(4) . . ?
C12_5 C11_5 C2' 119.0(4) . . ?
C12_5 C11_5 C16_5 118.0(3) . . ?
C16_5 C11_5 C2' 122.8(4) . . ?
C13_5 C12_5 C11_5 121.4(3) . . ?
C14_5 C13_5 C12_5 119.5(4) . . ?
C15_5 C14_5 C13_5 120.3(3) . . ?
C14_5 C15_5 C16_5 120.3(4) . . ?
C15_5 C16_5 C11_5 120.5(3) . . ?
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
0 0 -2 147.29 5.65
0 0 -3 0.51 0.42
0 0 -4 6243.02 201.84
0 0 -5 0.72 0.59
0 0 -6 2182.69 72.94
0 0 -7 1.02 0.78
0 0 -8 4952.28 162.78
0 0 -9 2.42 1.27
0 0 -9 2.47 1.51
0 0 -10 42.04 4.21
0 0 -10 48.79 5.51
0 0 -11 3.64 2.13
0 0 -12 716.51 31.79
0 0 -13 -0.64 1.65
0 0 -14 2061.04 77.84
0 0 -15 0.77 2.43
0 0 -16 1.67 2.33
0 0 -17 8.17 3.84
0 0 -18 3178.19 118.68
0 0 -19 -1.06 2.73
0 0 -20 4.53 3.59
0 0 -21 8.48 4.62
0 0 -22 880.28 46.37
0 0 -23 -1.35 4.03
0 0 23 2.63 4.16
0 0 -24 83.27 12.88
0 0 24 74.3 12.15
0 0 -25 -1.46 5.1
0 0 25 5.71 5
0 0 26 14.54 7.04
0 0 27 1.46 4.08
0 0 28 11.54 5.92
0 0 28 18.73 3.59
0 0 29 2 3.14
0 0 30 9.13 2.95
0 0 31 6.31 2.76
0 0 32 495.99 19.39
0 0 33 5.38 2.41
0 0 34 906.51 31.91
0 0 35 3.99 1.87
0 0 36 524.05 18.74
0 0 37 0.67 1.02
0 1 0 0.43 0.23
0 1 -1 70.84 2.95
0 -1 -1 75.6 2.98
0 1 -1 66.27 2.99
0 1 -2 212.93 8.21
0 -1 -2 216.09 8.22
0 -1 -2 209.15 7.88
0 -1 -3 137.26 6.47
0 -1 -3 153.86 6.85
0 1 -3 140.84 6.5
0 1 -4 1378.8 45.59
0 -1 -4 1262.41 45.35
0 -1 -4 1344.73 45.52
0 -1 -5 154.21 8.23
0 1 -5 179.8 8.65
0 -1 -5 169.27 8.26
0 -1 -6 4665.9 155.22
0 -1 -6 4644.59 154.62
0 1 -6 4807.13 155.33
0 1 -7 187.32 10.27
0 -1 -7 192.3 9.82
0 -1 -8 1077.09 40.22
0 1 -8 1137.34 41.58
0 1 -9 1298.58 47.66
0 -1 -9 1237.28 45.97
0 1 -10 661.74 28.1
0 -1 -10 626.74 26.31
0 -1 -11 999.04 40.39
0 1 -11 1168.94 43.44
0 1 -12 1365.66 50.27
0 -1 -12 1165.62 46.77
0 -1 -13 1077.29 44.14
0 1 -13 1248.01 47.9
0 1 -14 123.91 11
0 1 -15 9.2 3.63
0 1 -16 1039.53 46.17
0 1 -17 1517.45 63.15
0 1 -18 403.15 25.7
0 1 -19 337.68 23.26
0 1 -20 19.23 5.88
0 1 -21 42.29 8.18
0 1 -22 92.32 12.86
0 -1 22 76.99 5.09
0 -1 22 73.84 11.44
0 -1 23 166.55 17.73
0 1 23 166.42 17.41
0 1 -23 184.93 18.42
0 -1 23 190.93 9.08
0 -1 24 1279.4 58.59
0 1 -24 1210.11 58.05
0 1 24 1130.44 55.88
0 -1 24 1108.37 39.79
0 -1 -24 1106.99 56.46
0 1 25 169.39 18.36
0 -1 25 172.31 8.73
0 -1 25 175.97 18.84
0 -1 -25 159.69 18.05
0 1 -25 171.23 18.55
0 -1 26 1218.03 41.17
0 1 26 1204.4 57.91
0 -1 26 1091.21 39.94
0 1 27 126.09 15.79
0 -1 27 110.69 7.34
0 -1 27 114.52 15.22
0 -1 27 107.27 6.49
0 -1 28 67.51 11.99
0 -1 28 92.47 6.55
0 1 28 65.63 11.63
0 -1 29 590.48 23.11
0 -1 30 61.67 5.39
0 1 30 73.03 5.64
0 -1 31 174.36 8.92
0 1 31 157.46 8.75
0 1 32 25.94 3.43
0 -1 32 27.34 3.52
0 1 33 22.29 3.18
0 -1 33 20.5 3.06
0 1 34 202.62 9.11
0 -1 34 197.36 9.05
0 1 35 13.09 2.17
0 -1 35 16.48 2.23
0 -1 36 42.14 2.99
0 1 36 40.94 2.92
0 -1 37 3.48 1.15
0 1 37 1.64 1.08
0 -2 0 4306.41 139.26
0 2 0 4367.47 140.01
0 -2 1 173.45 6.97
0 2 -1 181.33 7.07
0 2 -2 1162.74 38.63
0 -2 -2 1149.57 38.31
0 -2 -2 1133.42 39.42
0 2 -2 1154.98 38.36
0 -2 -3 619.85 22.09
0 -2 -3 582.3 22.14
0 2 -3 662.69 22.19
0 -2 -4 1707.91 57.55
0 -2 -4 1687.9 56.83
0 2 -4 1718.38 57.53
0 -2 -5 4361.12 143.17
0 2 -5 4539.3 144.99
0 -2 -5 4357.83 144.86
0 -2 -6 4129.17 128.54
0 2 -6 3683.1 130.49
0 -2 -6 3846.51 130.76
0 -2 -7 2740.85 92.04
0 -2 -7 2796.85 91.78
0 -2 -7 2630.53 88.29
0 2 -7 2689.91 91.53
0 -2 -8 7535.26 251.92
0 2 -8 7786.85 252.08
0 -2 -8 8297.15 252.58
0 -2 -8 7490.91 247.75
0 2 -9 3040.52 103.73
0 -2 -9 2943.49 98.61
0 -2 -9 3106.73 103.86
0 -2 -9 3132.35 103.64
0 -2 -10 3323.08 111.56
0 2 -10 3295.3 111.84
0 -2 -10 3140.68 105.73
0 -2 -10 3498.64 112.38
0 -2 -11 2209.94 83.52
0 -2 -11 2189.84 82.77
0 2 -11 2488.63 84.48
0 -2 -11 2381.98 77.1
0 -2 -12 338.03 17.34
0 -2 -12 313.59 17.53
0 2 -12 347.96 18.09
0 -2 -12 288.69 11.33
0 2 -13 312.25 17.15
0 -2 -13 276.98 16.33
0 -2 -13 291.09 15.94
0 2 -14 69.73 8.11
0 -2 -14 57.19 7.46
0 -2 -14 77.47 7.96
0 -2 -15 887.88 38.76
0 2 -15 833.13 38.03
0 -2 -15 763.85 35.78
0 2 -16 1445.18 58.71
0 -2 -16 1369.91 58.17
0 -2 -17 234.09 17.7
0 2 -17 215.02 16.89
0 2 -18 55.94 8.78
0 -2 -18 43.93 7.94
0 -2 -19 9.46 4.44
0 2 -19 5.19 4.25
0 2 -20 438.4 28.52
0 -2 -20 482.44 29.4
0 -2 -21 571.5 33.4
0 -2 21 519.65 20.01
0 2 -21 520.97 32.03
0 -2 -22 19.07 6.6
0 2 -22 22.66 6.93
0 -2 22 18.18 2.79
0 -2 22 14.27 6.3
0 2 -23 234.41 20.66
0 -2 23 229.64 10.52
0 -2 -23 211.03 19.79
0 -2 23 194.27 9.81
0 2 23 223.89 19.54
0 -2 23 212.67 20.05
0 -2 24 239.46 11.26
0 2 24 250.44 21.54
0 -2 -24 233.62 21.53
0 -2 24 258.48 11.78
0 2 -24 262.36 22.46
0 -2 24 246.66 22.15
0 -2 25 158.29 17.69
0 -2 25 157.53 8.33
0 -2 25 170.41 9.12
0 -2 26 58.47 4.82
0 2 26 48.7 10.17
0 -2 26 49.15 10.6
0 -2 26 66.54 5.6
0 2 27 686.84 39.29
0 -2 27 681.96 40.61
0 -2 27 683.68 25.58
0 -2 27 622.22 24.46
0 -2 28 101.49 6.33
0 -2 28 90.98 14
0 -2 28 112.79 7.13
0 -2 29 19.05 3.4
0 -2 29 14.63 2.82
0 -2 30 265.29 12.27
0 -2 31 74.58 5.56
0 2 31 73.16 5.6
0 -2 32 271.42 11.92
0 2 32 266.04 12
0 2 33 18.3 2.92
0 -2 33 20.74 2.99
0 2 34 5.07 2.11
0 -2 34 2.97 1.88
0 -2 35 67.65 4.2
0 2 35 72.52 4.31
0 -2 36 10.37 1.69
0 2 36 11.29 1.75
0 -2 37 32.77 2.22
0 2 37 31.3 2.16
0 -3 0 2.05 0.49
0 3 0 -0.13 0.48
0 3 -1 252.58 10.37
0 -3 1 268.34 10
0 3 1 265.97 10.72
0 -3 2 7466.57 240.25
0 3 -2 7527.63 240.19
0 -3 -2 7249.93 238.94
0 3 -2 7549.82 239.04
0 3 -3 963.63 32.18
0 3 -3 927.42 32.6
0 -3 3 954.48 33.18
0 -3 -3 924.67 32.09
0 -3 -3 914.22 33.78
0 3 -4 4533.88 146.51
0 -3 -4 4373.91 147.31
0 -3 -4 4521.27 146.49
0 -3 -5 2637.85 90.02
0 3 -5 2735.64 90.16
0 -3 -5 2723.27 90.16
0 -3 -6 176.61 10.57
0 -3 -6 192.49 9.6
0 3 -6 167.09 9.16
0 -3 -6 183.63 8.81
0 3 -7 1019.67 38.3
0 -3 -7 1033.42 39.99
0 -3 -7 1046.3 38.52
0 -3 -7 1050.98 36.73
0 3 -8 347.71 16.76
0 -3 -8 374.39 17.15
0 -3 -8 370.67 14.89
0 -3 -8 374.88 18.28
0 -3 -9 48.85 5.16
0 -3 -9 42.6 5.23
0 3 -9 45.87 4.96
0 -3 -9 45.28 3.5
0 -3 -10 25.64 2.5
0 -3 -10 33.31 4.56
0 3 -10 20.71 3.85
0 -3 -10 21.59 3.99
0 -3 -11 32.69 2.76
0 -3 -11 32.21 4.7
0 -3 -11 32.35 4.97
0 3 -11 37.26 5.07
0 3 -12 53.16 6.4
0 -3 -12 55.19 6.53
0 -3 -12 64.6 7.13
0 -3 -13 1060.62 44.54
0 -3 -13 1077.72 44.7
0 3 -13 1081.8 44.69
0 3 -14 84.23 8.81
0 -3 -14 83.71 8.81
0 -3 -14 83.04 8.9
0 -3 -15 1358.32 56.52
0 3 -15 1362.05 56.34
0 -3 -15 1452.33 57.33
0 3 -16 3039.67 113.74
0 -3 -16 3199.39 113.92
0 -3 -16 3116.22 114.18
0 3 -17 36.78 6.71
0 -3 -17 41.19 7.24
0 -3 -18 268.02 19.87
0 3 -18 283.6 19.98
0 3 -19 1562.89 65.95
0 -3 -19 1530.54 65.98
0 -3 20 843.78 31.04
0 -3 -20 855.11 43.72
0 -3 20 902.52 31.55
0 -3 20 824.23 43.56
0 3 -20 904.18 43.95
0 -3 21 84.63 12.13
0 -3 21 108.81 6.31
0 -3 21 109.59 6.28
0 -3 -21 97.3 5.93
0 -3 -21 90.14 12.19
0 3 -21 98.48 12.6
0 -3 22 391.85 16.1
0 3 22 405.9 26.74
0 -3 22 362.53 27.05
0 3 -22 422.42 27.92
0 -3 -22 371.53 15.8
0 -3 22 428.98 16.59
0 -3 -22 367.16 26.7
0 -3 23 330.53 14.06
0 -3 23 308.79 13.68
0 3 23 335.44 24.05
0 3 -23 288.81 23.73
0 -3 -23 312.4 13.53
0 -3 -23 326.8 25.25
0 3 24 1508.24 66.44
0 -3 24 1430.9 50.92
0 -3 24 1501.2 51.4
0 -3 25 102.16 6.98
0 -3 25 103.02 6.57
0 3 25 99.6 13.24
0 -3 26 109.02 7.27
0 3 26 119.44 14.38
0 -3 26 111.52 6.93
0 3 27 7.55 4.6
0 -3 27 6.5 2.54
0 -3 27 4.3 3.03
0 -3 28 7.45 3.01
0 -3 28 1.72 2.14
0 -3 29 1.8 2.19
0 -3 29 3.36 2.77
0 -3 30 67.34 5.42
0 -3 31 9.75 3.01
0 3 32 75.47 5.3
0 -3 32 76.72 5.27
0 3 33 4.42 2.38
0 -3 33 4.48 2.26
0 3 34 480.28 17.74
0 -3 34 458.25 17.63
0 3 35 8.15 1.89
0 -3 35 7.16 1.73
0 3 36 18.38 1.94
0 -3 36 16.15 1.94
0 3 37 145.37 5.77
0 -3 37 145.18 5.82
0 -4 0 464.87 16.35
0 4 0 490.84 18.1
0 -4 1 461.51 16.65
0 4 1 469.22 17.93
0 4 -1 462.76 17.66
0 -4 2 0.72 0.61
0 4 -2 3.63 1.1
0 -4 3 701.4 26.1
0 4 -3 697.29 25.94
0 4 -3 732 24.68
0 4 -4 29.68 2.46
0 -4 4 29.51 3.07
0 -4 -4 32.13 4.04
0 -4 5 3818.53 124.67
0 -4 -5 3530.4 126.31
0 4 -5 3771.21 123.08
0 -4 -5 3742.12 123.08
0 -4 -6 1637.49 56.81
0 4 -6 1637.48 56.82
0 -4 -7 316.87 15.14
0 4 -7 362.17 15.6
0 -4 -8 281.09 14.07
0 4 -8 294.75 14.3
0 -4 -8 272.02 15.74
0 4 -9 38.58 4.51
0 -4 -9 36.23 5.31
0 -4 -9 35.6 4.4
0 -4 -10 326.75 16.77
0 -4 -10 326.82 18.39
0 4 -10 309.12 16.4
0 4 -11 916.36 38.04
0 -4 -11 946.68 38.4
0 -4 -11 961.45 40.47
0 -4 -12 2171.78 79.64
0 -4 -12 2080.92 77.18
0 4 -12 2099.27 77.06
0 -4 -13 2616.74 93.71
0 -4 -13 2565.72 95.39
0 4 -13 2573.3 93.28
0 -4 -14 481.79 25.46
0 -4 -14 506.44 27.12
0 4 -14 505.4 25.61
0 -4 -15 783.48 36.65
0 -4 -15 806.88 38.11
0 4 -15 783.3 36.41
0 -4 -16 4.88 3.1
0 4 -16 1.58 2.36
0 -4 -16 7.3 3.47
0 4 -17 39.41 6.76
0 -4 17 26.16 6.11
0 -4 -17 22.1 5.51
0 -4 -17 25.15 6.27
0 -4 18 1049.43 49.61
0 4 -18 1101.32 48.82
0 -4 -18 1056.96 48.87
0 -4 -19 5.13 3.6
0 -4 19 5.73 1.97
0 -4 19 9.32 1.89
0 4 -19 4.96 3.78
0 -4 19 4.47 3.74
0 -4 20 20.75 2.59
0 -4 -20 16.22 2.58
0 -4 -20 24.06 6.45
0 -4 20 18.9 2.85
0 -4 20 16.69 5.93
0 4 -20 14.82 5.15
0 4 21 594.93 32.5
0 -4 -21 611.34 34.7
0 -4 21 606.52 22.62
0 -4 21 568.85 34.75
0 4 -21 565.96 33.4
0 -4 21 582.31 22.4
0 -4 -21 567.54 22.24
0 -4 22 37.81 3.94
0 -4 -22 32.88 3.59
0 4 -22 46.09 8.82
0 -4 22 46.43 3.96
0 4 22 39.64 7.68
0 -4 22 33.12 8.13
0 -4 -22 36.58 7.82
0 4 23 144.38 15.28
0 -4 23 157.17 17.06
0 -4 23 139.99 8.17
0 -4 -23 157.27 8.32
0 -4 23 170 8.67
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10 0 7 586.89 20.7
10 0 8 120.97 6.15
10 0 8 97.69 4.93
10 0 9 107.05 5.83
10 0 9 107.03 4.98
10 0 10 2.31 1.74
10 0 10 1.79 1.07
10 0 -11 323.97 12.23
10 0 11 367.84 13.58
10 0 11 345.33 12.3
10 0 -12 17.21 1.67
10 0 12 20.03 2.28
10 0 12 14.54 1.38
10 0 -13 22.83 1.79
10 0 -14 45.57 2.55
10 0 -15 28.01 1.83
10 1 -14 58.69 2.81
10 1 -13 209.36 7.77
10 -1 12 92.97 4.89
10 -1 12 85.4 4.07
10 -1 11 15.79 2.15
10 -1 11 20.32 1.89
10 -1 10 103.55 5.69
10 -1 10 114.5 5.13
10 -1 9 33.78 2.56
10 -1 8 46.65 3.16
10 -1 7 55.05 3.53
10 -1 6 400.19 14.98
10 -1 5 276.28 11.06
10 -1 4 24.1 2.49
10 -1 3 214.87 9.17
10 -1 2 31.69 2.91
10 -1 1 34.06 2.84
10 1 -1 28.43 2.49
10 1 0 21.44 2.22
10 -1 0 15.91 2.24
10 1 1 23.81 2.3
10 -1 -1 25.07 2.57
10 1 2 -0.56 1.12
10 1 2 44.26 2.86
10 1 3 186.95 6.63
10 1 3 201.05 5.45
10 1 4 30.73 3.12
10 1 4 26.65 2.26
10 1 5 276.34 9.48
10 1 5 272.78 8.01
10 1 6 374.68 14.84
10 1 6 368.23 13.65
10 1 7 49.5 3.87
10 1 7 53.89 3.16
10 1 8 65.04 4.33
10 1 8 61.4 3.33
10 -1 -9 20.3 1.96
10 1 9 25.58 2.77
10 1 9 24.91 1.87
10 -1 -10 108.82 4.88
10 1 10 100.05 4.49
10 -1 -11 21.28 1.93
10 1 11 30.68 2.74
10 -1 -12 92.17 4.31
10 1 12 91.43 4.91
10 -1 -13 233.78 8.86
10 -1 -14 75.67 3.63
10 -1 -15 20.61 1.63
10 -2 12 108.19 4.86
10 -2 11 15.86 2.03
10 -2 11 19.47 1.88
10 -2 10 292.09 11.83
10 -2 10 301.87 11.34
10 -2 9 21.59 2.48
10 -2 9 21.25 2.12
10 -2 8 107.27 5.8
10 -2 8 110.5 5.39
10 -2 7 7.21 1.87
10 -2 7 10.38 1.81
10 -2 6 153.61 5.66
10 -2 6 176.49 5.3
10 -2 5 86.1 4.39
10 -2 5 85.84 3.91
10 -2 4 73.24 4.12
10 -2 4 64.25 3.48
10 2 -3 118.99 6.14
10 -2 3 192.74 7.38
10 2 -2 280.46 11.04
10 -2 2 288.65 11.51
10 2 -1 218.38 9.2
10 -2 1 238.17 9.73
10 2 -1 224.13 9.19
10 2 0 94.31 4.79
10 -2 0 92.86 5.13
10 2 0 80.06 4.48
10 2 1 212.41 9.21
10 2 1 231.54 9.14
10 -2 -1 236.53 9.74
10 2 2 290.8 11.29
10 2 2 275.4 10.9
10 -2 -2 293.17 11.67
10 2 3 155.98 7.18
10 2 3 168.28 6.94
10 2 4 67.63 3.94
10 2 4 65.56 4.44
10 2 4 57.19 3.38
10 2 5 95.88 5.01
10 2 5 102.66 5.6
10 2 5 89.81 4.42
10 2 6 145.39 6.68
10 2 6 155.77 7.37
10 2 6 146.44 6.1
10 2 7 5.5 1.83
10 -2 -8 108.14 5.09
10 2 8 123.06 6.07
10 -2 -9 16.78 1.87
10 2 9 15.51 2.25
10 -2 -10 292.23 11.13
10 2 10 310.9 11.96
10 -2 -11 13.97 1.67
10 2 11 13.59 1.97
10 -2 -12 96.83 4.51
10 -2 -13 104.09 4.68
10 -2 -14 147.61 6
10 -2 -15 75.92 3.52
10 -3 12 89.9 4.25
10 -3 11 92.83 4.49
10 -3 10 22.71 2.34
10 -3 10 21.59 2.08
10 -3 9 99.73 5.36
10 -3 9 116.28 5.32
10 -3 8 39.24 2.79
10 -3 8 40.22 2.65
10 3 -7 17.13 1.93
10 -3 7 20.15 2.31
10 3 -6 230.09 9.28
10 -3 6 221.84 9.86
10 -3 6 252.43 9.76
10 3 -5 108.1 5.28
10 -3 5 98.7 5.65
10 3 -4 52.85 3.5
10 -3 4 56.8 3.74
10 3 -3 22.15 2.38
10 -3 3 20.81 2.41
10 3 -2 258.37 10.35
10 -3 2 272.74 10.66
10 3 -2 246.06 9.84
10 3 -1 42.48 3.23
10 -3 1 44.68 3.35
10 3 -1 41.57 2.77
10 3 0 2.66 1.57
10 -3 0 4.02 1.59
10 3 0 3.83 1.15
10 3 1 45.9 3.34
10 3 1 45.76 2.76
10 -3 -1 46.16 3.45
10 3 2 271.3 10.74
10 3 2 249.91 9.84
10 -3 -2 285.06 10.96
10 3 3 18.08 2.35
10 -3 -3 17.49 2.36
10 3 4 57.73 3.79
10 3 5 100.65 5.24
10 3 6 216.34 9.01
10 3 6 212.96 9.22
10 -3 -7 20.39 1.99
10 3 7 25.74 2.5
10 3 7 24.87 2.51
10 -3 -8 37.26 2.65
10 3 8 43.99 3.25
10 -3 -9 98.71 4.67
10 3 9 101.42 5.14
10 -3 -10 26.11 2.16
10 -3 -11 85.08 4.14
10 -3 -12 85.47 4.09
10 -3 -13 147.91 6.08
10 -3 -14 113.2 4.81
10 -3 -15 30.72 1.93
10 -4 15 43.08 2.3
10 -4 12 5.57 1.13
10 -4 11 120.66 5.33
10 -4 10 157 6.65
10 4 -9 14.77 1.7
10 -4 9 15.5 1.84
10 4 -8 22.02 2.02
10 -4 8 20.71 2.08
10 4 -7 52.94 3.29
10 -4 7 51.08 3.33
10 4 -6 234.64 9.47
10 -4 6 241.05 9.66
10 4 -5 58.56 3.67
10 -4 5 65.11 3.84
10 4 -4 145.98 6.45
10 -4 4 150.42 6.57
10 4 -3 80.4 4.61
10 -4 3 91.32 4.79
10 4 -2 128.79 6.2
10 -4 2 131.46 6.28
10 4 -1 5.19 1.7
10 4 0 82.16 4.67
10 4 1 2.17 1.54
10 4 2 124.17 6.12
10 4 3 82.08 4.66
10 4 4 159.91 7.26
10 -4 -4 160.16 7.16
10 4 5 63.8 3.87
10 -4 -5 54.58 3.58
10 4 6 246.58 9.61
10 -4 -6 239.93 9.38
10 -4 -7 51.85 3.14
10 4 7 58.8 3.67
10 -4 -8 26.64 2.17
10 4 8 27.73 2.47
10 -4 -8 26.64 2.27
10 -4 -9 14.28 1.71
10 -4 -9 11.74 1.59
10 -4 -10 151.96 6.29
10 -4 -10 147.88 6.32
10 -4 -11 97.24 4.59
10 -4 -11 106.45 4.67
10 -4 -12 6.56 1.12
10 -4 -12 6.35 1.23
10 -4 -13 72.04 3.51
10 -4 -13 76.16 3.42
10 -4 -14 128.1 4.98
10 -4 -14 114.96 4.69
10 -5 13 32.95 1.97
10 -5 12 188.13 7.2
10 -5 11 56.28 2.86
10 -5 11 58.81 2.99
10 5 -10 145.46 6.29
10 -5 10 161.19 6.49
10 5 -9 27.47 2.14
10 -5 9 30.44 2.11
10 -5 9 31.16 2.29
10 5 -8 204.98 8.41
10 -5 8 227.24 8.65
10 5 -7 5.06 1.38
10 -5 7 4.03 1.1
10 -5 7 6.44 1.41
10 5 -6 192.51 7.61
10 -5 6 169.75 7
10 -5 6 177.21 7.49
10 5 -5 55.58 3.52
10 5 -4 43.49 3.1
10 5 -3 64.24 3.88
10 5 -2 28.56 2.6
10 5 -1 51.1 3.49
10 -5 1 57.63 3.5
10 5 0 34.49 2.88
10 -5 0 38.41 2.81
10 5 1 60.28 3.86
10 -5 -1 64.37 3.71
10 5 2 28.88 2.64
10 -5 -2 20.08 2.15
10 5 3 46.35 3.38
10 -5 -3 52.72 3.26
10 5 4 42.29 3.15
10 -5 -4 44.53 2.94
10 5 5 51.25 3.35
10 -5 -5 43.81 2.94
10 5 6 180.7 7.55
10 -5 -6 177.91 7.18
10 -5 -6 162.08 6.8
10 5 7 8.29 1.64
10 -5 -7 7.13 1.31
10 -5 -7 7.24 1.34
10 5 8 174.63 7.55
10 -5 -8 169.76 7.05
10 -5 -9 23.19 1.85
10 -5 -9 22.63 1.93
10 -5 -10 195 7.34
10 -5 -10 184.98 7.38
10 -5 -11 42.98 2.53
10 -5 -11 46.46 2.42
10 -5 -12 169.45 6.17
10 -5 -12 144.71 5.76
10 6 -10 34.71 2.11
10 -6 10 35.76 2.04
10 6 -9 41.09 2.42
10 -6 9 38.3 2.18
10 6 -8 53.44 2.96
10 -6 8 50.89 2.6
10 6 -7 207.46 8.19
10 6 -6 36.85 2.56
10 -6 6 31.76 2.34
10 6 -5 62.52 3.51
10 -6 5 57.42 3.29
10 6 -4 303.33 11.43
10 -6 4 293.47 11.17
10 6 -3 115.76 5.6
10 -6 3 125.89 5.5
10 6 -2 10.86 1.83
10 -6 2 11.4 1.55
10 6 -1 37.72 2.83
10 -6 1 38.54 2.61
10 6 0 40.89 2.97
10 -6 0 39.08 2.65
10 6 1 35.49 2.82
10 -6 -1 39.22 2.59
10 6 2 7.02 1.63
10 -6 -2 11 1.49
10 6 3 129.38 6.14
10 -6 -3 143.13 5.92
10 6 4 290.69 11.33
10 -6 -4 297.01 10.92
10 6 5 56.49 3.5
10 -6 -5 59.03 3.13
10 6 6 27.87 2.4
10 -6 -6 25.21 1.92
10 6 7 219.41 8.88
10 -6 -7 228.18 8.42
10 6 8 54.88 3.11
10 -6 -8 51.11 2.58
10 -6 -9 41.67 2.11
10 -6 -9 36.09 2.22
10 -6 -10 38.27 2.2
10 7 -9 86.32 3.71
10 7 -8 79.78 3.63
10 7 -7 48.11 2.68
10 -7 7 49.18 2.57
10 7 -6 26.54 2.01
10 -7 6 26.59 1.83
10 7 -5 14.9 1.66
10 -7 5 18.16 1.52
10 7 -4 29.07 2.17
10 -7 4 26.56 1.93
10 7 -3 118.24 5.22
10 -7 3 112.2 4.86
10 7 -2 63.99 3.56
10 -7 2 66.81 3.27
10 7 -1 37.31 2.59
10 -7 1 38.46 2.34
10 7 0 68.47 3.67
10 -7 0 65.6 3.26
10 7 1 35.71 2.6
10 -7 -1 39.25 2.26
10 7 2 73.02 3.81
10 -7 -2 68.11 3.3
10 7 3 121.33 5.37
10 -7 -3 115.27 4.81
10 7 4 24.29 2.03
10 -7 -4 21.63 1.53
10 -7 -5 16.14 1.27
10 8 -5 108.52 4.5
10 8 -4 50.15 2.62
10 8 5 130.38 5.25
11 0 0 0.13 0.69
11 0 1 0.6 0.67
11 0 -1 0.52 0.71
11 0 2 8.35 1.01
11 0 -2 8.78 1.14
11 0 3 2.96 0.73
11 0 -3 4.25 0.93
11 0 -4 18.2 1.48
11 0 -5 8.56 1.07
11 0 -6 47.27 2.43
11 0 -7 3.13 0.75
11 1 -5 15.38 1.22
11 -1 4 67.55 3.07
11 1 -4 67.79 3.01
11 -1 3 26.86 1.7
11 1 -3 20.12 1.45
11 -1 2 52.61 2.62
11 1 -2 46.16 2.34
11 -1 1 18.57 1.51
11 1 -1 16.99 1.28
11 -1 0 633.98 21.52
11 -1 -1 21.3 1.65
11 -1 -2 56.55 2.91
11 -1 -3 21.75 1.67
11 -1 -4 74.53 3.49
11 -1 -5 17.16 1.47
11 -1 -6 14.09 1.28
11 -1 -7 12.65 1.16
11 -1 -8 105.18 4.27
11 -2 5 112.04 4.5
11 -2 4 60.67 2.88
11 -2 3 28.91 1.87
11 -2 2 252.35 9.23
11 -2 1 67.72 3.26
11 -2 0 30.23 2
11 -2 -1 81.96 3.76
11 -2 -2 267.41 9.78
11 -2 -3 32.48 2.07
11 -2 -4 73.91 3.46
11 -2 -5 113.66 4.7
11 -2 -6 117.46 4.77
11 -2 -7 0.06 0.56
11 -3 5 52.95 2.52
11 -3 4 27.79 1.71
11 -3 3 30.08 1.84
11 -3 2 53.72 2.7
11 -3 1 44.69 2.42
11 -3 0 67.38 3.19
11 -3 -1 45.75 2.47
11 -3 -2 63.75 3.06
11 -3 -3 17.81 1.45
11 -3 -4 30.86 1.87
11 -4 3 13.47 1.13
11 -4 2 158.75 6
11 -4 1 156.53 5.94
11 -4 0 11.18 1.07
_iucr_refine_instructions_details
;
TITL wl-s2cl5br-ligand_a.res in P2(1)2(1)2(1)
wl-s2cl5br-ligand.res
created by SHELXL-2018/3 at 09:30:32 on 10-May-2018
REM Old TITL WL-S2Cl5Br-ligand in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1): R1 0.121, Rweak 0.044, Alpha 0.003
REM 1.191 for 33 systematic absences, Orientation as input
REM Flack x = 0.109 ( 0.022 ) from 3257 Parsons' quotients
REM Formula found by SHELXT: C44 O4 Cl2 Br2
CELL 1.54184 8.9198 14.4186 29.7333 90 90 90
ZERR 8 0.0001 0.0001 0.0002 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Br Cl O
UNIT 176 128 8 8 16
DFIX 0.955 0.002 O1 H1
DFIX 1.655 0.001 H1 O1'
SADI 0.002 C3' H3'b C3' H3'a
SADI 0.002 C3 H3a C3' H3'b
SADI 0.001 C4_2 C1' C4_3 C1'
SADI 0.001 C3 H3a C3 H3b
SADI 0.001 C2' C11_5 C2' C11_4
RIGU_ClBr 0.0002 0.0004 Br1 > C9
RIGU_phen 0.0002 0.0004 C11 > C16
ISOR_3 0.001 0.002 C4
ISOR_3 0.001 0.002 C5
ISOR_4 0.001 0.002 C11
EADP H3'b H3'a
EADP C11_4 C11_5
EADP C16_4 C16_5
EADP C15_4 C15_5
EADP C14_4 C14_5
EADP C13_4 C13_5
EADP C12_4 C12_5
EADP C5_2 C5_3
EADP C4_2 C4_3
EADP C9_2 C9_3
EADP C8_2 C8_3
EADP C7_2 C7_3
EADP C6_2 C6_3
EADP H3a H3b
EADP H3b H3'b
EADP Br1_2 Br1_3
EADP Cl1_3 Cl1_2
SAME_ClBr 0.002 0.004 Br1 > C9
SAME_phen 0.002 0.004 C11 > C16
L.S. 4
PLAN 20
BOND
list 4
fmap 2
acta
OMIT -4 2 31
OMIT 8 10 0
OMIT -8 10 1
OMIT -4 7 27
OMIT -4 7 28
OMIT 2 0 1
OMIT 3 4 0
OMIT 5 0 3
OMIT 0 0 2
REM
REM
REM
WGHT 0.029100 1.125300
EXTI 0.000188
FVAR 0.38400 0.86690 0.40982
C11 1 0.354705 0.549657 0.700336 11.00000 0.01417 0.01693 =
0.01975 -0.00154 -0.00038 0.00177
C1 1 0.525346 0.458530 0.642363 11.00000 0.01454 0.01824 =
0.01529 -0.00091 -0.00141 0.00051
C16 1 0.291482 0.530529 0.742267 11.00000 0.02702 0.01758 =
0.01993 0.00080 0.00085 -0.00039
AFIX 43
H16 2 0.265653 0.469817 0.749443 11.00000 -1.20000
AFIX 0
C2 1 0.370682 0.472380 0.666155 11.00000 0.01467 0.01582 =
0.01798 0.00029 -0.00066 0.00122
C15 1 0.266387 0.600716 0.773547 11.00000 0.02699 0.02552 =
0.01948 -0.00132 0.00343 -0.00108
AFIX 43
H15 2 0.223663 0.586644 0.801250 11.00000 -1.20000
AFIX 0
C3 1 0.391292 0.499658 0.617678 11.00000 0.01843 0.01889 =
0.01735 0.00172 -0.00164 0.00291
H3A 2 0.395929 0.566825 0.609807 11.00000 0.02113
H3B 2 0.345956 0.458600 0.594366 11.00000 0.02113
H1 2 10.491720 10.254860 10.599480 11.00000 -1.50000
C14 1 0.304850 0.691292 0.763510 11.00000 0.02380 0.02315 =
0.02846 -0.00993 0.00597 -0.00170
AFIX 43
H14 2 0.286902 0.738493 0.784135 11.00000 -1.20000
AFIX 0
C13 1 0.370326 0.710825 0.722430 11.00000 0.03263 0.01771 =
0.03870 -0.00555 0.01220 -0.00533
AFIX 43
H13 2 0.398450 0.771373 0.715718 11.00000 -1.20000
AFIX 0
C12 1 0.394598 0.640814 0.691009 11.00000 0.02669 0.01972 =
0.02676 -0.00167 0.01113 -0.00205
AFIX 43
H12 2 0.438031 0.655233 0.663447 11.00000 -1.20000
AFIX 0
C10 1 0.564751 0.362043 0.628047 11.00000 0.01409 0.01854 =
0.01574 -0.00046 0.00136 0.00054
C17 1 0.279592 0.387843 0.677457 11.00000 0.01679 0.01656 =
0.01569 -0.00310 0.00057 -0.00058
C18 1 0.340385 0.312932 0.700925 11.00000 0.01625 0.02033 =
0.02509 0.00176 -0.00179 -0.00026
AFIX 43
H18 2 0.441920 0.312903 0.708033 11.00000 -1.20000
AFIX 0
C19 1 0.251716 0.238551 0.713805 11.00000 0.02686 0.01997 =
0.03021 0.00402 -0.00186 -0.00130
AFIX 43
H19 2 0.294162 0.188530 0.728897 11.00000 -1.20000
AFIX 0
C20 1 0.099737 0.238883 0.704149 11.00000 0.02384 0.02900 =
0.03455 0.00499 -0.00174 -0.00961
AFIX 43
H20 2 0.039729 0.189378 0.712977 11.00000 -1.20000
AFIX 0
C21 1 0.037447 0.313342 0.681263 11.00000 0.01719 0.03461 =
0.03332 0.00170 -0.00484 -0.00449
AFIX 43
H21 2 -0.064702 0.314027 0.675006 11.00000 -1.20000
AFIX 0
C22 1 0.127354 0.386953 0.667655 11.00000 0.01785 0.02319 =
0.02316 -0.00019 -0.00255 0.00153
AFIX 43
H22 2 0.085133 0.436080 0.651833 11.00000 -1.20000
AFIX 0
O1 5 0.466488 0.318790 0.604308 11.00000 0.02080 0.02238 =
0.02825 -0.01057 -0.00700 0.00113
O2 5 0.688821 0.328445 0.638382 11.00000 0.01708 0.01927 =
0.02638 -0.00389 -0.00332 0.00329
C1' 1 0.697723 0.017546 0.581575 11.00000 0.01697 0.01692 =
0.01701 -0.00075 0.00189 -0.00145
C2' 1 0.708775 0.007110 0.529034 11.00000 0.01753 0.01780 =
0.01650 -0.00246 -0.00152 0.00005
C3' 1 0.582786 -0.036075 0.555016 11.00000 0.01883 0.01849 =
0.02183 -0.00206 0.00183 -0.00197
H3'A 2 0.586675 -0.104041 0.561093 11.00000 0.02113
H3'B 2 0.479924 -0.009420 0.552765 11.00000 0.02113
C10' 1 0.652870 0.113461 0.596152 11.00000 0.01822 0.01791 =
0.01369 0.00056 0.00272 -0.00257
C17' 1 0.674113 0.090099 0.499821 11.00000 0.02105 0.02206 =
0.01544 -0.00371 0.00214 0.00327
C18' 1 0.763272 0.169466 0.500711 11.00000 0.02515 0.02525 =
0.02127 0.00046 0.00450 -0.00183
AFIX 43
H18' 2 0.843053 0.173411 0.520757 11.00000 -1.20000
AFIX 0
C19' 1 0.733108 0.242916 0.471626 11.00000 0.04175 0.02330 =
0.02976 0.00308 0.01251 0.00222
AFIX 43
H19' 2 0.792144 0.296050 0.472488 11.00000 -1.20000
AFIX 0
C20' 1 0.615542 0.236858 0.441504 11.00000 0.04577 0.03356 =
0.02671 0.00835 0.01078 0.02001
AFIX 43
H20' 2 0.596755 0.285513 0.421759 11.00000 -1.20000
AFIX 0
C21' 1 0.526064 0.159001 0.440617 11.00000 0.03502 0.04345 =
0.02510 0.00019 -0.00350 0.01684
AFIX 43
H21' 2 0.446103 0.155488 0.420617 11.00000 -1.20000
AFIX 0
C22' 1 0.555572 0.085556 0.469729 11.00000 0.02415 0.02976 =
0.02308 -0.00424 -0.00132 0.00541
AFIX 43
H22' 2 0.495217 0.032985 0.468978 11.00000 -1.20000
AFIX 0
O1' 5 0.525848 0.144260 0.588457 11.00000 0.01810 0.02178 =
0.02867 -0.00430 0.00141 0.00288
O2' 5 0.757652 0.160074 0.616148 11.00000 0.02292 0.01768 =
0.02593 -0.00408 -0.00325 0.00001
AFIX 147 0.9550
H2' 2 0.722353 0.221163 0.622642 11.00000 -1.20000
AFIX 0
RESI ClBr 1
BR1 3 0.936077 0.696487 0.583548 11.00000 0.03892 0.03489 =
0.03675 0.00310 0.01412 -0.01405
CL1 4 0.663397 0.442806 0.739036 11.00000 0.02551 0.02402 =
0.01970 0.00527 -0.00592 -0.00326
C4 1 0.660500 0.515906 0.654442 11.00000 0.01478 0.01631 =
0.01928 -0.00139 0.00088 0.00112
C5 1 0.733147 0.511606 0.695880 11.00000 0.01927 0.01431 =
0.02076 -0.00130 -0.00192 0.00175
C6 1 0.864206 0.560428 0.704496 11.00000 0.01991 0.01915 =
0.02745 -0.00541 -0.00139 -0.00015
AFIX 43
H6 2 0.910213 0.555690 0.732470 11.00000 -1.20000
AFIX 0
C7 1 0.926759 0.616385 0.671364 11.00000 0.02318 0.02002 =
0.03171 -0.00450 0.00192 -0.00123
AFIX 43
H7 2 1.014249 0.649652 0.676768 11.00000 -1.20000
AFIX 0
C8 1 0.855267 0.621232 0.630118 11.00000 0.02024 0.02214 =
0.02916 -0.00187 0.00547 -0.00182
C9 1 0.724599 0.572649 0.621584 11.00000 0.02017 0.01884 =
0.02243 0.00032 0.00357 -0.00017
AFIX 43
H9 2 0.678821 0.577838 0.593595 11.00000 -1.20000
AFIX 0
RESI ClBr 2
PART 1
BR1 3 1.259707 0.014668 0.638274 21.00000 0.01910 0.05662 =
0.03583 -0.00398 -0.00460 -0.00176
CL1 4 0.589265 -0.134776 0.650622 21.00000 0.02744 0.04152 =
0.03543 0.01671 0.00148 -0.00947
C4 1 0.808430 -0.027557 0.612803 21.00000 0.01930 0.01631 =
0.01753 -0.00287 0.00138 0.00170
C5 1 0.772171 -0.094869 0.644671 21.00000 0.02359 0.01901 =
0.02174 0.00050 0.00276 0.00123
C6 1 0.877942 -0.131432 0.674084 21.00000 0.02791 0.02589 =
0.02454 0.00126 0.00060 0.00579
AFIX 43
H6 2 0.850081 -0.177043 0.694559 21.00000 -1.20000
AFIX 0
C7 1 1.025208 -0.100009 0.672974 21.00000 0.02762 0.03032 =
0.02406 -0.00039 -0.00020 0.00536
AFIX 43
H7 2 1.097100 -0.123986 0.692416 21.00000 -1.20000
AFIX 0
C8 1 1.061449 -0.032002 0.642065 21.00000 0.02282 0.02634 =
0.02074 -0.00430 -0.00073 0.00593
C9 1 0.956370 0.004172 0.612670 21.00000 0.01927 0.01793 =
0.01937 -0.00412 0.00098 0.00131
AFIX 43
H9 2 0.984673 0.050300 0.592524 21.00000 -1.20000
AFIX 0
RESI ClBr 3
PART 0
PART 2
BR1 3 1.259738 -0.023956 0.636972 -21.00000 0.01910 0.05662 =
0.03583 -0.00398 -0.00460 -0.00176
CL1 4 0.570072 -0.138079 0.644064 -21.00000 0.02744 0.04152 =
0.03543 0.01671 0.00148 -0.00947
C4 1 0.803714 -0.036453 0.610877 -21.00000 0.01930 0.01631 =
0.01753 -0.00287 0.00138 0.00170
C5 1 0.755571 -0.101243 0.642532 -21.00000 0.02359 0.01901 =
0.02174 0.00050 0.00276 0.00123
C6 1 0.850944 -0.135969 0.675429 -21.00000 0.02791 0.02589 =
0.02454 0.00126 0.00060 0.00579
AFIX 43
H6 2 0.813358 -0.174412 0.697871 -21.00000 -1.20000
AFIX 0
C7 1 1.002486 -0.113339 0.674852 -21.00000 0.02762 0.03032 =
0.02406 -0.00039 -0.00020 0.00536
AFIX 43
H7 2 1.067272 -0.135492 0.696879 -21.00000 -1.20000
AFIX 0
C8 1 1.054027 -0.056906 0.640552 -21.00000 0.02282 0.02634 =
0.02074 -0.00430 -0.00073 0.00593
C9 1 0.956547 -0.015458 0.610398 -21.00000 0.01927 0.01793 =
0.01937 -0.00412 0.00098 0.00131
AFIX 43
H9 2 0.993325 0.026912 0.589555 -21.00000 -1.20000
AFIX 0
RESI phen 4
PART 0
PART 1
C11 1 0.832455 -0.051449 0.509590 31.00000 0.02146 0.01957 =
0.01741 0.00196 0.00068 0.00118
C12 1 0.802766 -0.141294 0.494315 31.00000 0.02184 0.01849 =
0.01990 0.00268 -0.00323 0.00295
AFIX 43
H12 2 0.705807 -0.164650 0.496305 31.00000 -1.20000
AFIX 0
C13 1 0.915746 -0.196426 0.476178 31.00000 0.02237 0.01868 =
0.02861 -0.00027 -0.00069 0.00156
AFIX 43
H13 2 0.893364 -0.254380 0.464202 31.00000 -1.20000
AFIX 0
C14 1 1.062157 -0.163872 0.476181 31.00000 0.02235 0.02063 =
0.02479 0.00225 -0.00138 0.00131
AFIX 43
H14 2 1.139558 -0.202354 0.466645 31.00000 -1.20000
AFIX 0
C15 1 1.093629 -0.074775 0.490242 31.00000 0.02137 0.02168 =
0.02262 0.00162 0.00220 -0.00020
AFIX 43
H15 2 1.191656 -0.052881 0.489346 31.00000 -1.20000
AFIX 0
C16 1 0.978980 -0.017537 0.505775 31.00000 0.02164 0.02167 =
0.01699 0.00239 0.00046 0.00059
AFIX 43
H16 2 0.999876 0.043531 0.513653 31.00000 -1.20000
AFIX 0
RESI phen 5
PART 0
PART 2
C11 1 0.822242 -0.059200 0.509794 -31.00000 0.02146 0.01957 =
0.01741 0.00196 0.00068 0.00118
C12 1 0.772014 -0.140297 0.488827 -31.00000 0.02184 0.01849 =
0.01990 0.00268 -0.00323 0.00295
AFIX 43
H12 2 0.669854 -0.153114 0.488168 -31.00000 -1.20000
AFIX 0
C13 1 0.871583 -0.202170 0.468945 -31.00000 0.02237 0.01868 =
0.02861 -0.00027 -0.00069 0.00156
AFIX 43
H13 2 0.836287 -0.255982 0.455335 -31.00000 -1.20000
AFIX 0
C14 1 1.023957 -0.182987 0.469576 -31.00000 0.02235 0.02063 =
0.02479 0.00225 -0.00138 0.00131
AFIX 43
H14 2 1.091183 -0.224417 0.456616 -31.00000 -1.20000
AFIX 0
C15 1 1.076171 -0.102673 0.489358 -31.00000 0.02137 0.02168 =
0.02262 0.00162 0.00220 -0.00020
AFIX 43
H15 2 1.178480 -0.090273 0.489752 -31.00000 -1.20000
AFIX 0
C16 1 0.976182 -0.040031 0.508758 -31.00000 0.02164 0.02167 =
0.01699 0.00239 0.00046 0.00059
AFIX 43
H16 2 1.011972 0.014932 0.521114 -31.00000 -1.20000
AFIX 0
HKLF 4
REM wl-s2cl5br-ligand_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0621, GooF = S = 1.057, Restrained GooF = 1.071 for all data
REM R1 = 0.0242 for 7700 Fo > 4sig(Fo) and 0.0253 for all 7890 data
REM 528 parameters refined using 308 restraints
END
WGHT 0.0291 1.1253
REM Highest difference peak 0.475, deepest hole -0.390, 1-sigma level 0.049
Q1 1 1.0011 0.6559 0.5927 11.00000 0.05 0.47
Q2 1 1.1872 -0.0162 0.6421 11.00000 0.05 0.32
Q3 1 1.0601 -0.0764 0.6591 11.00000 0.05 0.31
Q4 1 0.8050 0.6075 0.6232 11.00000 0.05 0.29
Q5 1 0.8751 -0.0227 0.6104 11.00000 0.05 0.27
Q6 1 0.9122 0.6213 0.6507 11.00000 0.05 0.26
Q7 1 0.7566 -0.0033 0.5997 11.00000 0.05 0.26
Q8 1 0.5490 0.4061 0.6361 11.00000 0.05 0.24
Q9 1 0.4709 0.4779 0.6262 11.00000 0.05 0.23
Q10 1 0.9557 -0.1388 0.6686 11.00000 0.05 0.23
Q11 1 0.3237 0.3486 0.6796 11.00000 0.05 0.23
Q12 1 1.2743 -0.0794 0.6336 11.00000 0.05 0.23
Q13 1 0.8991 -0.0470 0.5081 11.00000 0.05 0.22
Q14 1 0.5954 0.4860 0.6478 11.00000 0.05 0.22
Q15 1 1.0189 -0.0038 0.6308 11.00000 0.05 0.21
Q16 1 0.3567 0.4863 0.6424 11.00000 0.05 0.21
Q17 1 0.3337 0.4350 0.6734 11.00000 0.05 0.21
Q18 1 0.8149 -0.1212 0.6581 11.00000 0.05 0.21
Q19 1 0.1973 0.3854 0.6767 11.00000 0.05 0.21
Q20 1 0.7811 0.5460 0.7053 11.00000 0.05 0.20
REM The information below was added by Olex2.
REM
REM R1 = 0.0242 for 7700 Fo > 4sig(Fo) and 0.0253 for all 23809 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.47, deepest hole -0.39
REM Mean Shift 0.001, Max Shift -0.006.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0253
REM R1_gt = 0.0242
REM wR_ref = 0.0621
REM GOOF = 1.057
REM Shift_max = -0.006
REM Shift_mean = 0.001
REM Reflections_all = 23809
REM Reflections_gt = 7700
REM Parameters = n/a
REM Hole = -0.39
REM Peak = 0.47
REM Flack = -0.010(5)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id WL-S2Cl5Br-ligand
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.312
_oxdiff_exptl_absorpt_empirical_full_min 0.792