#------------------------------------------------------------------------------
#$Date: 2023-06-29 13:44:46 +0300 (Thu, 29 Jun 2023) $
#$Revision: 284608 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/32/7713248.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7713248
loop_
_publ_author_name
'Lindquist-Kleissler, Brent'
'Johnstone, Timothy C.'
_publ_section_title
;
 Models of the putative antimony(V)-diolate motifs in antileishmanial
 pentavalent antimonial drugs.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01623d
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H27 O2 Sb'
_chemical_formula_sum            'C24 H27 O2 Sb'
_chemical_formula_weight         469.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-12-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-27 deposited with the CCDC.	2023-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.1979(5)
_cell_length_b                   16.3230(8)
_cell_length_c                   16.9475(6)
_cell_measurement_reflns_used    19603
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9320
_cell_measurement_theta_min      4.7160
_cell_volume                     4204.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00 -48.00   0.50    0.95    --  -49.41 145.00 136.00   50
  2  ω   -119.00 -75.00   0.50    0.95    --  -49.41-127.00-107.00   88
  3  ω   -105.00 -61.00   0.50    0.95    --  -49.41-145.00  83.00   88
  4  ω    -65.00 -40.00   0.50    0.95    --  -49.41 127.00 -32.00   50
  5  ω     54.00 103.00   0.50    0.95    --   49.41-145.00  83.00   98
  6  ω     38.00  95.00   0.50    0.95    --   49.41-127.00-107.00  114
  7  ω    -75.00 -50.00   0.50    3.80    --  -84.25 127.00 -32.00   50
  8  ω    -62.00 -37.00   0.50    3.80    --  -84.25 145.00 136.00   50
  9  ω   -113.00 -75.00   0.50    3.80    --  -84.25-127.00-107.00   76
 10  ω    111.00 136.00   0.50    3.80    --  105.75 127.00 -32.00   50
 11  ω     75.00 112.00   0.50    3.80    --  105.75-127.00-107.00   74
 12  ω    101.00 126.00   0.50    3.80    --  105.75-145.00  83.00   50
 13  ω     81.00 141.00   0.50    3.80    --  105.75 145.00 136.00  120
 14  ω     46.00  71.00   0.50    3.80    --  105.75-127.00-107.00   50
 15  ω   -121.00 -94.00   0.50    0.95    --  -49.41 -57.00 -60.00   54
 16  ω   -120.00 -82.00   0.50    0.95    --  -49.41 -57.00  60.00   76
 17  ω    -23.00  23.00   0.50    0.95    --  -49.41  19.00  60.00   92
 18  ω    -25.00  10.00   0.50    0.95    --  -49.41  19.00 120.00   70
 19  ω   -120.00 -83.00   0.50    0.95    --  -49.41 -57.00 150.00   74
 20  ω   -115.00 -87.00   0.50    0.95    --  -49.41-125.00 -60.00   56
 21  ω   -118.00 -87.00   0.50    0.95    --  -49.41-125.00   0.00   62
 22  ω   -117.00 -83.00   0.50    0.95    --  -49.41 -57.00-150.00   68
 23  ω   -118.00 -84.00   0.50    0.95    --  -49.41 -57.00 -30.00   68
 24  ω     89.00 115.00   0.50    0.95    --   49.41  57.00 120.00   52
 25  ω   -143.00-117.00   0.50    3.80    --  -84.25 -57.00 -90.00   52
 26  ω    -41.00 -15.00   0.50    3.80    --  -84.25  38.00 -90.00   52
 27  ω   -131.00-106.00   0.50    3.80    --  -84.25-145.00  83.00   50
 28  ω    -42.00 -15.00   0.50    3.80    --  -84.25  38.00 -30.00   54
 29  ω     41.00 105.00   0.50    3.80    --  105.75-125.00  90.00  128
 30  ω     63.00  89.00   0.50    3.80    --  105.75 -77.00 -60.00   52
 31  ω     59.00 107.00   0.50    3.80    --  105.75-125.00 -60.00   96
 32  ω     35.00  67.00   0.50    3.80    --  105.75 -57.00-150.00   64
 33  ω     94.00 173.00   0.50    3.80    --  105.75  57.00-120.00  158
 34  ω     34.00  67.00   0.50    3.80    --  105.75 -57.00 -90.00   66
 35  ω     35.00  67.00   0.50    3.80    --  105.75 -57.00  60.00   64
 36  ω     98.00 177.00   0.50    3.80    --  105.75  38.00 -30.00  158
 37  ω     99.00 175.00   0.50    3.80    --  105.75  57.00 120.00  152
 38  ω     36.00  67.00   0.50    3.80    --  105.75 -57.00 -60.00   62
 39  ω     54.00 106.00   0.50    3.80    --  105.75 -99.00 120.00  104
 40  ω     41.00  90.00   0.50    3.80    --  105.75-125.00-180.00   98
 41  ω     43.00 103.00   0.50    3.80    --  105.75 -99.00 -30.00  120
 42  ω     36.00  64.00   0.50    3.80    --  105.75 -99.00-120.00   56
 43  ω     77.00 106.00   0.50    3.80    --  105.75 -99.00-120.00   58
 44  ω     64.00 106.00   0.50    3.80    --  105.75-125.00-150.00   84
 45  ω     36.00  66.00   0.50    3.80    --  105.75 -57.00-120.00   60
 46  ω     81.00 106.00   0.50    3.80    --  105.75 -99.00  60.00   50
 47  ω    102.00 164.00   0.50    3.80    --  105.75  77.00   0.00  124
 48  ω    102.00 176.00   0.50    3.80    --  105.75  38.00  60.00  148
 49  ω     37.00 106.00   0.50    3.80    --  105.75 -99.00  30.00  138
 50  ω     44.00  70.00   0.50    3.80    --  105.75 -77.00 150.00   52
 51  ω     34.00  61.00   0.50    3.80    --  105.75 -57.00  90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0774953000
_diffrn_orient_matrix_UB_12      0.0328366000
_diffrn_orient_matrix_UB_13      0.0493313000
_diffrn_orient_matrix_UB_21      -0.0320169000
_diffrn_orient_matrix_UB_22      -0.0884080000
_diffrn_orient_matrix_UB_23      0.0141116000
_diffrn_orient_matrix_UB_31      0.0569440000
_diffrn_orient_matrix_UB_32      -0.0050536000
_diffrn_orient_matrix_UB_33      0.0749703000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60946
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.072
_diffrn_reflns_theta_min         3.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.519
_exptl_absorpt_correction_T_max  0.65037
_exptl_absorpt_correction_T_min  0.62586
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       Block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.047
_exptl_crystal_size_rad          0.030
_refine_diff_density_max         1.897
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.001(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0528P)²+8.3502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6896
_reflns_number_total             7984
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt01623d2.cif
_cod_data_source_block           6
_cod_database_code               7713248
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Sb O2 C24 H27'
_chemical_oxdiff_usercomment     BLK0543
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.999(13)
 0.001(13)
2. 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
3.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C115(H115), C116(H116), C122(H122), C123(H123),
 C125(H125), C126(H126), C132(H132), C133(H133), C135(H135), C136(H136),
 C212(H212), C213(H213), C215(H215), C216(H216), C222(H222), C223(H223),
 C225(H225), C226(H226), C232(H232), C233(H233), C235(H235), C236(H236)
3.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C117(H11A,H11B,H11C), C127(H12A,H12B,H12C), C137(H13A,H13B,
 H13C), C6(H6A,H6B,H6C), C217(H21A,H21B,H21C), C227(H22A,H22B,H22C), C237(H23A,
 H23B,H23C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.163
_oxdiff_exptl_absorpt_empirical_full_min 0.533
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'
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
Sb1 Sb 0.61602(3) 0.55026(4) 0.12565(3) 0.02709(16) Uani 1 1 d . . . . .
O11 O 0.6422(5) 0.4402(5) 0.1682(4) 0.0389(15) Uani 1 1 d . . . . .
O12 O 0.6137(4) 0.5781(4) 0.2436(4) 0.0334(15) Uani 1 1 d . . . . .
C1 C 0.6499(7) 0.4366(7) 0.2523(6) 0.040(2) Uani 1 1 d . . . . .
H1A H 0.699076 0.399889 0.267034 0.048 Uiso 1 1 calc R U . . .
H1B H 0.595055 0.414105 0.275241 0.048 Uiso 1 1 calc R U . . .
C2 C 0.6666(7) 0.5223(7) 0.2850(6) 0.037(2) Uani 1 1 d . . . . .
H2 H 0.729732 0.536719 0.275843 0.044 Uiso 1 1 calc R U . . .
C3 C 0.6481(6) 0.5264(7) 0.3735(7) 0.042(2) Uani 1 1 d . . . . .
H3A H 0.671038 0.577926 0.394816 0.063 Uiso 1 1 calc R U . . .
H3B H 0.676826 0.480179 0.399958 0.063 Uiso 1 1 calc R U . . .
H3C H 0.584444 0.523617 0.382547 0.063 Uiso 1 1 calc R U . . .
C111 C 0.6114(6) 0.4921(6) 0.0121(6) 0.030(2) Uani 1 1 d . . . . .
C112 C 0.6073(7) 0.4078(7) -0.0001(6) 0.036(2) Uani 1 1 d . . . . .
H112 H 0.607797 0.372058 0.044154 0.043 Uiso 1 1 calc R U . . .
C113 C 0.6026(7) 0.3748(7) -0.0753(6) 0.041(2) Uani 1 1 d . . . . .
H113 H 0.598914 0.317100 -0.081732 0.049 Uiso 1 1 calc R U . . .
C114 C 0.6032(6) 0.4248(7) -0.1411(6) 0.041(3) Uani 1 1 d . . . . .
C115 C 0.6101(6) 0.5080(6) -0.1321(7) 0.035(2) Uani 1 1 d . . . . .
H115 H 0.612971 0.542363 -0.177241 0.042 Uiso 1 1 calc R U . . .
C116 C 0.6131(5) 0.5428(6) -0.0558(5) 0.0273(18) Uani 1 1 d . . . . .
H116 H 0.616258 0.600573 -0.049937 0.033 Uiso 1 1 calc R U . . .
C117 C 0.6000(7) 0.3872(8) -0.2226(6) 0.049(3) Uani 1 1 d . . . . .
H11A H 0.584765 0.429492 -0.261345 0.074 Uiso 1 1 calc R U . . .
H11B H 0.555393 0.343808 -0.223765 0.074 Uiso 1 1 calc R U . . .
H11C H 0.657601 0.363918 -0.235624 0.074 Uiso 1 1 calc R U . . .
C121 C 0.4952(5) 0.6138(7) 0.1168(6) 0.027(2) Uani 1 1 d . . . . .
C122 C 0.4303(5) 0.5879(6) 0.0645(5) 0.026(2) Uani 1 1 d . . . . .
H122 H 0.440809 0.542141 0.031131 0.031 Uiso 1 1 calc R U . . .
C123 C 0.3500(6) 0.6290(6) 0.0609(6) 0.032(2) Uani 1 1 d . . . . .
H123 H 0.305720 0.609940 0.025810 0.039 Uiso 1 1 calc R U . . .
C124 C 0.3333(6) 0.6971(6) 0.1076(5) 0.029(2) Uani 1 1 d . . . . .
C125 C 0.3985(6) 0.7238(6) 0.1590(6) 0.036(2) Uani 1 1 d . . . . .
H125 H 0.388972 0.771228 0.190373 0.044 Uiso 1 1 calc R U . . .
C126 C 0.4777(6) 0.6816(6) 0.1647(5) 0.030(2) Uani 1 1 d . . . . .
H126 H 0.520671 0.699057 0.201726 0.036 Uiso 1 1 calc R U . . .
C127 C 0.2468(6) 0.7432(7) 0.0991(6) 0.037(2) Uani 1 1 d . . . . .
H12A H 0.241233 0.763811 0.045000 0.056 Uiso 1 1 calc R U . . .
H12B H 0.245754 0.789281 0.136096 0.056 Uiso 1 1 calc R U . . .
H12C H 0.197722 0.706133 0.110637 0.056 Uiso 1 1 calc R U . . .
C131 C 0.7288(5) 0.6230(6) 0.1060(5) 0.026(2) Uani 1 1 d . . . . .
C132 C 0.7359(5) 0.7029(6) 0.1349(5) 0.031(2) Uani 1 1 d . . . . .
H132 H 0.687143 0.727552 0.160682 0.037 Uiso 1 1 calc R U . . .
C133 C 0.8148(5) 0.7470(6) 0.1259(6) 0.0309(19) Uani 1 1 d . . . . .
H133 H 0.818446 0.801824 0.144435 0.037 Uiso 1 1 calc R U . . .
C134 C 0.8873(6) 0.7109(6) 0.0902(5) 0.031(2) Uani 1 1 d . . . . .
C135 C 0.8790(6) 0.6310(6) 0.0605(6) 0.034(2) Uani 1 1 d . . . . .
H135 H 0.927643 0.605937 0.034857 0.041 Uiso 1 1 calc R U . . .
C136 C 0.8009(6) 0.5883(7) 0.0680(6) 0.037(2) Uani 1 1 d . . . . .
H136 H 0.796334 0.534514 0.046946 0.044 Uiso 1 1 calc R U . . .
C137 C 0.9743(6) 0.7557(8) 0.0835(7) 0.042(3) Uani 1 1 d . . . . .
H13A H 0.967212 0.812123 0.102058 0.063 Uiso 1 1 calc R U . . .
H13B H 0.993338 0.756060 0.028219 0.063 Uiso 1 1 calc R U . . .
H13C H 1.018597 0.727734 0.115736 0.063 Uiso 1 1 calc R U . . .
Sb2 Sb 0.87637(3) 0.94671(4) 0.37895(3) 0.02898(16) Uani 1 1 d . . . . .
O21 O 0.8751(4) 1.0638(5) 0.3484(4) 0.0401(16) Uani 1 1 d . . . . .
O22 O 0.8548(4) 0.9317(4) 0.2601(4) 0.0334(15) Uani 1 1 d . . . . .
C4 C 0.8600(8) 1.0763(7) 0.2665(6) 0.046(3) Uani 1 1 d . . . . .
H4A H 0.893508 1.124821 0.248388 0.055 Uiso 1 1 calc R U . . .
H4B H 0.796696 1.086944 0.257301 0.055 Uiso 1 1 calc R U . . .
C5 C 0.8885(6) 1.0014(6) 0.2197(6) 0.036(2) Uani 1 1 d . . . . .
H5 H 0.954200 0.998461 0.220181 0.043 Uiso 1 1 calc R U . . .
C6 C 0.8578(7) 1.0006(7) 0.1354(7) 0.044(3) Uani 1 1 d . . . . .
H6A H 0.883072 0.953190 0.108168 0.066 Uiso 1 1 calc R U . . .
H6B H 0.876946 1.051060 0.109170 0.066 Uiso 1 1 calc R U . . .
H6C H 0.793478 0.997150 0.134028 0.066 Uiso 1 1 calc R U . . .
C211 C 0.8839(6) 0.9881(6) 0.5007(6) 0.026(2) Uani 1 1 d . . . . .
C212 C 0.8926(6) 1.0693(6) 0.5235(6) 0.036(2) Uani 1 1 d . . . . .
H212 H 0.895051 1.111239 0.484764 0.044 Uiso 1 1 calc R U . . .
C213 C 0.8979(7) 1.0893(7) 0.6035(7) 0.045(3) Uani 1 1 d . . . . .
H213 H 0.904390 1.145164 0.618170 0.054 Uiso 1 1 calc R U . . .
C214 C 0.8941(6) 1.0299(7) 0.6622(6) 0.039(2) Uani 1 1 d . . . . .
C215 C 0.8856(5) 0.9483(7) 0.6390(6) 0.035(2) Uani 1 1 d . . . . .
H215 H 0.883695 0.906401 0.677906 0.043 Uiso 1 1 calc R U . . .
C216 C 0.8797(5) 0.9273(6) 0.5587(5) 0.0269(19) Uani 1 1 d . . . . .
H216 H 0.872934 0.871532 0.543737 0.032 Uiso 1 1 calc R U . . .
C217 C 0.8968(8) 1.0526(10) 0.7480(7) 0.059(3) Uani 1 1 d . . . . .
H21A H 0.925074 1.106214 0.754037 0.089 Uiso 1 1 calc R U . . .
H21B H 0.930398 1.011297 0.777202 0.089 Uiso 1 1 calc R U . . .
H21C H 0.836695 1.055175 0.768833 0.089 Uiso 1 1 calc R U . . .
C221 C 0.7664(5) 0.8688(6) 0.3922(5) 0.028(2) Uani 1 1 d . . . . .
C222 C 0.7004(6) 0.8889(7) 0.4459(5) 0.032(2) Uani 1 1 d . . . . .
H222 H 0.708618 0.932917 0.481779 0.039 Uiso 1 1 calc R U . . .
C223 C 0.6221(6) 0.8440(7) 0.4466(5) 0.033(2) Uani 1 1 d . . . . .
H223 H 0.577194 0.857715 0.483319 0.040 Uiso 1 1 calc R U . . .
C224 C 0.6092(6) 0.7802(6) 0.3947(5) 0.034(2) Uani 1 1 d . . . . .
C225 C 0.6771(6) 0.7563(6) 0.3434(5) 0.033(2) Uani 1 1 d . . . . .
H225 H 0.670503 0.709905 0.310049 0.039 Uiso 1 1 calc R U . . .
C226 C 0.7548(6) 0.8026(6) 0.3424(5) 0.030(2) Uani 1 1 d . . . . .
H226 H 0.800435 0.788179 0.306753 0.036 Uiso 1 1 calc R U . . .
C227 C 0.5225(7) 0.7349(8) 0.3916(7) 0.044(3) Uani 1 1 d . . . . .
H22A H 0.499853 0.727624 0.445292 0.065 Uiso 1 1 calc R U . . .
H22B H 0.531324 0.681153 0.367081 0.065 Uiso 1 1 calc R U . . .
H22C H 0.480168 0.766571 0.360451 0.065 Uiso 1 1 calc R U . . .
C231 C 0.9998(5) 0.8861(7) 0.3724(6) 0.029(2) Uani 1 1 d . . . . .
C232 C 1.0208(6) 0.8417(7) 0.3039(6) 0.033(2) Uani 1 1 d . . . . .
H232 H 0.980710 0.839851 0.260978 0.039 Uiso 1 1 calc R U . . .
C233 C 1.1005(6) 0.8009(6) 0.2994(6) 0.037(2) Uani 1 1 d . . . . .
H233 H 1.113931 0.770520 0.253121 0.044 Uiso 1 1 calc R U . . .
C234 C 1.1609(5) 0.8028(6) 0.3601(6) 0.033(2) Uani 1 1 d . . . . .
C235 C 1.1408(6) 0.8493(8) 0.4268(6) 0.040(2) Uani 1 1 d . . . . .
H235 H 1.182124 0.852717 0.468779 0.048 Uiso 1 1 calc R U . . .
C236 C 1.0613(6) 0.8906(7) 0.4327(6) 0.033(2) Uani 1 1 d . . . . .
H236 H 1.048838 0.922182 0.478404 0.039 Uiso 1 1 calc R U . . .
C237 C 1.2475(6) 0.7569(6) 0.3566(6) 0.040(2) Uani 1 1 d . . . . .
H23A H 1.246934 0.712284 0.395233 0.059 Uiso 1 1 calc R U . . .
H23B H 1.295895 0.794601 0.368715 0.059 Uiso 1 1 calc R U . . .
H23C H 1.255741 0.734291 0.303553 0.059 Uiso 1 1 calc R U . . .
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -2 -1 0.0281
1 -1 0 0.0294
-1 1 0 0.0436
-2 1 -2 0.0321
2 -1 2 0.0279
0 -1 -2 0.0438
0 1 2 0.0264
2 2 -1 0.0114
1 -1 2 0.0303
1 2 0 0.0173
1 2 1 0.0177
0 -1 0 0.0301
-1 0 2 0.0352
0 -2 1 0.0227
-1 -2 1 0.0247
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
O11 Sb1 O12 81.3(3) . . ?
O11 Sb1 C111 86.1(3) . . ?
O11 Sb1 C121 130.3(3) . . ?
O11 Sb1 C131 113.9(3) . . ?
O12 Sb1 C111 166.2(3) . . ?
O12 Sb1 C121 86.9(3) . . ?
O12 Sb1 C131 92.5(3) . . ?
C121 Sb1 C111 97.2(4) . . ?
C131 Sb1 C111 97.7(4) . . ?
C131 Sb1 C121 114.7(4) . . ?
C1 O11 Sb1 114.7(6) . . ?
C2 O12 Sb1 109.6(6) . . ?
O11 C1 H1A 109.7 . . ?
O11 C1 H1B 109.7 . . ?
O11 C1 C2 109.7(8) . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
O12 C2 C1 108.5(8) . . ?
O12 C2 H2 108.6 . . ?
O12 C2 C3 111.0(8) . . ?
C1 C2 H2 108.6 . . ?
C1 C2 C3 111.4(9) . . ?
C3 C2 H2 108.6 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C112 C111 Sb1 124.8(8) . . ?
C112 C111 C116 117.2(9) . . ?
C116 C111 Sb1 118.0(7) . . ?
C111 C112 H112 119.3 . . ?
C113 C112 C111 121.5(11) . . ?
C113 C112 H112 119.3 . . ?
C112 C113 H113 119.6 . . ?
C114 C113 C112 120.9(10) . . ?
C114 C113 H113 119.6 . . ?
C113 C114 C117 119.9(10) . . ?
C115 C114 C113 119.6(10) . . ?
C115 C114 C117 120.4(11) . . ?
C114 C115 H115 119.9 . . ?
C114 C115 C116 120.2(10) . . ?
C116 C115 H115 119.9 . . ?
C111 C116 H116 119.7 . . ?
C115 C116 C111 120.5(9) . . ?
C115 C116 H116 119.7 . . ?
C114 C117 H11A 109.5 . . ?
C114 C117 H11B 109.5 . . ?
C114 C117 H11C 109.5 . . ?
H11A C117 H11B 109.5 . . ?
H11A C117 H11C 109.5 . . ?
H11B C117 H11C 109.5 . . ?
C122 C121 Sb1 120.8(8) . . ?
C122 C121 C126 118.4(8) . . ?
C126 C121 Sb1 120.8(7) . . ?
C121 C122 H122 119.9 . . ?
C121 C122 C123 120.1(9) . . ?
C123 C122 H122 119.9 . . ?
C122 C123 H123 119.3 . . ?
C124 C123 C122 121.4(8) . . ?
C124 C123 H123 119.3 . . ?
C123 C124 C125 118.6(8) . . ?
C123 C124 C127 120.0(8) . . ?
C125 C124 C127 121.3(9) . . ?
C124 C125 H125 119.9 . . ?
C124 C125 C126 120.3(9) . . ?
C126 C125 H125 119.9 . . ?
C121 C126 H126 119.4 . . ?
C125 C126 C121 121.1(9) . . ?
C125 C126 H126 119.4 . . ?
C124 C127 H12A 109.5 . . ?
C124 C127 H12B 109.5 . . ?
C124 C127 H12C 109.5 . . ?
H12A C127 H12B 109.5 . . ?
H12A C127 H12C 109.5 . . ?
H12B C127 H12C 109.5 . . ?
C132 C131 Sb1 122.2(6) . . ?
C136 C131 Sb1 118.9(7) . . ?
C136 C131 C132 118.8(9) . . ?
C131 C132 H132 119.8 . . ?
C131 C132 C133 120.4(8) . . ?
C133 C132 H132 119.8 . . ?
C132 C133 H133 119.8 . . ?
C134 C133 C132 120.4(9) . . ?
C134 C133 H133 119.8 . . ?
C133 C134 C135 118.7(8) . . ?
C133 C134 C137 121.4(9) . . ?
C135 C134 C137 119.9(9) . . ?
C134 C135 H135 119.6 . . ?
C136 C135 C134 120.8(9) . . ?
C136 C135 H135 119.6 . . ?
C131 C136 H136 119.6 . . ?
C135 C136 C131 120.9(10) . . ?
C135 C136 H136 119.6 . . ?
C134 C137 H13A 109.5 . . ?
C134 C137 H13B 109.5 . . ?
C134 C137 H13C 109.5 . . ?
H13A C137 H13B 109.5 . . ?
H13A C137 H13C 109.5 . . ?
H13B C137 H13C 109.5 . . ?
O21 Sb2 O22 81.8(3) . . ?
O21 Sb2 C211 87.1(3) . . ?
O21 Sb2 C221 126.9(3) . . ?
O21 Sb2 C231 116.4(4) . . ?
O22 Sb2 C211 167.3(3) . . ?
O22 Sb2 C221 84.6(3) . . ?
O22 Sb2 C231 92.0(3) . . ?
C221 Sb2 C211 97.3(3) . . ?
C221 Sb2 C231 115.1(4) . . ?
C231 Sb2 C211 98.5(4) . . ?
C4 O21 Sb2 113.4(7) . . ?
C5 O22 Sb2 108.7(6) . . ?
O21 C4 H4A 109.6 . . ?
O21 C4 H4B 109.6 . . ?
O21 C4 C5 110.3(9) . . ?
H4A C4 H4B 108.1 . . ?
C5 C4 H4A 109.6 . . ?
C5 C4 H4B 109.6 . . ?
O22 C5 C4 106.8(8) . . ?
O22 C5 H5 108.5 . . ?
O22 C5 C6 109.9(8) . . ?
C4 C5 H5 108.5 . . ?
C6 C5 C4 114.5(9) . . ?
C6 C5 H5 108.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C212 C211 Sb2 124.5(8) . . ?
C212 C211 C216 119.2(9) . . ?
C216 C211 Sb2 116.3(7) . . ?
C211 C212 H212 120.0 . . ?
C211 C212 C213 120.0(10) . . ?
C213 C212 H212 120.0 . . ?
C212 C213 H213 119.1 . . ?
C214 C213 C212 121.9(10) . . ?
C214 C213 H213 119.1 . . ?
C213 C214 C215 118.0(9) . . ?
C213 C214 C217 121.3(11) . . ?
C215 C214 C217 120.7(11) . . ?
C214 C215 H215 119.6 . . ?
C214 C215 C216 120.7(9) . . ?
C216 C215 H215 119.6 . . ?
C211 C216 C215 120.3(9) . . ?
C211 C216 H216 119.9 . . ?
C215 C216 H216 119.9 . . ?
C214 C217 H21A 109.5 . . ?
C214 C217 H21B 109.5 . . ?
C214 C217 H21C 109.5 . . ?
H21A C217 H21B 109.5 . . ?
H21A C217 H21C 109.5 . . ?
H21B C217 H21C 109.5 . . ?
C222 C221 Sb2 119.8(7) . . ?
C226 C221 Sb2 120.4(7) . . ?
C226 C221 C222 119.4(9) . . ?
C221 C222 H222 120.1 . . ?
C221 C222 C223 119.7(9) . . ?
C223 C222 H222 120.1 . . ?
C222 C223 H223 119.6 . . ?
C224 C223 C222 120.8(9) . . ?
C224 C223 H223 119.6 . . ?
C223 C224 C225 120.0(9) . . ?
C223 C224 C227 121.1(9) . . ?
C225 C224 C227 118.9(9) . . ?
C224 C225 H225 120.8 . . ?
C226 C225 C224 118.5(9) . . ?
C226 C225 H225 120.8 . . ?
C221 C226 C225 121.5(9) . . ?
C221 C226 H226 119.3 . . ?
C225 C226 H226 119.3 . . ?
C224 C227 H22A 109.5 . . ?
C224 C227 H22B 109.5 . . ?
C224 C227 H22C 109.5 . . ?
H22A C227 H22B 109.5 . . ?
H22A C227 H22C 109.5 . . ?
H22B C227 H22C 109.5 . . ?
C232 C231 Sb2 119.0(7) . . ?
C236 C231 Sb2 122.2(7) . . ?
C236 C231 C232 118.8(8) . . ?
C231 C232 H232 120.2 . . ?
C233 C232 C231 119.5(8) . . ?
C233 C232 H232 120.2 . . ?
C232 C233 H233 119.0 . . ?
C234 C233 C232 122.0(9) . . ?
C234 C233 H233 119.0 . . ?
C233 C234 C235 118.1(8) . . ?
C233 C234 C237 122.5(9) . . ?
C235 C234 C237 119.4(9) . . ?
C234 C235 H235 119.6 . . ?
C236 C235 C234 120.8(9) . . ?
C236 C235 H235 119.6 . . ?
C231 C236 C235 120.6(9) . . ?
C231 C236 H236 119.7 . . ?
C235 C236 H236 119.7 . . ?
C234 C237 H23A 109.5 . . ?
C234 C237 H23B 109.5 . . ?
C234 C237 H23C 109.5 . . ?
H23A C237 H23B 109.5 . . ?
H23A C237 H23C 109.5 . . ?
H23B C237 H23C 109.5 . . ?
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
Sb1 O11 1.977(7) . ?
Sb1 O12 2.049(6) . ?
Sb1 C111 2.147(10) . ?
Sb1 C121 2.114(9) . ?
Sb1 C131 2.111(9) . ?
O11 C1 1.431(12) . ?
O12 C2 1.402(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.526(15) . ?
C2 H2 1.0000 . ?
C2 C3 1.528(15) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C111 C112 1.393(14) . ?
C111 C116 1.417(13) . ?
C112 H112 0.9500 . ?
C112 C113 1.385(14) . ?
C113 H113 0.9500 . ?
C113 C114 1.382(16) . ?
C114 C115 1.371(15) . ?
C114 C117 1.512(14) . ?
C115 H115 0.9500 . ?
C115 C116 1.413(14) . ?
C116 H116 0.9500 . ?
C117 H11A 0.9800 . ?
C117 H11B 0.9800 . ?
C117 H11C 0.9800 . ?
C121 C122 1.392(13) . ?
C121 C126 1.397(14) . ?
C122 H122 0.9500 . ?
C122 C123 1.395(12) . ?
C123 H123 0.9500 . ?
C123 C124 1.387(13) . ?
C124 C125 1.390(13) . ?
C124 C127 1.522(12) . ?
C125 H125 0.9500 . ?
C125 C126 1.390(13) . ?
C126 H126 0.9500 . ?
C127 H12A 0.9800 . ?
C127 H12B 0.9800 . ?
C127 H12C 0.9800 . ?
C131 C132 1.396(14) . ?
C131 C136 1.392(13) . ?
C132 H132 0.9500 . ?
C132 C133 1.407(13) . ?
C133 H133 0.9500 . ?
C133 C134 1.388(13) . ?
C134 C135 1.404(14) . ?
C134 C137 1.515(13) . ?
C135 H135 0.9500 . ?
C135 C136 1.382(13) . ?
C136 H136 0.9500 . ?
C137 H13A 0.9800 . ?
C137 H13B 0.9800 . ?
C137 H13C 0.9800 . ?
Sb2 O21 1.980(7) . ?
Sb2 O22 2.055(6) . ?
Sb2 C211 2.175(9) . ?
Sb2 C221 2.113(9) . ?
Sb2 C231 2.123(8) . ?
O21 C4 1.421(13) . ?
O22 C5 1.423(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.521(15) . ?
C5 H5 1.0000 . ?
C5 C6 1.502(15) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C211 C212 1.387(14) . ?
C211 C216 1.397(13) . ?
C212 H212 0.9500 . ?
C212 C213 1.396(15) . ?
C213 H213 0.9500 . ?
C213 C214 1.391(17) . ?
C214 C215 1.395(15) . ?
C214 C217 1.502(14) . ?
C215 H215 0.9500 . ?
C215 C216 1.407(13) . ?
C216 H216 0.9500 . ?
C217 H21A 0.9800 . ?
C217 H21B 0.9800 . ?
C217 H21C 0.9800 . ?
C221 C222 1.393(13) . ?
C221 C226 1.382(13) . ?
C222 H222 0.9500 . ?
C222 C223 1.398(14) . ?
C223 H223 0.9500 . ?
C223 C224 1.378(14) . ?
C224 C225 1.405(13) . ?
C224 C227 1.511(14) . ?
C225 H225 0.9500 . ?
C225 C226 1.402(14) . ?
C226 H226 0.9500 . ?
C227 H22A 0.9800 . ?
C227 H22B 0.9800 . ?
C227 H22C 0.9800 . ?
C231 C232 1.405(14) . ?
C231 C236 1.386(13) . ?
C232 H232 0.9500 . ?
C232 C233 1.384(13) . ?
C233 H233 0.9500 . ?
C233 C234 1.380(14) . ?
C234 C235 1.395(14) . ?
C234 C237 1.515(12) . ?
C235 H235 0.9500 . ?
C235 C236 1.388(14) . ?
C236 H236 0.9500 . ?
C237 H23A 0.9800 . ?
C237 H23B 0.9800 . ?
C237 H23C 0.9800 . ?
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
Sb1 O11 C1 C2 -19.2(10) . . . . ?
Sb1 O12 C2 C1 -42.3(9) . . . . ?
Sb1 O12 C2 C3 -165.1(7) . . . . ?
Sb1 C111 C112 C113 178.6(7) . . . . ?
Sb1 C111 C116 C115 -179.9(6) . . . . ?
Sb1 C121 C122 C123 178.1(7) . . . . ?
Sb1 C121 C126 C125 179.8(8) . . . . ?
Sb1 C131 C132 C133 174.9(7) . . . . ?
Sb1 C131 C136 C135 -173.8(7) . . . . ?
O11 C1 C2 O12 40.4(11) . . . . ?
O11 C1 C2 C3 162.9(8) . . . . ?
C111 C112 C113 C114 1.0(16) . . . . ?
C112 C111 C116 C115 0.4(13) . . . . ?
C112 C113 C114 C115 1.2(15) . . . . ?
C112 C113 C114 C117 178.7(9) . . . . ?
C113 C114 C115 C116 -2.6(14) . . . . ?
C114 C115 C116 C111 1.8(13) . . . . ?
C116 C111 C112 C113 -1.8(15) . . . . ?
C117 C114 C115 C116 180.0(9) . . . . ?
C121 C122 C123 C124 1.4(15) . . . . ?
C122 C121 C126 C125 -1.8(15) . . . . ?
C122 C123 C124 C125 -0.4(15) . . . . ?
C122 C123 C124 C127 176.7(9) . . . . ?
C123 C124 C125 C126 -1.7(15) . . . . ?
C124 C125 C126 C121 2.8(15) . . . . ?
C126 C121 C122 C123 -0.3(14) . . . . ?
C127 C124 C125 C126 -178.8(9) . . . . ?
C131 C132 C133 C134 -1.8(14) . . . . ?
C132 C131 C136 C135 1.6(14) . . . . ?
C132 C133 C134 C135 2.6(14) . . . . ?
C132 C133 C134 C137 -177.0(9) . . . . ?
C133 C134 C135 C136 -1.4(14) . . . . ?
C134 C135 C136 C131 -0.7(15) . . . . ?
C136 C131 C132 C133 -0.3(13) . . . . ?
C137 C134 C135 C136 178.2(9) . . . . ?
Sb2 O21 C4 C5 -25.0(10) . . . . ?
Sb2 O22 C5 C4 -43.9(8) . . . . ?
Sb2 O22 C5 C6 -168.6(6) . . . . ?
Sb2 C211 C212 C213 -179.2(7) . . . . ?
Sb2 C211 C216 C215 178.9(6) . . . . ?
Sb2 C221 C222 C223 170.8(7) . . . . ?
Sb2 C221 C226 C225 -171.7(7) . . . . ?
Sb2 C231 C232 C233 -179.0(8) . . . . ?
Sb2 C231 C236 C235 179.2(8) . . . . ?
O21 C4 C5 O22 45.6(11) . . . . ?
O21 C4 C5 C6 167.4(9) . . . . ?
C211 C212 C213 C214 -0.5(15) . . . . ?
C212 C211 C216 C215 -0.8(13) . . . . ?
C212 C213 C214 C215 0.7(14) . . . . ?
C212 C213 C214 C217 -177.9(9) . . . . ?
C213 C214 C215 C216 -1.0(13) . . . . ?
C214 C215 C216 C211 1.1(13) . . . . ?
C216 C211 C212 C213 0.5(14) . . . . ?
C217 C214 C215 C216 177.6(9) . . . . ?
C221 C222 C223 C224 -0.2(15) . . . . ?
C222 C221 C226 C225 1.5(14) . . . . ?
C222 C223 C224 C225 3.7(15) . . . . ?
C222 C223 C224 C227 -176.0(10) . . . . ?
C223 C224 C225 C226 -4.6(14) . . . . ?
C224 C225 C226 C221 2.0(14) . . . . ?
C226 C221 C222 C223 -2.5(14) . . . . ?
C227 C224 C225 C226 175.2(9) . . . . ?
C231 C232 C233 C234 -0.7(16) . . . . ?
C232 C231 C236 C235 -2.6(16) . . . . ?
C232 C233 C234 C235 -1.5(16) . . . . ?
C232 C233 C234 C237 178.7(10) . . . . ?
C233 C234 C235 C236 1.7(16) . . . . ?
C234 C235 C236 C231 0.4(17) . . . . ?
C236 C231 C232 C233 2.7(16) . . . . ?
C237 C234 C235 C236 -178.6(10) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.999(13)
2 0.001(13)
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
-2.0070 -1.9862 -1.0123 0.0404 0.2256 -0.1801
0.9983 -0.9989 0.0001 -0.1102 0.0564 0.0619
-0.9983 0.9989 -0.0001 0.1102 -0.0564 -0.0619
-1.9976 0.9926 -2.0041 0.0885 -0.0521 -0.2690
1.9976 -0.9926 2.0041 -0.0885 0.0521 0.2690
-0.0010 -1.0053 -2.0039 -0.1318 0.0606 -0.1452
0.0010 1.0053 2.0039 0.1318 -0.0606 0.1452
1.9988 1.9973 -1.0036 -0.1388 -0.2547 0.0285
0.9987 -0.9932 2.0044 -0.0111 0.0841 0.2122
1.0001 1.9996 -0.0012 -0.0119 -0.2088 0.0468
1.0003 2.0025 1.0010 0.0376 -0.1949 0.1219
-0.0006 -0.9995 0.0004 -0.0328 0.0884 0.0050
-0.9985 0.0052 2.0046 0.1764 0.0598 0.0934
-0.0010 -1.9962 1.0030 -0.0160 0.1907 0.0852
-0.9999 -1.9967 1.0033 0.0614 0.2227 0.0284
