Transfer of Polyantimony Units
Heinl, Veronika; Seitz, Andreas; Balazs, Gabor; Seidl, Michael; Scheer, Manfred; Chemical Science  (2021) –; doi:10.1039/D1SC02498A

data_1563608
_publ_section_title
;
 Transfer of Polyantimony Units
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02498A
_journal_year                    2021
_chemical_formula_moiety         'C51 H87 Fe3 Sb2'
_chemical_formula_sum            'C51 H87 Fe3 Sb2'
_chemical_formula_weight         1111.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.11 svn.r3635 for OlexSys, GUI svn.r5848)
;
_audit_update_record
;
2021-04-23 deposited with the CCDC.	2021-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                87.329(2)
_cell_angle_beta                 89.4550(10)
_cell_angle_gamma                88.3190(10)
_cell_formula_units_Z            4
_cell_length_a                   12.3188(2)
_cell_length_b                   20.5303(4)
_cell_length_c                   20.5490(4)
_cell_measurement_reflns_used    31529
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      70.0560
_cell_measurement_theta_min      3.8600
_cell_volume                     5188.97(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.3-alpha (Bourhis et al., 2015)'
_computing_structure_solution
'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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   -113.00 -18.00   0.50   30.00    --  -43.64 -57.00 120.00  190
  2  \w   -125.00 -79.00   0.50   30.00    --  -43.64 -99.00-120.00   92
  3  \w     11.00 121.00   0.50   30.00    --   43.64  19.00-150.00  220
  4  \w     22.00  91.00   0.50  100.00    --   95.48 -30.00-150.00  138
  5  \w     22.00  91.00   0.50  100.00    --   95.48 -30.00 -90.00  138
  6  \w     22.00  91.00   0.50  100.00    --   95.48 -30.00 150.00  138
  7  \w     69.00 169.00   0.50  100.00    --   95.48  30.00  60.00  200
  8  \w     25.00  98.00   0.50  100.00    --   95.48 -45.00 120.00  146
  9  \w     71.00 166.00   0.50  100.00    --   95.48  45.00 150.00  190
 10  \w     12.00  66.00   0.50   30.00    --   43.64  77.00 -60.00  108
 11  \w     74.00 133.00   0.50   30.00    --   43.64 178.00  60.00  118
 12  \w     37.00 111.00   0.50  100.00    --   95.79 -77.00   0.00  148
 13  \w     13.00  46.00   0.50  100.00    --   95.79 -95.00 120.00   66
 14  \w     61.00 109.00   0.50  100.00    --   95.79 -95.00 120.00   96
 15  \w     52.00 109.00   0.50  100.00    --   95.79 -95.00-120.00  114
 16  \w   -125.00-100.00   0.50   30.00    --  -43.64 -99.00 -90.00   50
 17  \w    -66.00 -39.00   0.50   30.00    --  -43.64 -57.00-150.00   54
 18  \w     27.00  53.00   0.50  100.00    --   95.79 -45.00  30.00   52
 19  \w     97.00 123.00   0.50  100.00    --   95.79 125.00-120.00   52
 20  \w     81.00 106.00   0.50  100.00    --   95.79-125.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0769743000
_diffrn_orient_matrix_UB_12      0.0106200000
_diffrn_orient_matrix_UB_13      -0.0488120000
_diffrn_orient_matrix_UB_21      0.0553219000
_diffrn_orient_matrix_UB_22      -0.0448293000
_diffrn_orient_matrix_UB_23      -0.0379189000
_diffrn_orient_matrix_UB_31      -0.0616443000
_diffrn_orient_matrix_UB_32      -0.0499011000
_diffrn_orient_matrix_UB_33      0.0279375000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52581
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         63.180
_diffrn_reflns_theta_min         3.733
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.336
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (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_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         22736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+1.6931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20653
_reflns_number_total             22736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02498a2.cif
_cod_data_source_block           heve177_2_abs2
_cod_database_code               1563608
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C102H174Sb4Fe6
_chemical_oxdiff_usercomment     'colourless block'
_shelx_estimated_absorpt_t_max   0.535
_shelx_estimated_absorpt_t_min   0.163
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.18
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C71(H71), C22(H22), C39(H39), C56(H56), C37(H37), C54(H54), C5(H5), C73(H73),
 C20(H20), C3(H3), C88(H88), C90(H90)
2.b Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C93(H93a,H93b,H93c), C24(H24a,H24b,H24c), C80(H80a,H80b,
 H80c), C25(H25a,H25b,H25c), C68(H68a,H68b,H68c), C79(H79a,H79b,H79c), C7(H7a,
 H7b,H7c), C30(H30a,H30b,H30c), C58(H58a,H58b,H58c), C32(H32a,H32b,H32c),
 C28(H28a,H28b,H28c), C51(H51a,H51b,H51c), C8(H8a,H8b,H8c), C81(H81a,H81b,H81c),
  C11(H11a,H11b,H11c), C43(H43a,H43b,H43c), C26(H26a,H26b,H26c), C98(H98a,H98b,
 H98c), C62(H62a,H62b,H62c), C59(H59a,H59b,H59c), C101(H10a,H10b,H10c),
 C34(H34a,H34b,H34c), C64(H64a,H64b,H64c), C76(H76a,H76b,H76c), C96(H96a,H96b,
 H96c), C84(H84a,H84b,H84c), C29(H29a,H29b,H29c), C46(H46a,H46b,H46c), C92(H92a,
 H92b,H92c), C67(H67a,H67b,H67c), C47(H47a,H47b,H47c), C77(H77a,H77b,H77c),
 C45(H45a,H45b,H45c), C94(H94a,H94b,H94c), C9(H9a,H9b,H9c), C63(H63a,H63b,H63c),
  C41(H41a,H41b,H41c), C12(H12a,H12b,H12c), C97(H97a,H97b,H97c), C42(H42a,H42b,
 H42c), C13(H13a,H13b,H13c), C83(H83a,H83b,H83c), C16(H16a,H16b,H16c), C75(H75a,
 H75b,H75c), C50(H50a,H50b,H50c), C49(H49a,H49b,H49c), C60(H60a,H60b,H60c),
 C66(H66a,H66b,H66c), C100(H10d,H10e,H10f), C17(H17a,H17b,H17c), C85(H85a,H85b,
 H85c), C15(H15a,H15b,H15c), C102(H10g,H10h,H10i)
;
_shelx_res_checksum              30014
_shelx_hkl_checksum              93948
_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 3.045
_oxdiff_exptl_absorpt_empirical_full_min 0.461