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

data_1563607
_publ_section_title
;
 Transfer of Polyantimony Units
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02498A
_journal_year                    2021
_chemical_formula_moiety         'C68 H116 Co4 Sb4'
_chemical_formula_sum            'C68 H116 Co4 Sb4'
_chemical_formula_weight         1656.32
_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_Hall           'P 62 2 (0 0 4)'
_space_group_name_H-M_alt        'P 62 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-23 deposited with the CCDC.	2021-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.0892(8)
_cell_length_b                   13.0892(8)
_cell_length_c                   36.0383(18)
_cell_measurement_reflns_used    6280
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      72.5100
_cell_measurement_theta_min      4.5880
_cell_volume                     5347.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5096
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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      5.00 121.00   0.50   30.00    --   39.65  77.00-180.00  232
  2  \w     73.00 178.00   0.50  100.00    --  107.66  77.00   0.00  210
  3  \w     73.00 178.00   0.50  100.00    --  107.66  77.00 -90.00  210
  4  \w     73.00 178.00   0.50  100.00    --  107.66  77.00 -30.00  210
  5  \w     73.00 178.00   0.50  100.00    --  107.66  77.00 -60.00  210
  6  \w    -98.00 -18.00   0.50   30.00    --  -39.65 125.00 -60.00  160
  7  \w      9.00 116.00   0.50   30.00    --   39.65  57.00  60.00  214
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1081830000
_diffrn_orient_matrix_UB_12      0.1045376000
_diffrn_orient_matrix_UB_13      0.0181064000
_diffrn_orient_matrix_UB_21      -0.0387320000
_diffrn_orient_matrix_UB_22      -0.0603895000
_diffrn_orient_matrix_UB_23      0.0381243000
_diffrn_orient_matrix_UB_31      0.0723694000
_diffrn_orient_matrix_UB_32      -0.0621020000
_diffrn_orient_matrix_UB_33      -0.0066621000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            19596
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.933
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.176
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.37b (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.722
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 1075 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.041(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3543
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0468
_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/[\s^2^(Fo^2^)+(0.0392P)^2^+28.1951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.630
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3117
_reflns_number_total             3543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02498a2.cif
_cod_data_source_block           heve124_2_abs
_cod_original_cell_volume        5347.1(7)
_cod_original_sg_symbol_Hall     'P 62 2c (0 0 1)'
_cod_database_code               1563607
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C52H84Sb4Co4
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C8A-C6 \\sim C8B-C6 \\sim C9A-C6 \\sim C9B-C6 \\sim C7B-C6 \\sim C7A-C6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C9A \\sim C9B \\sim C6 \\sim C7A \\sim C7B \\sim C8B \\sim C8A: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
4. Others
 Fixed Sof: C8A(0.72) H8AA(0.72) H8AB(0.72) H8AC(0.72) C7A(0.72) H7AA(0.72)
 H7AB(0.72) H7AC(0.72) C9A(0.72) H9AA(0.72) H9AB(0.72) H9AC(0.72) C9B(0.28)
 H9BA(0.28) H9BB(0.28) H9BC(0.28) C8B(0.28) H8BA(0.28) H8BB(0.28) H8BC(0.28)
 C7B(0.28) H7BA(0.28) H7BB(0.28) H7BC(0.28)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C8A(H8AA,H8AB,
 H8AC), C7A(H7AA,H7AB,H7AC), C9A(H9AA,H9AB,H9AC), C17(H17A,H17B,H17C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C9B(H9BA,H9BB,H9BC), C8B(H8BA,H8BB,H8BC),
 C7B(H7BA,H7BB,H7BC)
;
_shelx_res_checksum              28918
_shelx_hkl_checksum              56774
_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 1.754
_oxdiff_exptl_absorpt_empirical_full_min 0.760