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

data_1563610
_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 Ni4 Sb4, C17 H29 Ni0.5'
_chemical_formula_sum            'C85 H145 Ni4.5 Sb4'
_chemical_formula_weight         1918.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 92.226(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   46.3369(13)
_cell_length_b                   19.0535(5)
_cell_length_c                   19.5836(6)
_cell_measurement_reflns_used    12138
_cell_measurement_temperature    122.97(13)
_cell_measurement_theta_max      73.4950
_cell_measurement_theta_min      3.6320
_cell_volume                     17276.9(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      122.97(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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      2.00  98.00   1.00   45.00    --   41.73-125.00 -90.00   96
  2  \w     17.00 116.00   1.00   45.00    --   41.73  37.00 150.00   99
  3  \w     30.00  69.00   1.00  180.00    --  106.46 -30.00  30.00   39
  4  \w     30.00  69.00   1.00  180.00    --  106.46 -30.00  60.00   39
  5  \w     73.00 158.00   1.00  180.00    --  106.46 125.00-180.00   85
  6  \w     30.00 139.00   1.00  180.00    --  106.46 -77.00 150.00  109
  7  \w     30.00  69.00   1.00  180.00    --  106.46 -30.00 120.00   39
  8  \w     77.00 158.00   1.00  180.00    --  106.46  61.00 -60.00   81
  9  \w     78.00 158.00   1.00  180.00    --  106.46  30.00 -90.00   80
 10  \w      9.00 118.00   1.00   45.00    --   41.73  77.00-120.00  109
 11  \w     14.00 115.00   1.00   45.00    --   41.73  57.00  30.00  101
 12  \w     30.00  69.00   1.00  180.00    --  106.46 -30.00 -90.00   39
 13  \w     54.00 142.00   1.00  180.00    --  106.46  15.00 120.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0062126000
_diffrn_orient_matrix_UB_12      0.0114039000
_diffrn_orient_matrix_UB_13      0.0770313000
_diffrn_orient_matrix_UB_21      0.0211241000
_diffrn_orient_matrix_UB_22      0.0596404000
_diffrn_orient_matrix_UB_23      -0.0161011000
_diffrn_orient_matrix_UB_31      -0.0249602000
_diffrn_orient_matrix_UB_32      0.0533755000
_diffrn_orient_matrix_UB_33      0.0015181000
_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  0.0569
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47158
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.350
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.074
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             7880
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         15359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12426
_reflns_number_total             15359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02498a2.cif
_cod_data_source_block           mc_abs
_cod_original_formula_sum        'C85 H145 Ni4.50 Sb4'
_cod_database_code               1563610
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C85H145Ni4.5Sb4
_reflns_odcompleteness_completeness 99.36
_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.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C35(H35), C52(H52), C55(H55), C21(H21), C4(H4), C1(H1), C38(H38),
 C72(H72), C69(H69)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C66(H66A,H66B,H66C), C17(H17A,H17B,H17C), C33(H33A,H33B,
 H33C), C67(H67A,H67B,H67C), C59(H59A,H59B,H59C), C32(H32A,H32B,H32C), C64(H64A,
 H64B,H64C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C16(H16A,H16B,H16C),
 C34(H34A,H34B,H34C), C45(H45A,H45B,H45C), C58(H58A,H58B,H58C), C60(H60A,H60B,
 H60C), C68(H68A,H68B,H68C), C76(H76A,H76B,H76C), C75(H75A,H75B,H75C), C42(H42A,
 H42B,H42C), C29(H29A,H29B,H29C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C),
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C13(H13A,H13B,H13C), C84(H84A,H84B,H84C), C7(H7A,H7B,H7C), C62(H62A,H62B,H62C),
  C50(H50A,H50B,H50C), C28(H28A,H28B,H28C), C79(H79A,H79B,H79C), C77(H77A,H77B,
 H77C), C63(H63A,H63B,H63C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C30(H30A,
 H30B,H30C), C11(H11A,H11B,H11C), C49(H49A,H49B,H49C), C80(H80A,H80B,H80C),
 C51(H51A,H51B,H51C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C85(H85A,H85B,
 H85C)
;
_shelx_res_checksum              29492
_shelx_hkl_checksum              3521
_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 1.691
_oxdiff_exptl_absorpt_empirical_full_min 0.463