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

data_1563609
_publ_section_title
;
 Transfer of Polyantimony Units
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02498A
_journal_year                    2021
_chemical_formula_moiety         'C120 H105 Co3 Sb2, C7 H8'
_chemical_formula_sum            'C127 H113 Co3 Sb2'
_chemical_formula_weight         2059.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 91.1760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0588(2)
_cell_length_b                   19.7981(2)
_cell_length_c                   30.5084(4)
_cell_measurement_reflns_used    17388
_cell_measurement_temperature    128.5(3)
_cell_measurement_theta_max      74.3650
_cell_measurement_theta_min      3.0730
_cell_volume                     9697.6(2)
_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-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      128.5(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -50.00  27.00   1.00   20.00    --  -44.08  38.00 150.00   77
  2  \w   -116.00 -14.00   1.00   20.00    --  -44.08 -77.00-150.00  102
  3  \w     36.00  98.00   1.00   80.00    --  104.50 -45.00 -90.00   62
  4  \w     33.00 135.00   1.00   80.00    --  104.50 -77.00  90.00  102
  5  \w     38.00  98.00   1.00   80.00    --  104.50 -45.00  90.00   60
  6  \w     36.00  91.00   1.00   80.00    --  104.50 -45.00 -30.00   55
  7  \w     79.00 175.00   1.00   80.00    --  104.50  77.00-150.00   96
;
_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      -0.0134303000
_diffrn_orient_matrix_UB_12      0.0732681000
_diffrn_orient_matrix_UB_13      0.0153141000
_diffrn_orient_matrix_UB_21      0.0559437000
_diffrn_orient_matrix_UB_22      -0.0133436000
_diffrn_orient_matrix_UB_23      0.0406955000
_diffrn_orient_matrix_UB_31      0.0767788000
_diffrn_orient_matrix_UB_32      0.0225483000
_diffrn_orient_matrix_UB_33      -0.0257078000
_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  0.0252
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34451
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         2.661
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.690
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             4232
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.443
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         17148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0387P)^2^+6.9890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15212
_reflns_number_total             17148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02498a2.cif
_cod_data_source_block           sean349_block
_cod_database_code               1563609
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C127H113Co3Sb2
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.459
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C20(H20A,H20B), C114(H11A,H11B), C74(H74A,H74B), C34(H34A,
 H34B), C107(H10C,H10D), C13(H13A,H13B), C93(H93A,H93B), C67(H67A,H67B),
 C46(H46A,H46B), C27(H27A,H27B), C86(H86A,H86B), C60(H60A,H60B), C6(H6A,H6B),
 C53(H53A,H53B)
2.b Aromatic/amide H refined with riding coordinates:
 C70(H70), C69(H69), C55(H55), C12(H12), C106(H106), C26(H26), C19(H19),
 C71(H71), C73(H73), C99(H99), C80(H80), C104(H104), C36(H36), C22(H22),
 C105(H105), C62(H62), C49(H49), C102(H102), C48(H48), C52(H52), C76(H76),
 C56(H56), C72(H72), C66(H66), C57(H57), C88(H88), C95(H95), C50(H50),
 C126(H126), C125(H125), C109(H109), C15(H15), C113(H113), C79(H79), C120(H120),
  C30(H30), C59(H59), C97(H97), C123(H123), C96(H96), C33(H33), C29(H29),
 C11(H11), C92(H92), C89(H89), C32(H32), C124(H124), C31(H31), C127(H127),
 C23(H23), C58(H58), C119(H119), C103(H103), C8(H8), C116(H116), C37(H37),
 C51(H51), C98(H98), C78(H78), C25(H25), C118(H118), C40(H40), C65(H65),
 C112(H112), C39(H39), C63(H63), C24(H24), C18(H18), C64(H64), C77(H77),
 C110(H110), C9(H9), C90(H90), C111(H111), C117(H117), C38(H38), C10(H10),
 C91(H91), C17(H17), C16(H16)
2.c Idealised Me refined as rotating group:
 C121(H12A,H12B,H12C)
;
_shelx_res_checksum              62922
_shelx_hkl_checksum              90717
_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 1.367
_oxdiff_exptl_absorpt_empirical_full_min 0.807