Synthesis of polyantimony ligand complexes starting from Cp*4Sb4
Heinl, Veronika; Balázs, Gábor; Seidl, Michael; Scheer, Manfred; Chemical Communications  (2022) –; doi:10.1039/D1CC06770B

data_7129633
_publ_section_title
;
 Synthesis of polyantimony ligand complexes starting from Cp*4Sb4
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06770B
_journal_year                    2022
_chemical_formula_moiety         'C60 H84 Fe4 O8 Sb4, C2 H3 N'
_chemical_formula_sum            'C62 H87 Fe4 N O8 Sb4'
_chemical_formula_weight         1684.72
_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
_audit_creation_date             2021-08-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2022-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                88.540(2)
_cell_angle_beta                 85.7954(18)
_cell_angle_gamma                75.637(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2505(2)
_cell_length_b                   18.2944(5)
_cell_length_c                   18.7216(4)
_cell_measurement_reflns_used    16621
_cell_measurement_temperature    123.00(13)
_cell_measurement_theta_max      70.0870
_cell_measurement_theta_min      3.9760
_cell_volume                     3391.82(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.939
_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  26.00   1.00   15.00    --  -44.33  38.00-150.00   76
  2  \w    -25.00  68.00   1.00   15.00    --   44.33 -57.00 -90.00   93
  3  \w     20.00 114.00   1.00   15.00    --   44.33  57.00  60.00   94
  4  \w     21.00 125.00   1.00   60.00    --   95.48 -15.00  30.00  104
  5  \w     25.00  80.00   1.00   60.00    --   95.48 -30.00 120.00   55
  6  \w     14.00 109.00   1.00   60.00    --   95.48 -94.00   0.00   95
  7  \w     24.00  91.00   1.00   60.00    --   95.48 -30.00-150.00   67
  8  \w     32.00 109.00   1.00   60.00    --   95.48 -94.00-120.00   77
  9  \w     82.00 163.00   1.00   60.00    --   95.48  45.00  30.00   81
 10  \w     24.00 126.00   1.00   60.00    --   95.48 -77.00  60.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0100929000
_diffrn_orient_matrix_UB_12      0.0718652000
_diffrn_orient_matrix_UB_13      0.0173036000
_diffrn_orient_matrix_UB_21      -0.1234271000
_diffrn_orient_matrix_UB_22      0.0311681000
_diffrn_orient_matrix_UB_23      -0.0285957000
_diffrn_orient_matrix_UB_31      -0.0664464000
_diffrn_orient_matrix_UB_32      -0.0059484000
_diffrn_orient_matrix_UB_33      0.0666567000
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27519
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         70.024
_diffrn_reflns_theta_min         3.093
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.588
_exptl_absorpt_correction_T_max  0.477
_exptl_absorpt_correction_T_min  0.177
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       plate
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.101
_refine_diff_density_max         2.524
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         16401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0701P)^2^+2.4807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15071
_reflns_number_total             16401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06770b2.cif
_cod_data_source_block           heve209_b_ap_abs_gaus
_cod_original_cell_volume        3391.80(15)
_cod_database_code               7129633
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C62H87Fe4NO8Sb4
_shelx_estimated_absorpt_t_max   0.320
_shelx_estimated_absorpt_t_min   0.138
_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:
 C19(H19), C4(H4), C21(H21), C37(H37), C6(H6), C36(H36), C49(H49), C22(H22),
 C7(H7), C34(H34), C51(H51), C52(H52)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C62(H62A,H62B,H62C), C14(H14A,H14B,
 H14C), C13(H13A,H13B,H13C), C30(H30A,H30B,H30C), C11(H11A,H11B,H11C), C24(H24A,
 H24B,H24C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C10(H10A,H10B,H10C),
 C41(H41A,H41B,H41C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C), C44(H44A,H44B,H44C),
  C39(H39A,H39B,H39C), C55(H55A,H55B,H55C), C40(H40A,H40B,H40C), C43(H43A,H43B,
 H43C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C45(H45A,
 H45B,H45C), C60(H60A,H60B,H60C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              66223
_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 2.239
_oxdiff_exptl_absorpt_empirical_full_min 0.550