Bisstibane−Distibane conversion via consecutive single-electron oxidation and reduction reaction
Gehlhaar, Alexander; Weinert, Hanns Micha; Wölper, Christoph; Semleit, Nina; Haberhauer, Gebhard; Schulz, Stephan; Chemical Communications  (2022) –; doi:10.1039/D2CC01986H

data_7130088
_publ_section_title
;
 Bisstibane&#x2212;Distibane conversion via consecutive single-electron
 oxidation and reduction reaction
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01986H
_journal_year                    2022
_chemical_formula_sum            'C79 H75 B F20 Sb2'
_chemical_formula_weight         1658.70
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-03-09 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                82.723(8)
_cell_angle_beta                 80.545(8)
_cell_angle_gamma                78.391(8)
_cell_formula_units_Z            2
_cell_length_a                   14.118(3)
_cell_length_b                   15.623(3)
_cell_length_c                   17.104(3)
_cell_measurement_reflns_used    9141
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.46
_cell_measurement_theta_min      2.81
_cell_volume                     3628.0(12)
_computing_cell_refinement       'BRUKER APEX3(v2019.1-0)'
_computing_data_collection       'BRUKER APEX3(v2019.1-0)'
_computing_data_reduction        'BRUKER APEX3(v2019.1-0)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'BRUKER APEX3(v2019.1-0)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker D8 KAPPA II (APEX II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/QUEEN'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            230758
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.920
_diffrn_reflns_theta_min         1.780
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.417
_exptl_crystal_size_min          0.250
_refine_diff_density_max         2.988
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         28346
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0153P)^2^+4.4685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24467
_reflns_number_total             28346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01986h2.cif
_cod_data_source_block           alf_121_dm
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        3627.9(12)
_cod_database_code               7130088
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.715
_shelx_estimated_absorpt_t_max   0.818
_shelx_res_checksum              8895
_shelx_hkl_checksum              85667