Metal-coordinated distibene and dibismuthene dications - isoelectronic analogues of butadiene dications.
Weinert, Hanns M.; Schulte, Yannick; Gehlhaar, Alexander; Wölper, Christoph; Haberhauer, Gebhard; Schulz, Stephan; Chemical communications (Cambridge, England) 59 (2023) 7755–7758; doi:10.1039/d3cc01844j

data_7131816
_publ_section_title
;
 Metal-coordinated distibene and dibismuthene dications - isoelectronic
 analogues of butadiene dications.
;
_journal_issue                   50
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7755
_journal_page_last               7758
_journal_paper_doi               10.1039/d3cc01844j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_sum            'C73 H102 Bi F3 Ga2 N8 O3 S'
_chemical_formula_weight         1577.10
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-05-09 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.813(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8030(14)
_cell_length_b                   27.401(3)
_cell_length_c                   26.932(3)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      2.36
_cell_volume                     9360.4(18)
_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 0.996
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            338101
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.679
_diffrn_reflns_theta_min         1.671
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.515
_exptl_absorpt_correction_T_max  0.39
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Blessing, Acta Cryst 1995 A51 33-38'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       prism
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.067
_refine_diff_density_max         2.788
_refine_diff_density_min         -4.260
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         28923
_refine_ls_number_restraints     316
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0295P)^2^+14.1716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20074
_reflns_number_total             28923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01844j2.cif
_cod_data_source_block           mw_149_2m_sq
_cod_original_cell_volume        9360.5(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7131816
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.539
_shelx_estimated_absorpt_t_max   0.850
_exptl_absorpt_special_details
;
 Crystal faces:

     H       K       L      d(mm)

   1.000   0.000   0.000   0.02100
   1.000   1.000  -1.000   0.02400
  -1.000  -1.000  -1.000   0.11400
   0.000   0.000  -1.000   0.01800
   0.000   0.000   1.000   0.04800
   0.000   1.000   1.000   0.03300
   0.000  -1.000  -1.000   0.01500
   0.000  -1.000   1.000   0.06700
   0.000   1.000  -1.000   0.01200
  -1.000   0.000   1.000   0.12900
  -1.000   2.000  -1.000   0.08400
   1.000  -2.000   1.000   0.04200
;
_shelx_res_checksum              21740
_shelx_fab_checksum              60713