Donor-Stabilized Antimony(I) and Bismuth(I) Ions: Heavier Valence Isoelectronic Analogues of Carbones.
Siddiqui, Mujahuddin M.; Sarkar, Samir Kumar; Nazish, Mohd; Morganti, Massimiliano; Köhler, Christian; Cai, Jiali; Zhao, Lili; Herbst-Irmer, Regine; Stalke, Dietmar; Frenking, Gernot; Roesky, Herbert W.; Journal of the American Chemical Society 143 (2021) 1301–1306; doi:10.1021/jacs.0c12084

data_4135610
_publ_section_title
;
 Donor-Stabilized Antimony(I) and Bismuth(I) Ions: Heavier Valence
 Isoelectronic Analogues of Carbones.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1301
_journal_page_last               1306
_journal_paper_doi               10.1021/jacs.0c12084
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         '(C40 H62 N2 Sb), (C F3 O3 S), 0.5 (C7 H8)'
_chemical_formula_sum            'C44.5 H66 F3 N2 O3 S Sb'
_chemical_formula_weight         887.80
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.02(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.189(2)
_cell_length_b                   15.330(2)
_cell_length_c                   32.284(4)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.075
_cell_measurement_theta_min      2.2845
_cell_volume                     4544.9(13)
_computing_cell_refinement       'SAINT V8.40A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.40A'
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_computing_publication_material  'XP Version 5.1'
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_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            80806
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.154
_diffrn_reflns_theta_min         1.262
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       needle
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.704
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         10055
_refine_ls_number_restraints     2052
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+4.0600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8433
_reflns_number_total             10055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c12084_si_003.cif
_cod_data_source_block           gross2klein
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C44.50 H66 F3 N2 O3 S Sb'
_cod_database_code               4135610
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              62470
_shelx_hkl_checksum              75751