Cyanido Antimonate(III) and Bismuthate(III) Anions.
Arlt, Sören; Harloff, Jörg; Schulz, Axel; Stoffers, Alrik; Villinger, Alexander; Inorganic chemistry 55 (2016) 12321–12328; doi:10.1021/acs.inorgchem.6b02174

data_4349247
_publ_section_title
;
 Cyanido Antimonate(III) and Bismuthate(III) Anions.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12321
_journal_page_last               12328
_journal_paper_doi               10.1021/acs.inorgchem.6b02174
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '3(C24 H20 P +), C6 Bi N6 3-'
_chemical_formula_sum            'C78 H60 Bi N6 P3'
_chemical_formula_weight         1383.21
_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_method           SHELXL-2013
_cell_angle_alpha                96.274(2)
_cell_angle_beta                 112.1270(10)
_cell_angle_gamma                109.475(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2170(5)
_cell_length_b                   15.1544(5)
_cell_length_c                   17.7507(5)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      2.54
_cell_volume                     3217.00(19)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            105722
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.206
_exptl_absorpt_coefficient_mu    2.865
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.6031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       prism
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         23100
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.4952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19481
_reflns_number_total             23100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02174_si_002.cif
_cod_data_source_block           av_as969293_PPh4_6_Bi2CN11_CN
_cod_database_code               4349247
_shelx_estimated_absorpt_t_min   0.470
_shelx_estimated_absorpt_t_max   0.657
_shelxl_version_number           2013-4
_shelx_res_checksum              83404
_shelx_hkl_checksum              37938