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_4349250
_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(C36 H30 N P2 +), C6 Bi N6 3-'
_chemical_formula_sum            'C114 H90 Bi N9 P6'
_chemical_formula_weight         1980.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0495(7)
_cell_length_b                   20.7536(8)
_cell_length_c                   24.2348(8)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.22
_cell_volume                     9581.1(6)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1085
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            184982
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.654
_diffrn_reflns_theta_min         0.840
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_refine_diff_density_max         2.555
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 10027 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         37800
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                25633
_reflns_number_total             37800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02174_si_002.cif
_cod_data_source_block           av_as969_475_PNP_3_BiCN6
_cod_database_code               4349250
_shelx_estimated_absorpt_t_min   0.615
_shelx_estimated_absorpt_t_max   0.841
_shelxl_version_number           2013-4
_shelx_res_checksum              31555
_shelx_hkl_checksum              40830