Hypervalent 5?Bi?12 derivatives containing dichalcogenoimidodiphosphinato ligands. Crystal structure and solution behaviour of [2-(Me2NCH2)C6H4]BiCl[(XPR2)(YPR?2)N] (X, Y = O, S, Se; R, R? = Me, Ph)
Balazs, Lucia; Stanga, Olimpiu; Breunig, Hans J.; Silvestru, Cristian; Dalton Transactions  (2003) 2237–; doi:10.1039/b301290e

data_7012802
_publ_section_title
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 Hypervalent 5?Bi?12 derivatives containing
 dichalcogenoimidodiphosphinato ligands. Crystal structure and solution
 behaviour of [2-(Me2NCH2)C6H4]BiCl[(XPR2)(YPR?2)N] (X, Y = O, S, Se;
 R, R? = Me, Ph)
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_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2237
_journal_paper_doi               10.1039/b301290e
_journal_year                    2003
_chemical_formula_sum            'C23 H28 Bi Cl N2 O P2 S'
_chemical_formula_weight         686.90
_chemical_name_systematic        ?
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.4890(10)
_cell_length_b                   19.2340(10)
_cell_length_c                   21.543(2)
_cell_measurement_reflns_used    89
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15.023
_cell_measurement_theta_min      2.319
_cell_volume                     5174.9(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7205
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.140
_exptl_absorpt_correction_T_max  0.240
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Walker & Stuart, 1983'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloks
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+7.5225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                3065
_reflns_number_total             5868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301290e.txt
_cod_data_source_block           cs7
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7012802