Heavy Group 15 Element Compounds of a Sterically Demanding Bis(iminophosphorane)methanide and -methanediide
Sindlinger, Christian P.; Stasch, Andreas; Wesemann, Lars; Organometallics 33 (2014) 322–; doi:10.1021/om401059x

data_4082527
_publ_section_title
;
 Heavy Group 15 Element Compounds of a Sterically Demanding
 Bis(iminophosphorane)methanide and -methanediide
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              322
_journal_paper_doi               10.1021/om401059x
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C52 H62 Bi Cl2 N2 P2'
_chemical_formula_weight         1056.86
_chemical_name_common            L2BiCl2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.4740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0435(5)
_cell_length_b                   17.7779(8)
_cell_length_c                   23.3800(10)
_cell_measurement_reflns_used    597
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      31.5125
_cell_measurement_theta_min      2.0977
_cell_volume                     4847.0(4)
_computing_cell_refinement       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40518
_diffrn_reflns_theta_full        27.25
_diffrn_reflns_theta_max         27.25
_diffrn_reflns_theta_min         1.75
_diffrn_source_type              'micro source'
_exptl_absorpt_coefficient_mu    3.850
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear light yellow-green'
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Bloc
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.331
_refine_diff_density_min         -1.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         10784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                8624
_reflns_number_total             10784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401059x_si_002.cif
_cod_data_source_block           I
_cod_database_code               4082527