Hexaphenyl carbodiphosphorane adducts of heavier group 15 element trichlorides: syntheses, properties and reactivities.
Münzer, Jörn E; Kneusels, Nis-Julian H; Weinert, Bastian; Neumüller, Bernhard; Kuzu, Istemi; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11076–11085; doi:10.1039/c9dt01784d

data_7700303
_publ_section_title
;
 Hexaphenyl carbodiphosphorane adducts of heavier group 15 element
 trichlorides: syntheses, properties and reactivities.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11076
_journal_page_last               11085
_journal_paper_doi               10.1039/c9dt01784d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '[SbCl~3~(C{PPh~3~})]^.^0.5Et~2~'
_chemical_formula_sum            'C39 H35 Cl3 O0.5 P2 Sb'
_chemical_formula_weight         801.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-06-04 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.51(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.541(1)
_cell_length_b                   39.489(2)
_cell_length_c                   17.598(1)
_cell_measurement_reflns_used    6000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.6
_cell_volume                     7091.6(9)
_computing_cell_refinement       'IPDS II (Stoe)'
_computing_data_collection       'IPDS II (Stoe)'
_computing_data_reduction        'IPDS II (Stoe)'
_computing_publication_material  'WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'IPDS II (Stoe)'
_diffrn_measurement_method       'IPDS II (Stoe)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.1247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12046
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.884
_diffrn_reflns_theta_min         1.579
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'X-red32/X-area (Stoe)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       needles
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   0.76
_exptl_transmission_factor_min   0.49
_refine_diff_density_max         1.546
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 2845 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         12046
_refine_ls_number_restraints     725
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.983
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                8749
_reflns_number_total             12046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01784d2.cif
_cod_data_source_block           CCDC_1908267
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700302--7700307.cif.
;
_cod_original_formula_sum        'C39 H35 Cl3 O0.50 P2 Sb'
_cod_database_code               7700303
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              4189