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_7700302
_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         '[PCl~2~(C{PPh~3~})]Cl'
_chemical_formula_sum            'C37 H30 Cl3 P3'
_chemical_formula_weight         673.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                72.67(1)
_cell_angle_beta                 73.44(1)
_cell_angle_gamma                65.28(1)
_cell_formula_units_Z            2
_cell_length_a                   10.687(1)
_cell_length_b                   11.378(1)
_cell_length_c                   15.429(1)
_cell_measurement_reflns_used    158
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      7.9
_cell_volume                     1598.7(3)
_computing_cell_refinement       'SAINT (Bruker)'
_computing_data_collection       'APEX2 (Bruker)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_publication_material  'WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2015 (Sheldrick, 2015)'
_computing_structure_solution
;
 SIR-92 (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla, Polidori,
        Camalli, 1992)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'D8 QUEST (Bruker)'
_diffrn_measurement_method       'APEX2 (Bruker)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            80804
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.183
_diffrn_reflns_theta_min         2.207
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       plates
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   1.0
_exptl_transmission_factor_min   0.97
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.9913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6414
_reflns_number_total             7085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01784d2.cif
_cod_data_source_block           '[1]Cl_(CCDC_1908265)'
_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_database_code               7700302
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.87
_shelx_estimated_absorpt_t_max   0.91
_shelx_res_checksum              73381