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_7700305
_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         'C37 H30 As Cl2 P2, Cl4 Ga'
_chemical_formula_sum            'C37 H30 As Cl6 Ga P2'
_chemical_formula_weight         893.89
_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     dual
_audit_creation_date             2019-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-04 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                67.318(7)
_cell_angle_beta                 72.364(7)
_cell_angle_gamma                89.533(7)
_cell_formula_units_Z            2
_cell_length_a                   10.7120(9)
_cell_length_b                   12.9281(12)
_cell_length_c                   15.1481(13)
_cell_measurement_reflns_used    16700
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      1.48
_cell_volume                     1830.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16235
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.541
_exptl_absorpt_coefficient_mu    2.202
_exptl_absorpt_correction_T_max  0.5883
_exptl_absorpt_correction_T_min  0.4082
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'STOE LANA'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_recrystallization_method
'crystallization from toluene at ambient temperature'
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.085
_exptl_crystal_size_rad          0.092
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0535P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6567
_reflns_number_total             7982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01784d2.cif
_cod_data_source_block           '[3][GaCl4]_(CCDC_1908266)'
_cod_depositor_comments
'Adding full bibliography for 7700302--7700307.cif.'
_cod_database_code               7700305
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C13(H13), C21(H21), C27(H27), C31(H31), C19(H19), C36(H36), C3(H3),
 C12(H12), C33(H33), C30(H30), C23(H23), C7(H7), C24(H24), C22(H22), C28(H28),
 C35(H35), C29(H29), C25(H25), C34(H34), C15(H15), C16(H16), C5(H5), C9(H9),
 C17(H17), C18(H18), C6(H6), C10(H10), C4(H4), C11(H11)
;
_shelx_res_checksum              29979
_olex2_submission_special_instructions 'No special instructions were received'