Simple conversion of trisodium phosphide, Na3P, into silyl- and cyanophosphides and structure of a terminal silver phosphide
Grützmacher, Hansjörg; Le Corre, Grégoire; Dalton Transactions  (2022) –; doi:10.1039/D1DT04223H

data_7709339
_publ_section_title
;
 Simple conversion of trisodium phosphide, Na3P, into silyl- and
 cyanophosphides and structure of a terminal silver phosphide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04223H
_journal_year                    2022
_chemical_formula_moiety         'C24 H20 P, Cl6 P Si2'
_chemical_formula_sum            'C24 H20 Cl6 P2 Si2'
_chemical_formula_weight         639.24
_chemical_melting_point          413
_chemical_name_systematic
'Bis(trichlorosilyl)phoshanide tetraphenylphosphonium salt'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-06 deposited with the CCDC.	2022-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.5010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2251(5)
_cell_length_b                   14.2041(5)
_cell_length_c                   15.3777(5)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.36
_cell_volume                     2840.33(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            68524
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.074
_diffrn_reflns_theta_min         2.357
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0770 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.9020. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         8192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0201P)^2^+3.3189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6271
_reflns_number_total             8192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04223h2.cif
_cod_data_source_block           glc20963_0m
_cod_depositor_comments
;

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C1.81 H1.51 Cl0.45 P0.15 Si0.15'
_cod_original_formula_weight         48.24
_cod_original_formula_moiety         '0.08(C24 H20 P), 0.08(Cl6 P Si2)'
_cod_original_formula_units_Z            53
_cod_database_code               7709339
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.841
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C0F(H0F), C0G(H0G), C0H(H0H), C0I(H0I), C0J(H0J), C0K(H0K), C0L(H0L),
 C0M(H0M), C0N(H0N), C0O(H0O), C0P(H0P), C0Q(H0Q), C0R(H0R), C0S(H0S), C0T(H0T),
  C0U(H0U), C0V(H0V), C0W(H0W), C0X(H0X), C0Y(H0Y)
;
_shelx_res_checksum              90426
_shelx_hkl_checksum              49131
_olex2_submission_special_instructions 'No special instructions were received'