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_7709337
_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         'C46 H41 O P Si2'
_chemical_formula_sum            'C46 H41 O P Si2'
_chemical_formula_weight         696.98
_chemical_melting_point          602
_chemical_name_systematic
(E)-(mesityl((triphenylsilyl)oxy)methylene)(triphenylsilyl)phosphane
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8439(2)
_cell_length_b                   17.8101(3)
_cell_length_c                   21.7832(4)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.40
_cell_measurement_theta_min      3.20
_cell_volume                     3819.05(12)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62386
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.588
_diffrn_reflns_theta_min         3.205
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6255
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 2962 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0409P)^2^+0.9715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7041
_reflns_number_total             7558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04223h2.cif
_cod_data_source_block           glc2117_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            'C9.68 H8.63 O0.21 P0.21 Si0.42'
_cod_original_formula_weight         146.72
_cod_original_formula_moiety         '0.21(C46 H41 O P Si2)'
_cod_original_formula_units_Z            19
_cod_database_code               7709337
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.744
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C40(H40), C36(H36), C5(H5), C32(H32), C24(H24), C7(H7),
 C46(H46), C37(H37), C12(H12), C14(H14), C30(H30), C42(H42), C39(H39), C31(H31),
  C28(H28), C45(H45), C34(H34), C33(H33), C38(H38), C20(H20), C19(H19),
 C15(H15), C25(H25), C44(H44), C27(H27), C22(H22), C43(H43), C26(H26), C21(H21),
  C13(H13)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              65026
_shelx_hkl_checksum              32563
_olex2_submission_special_instructions 'No special instructions were received'