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_7709340
_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 H51 Cu N3 P Si'
_chemical_formula_sum            'C46 H51 Cu N3 P Si'
_chemical_formula_weight         768.54
_chemical_melting_point          450
_chemical_name_systematic
Cyano(triphenylsilyl)phosphanido[1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene]copper(I)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-28
_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                   21.5909(6)
_cell_length_b                   10.7125(3)
_cell_length_c                   18.4005(4)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.19
_cell_volume                     4255.90(19)
_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 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            74787
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.735
_diffrn_reflns_theta_min         2.187
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 3706 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9020
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0160P)^2^+1.0676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0547
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                8290
_reflns_number_total             9020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04223h2.cif
_cod_data_source_block           cucn
_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 H10.74 Cu0.21 N0.63 P0.21 Si0.21'
_cod_original_formula_weight         161.79
_cod_original_formula_moiety         '0.21(C46 H51 Cu N3 P Si)'
_cod_original_formula_units_Z            19
_cod_database_code               7709340
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.823
_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 Ternary CH refined with riding coordinates:
 C12(H12), C5(H5), C24(H24), C17(H17)
2.b Aromatic/amide H refined with riding coordinates:
 C45(H45), C46(H46), C9(H9), C21(H21), C40(H40), C8(H8), C38(H38), C36(H36),
 C10(H10), C44(H44), C22(H22), C42(H42), C20(H20), C37(H37), C34(H34), C41(H41),
  C43(H43), C35(H35), C30(H30), C28(H28), C31(H31), C32(H32), C29(H29)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C25(H25A,H25B,H25C), C13(H13A,H13B,
 H13C), C26(H26A,H26B,H26C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C)
;
_shelx_res_checksum              82980
_shelx_hkl_checksum              17176
_olex2_submission_special_instructions 'No special instructions were received'