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_7709338
_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_absolute_configuration syn
_chemical_formula_moiety         'C46 H51 Ag N3 P Si'
_chemical_formula_sum            'C46 H51 Ag N3 P Si'
_chemical_formula_weight         812.86
_chemical_melting_point          453
_chemical_name_systematic
Cyano(triphenylsilyl)phosphanido[1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene]silver(I)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-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             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                   9.5649(2)
_cell_length_b                   20.0490(3)
_cell_length_c                   21.8272(3)
_cell_measurement_reflns_used    16719
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.6640
_cell_measurement_theta_min      2.0350
_cell_volume                     4185.73(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -15.00  19.30   0.70   19.57    --  -16.28 -99.00 150.00   49
  2  \w    -90.00 -58.50   0.70   19.57    --  -16.28-179.00 -60.00   45
  3  \w      3.00  84.20   0.70   19.57    --   16.36  57.00 120.00  116
  4  \w      4.00  84.50   0.70   19.57    --   16.36  57.00  30.00  115
  5  \w      2.00  84.60   0.70   19.57    --   16.36  57.00 -60.00  118
  6  \w     -2.00  84.10   0.70   19.57    --   16.36  57.00-150.00  123
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0365166000
_diffrn_orient_matrix_UB_12      0.0306958000
_diffrn_orient_matrix_UB_13      -0.0022639000
_diffrn_orient_matrix_UB_21      -0.0636967000
_diffrn_orient_matrix_UB_22      0.0175746000
_diffrn_orient_matrix_UB_23      0.0039617000
_diffrn_orient_matrix_UB_31      0.0103592000
_diffrn_orient_matrix_UB_32      0.0000054000
_diffrn_orient_matrix_UB_33      0.0321845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36466
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.014
_diffrn_reflns_theta_min         1.866
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 3693 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.202(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0253P)^2^+1.1450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                9188
_reflns_number_total             9768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04223h2.cif
_cod_data_source_block           exp_5191
_cod_depositor_comments
;

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C10.22 H11.33 Ag0.22 N0.67 P0.22 Si0.22'
_cod_original_formula_weight         180.63
_cod_original_formula_moiety         '0.22(C46 H51 Ag N3 P Si)'
_cod_original_formula_units_Z            18
_cod_database_code               7709338
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_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:
 C00A(H00A), C00R(H00R), C00W(H00W), C012(H012)
2.b Aromatic/amide H refined with riding coordinates:
 C006(H006), C009(H009), C00F(H00F), C00I(H00I), C00J(H00J), C00K(H00K),
 C00M(H00M), C00N(H00N), C00O(H00O), C00S(H00S), C00T(H00T), C00U(H00U),
 C00X(H00X), C010(H010), C011(H011), C014(H014), C015(H015), C016(H016),
 C017(H017), C019(H019), C01A(H01G), C01B(H01H), C01C(H01I)
2.c Idealised Me refined as rotating group:
 C00Q(H00B,H00C,H00D), C00Y(H00E,H00G,H00H), C013(H01A,H01B,H01C), C018(H01D,
 H01E,H01F), C01D(H01J,H01K,H01L), C01E(H01M,H01N,H01O), C01F(H01P,H01Q,H01R),
 C01G(H01S,H01T,H01U)
;
_shelx_res_checksum              48209
_shelx_hkl_checksum              85025
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.897