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_7709336
_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         'C36 H30 P Si2, C14 H29 Na O7'
_chemical_formula_sum            'C50 H59 Na O7 P Si2'
_chemical_formula_weight         882.11
_chemical_melting_point          600
_chemical_name_systematic
'Bis(triphenylsilyl)phosphanide sodium(18-crown-6)(1,2-dimethoxyethane)1/2 salt'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-06
_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                98.695(2)
_cell_angle_beta                 107.907(2)
_cell_angle_gamma                101.613(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2084(3)
_cell_length_b                   12.5732(4)
_cell_length_c                   16.8295(5)
_cell_measurement_reflns_used    18287
_cell_measurement_temperature    100.01(15)
_cell_measurement_theta_max      30.7380
_cell_measurement_theta_min      1.8990
_cell_volume                     2344.09(13)
_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_temperature      100
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.922
_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    -39.00  48.00   1.00   25.00    --  -20.71  57.00-120.00   87
  2  \w    -91.00   2.00   1.00   25.00    --  -20.71 -38.00-180.00   93
  3  \w    -25.00  20.00   1.00   25.00    --  -20.71 -99.00 150.00   45
  4  \w    -84.00  -5.00   1.00   25.00    --  -20.71 138.00   4.51   79
  5  \w     -7.00  90.00   1.00   25.00    --   21.18  77.00 -90.00   97
  6  \w    -25.00  62.00   1.00   25.00    --   21.18 -99.00 -90.00   87
  7  \w    -47.00  40.00   1.00   25.00    --   21.18 -57.00 -30.00   87
  8  \w    -48.00  50.00   1.00   25.00    --   21.18 -77.00 150.00   98
  9  \w      3.00  90.00   1.00   25.00    --   21.18  57.00 120.00   87
 10  \w      3.00  90.00   1.00   25.00    --   21.18  57.00  30.00   87
 11  \w    -89.00  -2.00   1.00   25.00    --  -20.71 -57.00 -30.00   87
 12  \w    -75.00   4.00   1.00   25.00    --  -20.71 124.00 -90.00   79
 13  \w     -4.00  75.00   1.00   25.00    --   21.18-124.00-169.00   79
 14  \w     34.00  95.00   1.00   25.00    --   21.18 179.00-180.00   61
 15  \w     34.00  95.00   1.00   25.00    --   21.18 179.00-120.00   61
 16  \w      3.00  90.00   1.00   25.00    --   21.18  57.00-180.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            73742
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.877
_diffrn_reflns_theta_min         1.698
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88692
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             938
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-dimethoxyethane'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         13648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0352P)^2^+1.0164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10883
_reflns_number_total             13648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04223h2.cif
_cod_data_source_block           glc3010
_cod_original_cell_volume        2344.08(12)
_cod_database_code               7709336
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C)
;
_shelx_res_checksum              14100
_shelx_hkl_checksum              30226
_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
;