Phosphorus-containing polycarbosilazanes: synthesis <i>via</i> dehydrocoupling catalysis and flame-retardant properties.
Soran, Albert; Chapple, Peter M.; Longuet, Claire; Sonnier, Rodolphe; Cordier, Marie; Carpentier, Jean-François; Sarazin, Yann; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2037–2054; doi:10.1039/d4dt03172e

data_7717745
_publ_section_title
;
 Phosphorus-containing polycarbosilazanes: synthesis <i>via</i>
 dehydrocoupling catalysis and flame-retardant properties.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2037
_journal_page_last               2054
_journal_paper_doi               10.1039/d4dt03172e
_journal_volume                  54
_journal_year                    2025
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C37 H32 N P Si'
_chemical_formula_sum            'C37 H32 N P Si'
_chemical_formula_weight         549.69
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-09-18 deposited with the CCDC.	2024-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                89.561(5)
_cell_angle_beta                 79.782(5)
_cell_angle_gamma                83.183(4)
_cell_formula_units_Z            4
_cell_length_a                   9.4488(11)
_cell_length_b                   17.913(2)
_cell_length_c                   17.982(2)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5177
_cell_measurement_theta_min      2.3019
_cell_measurement_wavelength     0.710730
_cell_volume                     2973.8(6)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'PLATON, A.L.Spek, Acta Cryst. 2009, D65, 148-155'
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
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_diffrn_orient_matrix_UB_13      -0.0411951
_diffrn_orient_matrix_UB_21      -0.0002298
_diffrn_orient_matrix_UB_22      0.0490036
_diffrn_orient_matrix_UB_23      0.0263161
_diffrn_orient_matrix_UB_31      0.0996859
_diffrn_orient_matrix_UB_32      0.0043946
_diffrn_orient_matrix_UB_33      -0.0283565
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0836
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11213
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.206
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.018
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         11213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1557
_refine_ls_R_factor_gt           0.1424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+27.5752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3788
_refine_ls_wR_factor_ref         0.3868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9426
_reflns_number_total             11213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt03172e2.cif
_cod_data_source_block           4-Ph2P-C6H4CH2NHSiPh3
_cod_depositor_comments
'Adding full bibliography for 7717745--7717746.cif.'
_cod_database_code               7717745
_shelx_res_checksum              61783
_shelx_hkl_checksum              49