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_7717746
_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_formula_moiety         'C18 H17 P Si'
_chemical_formula_sum            'C18 H17 P Si'
_chemical_formula_weight         292.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 91.869(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8294(9)
_cell_length_b                   8.7426(7)
_cell_length_c                   16.9192(10)
_cell_measurement_reflns_used    1267
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      2.62
_cell_volume                     1601.0(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker APEX5 2023.9-2'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_publication_material  'Bruker APEX5 2023.9-2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24922
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'Incoatec Mo--I\mS 3.0 microfocus source'
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.3302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3654
_reflns_number_total             3981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03172e2.cif
_cod_data_source_block           0138alb
_cod_depositor_comments
'Adding full bibliography for 7717745--7717746.cif.'
_cod_database_code               7717746
_shelx_res_checksum              83032
_shelx_hkl_checksum              11856