Multi-site reduction of hexachlorophosphazene to low-valent PN heterocycles and extension to the reduction of poly-chlorophosphazene
LaPierre, Etienne A.; Suvinen, Roope A.; Patrick, Brian O.; Tuononen, Heikki M.; Manners, Ian; Chemical Science 16 (2025) 9820–9832; doi:10.1039/D4SC07559E

data_1574501
_publ_section_title
;
 Multi-site reduction of hexachlorophosphazene to low-valent PN
 heterocycles and extension to the reduction of poly-chlorophosphazene
;
_journal_issue                   22
_journal_name_full               'Chemical Science'
_journal_page_first              9820
_journal_page_last               9832
_journal_paper_doi               10.1039/D4SC07559E
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C40 H62 Cl2 N5 P3 Se2'
_chemical_formula_sum            'C40 H62 Cl2 N5 P3 Se2'
_chemical_formula_weight         934.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-09-11 deposited with the CCDC.	2025-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.540(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9105(7)
_cell_length_b                   9.9902(4)
_cell_length_c                   25.0966(10)
_cell_measurement_reflns_used    8216
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.31
_cell_volume                     4414.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'LinXTL v. 5.9.9 (Spasyuk, 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25376
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.440
_diffrn_reflns_theta_min         1.651
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0395P)^2^+3.0643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4047
_reflns_number_total             5510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07559e2.cif
_cod_data_source_block           im038_a
_cod_depositor_comments
'Adding full bibliography for 1574493--1574501.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1574501
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.623
_shelx_estimated_absorpt_t_max   0.909
_shelx_res_checksum              90337