Synthesis and structural studies (1H, 13C, 31P NMR and X-ray) of new C-bonded cyclotriphosphazenes with heterocyclic substituents from novel phosphinic acid derivatives
Virginie Vicente; Alain Fruchier; Marc Taillefer; Corinne Combes-Chamalet; Ian J. Scowen; Françoise Plénat; Henri-Jean Cristau; New J. Chem. 28 (2004) 418–424; doi:10.1039/b311046j

data_7050220
_publ_section_title
;
 Synthesis and structural studies (1H, 13C, 31P NMR and X-ray) of new
 C-bonded cyclotriphosphazenes with heterocyclic substituents from
 novel phosphinic acid derivatives
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              418
_journal_page_last               424
_journal_paper_doi               10.1039/b311046j
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C24 H18 N3 P3 S6'
_chemical_formula_weight         633.68
_chemical_name_systematic
;
Hexa-2-thienylcyclotrphosphazene
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.044(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2770(16)
_cell_length_b                   9.1335(10)
_cell_length_c                   13.561(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_volume                     1370.9(3)
_computing_cell_refinement       'IPDS software (Stoe, 1996)'
_computing_data_collection       'IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP-III( Burnett and Johnson,1996)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR97 (Altomare, et al.,1999)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13519
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5198
_refine_ls_number_restraints     433
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.4685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                4995
_reflns_number_total             5198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311046j.txt
_cod_data_source_block           taille2
_cod_database_code               7050220