A Spirocyclic System Comprising Both Phosphazane and Phosphazene Rings
Richards, Philip I.; Steiner, Alexander; Inorganic Chemistry 44 (2005) 275–281; doi:10.1021/ic048665f

data_4308370
_publ_section_title
;
 A Spirocyclic System Comprising Both Phosphazane and Phosphazene Rings
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              275
_journal_page_last               281
_journal_paper_doi               10.1021/ic048665f
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C43 H74 Cl3 N9 P6'
_chemical_formula_weight         1009.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.729(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.132(4)
_cell_length_b                   16.755(4)
_cell_length_c                   19.004(4)
_cell_measurement_temperature    150(2)
_cell_volume                     5134(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex'
_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  0.0790
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20323
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         6678
_refine_ls_number_restraints     571
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+10.0857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2303
_reflns_number_gt                4833
_reflns_number_total             6678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048665from20040923_075833_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        5135(2)
_cod_database_code               4308370