Syntheses of Novel Exo and Endo Isomers of Ansa-Substituted Fluorophosphazenes and Their Facile Transformations into Spiro Isomers in the Presence of Fluoride Ions
K. Muralidharan; N. Dastagiri Reddy; Anil J. Elias; Inorganic Chemistry 39 (2000) 3988–3994; doi:10.1021/ic0001863

data_4321314
_publ_section_title
;
 Syntheses of Novel Exo and Endo Isomers of Ansa-Substituted
 Fluorophosphazenes and Their Facile Transformations into Spiro Isomers in
 the Presence of Fluoride Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3988
_journal_page_last               3994
_journal_paper_doi               10.1021/ic0001863
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C9 H11 F4 N3 O2 P4 S'
_chemical_formula_weight         425.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.39
_cell_angle_beta                 80.65
_cell_angle_gamma                70.67
_cell_formula_units_Z            2
_cell_length_a                   8.006
_cell_length_b                   8.685
_cell_length_c                   13.006
_cell_measurement_temperature    293(2)
_cell_volume                     841.977
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2391
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.8860
_exptl_absorpt_correction_T_min  0.8357
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.930
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                1841
_reflns_number_total             2201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0001863_4.cif
_cod_data_source_block           muaj4
_cod_original_cell_volume        842.0
_cod_database_code               4321314