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_4321312
_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            'C13 H15 F4 Fe N3 O2 P4 S'
_chemical_formula_weight         533.07
_chemical_name_systematic
;
 ?
;
_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                109.55
_cell_angle_beta                 97.07
_cell_angle_gamma                111.79
_cell_formula_units_Z            4
_cell_length_a                   11.209
_cell_length_b                   13.965
_cell_length_c                   14.969
_cell_measurement_temperature    293(2)
_cell_volume                     1966.717
_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  0.0101
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5435
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  0.7880
_exptl_absorpt_correction_T_min  0.7053
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0031(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         5119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          2.124
_refine_ls_shift/su_mean         0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                4375
_reflns_number_total             5119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0001863_2.cif
_cod_data_source_block           muaj2
_cod_original_cell_volume        1966.8
_cod_database_code               4321312