Preparation of the First Examples of Ansa-Spiro Substituted Fluorophosphazenes and Their Structural Studies: Analysis of C-H...F-P Weak Interactions in Substituted Fluorophosphazenes
K. Muralidharan; Anil J. Elias; Inorganic Chemistry 42 (2003) 7535–7543; doi:10.1021/ic034712c

data_4312497
_publ_section_title
;
 Preparation of the First Examples of Ansa-Spiro Substituted
 Fluorophosphazenes and Their Structural Studies: Analysis of C-H...F-P
 Weak Interactions in Substituted Fluorophosphazenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7535
_journal_page_last               7543
_journal_paper_doi               10.1021/ic034712c
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C26 H30 F2 Fe2 N3 O4 P5 S2'
_chemical_formula_weight         817.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 91.801(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   21.238(5)
_cell_length_b                   13.301(5)
_cell_length_c                   23.594(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6662(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_sigmaI/netI    0.1188
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8676
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    0.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                2312
_reflns_number_total             4344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034712csi20030913_102226_1.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;

2020-11-01
Z value changed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            4
_cod_database_code               4312497