Ansa versus Spiro Substitution of Cyclophosphazenes: Is Fluorination Essential for Ansa to Spiro Transformation of Cyclophosphazenes?
K. Muralidharan; P. Venugopalan; Anil J. Elias; Inorganic Chemistry 42 (2003) 3176–3182; doi:10.1021/ic034119v

data_4313668
_publ_section_title
;
 Ansa versus Spiro Substitution of Cyclophosphazenes: Is Fluorination
 Essential for Ansa to Spiro Transformation of Cyclophosphazenes?
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3176
_journal_page_last               3182
_journal_paper_doi               10.1021/ic034119v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C13 H15 Cl4 Fe1 N3 O2 P4 S1'
_chemical_formula_sum            'C13 H15 Cl4 Fe N3 O2 P4 S'
_chemical_formula_weight         598.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.894(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   20.941(5)
_cell_length_b                   9.434(5)
_cell_length_c                   23.663(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4557(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1408
_diffrn_reflns_av_sigmaI/netI    0.2382
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8201
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00056(2)
_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   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.2490
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0040P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                2731
_reflns_number_total             7969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034119vrom20030203_123527_2.cif
_cod_data_source_block           compound4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C13 H15 Cl4 Fe1 N3 O2 P4 S1'
_cod_database_code               4313668