Syntheses and Experimental Studies on the Relative Stabilities of Spiro, Ansa, and Bridged Derivatives of Cyclic Tetrameric Fluorophosphazene
Anil J. Elias; Brendan Twamley; Jean'ne M. Shreeve; Inorganic Chemistry 40 (2001) 2120–2126; doi:10.1021/ic001294s

data_4319568
_publ_section_title
;
 Syntheses and Experimental Studies on the Relative Stabilities of Spiro,
 Ansa, and Bridged Derivatives of Cyclic Tetrameric Fluorophosphazene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2120
_journal_page_last               2126
_journal_paper_doi               10.1021/ic001294s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C4 H4 F10 N4 O2 P4'
_chemical_formula_weight         453.99
_chemical_name_common            spiro-[(CF2CH2O)2PHN][F2PN]3
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.8938(2)
_cell_length_b                   10.2999(2)
_cell_length_c                   20.96840(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.05
_cell_measurement_theta_min      1.94
_cell_volume                     2784.71(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Siemens SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18868
_diffrn_reflns_theta_full        29.05
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        '< 0.01%'
_diffrn_standards_interval_count 'beginning and end'
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.8495
_exptl_absorpt_correction_T_min  0.7982
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0249P)^2^+7.1538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                2986
_reflns_number_total             3468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001294s_1.cif
_cod_data_source_block           bt100
_cod_database_code               4319568