Syntheses and Reactions of the Fluorinated Cyclic Thionylphosphazene NSO(Ar)[NPF2]2 (Ar = 4-t-BuC6H4-) with Difunctional Reagents
Anil J. Elias; Brendan Twamley; Jean'ne M. Shreeve; Inorganic Chemistry 40 (2001) 2287–2291; doi:10.1021/ic001295k

data_4319638
_publ_section_title
;
 Syntheses and Reactions of the Fluorinated Cyclic Thionylphosphazene
 NSO(Ar)[NPF2]2 (Ar = 4-t-BuC6H4-) with Difunctional Reagents
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2287
_journal_page_last               2291
_journal_paper_doi               10.1021/ic001295k
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C13 H19 F2 N3 O3 P2 S'
_chemical_formula_weight         397.31
_chemical_name_common            ansa-thionylphosphazene
_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                111.302(2)
_cell_angle_beta                 98.453(2)
_cell_angle_gamma                101.392(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5112(10)
_cell_length_b                   10.1847(12)
_cell_length_c                   11.3687(13)
_cell_measurement_reflns_used    998
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.23
_cell_volume                     873.87(18)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9631
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        '< 0.1'
_diffrn_standards_interval_count 'beginning and end'
_diffrn_standards_number         '100 frames remeasured'
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  0.8811
_exptl_absorpt_correction_T_min  0.8107
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0402P)^2^+1.3478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                2419
_reflns_number_total             3060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001295k_2.cif
_cod_data_source_block           bt196
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319638