A Novel Synthesis of Hexakis(trifluoromethyl)cyclotriphosphazene. Single-Crystal X-ray Structures of N3P3(CF3)6 and N3P3F6
Rajendra Prasad Singh; Ashwani Vij; Robert L. Kirchmeier; Jean'ne M. Shreeve; Inorganic Chemistry 39 (2000) 375–377; doi:10.1021/ic9909781

data_4300150
_publ_section_title
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A Novel Synthesis of Hexakis(trifluoromethyl)cyclotriphosphazene.
Single-Crystal X-ray Structures of N3P3(CF3)6 and N3P3F6
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              375
_journal_page_last               377
_journal_paper_doi               10.1021/ic9909781
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'N3 P3 (CF3)6'
_chemical_formula_sum            'C6 F18 N3 P3'
_chemical_formula_weight         549.00
_chemical_melting_point          337
_chemical_name_common            Hexakis(trifluoromethyl)cyclotriphosphazene
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.8510(10)
_cell_angle_beta                 75.5130(10)
_cell_angle_gamma                68.927(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5891(8)
_cell_length_b                   8.9195(8)
_cell_length_c                   12.5198(11)
_cell_measurement_reflns_used    2372
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      1.68
_cell_volume                     865.89(14)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 0.820
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker CCD Diffractometer'
_diffrn_measurement_method       '\w scans'
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3892
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_time  'before and after data collection'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.962260
_exptl_absorpt_correction_T_min  0.567992
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.028(4)
_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   1.046
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0632
_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^)+(0.1012P)^2^+0.0195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1727
_reflns_number_gt                1837
_reflns_number_total             2442
_reflns_threshold_expression     >2sigma(I)
_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_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_cell_volume        865.90(14)
_cod_database_code               4300150