Monospiroaryloxyphosphazenes: <i>p</i>-Fluorophenoxy Derivatives Containing the 1,2-Phenylenedioxy and 2,3-Naphthalenedioxy Groups
Vij, A.; Staples, R. J.; Kirchmeier, R. L.; Shreeve, J. M.; Acta Crystallographica Section C 52 (1996) 2515–2520; doi:10.1107/S0108270196005859

data_2005501
_publ_section_title
;
 Monospiroaryloxyphosphazenes: <i>p</i>-Fluorophenoxy Derivatives
 Containing the 1,2-Phenylenedioxy and 2,3-Naphthalenedioxy Groups
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2515
_journal_page_last               2520
_journal_paper_doi               10.1107/S0108270196005859
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C30 H20 F4 N3 O6 P3'
_chemical_formula_weight         687.40
_chemical_name_common
;
Monospiro(1,2-phenylenedioxy)tetrakis(parafluorophenoxy)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'
_audit_creation_method           SHELXL
_cell_angle_alpha                62.0400(10)
_cell_angle_beta                 74.1750(10)
_cell_angle_gamma                63.7950(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3869(3)
_cell_length_b                   12.6938(4)
_cell_length_c                   12.8468(4)
_cell_measurement_reflns_used    131
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      1.8
_cell_volume                     1466.53(8)
_computing_cell_refinement       'Siemens SMART 4.043'
_computing_data_collection       'Siemens SMART 4.043'
_computing_data_reduction        'Siemens SAINT 4.035'
_computing_molecular_graphics    'Siemens SHELXTL 5.03'
_computing_publication_material  'Siemens SHELXTL 5.03'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       \w
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8172
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 'start and end of data collection'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.8434
_exptl_absorpt_correction_type   'semi-empirical (Siemens, 1995a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.338
_refine_ls_extinction_coef       0.0067(8)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_hydrogen_treatment
;
H atoms obtained from difference map and all parameters refined, with
C---H 0.90(3)--0.99(3)\%A
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         5587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_obs          0.0454
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(Fo^2^) + (0.0472P)^2^ + 1.3332P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1157
_refine_ls_wR_factor_obs         0.1051
_reflns_number_observed          4645
_reflns_number_total             5588
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1172.cif
_cod_data_source_block           1
_cod_database_code               2005501