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_2005502
_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            'C34 H22 F4 N3 O6 P3'
_chemical_formula_weight         737.46
_chemical_name_common
;
Monospiro(2,3-naphthalenedioxy)tetrakis(parafluorophenoxy)cyclotriphosphazene
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.13250(10)
_cell_length_b                   26.5942(3)
_cell_length_c                   29.8727(5)
_cell_measurement_reflns_used    214
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      23.23
_cell_measurement_theta_min      1.53
_cell_volume                     6460.79(15)
_computing_cell_refinement       'Siemens SMART 4.035'
_computing_data_collection       'Siemens SMART 4.035'
_computing_data_reduction        'Siemens SAINT 4.032'
_computing_molecular_graphics    'Siemens SHELXTL 5.03'
_computing_publication_material  'Siemens SHELXTL 5.03'
_computing_structure_refinement  'SHELXL93 (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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23340
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 'start and end of data collection'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.9757
_exptl_absorpt_correction_T_min  0.8597
_exptl_absorpt_correction_type   'semi-empirical (Siemens, 1995a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.286
_refine_ls_extinction_coef       0.00093(10)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.085
_refine_ls_goodness_of_fit_obs   1.149
_refine_ls_hydrogen_treatment
;
H atoms obtained from difference map and all parameters refined, with
C---H 0.83(3)--0.97(4)\%A
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         4601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.340
_refine_ls_restrained_S_obs      1.149
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_obs          0.0468
_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^(F~o~^2^) + (0.0283P)^2^ + 5.2062P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1125
_refine_ls_wR_factor_obs         0.0818
_reflns_number_observed          3449
_reflns_number_total             4602
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1172.cif
_cod_data_source_block           2
_cod_original_cell_volume        6460.8(2)
_cod_database_code               2005502