4',4',6',6'-Tetrachloro-3-(4,6-dimethylpyridin-2-yl)-3,4-dihydrospiro[1,3,2-benzoxazaphosphinine-2,2'-(2λ^5^,4λ^5^,6λ^5^-cyclotriphosphazene)]
Çaylak, Nagihan; Hökelek, Tuncer; Büyükgüngör, Orhan; Dal, Hakan; Süzen, Yasemin; Kılıç, Zeynel; Acta Crystallographica Section E 61 (2005) o1557–o1560; doi:10.1107/S1600536805013383

data_2206097
_publ_section_title
4',4',6',6'-Tetrachloro-3-(4,6-dimethylpyridin-2-yl)-3,4-dihydrospiro[1,3,2-benzoxazaphosphinine-2,2'-(2\l^5^,4\l^5^,6\l^5^-cyclotriphosphazene)]
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1557
_journal_page_last               o1560
_journal_paper_doi               10.1107/S1600536805013383
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C14 H14 Cl4 N5 O P3'
_chemical_formula_moiety         'C14 H14 Cl4 N5 O P3'
_chemical_formula_sum            'C14 H14 Cl4 N5 O P3'
_chemical_formula_weight         503.01
_chemical_name_systematic
;
4',4',6',6'-Tetrachloro-3-(4,6-dimethylpyridin-2-yl)-3,4-dihydrospiro[1,3,2-
benzoxazaphosphinine-2,2'-(2\l^5^,4\l^5^,6\l^5^-cyclotriphosphazene)]
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9310(5)
_cell_length_b                   11.9091(10)
_cell_length_c                   21.3948(15)
_cell_measurement_reflns_used    5847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      1.71
_cell_volume                     2020.8(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        X-RED
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       \f
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9087
_diffrn_reflns_theta_full        27.05
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.452
_refine_ls_abs_structure_details 'Flack (1983), with 1667 Friedel pairs'
_refine_ls_abs_structure_Flack   0.06(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0536P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                3874
_reflns_number_total             4149
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6350.cif
_cod_data_source_block           I
_cod_database_code               2206097
_cod_database_fobs_code          2206097