4',4',6',6'-Tetrachloro-3,4-dihydro-3-(6-methylpyridin-2-yl)spiro[1,3,2-benzoxazaphosphinine-2,2'-(2λ^5^,4λ^5^,6λ^5^-cyclotriphosphazene)]
Tercan, Barış; Hökelek, Tuncer; Dal, Hakan; Süzen, Yasemin; Kılıç, Zeynel; Acta Crystallographica Section C 60 (2004) o639–o641; doi:10.1107/S0108270104016518

data_2014216
_publ_section_title
4',4',6',6'-Tetrachloro-3,4-dihydro-3-(6-methylpyridin-2-yl)spiro[1,3,2-benzoxazaphosphinine-2,2'-(2\l^5^,4\l^5^,6\l^5^-cyclotriphosphazene)]
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o639
_journal_page_last               o641
_journal_paper_doi               10.1107/S0108270104016518
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C13 H12 Cl4 N5 O P3'
_chemical_formula_moiety         'C13 H12 Cl4 N5 O P3'
_chemical_formula_sum            'C13 H12 Cl4 N5 O P3'
_chemical_formula_weight         488.99
_chemical_name_systematic
;
4',4',6',6'-Tetrachloro-3,4-dihydro-3-(6-methylpyridin-2-yl)spiro[1,3,2-
benzoxazaphosphinine-2,2'-(2\l^5^,4\l^5^,6\l^5^-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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.131(2)
_cell_angle_beta                 87.5980(10)
_cell_angle_gamma                81.992(2)
_cell_formula_units_Z            2
_cell_length_a                   8.98340(10)
_cell_length_b                   9.5110(2)
_cell_length_c                   11.9857(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      11
_cell_volume                     1004.26(3)
_computing_cell_refinement       'CAD-4 Express'
_computing_data_collection       'CAD-4 Express (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4003
_diffrn_reflns_theta_full        74.15
_diffrn_reflns_theta_max         74.15
_diffrn_reflns_theta_min         7.02
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.756
_exptl_absorpt_correction_T_max  0.212
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.367
_refine_ls_extinction_coef       0.088(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0631
_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^)+(0.1278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                2661
_reflns_number_total             3909
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1184.cif
_cod_data_source_block           I
_cod_database_code               2014216
_cod_database_fobs_code          2014216