4',4',6',6'-Tetrachloro-2-(6-methylpyridin-2-yl)-1<i>H</i>,2<i>H</i>-spiro[naphtho[1,2-<i>e</i>][1,3,2]oxazaphosphinine-3,2'-[1,3,5,2,4,6]triazatriphosphinine]
Işıklan, Muhammet; Sonkaya, Ömer; Hökelek, Tuncer; Acta Crystallographica Section E 69 (2013) o861–o862; doi:10.1107/S1600536813012348

data_2238094
_publ_section_title
;
 4',4',6',6'-Tetrachloro-2-(6-methylpyridin-2-yl)-1<i>H</i>,2<i>H</i>-spiro[naphtho[1,2-<i>e</i>][1,3,2]oxazaphosphinine-3,2'-[1,3,5,2,4,6]triazatriphosphinine]
;
_journal_coeditor_code           XU5701
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o861
_journal_page_last               o862
_journal_paper_doi               10.1107/S1600536813012348
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C17 H14 Cl4 N5 O P3'
_chemical_formula_moiety         'C17 H14 Cl4 N5 O P3'
_chemical_formula_sum            'C17 H14 Cl4 N5 O P3'
_chemical_formula_weight         539.04
_chemical_name_systematic
4',4',6',6'-Tetrachloro-2-(6-methylpyridin-2-yl)-1<i>H</i>,2<i>H</i>-spiro[naphtho[1,2-<i>e</i>][1,3,2]oxazaphosphinine-3,2'-[1,3,5,2,4,6]triazatriphosphinine]
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.7784(5)
_cell_length_b                   7.8573(3)
_cell_length_c                   25.1034(5)
_cell_measurement_reflns_used    2741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.48
_cell_volume                     4295.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'WinGX (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22083
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.9390
_exptl_absorpt_correction_T_min  0.7517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.768
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0611P)^2^+1.3984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                3446
_reflns_number_total             5297
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5701.cif
_cod_data_source_block           I
_cod_database_code               2238094
_cod_database_fobs_code          2238094