Phosphorus-nitrogen compounds. 14. Synthesis, stereogenism, and structural investigations of novel n/o spirocyclic phosphazene derivatives.
Ilter, Elif Ece; Asmafiliz, Nuran; Kiliç, Zeynel; Isiklan, Muhammet; Hökelek, Tuncer; Caylak, Nagihan; Sahin, Ertan; Inorganic chemistry 46 (2007) 9931–9944; doi:10.1021/ic701216f

data_4339690
_publ_section_title
;
 Phosphorus-nitrogen compounds. 14. Synthesis, stereogenism, and
 structural investigations of novel n/o spirocyclic phosphazene
 derivatives.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9931
_journal_page_last               9944
_journal_paper_doi               10.1021/ic701216f
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C10 H13 Cl4 N4 O P3'
_chemical_formula_sum            'C10 H13 Cl4 N4 O P3'
_chemical_formula_weight         439.95
_chemical_name_systematic
;
 3-Propyl-4,4,6,6-tetrachloro-3,4-dihydro-spiro[1,3,2-benzoxazaphosphorine-
 [2(lambda)**5,4(lambda)**5,6(lambda)**5][1,3,5,2,4,6]triazatriphosphorine
;
_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                93.663(13)
_cell_angle_beta                 92.424(10)
_cell_angle_gamma                107.067(13)
_cell_formula_units_Z            4
_cell_length_a                   9.5684(11)
_cell_length_b                   11.5791(19)
_cell_length_c                   17.129(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.7
_cell_measurement_theta_min      3.6
_cell_volume                     1806.8(4)
_computing_cell_refinement       'CAD4 Express'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4 Diffractometer'
_diffrn_measurement_method       'non-profiled omega 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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.1291
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7226
_diffrn_reflns_theta_full        74.21
_diffrn_reflns_theta_max         74.21
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.524
_exptl_absorpt_correction_T_max  0.278
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North et al. (1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.741
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_gt           0.0808
_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^)+(0.1408P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2670
_reflns_number_gt                3388
_reflns_number_total             7119
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701216f-file006.cif
_cod_data_source_block           compound_4a
_cod_database_code               4339690