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_4339692
_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         'C20 H26 Cl2 N5 O2 P3'
_chemical_formula_sum            'C20 H26 Cl2 N5 O2 P3'
_chemical_formula_weight         532.27
_chemical_name_systematic
;
 6,6-Dichloro-bis{3-propyl-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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 99.111(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   9.311(5)
_cell_length_b                   22.628(5)
_cell_length_c                   12.208(5)
_cell_measurement_reflns_used    7553
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.6183
_cell_measurement_theta_min      2.2151
_cell_volume                     2539.6(18)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        CrystalClear
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID-S'
_diffrn_measurement_method       '\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  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            70088
_diffrn_reflns_theta_full        30.58
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0773
_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^)+(0.0911P)^2^+1.2039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2330
_reflns_number_gt                4292
_reflns_number_total             7766
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701216f-file006.cif
_cod_data_source_block           compound_5a
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4339692