4,4,6,6-Tetrachloro-1',3'-[2,2'-(3-oxapentane-1,5-dioxy)dibenzyl]- 2λ^5^,4λ^5^,6λ^5^-cyclotriphosphazene-2-spiro-2'-1,3,2-diazaphospholane benzene hemisolvate
Tercan, Barış; Hökelek, Tuncer; Bilge, Selen; Demiriz, Şemsay; Kılıç, Zeynel; Acta Crystallographica, Section E 60 (2004) o1369–o1372; doi:10.1107/S1600536804017118

data_2204100
_publ_section_title
;
4,4,6,6-Tetrachloro-1',3'-[2,2'-(3-oxapentane-1,5-dioxy)dibenzyl]-
2\l^5^,4\l^5^,6\l^5^-cyclotriphosphazene-2-spiro-2'-1,3,2-diazaphospholane
benzene hemisolvate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              o1369
_journal_page_last               o1372
_journal_paper_doi               10.1107/S1600536804017118
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C20 H24 Cl4 N5 O3 P3 , 0.5C6 H6'
_chemical_formula_moiety         'C20 H24 Cl4 N5 O3 P3 , 0.5C6 H6'
_chemical_formula_sum            'C23 H27 Cl4 N5 O3 P3'
_chemical_formula_weight         656.23
_chemical_name_systematic
;
4,4,6,6-Tetrachloro-1',3'-[2,2'-(3-oxapentane-1,5-dioxy)dibenzyl]-
2\l^5^,4\l^5^,6\l^5^-cyclotriphosphazene-2-spiro-2'-1,3,2-diazaphospholane
benzene hemisolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 95.23(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.531(5)
_cell_length_b                   13.431(3)
_cell_length_c                   24.043(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      12
_cell_volume                     5959(2)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD-4 (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'
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10505
_diffrn_reflns_theta_full        74.21
_diffrn_reflns_theta_max         74.21
_diffrn_reflns_theta_min         3.69
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.432
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.498
_refine_diff_density_min         -1.242
_refine_ls_extinction_coef       0.0023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5113
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1326P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1970
_reflns_number_gt                3612
_reflns_number_total             5913
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6263.cif
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2204100