7,11-(Butane-1,4-diyldioxydi-<i>o</i>-phenylenedimethylene)-6,6-dichloro-4,4-bis(pyrrolidin-1-yl)-2λ^5^,4λ^5^,6λ^5^-triphosphaza-1,3,5,7,11-pentaazaspiro[5.5]undeca-1,3,5-triene
Tercan, Barış; Hökelek, Tuncer; Büyükgüngör, Orhan; Asmafiliz, Nuran; İlter, Elif Ece; Kılıç, Zeynel; Acta Crystallographica Section E 61 (2005) o2145–o2147; doi:10.1107/S1600536805018362

data_2206145
_publ_section_title
7,11-(Butane-1,4-diyldioxydi-<i>o</i>-phenylenedimethylene)-6,6-dichloro-4,4-bis(pyrrolidin-1-yl)-2\l^5^,4\l^5^,6\l^5^-triphosphaza-1,3,5,7,11-pentaazaspiro[5.5]undeca-1,3,5-triene
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2145
_journal_page_last               o2147
_journal_paper_doi               10.1107/S1600536805018362
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C29 H42 Cl2 N7 O2 P3'
_chemical_formula_moiety         'C29 H42 Cl2 N7 O2 P3'
_chemical_formula_sum            'C29 H42 Cl2 N7 O2 P3'
_chemical_formula_weight         684.51
_chemical_name_systematic
;
7,11-[Butane-1,4-diyldioxydi-o-phenylenedimethylene]-6,6-dichloro-
4,4-bis(pyrrolidin-1-yl)-2\l^5^,4\l^5^,6\l^5^-triphosphaza-1,3,5,7,11-
pentaazaspiro[5.5]undeca-1,3,5-triene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.023(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2618(4)
_cell_length_b                   23.6323(8)
_cell_length_c                   15.1606(7)
_cell_measurement_reflns_used    44825
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      1.38
_cell_volume                     3233.0(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_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      100
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS-II'
_diffrn_measurement_method       '\f 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  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45677
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  0.8855
_exptl_absorpt_correction_T_min  0.8412
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.448
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         6351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.053P)^2^+0.4055P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                5232
_reflns_number_total             6351
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6432.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2206145
_cod_database_fobs_code          2206145