4-Phenyl-14,18-dithia-4-phosphatricyclo[18.4.0.0^7,12^]tetracosa-2,5-dien-4-one benzene hemisolvate
Wieczorek, Wanda; Trzesowska, Agata; Kruszynski, Rafal; Acta Crystallographica Section E 61 (2005) o3304–o3306; doi:10.1107/S1600536805029181

data_2206879
_publ_section_title
;4-Phenyl-14,18-dithia-4-phosphatricyclo[18.4.0.0^7,12^]tetracosa-2,5-dien-4-one
 benzene hemisolvate
;
_journal_coeditor_code           BT6735
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3304
_journal_page_last               o3306
_journal_paper_doi               10.1107/S1600536805029181
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C27 H27 O P S2, 0.5C6 H6'
_chemical_formula_moiety         'C27 H27 O P S2, 0.5C6 H6'
_chemical_formula_sum            'C30 H30 O P S2'
_chemical_formula_weight         501.67
_chemical_name_systematic
;
4-Phenyl-14,18-dithia-4-phosphatricyclo[18.4.0.0^7,12^]tetracosa-2,5-
dien-4-one benzene solvate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.920(10)
_cell_angle_beta                 91.520(10)
_cell_angle_gamma                100.830(10)
_cell_formula_units_Z            2
_cell_length_a                   5.4920(10)
_cell_length_b                   14.0980(10)
_cell_length_c                   18.0560(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291.3(3)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      5.0
_cell_volume                     1340.4(3)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software'
_computing_molecular_graphics
;
MERCURY (Version 1.4; Bruno et al., 2002) and ORTEP-3 (Windows Version
1.062;  Farrugia 1997)
;
_computing_publication_material  'SHELXL97  and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291.3(3)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6116
_diffrn_reflns_theta_full        74.95
_diffrn_reflns_theta_max         74.95
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        11.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.513
_exptl_absorpt_correction_T_max  0.507
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 1999)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.564
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1002P)^2^+0.714P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                5155
_reflns_number_total             5512
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6735.cif
_cod_data_source_block           I
_cod_database_code               2206879
_cod_database_fobs_code          2206879