8b,8c-Diphenyl-2,6-bis(4-pyridylmethyl)perhydro-2,3a,4a,6,7a,8a-hexaazacyclopenta[<i>def</i>]fluorene-4,8-dithione chloroform solvate
Deng, Cong; Shu, Wenming; Zhang, Dongxue; Acta Crystallographica Section E 66 (2010) o1524–; doi:10.1107/S1600536810020040

data_2226391
_publ_section_title
;
 8b,8c-Diphenyl-2,6-bis(4-pyridylmethyl)perhydro-2,3a,4a,6,7a,8a-hexaazacyclopenta[<i>def</i>]fluorene-4,8-dithione
 chloroform solvate
;
_journal_coeditor_code           CV2714
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1524
_journal_paper_doi               10.1107/S1600536810020040
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C32 H30 N8 S2, C H Cl3'
_chemical_formula_moiety         'C32 H30 N8 S2, C H Cl3'
_chemical_formula_sum            'C33 H31 Cl3 N8 S2'
_chemical_formula_weight         710.13
_chemical_name_systematic
;
8b,8c-Diphenyl-2,6-bis(4-pyridylmethyl)perhydro-2,3a,4a,6,7a,8a-
hexaazacyclopenta[<i>def</i>]fluorene-4,8-dithione chloroform 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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.9780(10)
_cell_angle_beta                 91.6990(10)
_cell_angle_gamma                98.5000(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5381(6)
_cell_length_b                   12.1712(8)
_cell_length_c                   14.8765(9)
_cell_measurement_temperature    294(2)
_cell_volume                     1673.81(18)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.1093
_diffrn_reflns_av_sigmaI/netI    0.1743
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11061
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.9576
_exptl_absorpt_correction_T_min  0.9178
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.393
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.1761
_refine_ls_R_factor_gt           0.0621
_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^)+(0.1041P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.2103
_reflns_number_gt                2136
_reflns_number_total             5690
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv2714.cif
_cod_data_source_block           I
_cod_database_code               2226391
_cod_database_fobs_code          2226391