2,6-Bis(2-hydroxyethyl)-8b,8c-diphenylperhydro-2,3a,4a,6,7a,8a-hexaazacyclopenta[<i>def</i>]fluorene-4,8-dithione
Wang, Zihua; Xi, Hailing; Acta Crystallographica Section E 65 (2009) o1426–; doi:10.1107/S1600536809019230

data_2221984
_publ_section_title
2,6-Bis(2-hydroxyethyl)-8b,8c-diphenylperhydro-2,3a,4a,6,7a,8a-hexaazacyclopenta[<i>def</i>]fluorene-4,8-dithione
_journal_coeditor_code           CV2558
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1426
_journal_paper_doi               10.1107/S1600536809019230
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C24 H28 N6 O2 S2'
_chemical_formula_moiety         'C24 H28 N6 O2 S2'
_chemical_formula_sum            'C24 H28 N6 O2 S2'
_chemical_formula_weight         496.64
_chemical_name_systematic
;
2,6-Bis(2-hydroxyethyl)-8b,8c-diphenylperhydro-2,3a,4a,6,7a,8a-
hexaazacyclopenta[<i>def</i>]fluorene-4,8-dithione
;
_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                 95.9170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8207(3)
_cell_length_b                   11.9259(3)
_cell_length_c                   18.7222(5)
_cell_measurement_reflns_used    7811
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.55
_cell_volume                     2403.16(11)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_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      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26638
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9748
_exptl_absorpt_correction_T_min  0.9271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick,1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5248
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0492
_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^)+(0.086P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1407
_reflns_number_gt                3908
_reflns_number_total             5248
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2558.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2221984
_cod_database_fobs_code          2221984