(4<i>R</i>,11<i>R</i>)-9-(1-hydroxypropan-2-yl)-4,11-diphenyl-1,3,5,7,9-pentaazatricyclo[5.3.1.0^4,11^]undecane-2,6-dithione
Wang, Meng; Wang, Jungang; Xiang, Jiacheng; Acta Crystallographica Section E 67 (2011) o2060–; doi:10.1107/S160053681102736X

data_2231249
_publ_section_title
;
 (4<i>R</i>,11<i>R</i>)-9-(1-hydroxypropan-2-yl)-4,11-diphenyl-1,3,5,7,9-pentaazatricyclo[5.3.1.0^4,11^]undecane-2,6-dithione
;
_journal_coeditor_code           PK2329
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2060
_journal_paper_doi               10.1107/S160053681102736X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H23 N5 O S2'
_chemical_formula_moiety         'C21 H23 N5 O S2'
_chemical_formula_sum            'C21 H23 N5 O S2'
_chemical_formula_weight         425.58
_chemical_name_common
;
(2a<i>R</i>,2b<i>R</i>)-6-(1-Hydroxypropan-2-yl)-2a,2b-diphenyl-2a,2b,6,7-
tetrahydro-5<i>H</i>-2,3,4a,6,7a-pentaazacyclopenta[<i>cd</i>]indene-
1,4(2<i>H</i>,3<i>H</i>)-dithione
;
_chemical_name_systematic
;
(4<i>R</i>,11<i>R</i>)-9-(1-hydroxypropan-2-yl)-4,11-diphenyl-1,3,5,7,9-
pentaazatricyclo[5.3.1.0^4,11^]undecane-2,6-dithione
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 100.169(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0030(9)
_cell_length_b                   12.6382(13)
_cell_length_c                   18.5830(2)
_cell_measurement_reflns_used    4930
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2081.2(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
'PLATON (Spek, 2009), SHELXL97 (Sheldrick, 2008) and pubCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART 4K 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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14076
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.251
_refine_ls_abs_structure_details 'Flack (1983), 4300 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9634
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0728P)^2^+0.1223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                8871
_reflns_number_total             9634
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2329.cif
_cod_data_source_block           I
_cod_original_cell_volume        2081.2(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2231249
_cod_database_fobs_code          2231249