2-(10',10'-Dimethyl-3'-sulfanylidene-4'-azatricyclo[5.2.1.0^1,5^]decan-2'-yl)-10,10-dimethyl-4-azatricyclo[5.2.1.0^1,5^]decane-3-thione
Walker, Ashley; Forsyth, Craig M.; Perlmutter, Patrick; Acta Crystallographica Section E 69 (2013) o1282–; doi:10.1107/S1600536813019211

data_2238354
_publ_section_title
;
 2-(10',10'-Dimethyl-3'-sulfanylidene-4'-azatricyclo[5.2.1.0^1,5^]decan-2'-yl)-10,10-dimethyl-4-azatricyclo[5.2.1.0^1,5^]decane-3-thione
;
_journal_coeditor_code           GW2136
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1282
_journal_paper_doi               10.1107/S1600536813019211
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C28 H40 N2 O2 S2'
_chemical_formula_moiety         'C28 H40 N2 O2 S2'
_chemical_formula_sum            'C28 H40 N2 O2 S2'
_chemical_formula_weight         500.74
_chemical_name_systematic
2-(10',10'-Dimethyl-3'-sulfanylidene-4'-azatricyclo[5.2.1.0^1,5^]decan-2'-yl)-10,10-dimethyl-4-azatricyclo[5.2.1.0^1,5^]decane-3-thione
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8159(3)
_cell_length_b                   13.8159(3)
_cell_length_c                   13.5221(6)
_cell_measurement_reflns_used    4395
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      2.57
_cell_volume                     2581.09(14)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  '<i>CIFTAB</i> (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEX CCD'
_diffrn_measurement_method       'thin slice \f and \w 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  0.0520
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18157
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.144
_diffrn_reflns_theta_min         2.107
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.302
_refine_ls_abs_structure_details
;
Parsons & Flack (2004);
Flack x determined using 1367 quotients [(I+)-(I-)]/[(I+)+(I-)]
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0528
_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
;
 w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.8743P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                3601
_reflns_number_total             3814
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gw2136.cif
_cod_data_source_block           I
_cod_original_cell_volume        2581.09(16)
_cod_database_code               2238354
_cod_database_fobs_code          2238354
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.981
_shelx_hkl_checksum              46391
_shelx_res_checksum              23007
_shelxl_version_number           20.13