6,6-Diphenyl-6,7-dihydro-5<i>H</i>-1,3,4,8-tetrathia-6-stannazulene-2-thione and 6,6'-spirobi[6,7-dihydro-5<i>H</i>-1,3,4,8-tetrathia-6-stannazulene]-2,2'-dithione
Harrison, William T. A.; Howie, R. Alan; Skakle, Janet M. S.; Wardell, James L.; Acta Crystallographica Section C 58 (2002) m351–m354; doi:10.1107/S0108270102007898

data_2012779
_publ_section_title
;6,6-Diphenyl-6,7-dihydro-5<i>H</i>-1,3,4,8-tetrathia-6-stannazulene-2-thione
 and
 6,6'-spirobi[6,7-dihydro-5<i>H</i>-1,3,4,8-tetrathia-6-stannazulene]-2,2'-dithione
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m351
_journal_page_last               m354
_journal_paper_doi               10.1107/S0108270102007898
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Sn (C17 H14 S5)]'
_chemical_formula_moiety         'C17 H14 S5 Sn'
_chemical_formula_sum            'C17 H14 S5 Sn'
_chemical_formula_weight         497.27
_chemical_name_systematic
;
6,6-Diphenyl-6,7-dihydro-5H-1,3,4,8-tetrathia-6-stannaazulene-2-thione
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 103.8400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6706(5)
_cell_length_b                   8.5319(6)
_cell_length_c                   13.3143(9)
_cell_measurement_reflns_used    3614
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.78
_cell_volume                     956.35(11)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      303(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\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  0.038
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6046
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'dark red-brown'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.12
_refine_diff_density_min         -0.58
_refine_ls_abs_structure_details 'Flack (1983), 1133 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3107
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.042
_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^)+(0.0677P)^2^+1.2361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.110
_refine_ls_wR_factor_ref         0.118
_reflns_number_gt                2767
_reflns_number_total             3107
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tr1026.cif
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2012779
_cod_database_fobs_code          2012779