Formation of thiolene versus dithiolene species from TTBEO. Crystal structures of [Au(ddtCO2Et)(PPh3)] and [Sn(ddtCO2Et)2Me2] {TTBEO = 2,5,7,9-tetrathiabicyclo[4.3.0]non-1(6)-en-8-one; ddtCO2Et = 3-(ethoxycarbonylsulfanyl)-5,6-dihydro-1,4-dithiine-2-thiolate}
Cerrada, Elena; García, J. Felipe; Laguna, Mariano; Terroba, Raquel; Villacampa, M. Dolores; Journal of the Chemical Society, Dalton Transactions  (1998) 3511–; doi:10.1039/a805064c

data_7027977
_publ_section_title
;
 Formation of thiolene versus dithiolene species from TTBEO. Crystal
 structures of [Au(ddtCO2Et)(PPh3)] and [Sn(ddtCO2Et)2Me2]
 {TTBEO&#x2005;=&#x2005;2,5,7,9-tetrathiabicyclo[4.3.0]non-1(6)-en-8-one;
 ddtCO2Et&#x2005;=&#x2005;3-(ethoxycarbonylsulfanyl)-5,6-dihydro-1,4-dithiine-2-thiolate}
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3511
_journal_paper_doi               10.1039/a805064c
_journal_year                    1998
_chemical_formula_sum            'C16 H24 O4 S8 Sn'
_chemical_formula_weight         655.52
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.53(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.623(3)
_cell_length_b                   20.585(4)
_cell_length_c                   17.012(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      7.5
_cell_volume                     2669.4(13)
_computing_cell_refinement       Dif4
_computing_data_collection       Dif4
_computing_data_reduction        Redu4
_computing_molecular_graphics    'Siemens xp'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens Stoe AED-2'
_diffrn_measurement_method       Omega/Theta
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0934
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5826
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment
'methyls bonded to tin as rigid groups, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_obs          0.0540
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+2.1387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1014
_refine_ls_wR_factor_obs         0.0833
_reflns_number_observed          2764
_reflns_number_total             4687
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            c805064sup1.cif
_cod_data_source_block           lola16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+2.1387P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+2.1387P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027977