Reaction of Thiamine Diphosphate Hydrochloride (H3TDPCl) With Methylphenyltin(IV) Dichloride in Water. Molecular and Crystal Structures of the Oxygen-Capped Cluster [{SnMe(HTDP)(OH)}3O](OH).21H2O, in Which Thiamine Diphosphate Coordinates via Its Terminal Phosphate Group
José S. Casas; Eduardo E. Castellano; María D. Couce; María S. García-Tasende; Agustín Sánchez; José Sordo; Carmen Taboada; Ezequiel M. Vázquez-López; Inorganic Chemistry 40 (2001) 946–951; doi:10.1021/ic001088k

data_4319330
_publ_contact_author_address
; Departamento de Qu\'imica Inorg\'anica 
  Facultade de Farmacia 
  Universidade de Santiago de Compostela 
  15706 Santiago de Compostela 
  Galicia, Spain 
;
_publ_contact_author_email       qiscasas@usc.es
_publ_contact_author_fax         '0034 981 594636'
_publ_contact_author_name        'Dr. Jos\'e S. Casas Fern\'andez'
_publ_contact_author_phone       '0034 981 594912'
_publ_section_title
;
 Reaction of Thiamine Diphosphate Hydrochloride (H3TDPCl) With
 Methylphenyltin(IV) Dichloride in Water. Molecular and Crystal Structures
 of the Oxygen-Capped Cluster [{SnMe(HTDP)(OH)}3O](OH).21H2O, in Which
 Thiamine Diphosphate Coordinates via Its Terminal Phosphate Group
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              946
_journal_page_last               951
_journal_paper_doi               10.1021/ic001088k
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C39 H106 N12 O47 P6 S3 Sn3'
_chemical_formula_weight         2133.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   24.485(3)
_cell_length_b                   24.485(3)
_cell_length_c                   27.103(3)
_cell_measurement_temperature    293(2)
_cell_volume                     14072(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.1043
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12524
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6528
_exptl_crystal_size_max          .188
_exptl_crystal_size_mid          .148
_exptl_crystal_size_min          .114
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5901
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                3283
_reflns_number_total             5901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001088k.cif
_cod_data_source_block           snmecoca
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        14071(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4319330