Formation of a Novel Trinuclear Spirostannoxane Tin(IV) Compound. Crystal and Molecular Structure of [Sn(nBu)(Cl){(OCH2CH2S)2Sn(nBu)}2] and the Stannolane [(nBu)Sn(SCH2CH2O)SCH2CH2OH]
Raymundo Cea-Olivares; L. Adriana Gómez-Ortiz; Verónica García-Montalvo; Rubén L. Gaviño-Ramírez; Simón Hernández-Ortega; Inorganic Chemistry 39 (2000) 2284–2288; doi:10.1021/ic991318z

data_4320979
_publ_contact_author_address
;       Instituto de Qu\'imica, UNAM 
        Circuito Exterior 
        Cd. Universitaria 
        Delegaci\'on Coyoac\'an 
        M\'exico D.F. 04510 
        M\'exico 
;
_publ_contact_author_email       cea@servidor.unam.mx
_publ_contact_author_fax         '52 5 616 2203 '
_publ_contact_author_name        'Raymundo Cea-Olivares'
_publ_contact_author_phone       '52 5 622 4415'
_publ_section_title
;
 Formation of a Novel Trinuclear Spirostannoxane Tin(IV) Compound. Crystal
 and Molecular Structure of [Sn(nBu)(Cl){(OCH2CH2S)2Sn(nBu)}2] and the
 Stannolane [(nBu)Sn(SCH2CH2O)SCH2CH2OH]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2284
_journal_page_last               2288
_journal_paper_doi               10.1021/ic991318z
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C20 H43 Cl O4 S4 Sn3'
_chemical_formula_weight         867.30
_chemical_name_common            ASnCl
_chemical_name_systematic
; 
  ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 111.88
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.492(3)
_cell_length_b                   17.329(2)
_cell_length_c                   10.787(1)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      4.54
_cell_volume                     3207.7(7)
_computing_cell_refinement       'xscans ver 2.1 (Siemens 1994)'
_computing_data_collection       'xscans ver 2.1 (Siemens 1994)'
_computing_data_reduction        'xscans ver 2.1 (Siemens 1994)'
_computing_molecular_graphics    'XP SHELXTL/PC (Sheldrick 1990)'
_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 0.499
_diffrn_measured_fraction_theta_max 0.499
_diffrn_measurement_device_type  'Siemens P4/PC'
_diffrn_measurement_method       \w-2\q
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3327
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        <9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.684
_exptl_absorpt_correction_T_max  0.5721
_exptl_absorpt_correction_T_min  0.3706
_exptl_absorpt_correction_type   'semi-empirical based on psi-scan'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_coef       0.00010(6)
_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_all   1.061
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    'no refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0529P)^2^+0.6657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0939
_refine_ls_wR_factor_gt          0.0893
_reflns_number_gt                2814
_reflns_number_total             3101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991318z_2.cif
_cod_data_source_block           COMPOUND#1
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.6657P] 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^)+(0.0529P)^2^+0.6657P] 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      'C c'
_cod_database_code               4320979