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_4320978
_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            'C8 H18 O2 S2 Sn'
_chemical_formula_weight         329.03
_chemical_name_common            ASnBu-dimeric
_chemical_name_systematic
; 
  ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.468(2)
_cell_length_b                   10.393(1)
_cell_length_c                   16.479(2)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.86
_cell_measurement_theta_min      4.94
_cell_volume                     2477.9(5)
_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 0.823
_diffrn_measured_fraction_theta_max 0.823
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2601
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.370
_exptl_absorpt_correction_T_max  0.8735
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   'semi-empirical based on psi-scan'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       none
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'no applied'
_refine_ls_goodness_of_fit_all   0.910
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    'no refined except H on O2'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0972
_refine_ls_wR_factor_gt          0.0907
_reflns_number_gt                1444
_reflns_number_total             2043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991318z_1.cif
_cod_data_source_block           COMPOUND#2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] 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^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4320978