Bis(triphenyltin) Succinate and its Complex with Dimethyl Sulfoxide and Ethanol, and its Complex with Hexamethylphosphoramide
Ng, Seik Weng; Acta Crystallographica Section C 54 (1998) 745–750; doi:10.1107/S0108270197018908

data_2007389
_publ_section_title
;
 Bis(triphenyltin) Succinate and its Complex with Dimethyl Sulfoxide
 and Ethanol, and its Complex with Hexamethylphosphoramide
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              745
_journal_page_last               750
_journal_paper_doi               10.1107/S0108270197018908
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety
;
 [Sn4  (C4 H4 O4)2 (C6 H5)12 (C2 H6 O)~1/2~ (C2 H6 OS)~3/2~]
;
_chemical_formula_sum            'C84 H80 O10 S1.5 Sn4'
_chemical_formula_weight         1772.33
_chemical_name_systematic
;
 [Bis(triphenyltin) succinate]^.^[bis(triphenyltin)
 succinate^.^sesqui(dimethylsulfoxide)^.^hemiethanol]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                67.565(6)
_cell_angle_beta                 74.546(8)
_cell_angle_gamma                70.904(8)
_cell_formula_units_Z            2
_cell_length_a                   14.206(2)
_cell_length_b                   15.7770(10)
_cell_length_c                   20.198(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14.25
_cell_measurement_theta_min      14.00
_cell_volume                     3901.7(8)
_computing_cell_refinement       'CAD-4 VAX/PC'
_computing_data_collection       'CAD-4 VAX/PC (Enraf Nonius Delft, 1988)'
_computing_data_reduction        'Xtal3.0 (Hall & Stewart, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w scan'
_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  0.0105
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14344
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.11
_diffrn_standards_decay_%        9.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.669
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_hydrogen_treatment
;
 H atoms riding, U(H) = 1.5U~eq~(C);  hydroxy H atom
 calculated
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         13695
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_obs          .0373
_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^)+(0.0496P)^2^+3.8919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1010
_refine_ls_wR_factor_obs         .0900
_reflns_number_observed          10805
_reflns_number_total             13698
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sx1059.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0496P)^2^+3.8919P] 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^)+(0.0496P)^2^+3.8919P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3901.7(6)
_cod_database_code               2007389