Crystal structures of diaquadi-μ-hydroxido-tris[trimethyltin(IV)] diformatotrimethylstannate(IV) and di-μ-hydroxido-tris[trimethyltin(IV)] chloride monohydrate
Otte, Felix; Koller, Stephan G.; Golz, Christopher; Strohmann, Carsten; Acta Crystallographica Section E 72 (2016) 1499–1502; doi:10.1107/S2056989016014912

data_2241864
_publ_section_title
;
 Crystal structures of diaquadi-\m-hydroxido-tris[trimethyltin(IV)]
 diformatotrimethylstannate(IV) and di-\m-hydroxido-tris[trimethyltin(IV)]
 chloride monohydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1499
_journal_page_last               1502
_journal_paper_doi               10.1107/S2056989016014912
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Sn3 (C H3)9 (O H)2 (H2 O)2] [Sn (C H3)3 (C H O2)2]'
_chemical_formula_moiety         'C9 H13 O4 Sn3 +, C5 H11 O4 Sn -'
_chemical_formula_sum            'C7 H22 O4 Sn2'
_chemical_formula_weight         407.62
_chemical_name_systematic
;
Diaquadi-\m-hydroxido-tris[trimethyltin(IV)] diformatotrimethylstannate(IV)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0786(8)
_cell_length_b                   18.9529(14)
_cell_length_c                   6.6990(5)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    154
_cell_measurement_theta_max      60
_cell_measurement_theta_min      3
_cell_volume                     1406.60(18)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX3 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      154.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            56576
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.641
_diffrn_reflns_theta_min         2.829
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.539
_exptl_absorpt_correction_T_max  0.0380
_exptl_absorpt_correction_T_min  0.0159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.329
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1569 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.040(19)
_refine_ls_extinction_coef       0.00294(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         3966
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0135
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0094P)^2^+0.4247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0262
_refine_ls_wR_factor_ref         0.0266
_reflns_number_gt                3811
_reflns_number_total             3966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5326sup1.cif
_cod_data_source_block           1
_cod_database_code               2241864
_shelx_hkl_checksum              14277
_shelx_res_checksum              40683
_cod_database_fobs_code 2241864