Redetermination of the crystal structure of di-μ<sub>2</sub>-hydroxido-bis-[di-<i>tert</i>-butyl-chlorido-tin(IV)] at 100 K.
Reuter, Hans; IUCrData 8 (2023) x230056–; doi:10.1107/S2414314623000561

data_1569780
_publ_section_title
;
 Redetermination of the crystal structure of
 di-&#x3bc;<sub>2</sub>-hydroxido-bis-[di-<i>tert</i>-butyl-chlorido-tin(IV)]
 at 100&#x2005;K.
;
_journal_coeditor_code           TK4087
_journal_issue                   'Pt 1'
_journal_name_full               IUCrData
_journal_page_first              x230056
_journal_paper_doi               10.1107/S2414314623000561
_journal_volume                  8
_journal_year                    2023
_chemical_formula_iupac
;
[Sn2 (C4 H9)4 Cl2 (O H)2]
;
_chemical_formula_moiety         'C16 H38 Cl2 O2 Sn2'
_chemical_formula_sum            'C16 H38 Cl2 O2 Sn2'
_chemical_formula_weight         570.74
_chemical_name_systematic
;
Di-\m~2~-hydroxido-bis[di-<i>tert</i>-butylchloridotin(IV)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.4420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0632(3)
_cell_length_b                   16.9135(5)
_cell_length_c                   13.4178(3)
_cell_measurement_reflns_used    9559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.95
_cell_volume                     2352.60(11)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006) and Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            114387
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         3.109
_exptl_absorpt_coefficient_mu    2.355
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.488
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+1.0738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0329
_refine_ls_wR_factor_ref         0.0344
_reflns_number_gt                5148
_reflns_number_total             5668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tk4087.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1569780
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.853
_shelx_hkl_checksum              63927
_shelx_res_checksum              46492