Cyclic Dinuclear Organotin Cations Stabilized by Bulky Substituents
Wagner, Michael; Zobel, Bernhard; Dietz, Christina; Schollmeyer, Dieter; Jurkschat, Klaus; Organometallics 34 (2015) 5602–; doi:10.1021/acs.organomet.5b00829

data_4088061
_publ_section_title
;
 Cyclic Dinuclear Organotin Cations Stabilized by Bulky Substituents
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5602
_journal_paper_doi               10.1021/acs.organomet.5b00829
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C31 H82 Cl2 Si8 Sn2, 0.5(C3 H6 O)'
_chemical_formula_sum            'C32.5 H85 Cl2 O0.5 Si8 Sn2'
_chemical_formula_weight         1017.00
_chemical_melting_point          464
_chemical_name_systematic
2,2,-Bis{bis[bis(trimethylsilyl)methyl-chlorido-stannyl]}propane
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.4631(10)
_cell_length_b                   23.2026(5)
_cell_length_c                   16.3645(4)
_cell_measurement_reflns_used    17632
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.5170
_cell_measurement_theta_min      2.3020
_cell_volume                     10807.4(5)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28'
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'CrysAlisPro, Agilent Technologies, Version 1.171.36.28'
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'CrysAlisPro, Agilent Technologies, Version 1.171.36.28'
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_computing_publication_material  'enCIFer Version 1.5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'XcaliburS, Sapphire3'
_diffrn_measurement_method       '\w und \y scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            118841
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.200
_diffrn_reflns_theta_min         2.265
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       column
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         13761
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0483
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10334
_reflns_number_total             13761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00829_si_002.cif
_cod_data_source_block           compound1_3191o
_cod_original_formula_sum        'C32.50 H85 Cl2 O0.50 Si8 Sn2'
_cod_database_code               4088061
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              85801
_shelx_hkl_checksum              22576