Structural and Spectroscopic Characterization of Tin‒Tin Double Bonds in Cyclic Distannenes
Henning, Jens; Eichele, Klaus; Fink, Reinhold F.; Wesemann, Lars; Organometallics 33 (2014) 3904–; doi:10.1021/om500645b

data_4083975
_publ_section_title
;
 Structural and Spectroscopic Characterization of Tin--Tin Double Bonds in
 Cyclic Distannenes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3904
_journal_paper_doi               10.1021/om500645b
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
'C63 H62 Cl O Sn2, C18 H36 K N2 O6, 0.5(C6 H6)'
_chemical_formula_sum            'C84 H101 Cl K N2 O7 Sn2'
_chemical_formula_weight         1562.60
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.479(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.855(2)
_cell_length_b                   16.1315(15)
_cell_length_c                   21.0378(19)
_cell_measurement_temperature    100(2)
_cell_volume                     7753.7(12)
_computing_cell_refinement       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_collection       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (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 APEX--II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            218909
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.7511
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3244
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         17746
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+8.3001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                15385
_reflns_number_total             17746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500645b_si_002.cif
_cod_data_source_block           stannylstannide7+benzene
_cod_depositor_comments
'Adding full bibliography for 4083969--4083976.cif.'
_cod_original_cell_volume        7753.9(12)
_cod_database_code               4083975
_computing_bruker_data_scaling   'SADABS V2008/1 (Bruker AXS)'