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_4083969
_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         'C87 H110 O Sn2'
_chemical_formula_sum            'C87 H110 O Sn2'
_chemical_formula_weight         1409.13
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.880(2)
_cell_length_b                   14.880(2)
_cell_length_c                   34.579(7)
_cell_measurement_reflns_used    39815
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.58
_cell_measurement_theta_min      4.53
_cell_volume                     7656(2)
_computing_cell_refinement       x-Area
_computing_data_collection       x-Area
_computing_data_reduction        x-Area
_computing_molecular_graphics    'ortep for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS2'
_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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            35088
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.9170
_exptl_absorpt_correction_T_min  0.8053
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'x-red, x-shape'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack (1983), 2926 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+3.5526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                6445
_reflns_number_total             6963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500645b_si_002.cif
_cod_data_source_block           bisstannylene2
_cod_depositor_comments
'Adding full bibliography for 4083969--4083976.cif.'
_cod_original_cell_volume        7657(2)
_cod_original_sg_symbol_H-M      'P 43212'
_cod_database_code               4083969