Dynamic Behavior and Isomerization Equilibria of Distannenes Synthesized by Tin Hydride/Olefin Insertions: Characterization of the Elusive Monohydrido Bridged Isomer.
Wang, Shuai; McCrea-Hendrick, Madison L; Weinstein, Cory M.; Caputo, Christine A.; Hoppe, Elke; Fettinger, James C.; Olmstead, Marilyn M.; Power, Philip P.; Journal of the American Chemical Society 139 (2017) 6586–6595; doi:10.1021/jacs.7b02269

data_4131263
_publ_section_title
;
 Dynamic Behavior and Isomerization Equilibria of Distannenes Synthesized
 by Tin Hydride/Olefin Insertions: Characterization of the Elusive
 Monohydrido Bridged Isomer.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6586
_journal_page_last               6595
_journal_paper_doi               10.1021/jacs.7b02269
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C84 H124 Sn2, 3(C7 H8)'
_chemical_formula_sum            'C105 H148 Sn2'
_chemical_formula_weight         1647.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 111.7260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8482(3)
_cell_length_b                   13.05490(10)
_cell_length_c                   30.6387(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.49
_cell_volume                     9232.90(17)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'SMART (Version 5.054) (Bruker, 2002)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
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_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            21936
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.764
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.9026
_exptl_absorpt_correction_T_min  0.7954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.223
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8116
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0184P)^2^+27.0863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6333
_reflns_number_total             8116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02269_si_002.cif
_cod_data_source_block           EH36FFMI
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4131263
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.880
_shelx_res_checksum              48693
_shelx_hkl_checksum              73473