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_4131261
_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         'C64 H80 Sn2, C3 H6'
_chemical_formula_sum            'C67 H86 Sn2'
_chemical_formula_weight         1128.73
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-08
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 117.0750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2225(14)
_cell_length_b                   11.8023(7)
_cell_length_c                   23.2736(14)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.65
_cell_volume                     5924.3(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            78070
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         1.751
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6767
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0861 before and 0.0502 after correction.
The Ratio of minimum to maximum transmission is 0.9076.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            darkgreen
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       niddle
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         13573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          1.795
_refine_ls_shift/su_mean         0.229
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10670
_reflns_number_total             13573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02269_si_002.cif
_cod_data_source_block           vwsolved
_cod_database_code               4131261
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.728
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C30(H30), C47(H47), C50(H50), C59(H59), C62(H62)
2.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C17(H17), C18(H18), C19(H19), C26(H26), C27(H27),
 C28(H28), C37(H37), C38(H38), C39(H39), C43(H43), C44(H44), C45(H45), C55(H55),
  C56(H56), C57(H57), C67(H67)
2.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16C,H16B,H16A), C24(H24A,H24B,H24C), C25(H25B,H25A,H25C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52C,H52A,H52B), C60(H60A,H60B,
 H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64B,H64A,H64C), C65(H65A,
 H65B,H65C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'