A nitrogen-base catalyzed generation of organotin(ii) hydride from an organotin trihydride under reductive dihydrogen elimination
Sindlinger, Christian P.; Stasch, Andreas; Bettinger, Holger F.; Wesemann, Lars; Chem. Sci. 6 (2015) 4737–; doi:10.1039/C5SC01561H

data_1519932
_publ_section_title
;
 A nitrogen-base catalyzed generation of organotin(ii) hydride from an
 organotin trihydride under reductive dihydrogen elimination
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              4737
_journal_paper_doi               10.1039/C5SC01561H
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C48.5 H70 Sn'
_chemical_formula_weight         771.73
_chemical_name_common            TripTpSnCpMe5
_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_update_record
;
2015-04-23 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9849(4)
_cell_length_b                   15.9056(4)
_cell_length_c                   17.7408(4)
_cell_measurement_reflns_used    234
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.1099
_cell_measurement_theta_min      2.0708
_cell_volume                     4431.37(19)
_computing_cell_refinement       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_collection       'Bruker APEX2'
_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_detector_area_resol_mean 8.3333
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55843
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         1.82
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.854
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9783
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+3.0606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                7903
_reflns_number_total             9783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc01561h2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 1519930--1519932.cif.'
_cod_original_formula_sum        'C48.50 H70 Sn'
_cod_database_code               1519932