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_1519931
_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            'C89 H134 N2 Sn2'
_chemical_formula_weight         1469.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                84.881(2)
_cell_angle_beta                 89.932(2)
_cell_angle_gamma                82.556(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7122(5)
_cell_length_b                   15.3521(6)
_cell_length_c                   22.5773(9)
_cell_measurement_reflns_used    385
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      24.0628
_cell_measurement_theta_min      3.5900
_cell_volume                     4351.4(3)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51088
_diffrn_reflns_theta_full        26.88
_diffrn_reflns_theta_max         26.88
_diffrn_reflns_theta_min         1.86
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear pale yellow-green'
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.134
_refine_diff_density_max         3.805
_refine_diff_density_min         -0.903
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         18495
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0601P)^2^+7.4353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                14420
_reflns_number_total             18495
_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_database_code               1519931