Synthesis, Structure, and Reactivity of a Mononuclear Organozinc Hydride Complex: Facile Insertion of CO2 into a Zn-H Bond and CO2-Promoted Displacement of Siloxide Ligands
Wesley Sattler; Gerard Parkin; Journal of the American Chemical Society 133 (2011) 9708–9711; doi:10.1021/ja2035706

data_4106328
_publ_section_title
;
 Synthesis, Structure, and Reactivity of a Mononuclear Organozinc Hydride
 Complex: Facile Insertion of CO2 into a Zn-H Bond and CO2-Promoted
 Displacement of Siloxide Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9708
_journal_page_last               9711
_journal_paper_doi               10.1021/ja2035706
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C17 H13 N3 O2 S3 Zn'
_chemical_formula_weight         452.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0412(9)
_cell_length_b                   14.5162(10)
_cell_length_c                   9.1317(6)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.71
_cell_measurement_theta_min      2.65
_cell_volume                     1850.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31437
_diffrn_reflns_theta_full        31.77
_diffrn_reflns_theta_max         31.77
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.682
_exptl_absorpt_correction_T_max  0.9513
_exptl_absorpt_correction_T_min  0.7296
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         6280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0414P)^2^+0.4238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                4966
_reflns_number_total             6280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2035706_si_005.cif
_cod_data_source_block           fors10
_cod_database_code               4106328