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_4106325
_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            'C23 H21 N3 S3 Zn'
_chemical_formula_weight         500.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                87.096(2)
_cell_angle_beta                 83.984(2)
_cell_angle_gamma                75.395(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4946(15)
_cell_length_b                   9.3522(16)
_cell_length_c                   14.843(3)
_cell_measurement_reflns_used    7464
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      32.01
_cell_measurement_theta_min      2.49
_cell_volume                     1134.4(4)
_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      125(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18448
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.9599
_exptl_absorpt_correction_T_min  0.8309
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                5087
_reflns_number_total             6891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2035706_si_002.cif
_cod_data_source_block           znn2c2s10
_cod_original_cell_volume        1134.4(3)
_cod_database_code               4106325