Generation of a Doubly Bridging CO2 Ligand and Deoxygenation of CO2 by an (NHC)Ni(0) Complex
Chang Hoon Lee; David S. Laitar; Peter Mueller; Joseph P. Sadighi; Journal of the American Chemical Society 129 (2007) 13802–13803; doi:10.1021/ja075630g

data_4110158
_publ_section_title
;
 Generation of a Doubly Bridging CO2 Ligand and Deoxygenation of CO2 by an
 (NHC)Ni(0) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13802
_journal_page_last               13803
_journal_paper_doi               10.1021/ja075630g
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C74 H116 N4 Ni2 O2'
_chemical_formula_weight         1211.13
_chemical_name_systematic
;
 ?
;
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_symmetry_cell_setting           triclinic
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 91.346(19)
_cell_angle_gamma                112.839(12)
_cell_formula_units_Z            1
_cell_length_a                   10.704(6)
_cell_length_b                   12.403(8)
_cell_length_c                   14.597(9)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.10
_cell_measurement_theta_min      2.39
_cell_volume                     1733.8(18)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35482
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         8555
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.6204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
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_reflns_number_gt                6972
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075630gsi20070727_121441.cif
_cod_data_source_block           06021fin
_cod_original_cell_volume        1734.0(18)
_cod_database_code               4110158