Ligand-Based Reduction of CO2 to CO Mediated by an Anionic Niobium Nitride Complex
Jared S. Silvia; Christopher C. Cummins; Journal of the American Chemical Society 132 (2010) 2169–2171; doi:10.1021/ja910445r

data_4101927
_publ_contact_author_address
;Department of Chemistry
Massachusetts Institute of Technology
Cambridge, MA
02139
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
 Ligand-Based Reduction of CO2 to CO Mediated by an Anionic Niobium
 Nitride Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2169
_journal_page_last               2171
_journal_paper_doi               10.1021/ja910445r
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C42 H63 N4 Nb O3'
_chemical_formula_sum            'C42 H63 N4 Nb O3'
_chemical_formula_weight         764.87
_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                83.4910(10)
_cell_angle_beta                 81.0630(10)
_cell_angle_gamma                68.6630(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3420(8)
_cell_length_b                   13.7425(11)
_cell_length_c                   15.7297(13)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1725
_cell_measurement_theta_min      2.1640
_cell_volume                     2053.1(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 3.0 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2008)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39195
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.9674
_exptl_absorpt_correction_T_min  0.9182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         10081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0299P)^2^+1.4011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                8300
_reflns_number_total             10081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910445r_si_001_1.cif
_cod_data_source_block           tBu-2
_cod_database_code               4101927