Inverted-Sandwich Dichromium(I) Complexes Supported by Two β-Diketiminates: A Multielectron Reductant and Syntheses of Chromium Dioxo and Imido
Yi-Chou Tsai; Po-Yang Wang; Shin-An Chen; Jin-Ming Chen; Journal of the American Chemical Society 129 (2007) 8066–8067; doi:10.1021/ja072003i

data_4109619
_publ_section_title
;
 Inverted-Sandwich Dichromium(I) Complexes Supported by Two
 \b-Diketiminates: A Multielectron Reductant and Syntheses of Chromium
 Dioxo and Imido
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8066
_journal_page_last               8067
_journal_paper_doi               10.1021/ja072003i
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C65 H90 Cr2 N4'
_chemical_formula_sum            'C65 H90 Cr2 N4'
_chemical_formula_weight         1031.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.9060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7158(2)
_cell_length_b                   15.3840(2)
_cell_length_c                   24.9281(4)
_cell_measurement_reflns_used    29881
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      2.037
_cell_volume                     6464.82(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0868
_diffrn_reflns_av_sigmaI/netI    0.0906
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42814
_diffrn_reflns_theta_full        25.62
_diffrn_reflns_theta_max         25.62
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.9731
_exptl_absorpt_correction_T_min  0.8815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            purple(dark)
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       prism
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         12088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1018P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                7536
_reflns_number_total             12088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072003isi20070515_094631.cif
_cod_data_source_block           6207
_cod_original_cell_volume        6464.82(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4109619