Diamagnetic Group 6 Tetrakis(di-tert-butylketimido)metal(IV) Complexes
Rosanna A. D. Soriaga; Jennifer M. Nguyen; Thomas A. Albright; David M. Hoffman; Journal of the American Chemical Society 132 (2010) 18014–18016; doi:10.1021/ja108265y

data_4103716
_publ_section_title
;
 Diamagnetic Group 6 Tetrakis(di-tert-butylketimido)metal(IV) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18014
_journal_page_last               18016
_journal_paper_doi               10.1021/ja108265y
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C36 H72 Cr N4'
_chemical_formula_weight         612.98
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4797(6)
_cell_length_b                   15.5746(5)
_cell_length_c                   15.3467(5)
_cell_measurement_reflns_used    8160
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      1.81
_cell_volume                     3939.0(2)
_computing_cell_refinement       'SAINT v7.12A (Bruker-Nonius, 2004)'
_computing_data_collection       'APEX2 v1.0-27 (Bruker-Nonius, 2005)'
_computing_data_reduction        'SAINT v7.12A (Bruker-Nonius, 2004)'
_computing_structure_refinement  'SHELXL v6.12 (G.M. Sheldrick, 2001)'
_computing_structure_solution    'SHELXS v6.12 (G.M. Sheldrick, 2001)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 4K
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       CCD
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20377
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.9903
_exptl_absorpt_correction_T_min  0.8288
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XPREP (G.M. Sheldrick, 2001)'
_exptl_crystal_colour            Amber
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.157
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+3.1637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                2597
_reflns_number_total             3779
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ja108265y_si_002.cif
_cod_data_source_block           k1228
_cod_database_code               4103716