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_4103717
_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 Mo N4'
_chemical_formula_weight         656.92
_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                   16.5902(8)
_cell_length_b                   15.6242(8)
_cell_length_c                   15.5439(8)
_cell_measurement_reflns_used    6923
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      1.80
_cell_volume                     4029.1(4)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-Nonius 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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20806
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_T_max  0.9894
_exptl_absorpt_correction_T_min  0.8016
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'diamond column'
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3606
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.260
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+3.3894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                2252
_reflns_number_total             4034
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ja108265y_si_003.cif
_cod_data_source_block           k1188
_cod_database_code               4103717