Stabilizing High-Valent Metal Ions with a Ketimide Ligand Set: Synthesis of Mn(N=CtBu2)4
Richard A. Lewis; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 50 (2011) 4660–4668; doi:10.1021/ic200490v

data_4325119
_publ_section_title
;
 Stabilizing High-Valent Metal Ions with a Ketimide Ligand Set: Synthesis
 of Mn(N=CtBu2)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4660
_journal_page_last               4668
_journal_paper_doi               10.1021/ic200490v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C44 H88 Li2 Mn N4 O2'
_chemical_formula_weight         774.00
_chemical_name_systematic
; 
 di(Lithium tetrahydrofuran) Manganese(II) tetrakis(bistert-butyl ketimide) 
;
_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                 96.517(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.638(4)
_cell_length_b                   19.844(7)
_cell_length_c                   19.216(7)
_cell_measurement_temperature    150(2)
_cell_volume                     4788(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31130
_diffrn_reflns_theta_full        23.37
_diffrn_reflns_theta_max         23.37
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.570740
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         6906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0888P)^2^+3.5406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1847
_reflns_number_gt                4928
_reflns_number_total             6906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200490v_si_002_1.cif
_cod_data_source_block           Complex_1
_cod_database_code               4325119