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_4325120
_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            'C36 H72 Li Mn N4'
_chemical_formula_weight         622.86
_chemical_name_systematic
; 
 Lithium Manganese(III) tetrakis(bistert-butyl ketimide)
;
_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                   16.7762(12)
_cell_length_b                   15.2054(10)
_cell_length_c                   15.8446(11)
_cell_measurement_temperature    150(2)
_cell_volume                     4041.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       omega
_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  0.0976
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25658
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.287
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0054(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0767P)^2^+6.3826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1999
_reflns_number_gt                1860
_reflns_number_total             2929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200490v_si_002_2.cif
_cod_data_source_block           Complex_2
_cod_database_code               4325120