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_4325121
_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            'C52 H104 Li Mn N4 O8'
_chemical_formula_weight         975.27
_chemical_name_systematic
; 
 [Lithium di(1,4,7,10-tetraoxacyclododecane)] Manganese(III)
 tetrakis(bistert-butyl ketimide)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.791(5)
_cell_angle_beta                 92.476(5)
_cell_angle_gamma                90.013(5)
_cell_formula_units_Z            2
_cell_length_a                   13.611(3)
_cell_length_b                   13.612(3)
_cell_length_c                   16.360(4)
_cell_measurement_temperature    150(2)
_cell_volume                     2913.7(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1139
_diffrn_reflns_av_sigmaI/netI    0.1899
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24321
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.363
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         10977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.1654
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1781
_reflns_number_gt                4812
_reflns_number_total             10977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200490v_si_002_3.cif
_cod_data_source_block           Complex_3
_cod_original_cell_volume        2913.8(12)
_cod_database_code               4325121