Manganese Nitride Complexes in Oxidation States III, IV, and V: Synthesis and Electronic Structure
Henning Kropp; Amanda E. King; Marat M. Khusniyarov; Frank W. Heinemann; Kyle M. Lancaster; Serena DeBeer; Eckhard Bill; Karsten Meyer; Journal of the American Chemical Society 134 (2012) 15538–15544; doi:10.1021/ja306647c

data_4118643
_publ_contact_author
;
        Prof. Dr. K. Meyer
        Department of Chemistry and Pharmacy
        Inorganic Chemistry
        Universit\"at Erlangen-N\"urnberg
        Egerlandstr. 1
        D-91058 Erlangen
        Bundesrepublik Deutschland
;
_publ_contact_author_email       Karsten.Meyer@chemie.uni-erlangen.de
_publ_contact_author_fax         '049 9131 852-7367'
_publ_contact_author_phone       '049 9131 852-7360'
_publ_section_title
;
 Manganese Nitride Complexes in Oxidation States III, IV, and V: Synthesis
 and Electronic Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15538
_journal_page_last               15544
_journal_paper_doi               10.1021/ja306647c
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C39 H45 Mn N10, C24 H20 B, C2 H3 N'
_chemical_formula_sum            'C65 H68 B Mn N11'
_chemical_formula_weight         1069.05
_chemical_name_systematic
; 
 ? 
;
_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                 100.905(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.704(3)
_cell_length_b                   17.886(2)
_cell_length_c                   18.825(3)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     5853.4(15)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \w-rotations with 1.80 \% and 126 sec per frame
;
_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  0.1819
_diffrn_reflns_av_sigmaI/netI    0.1154
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            90410
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       prism
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         12873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0370P)^2^+2.3456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                7328
_reflns_number_total             12873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja306647c_si_002.cif
_cod_data_source_block           ak1016
_cod_original_sg_symbol_Hall     -P2yn
_cod_database_code               4118643