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_4118644
_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 N8, C24 H20 B, C4 H10 O'
_chemical_formula_sum            'C67 H75 B Mn N8 O'
_chemical_formula_weight         1074.10
_chemical_name_systematic
; 
 ? 
;
_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                77.915(4)
_cell_angle_beta                 85.171(4)
_cell_angle_gamma                60.516(4)
_cell_formula_units_Z            2
_cell_length_a                   12.513(3)
_cell_length_b                   12.686(3)
_cell_length_c                   21.618(5)
_cell_measurement_reflns_used    4633
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.52
_cell_measurement_theta_min      2.27
_cell_volume                     2920.3(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36068
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2009'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       plate
_exptl_crystal_F_000             1142
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         11494
_refine_ls_number_restraints     683
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+2.0674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1515
_reflns_number_gt                7143
_reflns_number_total             11494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja306647c_si_003.cif
_cod_data_source_block           ak1014
_cod_original_cell_volume        2920.3(11)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4118644