An isolable, metastable, geometrically unique manganese(IV) trihydrazide complex poised for reactivity
Shivaiah Vaddypally; Sandeep K.Kondaveeti; Michael Zdilla; Chem.Commun. 47 (2011) 9696–; doi:10.1039/c1cc13427b

data_7106787
_publ_section_title
;
 An isolable, metastable, geometrically unique manganese(IV) trihydrazide
 complex poised for reactivity
;
_journal_name_full               Chem.Commun.
_journal_page_first              9696
_journal_paper_doi               10.1039/c1cc13427b
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C44 H50 Li2 Mn N6 O2'
_chemical_formula_sum            'C44 H50 Li2 Mn N6 O2'
_chemical_formula_weight         763.72
_chemical_name_common
;bis(diethyletherlithium)
tris(N,N'diphenylhydrazido)manganate(IV)
;
_chemical_name_systematic
;
bis(diethyletherlithium) tris(N,N'diphenylhydrazido)manganate(IV)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.050(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9361(15)
_cell_length_b                   18.107(2)
_cell_length_c                   19.001(2)
_cell_measurement_reflns_used    10293
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.16
_cell_volume                     4083.8(8)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'COSMO (Bruker AXS)'
_computing_data_reduction        'SADABS (Bruker AXS)'
_computing_molecular_graphics    'SHELXL-97, XP (Sheldrick, 2008'
_computing_publication_material  'APEX2 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX II DUO'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17501
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_correction_T_min  0.9303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
18195 Corrected reflections written to file
Estimated minimum and maximum transmission: 0.6477 0.7456
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r = 0.2000
Lambda/2 correction factor = 0.0015
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0859P)^2^+7.2898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1641
_reflns_number_gt                3944
_reflns_number_total             4676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13427b.txt
_cod_data_source_block           1a
_cod_original_cell_volume        4083.7(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7106787