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_7106788
_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 H46 Li2 Mn N6 O2'
_chemical_formula_sum            'C44 H46 Li2 Mn N6 O2'
_chemical_formula_weight         759.69
_chemical_name_common
;bis(tetrahydrofuranlithium)
tris(N,N'diphenylhydrazido)manganate(IV)
;
_chemical_name_systematic
;
bis(tetrahydrofuranlithium) 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                 95.1030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0250(7)
_cell_length_b                   17.5310(10)
_cell_length_c                   18.7595(11)
_cell_measurement_reflns_used    6725
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.26
_cell_volume                     3939.0(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18662
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.9279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
19012 Corrected reflections written to file
Estimated minimum and maximum transmission: 0.6493 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    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0394P)^2^+3.4189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                3858
_reflns_number_total             4676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13427b.txt
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7106788