Synthesis of Tetranuclear, Four-Coordinate Manganese Clusters with "Pinned Butterfly" Geometry Formed by Metal-Mediated N-N Bond Cleavage in Diphenylhydrazine
Clifton R. Hamilton; Regina A. Baglia; Alexander D. Gordon; Michael J. Zdilla; Journal of the American Chemical Society 133 (2011) 4208–4211; doi:10.1021/ja110536t

data_4105825
_publ_section_title
;
 Synthesis of Tetranuclear, Four-Coordinate Manganese Clusters with
 "Pinned Butterfly" Geometry Formed by Metal-Mediated N-N Bond Cleavage in
 Diphenylhydrazine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4208
_journal_page_last               4211
_journal_paper_doi               10.1021/ja110536t
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'[(Mn +2)4 (C12 H10 N2 -2)3 (C6 H6 N -1)2 (C5 H5 N)4'] . 3 (C5 H5 N)'
_chemical_formula_sum            'C83 H77 Mn4 N15'
_chemical_formula_weight         1504.36
_chemical_name_systematic
;
bis(mu-3-N,N'-diphenylhydrazido)N,N'diphenylhydrazidobis(mu-phenylamido)
tetrapyridinetetramanganese(II)
;
_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                 109.392(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.764(3)
_cell_length_b                   14.0803(16)
_cell_length_c                   24.148(3)
_cell_measurement_reflns_used    51301
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.408
_cell_measurement_theta_min      2.249
_cell_volume                     7300.9(16)
_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      115(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX II DUO'
_diffrn_measurement_method       'phi/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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            50030
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9437
_exptl_absorpt_correction_T_min  0.8930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 51230 Corrected reflections written to file
 Estimated minimum and maximum transmission:  0.6672  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            red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       prism
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         16652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+3.1067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                11857
_reflns_number_total             16652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja110536t_si_002_3.cif
_cod_data_source_block           2a
_cod_original_cell_volume        7301.1(14)
_cod_database_code               4105825