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_4105823
_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)2 (C6 H6 N -1)2 (C6 H18 N1 Si2 -1)2 (C4 H8 O)2]'
_chemical_formula_sum            'C32 H64 Mn2 N4 O2 Si4'
_chemical_formula_weight         759.11
_chemical_name_systematic
; 
 bis(mu-phenylamido)bis(tetrahydrofuran)
bis[bis(trimethylsilyl)amido]dimanganese(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                 95.286(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.817(4)
_cell_length_b                   21.151(9)
_cell_length_c                   10.788(4)
_cell_measurement_reflns_used    39636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.871
_cell_measurement_theta_min      2.687
_cell_volume                     2003.3(15)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'COSMO (Bruker AXS)'
_computing_data_reduction        'SADABS (Bruker AXS)'
_computing_molecular_graphics    'XP, SHELXL-97 (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      100(2)
_diffrn_detector_area_resol_mean 8.333
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36437
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.8593
_exptl_absorpt_correction_T_min  0.7715
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.8359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                4306
_reflns_number_total             4836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja110536t_si_002_1.cif
_cod_data_source_block           1a
_cod_original_cell_volume        2003.4(14)
_cod_database_code               4105823