Mechanistic Elucidation of the Stepwise Formation of a Tetranuclear Manganese Pinned Butterfly Cluster via N-N Bond Cleavage, Hydrogen Atom Transfer, and Cluster Rearrangement.
Hamilton, Clifton R.; Gau, Michael R.; Baglia, Regina A.; McWilliams, Sean F.; Zdilla, Michael J.; Journal of the American Chemical Society  (2014) 141218154447008–; doi:10.1021/ja508244x

data_4123116
_publ_section_title
;
 Mechanistic Elucidation of the Stepwise Formation of a Tetranuclear
 Manganese Pinned Butterfly Cluster via N-N Bond Cleavage, Hydrogen Atom
 Transfer, and Cluster Rearrangement.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141218154447008
_journal_paper_doi               10.1021/ja508244x
_journal_year                    2014
_chemical_formula_moiety         'C34 H58 Mn2 N6 Si4'
_chemical_formula_sum            'C34 H58 Mn2 N6 Si4'
_chemical_formula_weight         773.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                100.650(7)
_cell_angle_beta                 94.510(7)
_cell_angle_gamma                96.956(7)
_cell_formula_units_Z            1
_cell_length_a                   8.746(3)
_cell_length_b                   10.811(4)
_cell_length_c                   11.224(4)
_cell_measurement_reflns_used    6379
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.004
_cell_measurement_theta_min      2.3635
_cell_volume                     1029.7(6)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'COSMO (Bruker AXS)'
_computing_data_reduction        'SADABS (Bruker AXS)'
_computing_molecular_graphics    'XP (Sheldrick, 2013)'
_computing_publication_material  'APEX2 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker Kappa APEX II DUO'
_diffrn_measurement_method       'Phi/omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11325
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.567
_diffrn_reflns_theta_min         1.856
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 11312 Corrected reflections written to file
 Estimated minimum and maximum transmission:  0.6971  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            'pale pink'
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4924
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+2.4264P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4212
_reflns_number_total             4924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508244x_si_002.cif
_cod_data_source_block           1bpy
_cod_original_cell_volume        1029.7(7)
_cod_database_code               4123116
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.878
_shelxl_version_number           2013-2
_shelx_res_checksum              4282
_shelx_hkl_checksum              15683