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_4123121
_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_absolute_configuration unk
_chemical_formula_moiety         '[Mn4N12C68H62], 4[NC5H5]'
_chemical_formula_sum            'C88 H82 Mn4 N16'
_chemical_formula_weight         1583.45
_chemical_melting_point          ?
_chemical_name_common            'Red House'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 116.311(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.516(5)
_cell_length_b                   15.842(4)
_cell_length_c                   16.591(5)
_cell_measurement_reflns_used    1286
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.095
_cell_measurement_theta_min      2.33
_cell_volume                     3891.3(19)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'TWINABS (Bruker-AXS)'
_computing_molecular_graphics    XP
_computing_publication_material  'APEX2 Report Generator'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Kappa APEX II DUO'
_diffrn_measurement_method       'Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1973
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18562
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.899
_diffrn_reflns_theta_min         1.369
_diffrn_source                   'fine-focused sealed tube'
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.745617
_exptl_absorpt_correction_T_min  0.588670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
   13373 Corrected reflections written to file twin4.hkl
 Reflections merged according to point-group 2     
 Minimum and maximum apparent transmission:  0.589084  0.745617
 Additional spherical absorption correction applied with mu*r =  0.2000

 HKLF 5 dataset constructed from all observed data
   31877 Corrected reflections written to file twin5.hkl
 Reflections not merged
 Single reflections that also occur in composites not omitted
 Racemic twinning not included for all components
 Second component not inverted relative to first
 Minimum and maximum apparent transmission:  0.588670  0.745617
 Additional spherical absorption correction applied with mu*r =  0.2000
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.215(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         18562
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1587
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.947
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                10251
_reflns_number_total             18562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508244x_si_002.cif
_cod_data_source_block           2py-polymorph
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'Not Determined' was changed to '?' -
the value is undefined or not
given.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 
;
_cod_original_cell_volume        3891.1(19)
_cod_database_code               4123121
_shelx_estimated_absorpt_t_min   0.643
_shelx_estimated_absorpt_t_max   0.955
_shelxl_version_number           2013-3
_shelx_res_checksum              50762
_shelx_hkl_checksum              64785