Preparation of a 'twisted basket'Mn4N8 cluster: a two-hydrogen-atom reduced analogue of the Mn4N8 pinned butterfly
Michael R. Gau; Clifton R. Hamilton; Michael J. Zdilla; Chem.Commun. 50 (2014) 7780–; doi:10.1039/C4CC02872D

data_7115271
_publ_section_title
;
 Preparation of a 'twisted basket'Mn4N8 cluster: a two-hydrogen-atom
 reduced analogue of the Mn4N8 pinned butterfly
;
_journal_name_full               Chem.Commun.
_journal_page_first              7780
_journal_paper_doi               10.1039/C4CC02872D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '[Mn4N12C68H64][NC5H5]'
_chemical_formula_sum            'C73 H69 Mn4 N13'
_chemical_formula_weight         1348.17
_chemical_name_common            'Twisted Basket Tetramanganese Cluster'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.5179(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6312(10)
_cell_length_b                   18.1096(13)
_cell_length_c                   27.002(2)
_cell_measurement_reflns_used    9197
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.37
_cell_volume                     6653.0(8)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'SADABS (Bruker-AXS)'
_computing_molecular_graphics    XP
_computing_publication_material  'APEX2 Report Generator (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      101(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            62461
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.987
_diffrn_reflns_theta_min         1.355
_diffrn_source                   'fine-focused sealed tube'
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 63424 Corrected reflections written to file mo_1276_0m.hkl
 Estimated minimum and maximum transmission:  0.6859  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    1.346
_exptl_crystal_description       Block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.370
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         15944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0185P)^2^+9.6585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13424
_reflns_number_total             15944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02872d2.cif
_cod_data_source_block           3monoclinicP
_cod_original_cell_volume        6653.1(8)
_cod_database_code               7115271
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.758
_shelxl_version_number           2013-3
_shelx_res_checksum              5951