Synthesis of a High-Valent, Four-Coordinate Manganese Cubane Cluster with a Pendant Mn Atom: Photosystem II-Inspired Manganese-Nitrogen Clusters
Shivaiah Vaddypally; Sandeep K. Kondaveeti; Michael J. Zdilla; Inorganic Chemistry 51 (2012) 3950–3952; doi:10.1021/ic300502s

data_4328870
_publ_section_title
;
 Synthesis of a High-Valent, Four-Coordinate Manganese Cubane Cluster with
 a Pendant Mn Atom: Photosystem II-Inspired Manganese-Nitrogen Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3950
_journal_page_last               3952
_journal_paper_doi               10.1021/ic300502s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'(Mn5 N12 Li3 C40 H90)0.08, (Mn4 N11 Li4 C40 H90)0.92, (C5 H12)'
_chemical_formula_sum            'C45 H102 Li3.92 Mn4.08 N11.08'
_chemical_formula_weight         1050.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.578(6)
_cell_length_b                   16.627(3)
_cell_length_c                   12.535(3)
_cell_measurement_reflns_used    8510
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.927
_cell_measurement_theta_min      2.458
_cell_volume                     6165(2)
_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      173(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II DUO'
_diffrn_measurement_method       '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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            42054
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.9349
_exptl_absorpt_correction_T_min  0.8480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
63683 Corrected reflections written to file
 Estimated minimum and maximum transmission:  0.6312  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            black
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       plate
_exptl_crystal_F_000             2254
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4601
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+16.5174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1784
_reflns_number_gt                3408
_reflns_number_total             4601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300502s_si_002_2.cif
_cod_data_source_block           1a_1
_cod_database_code               4328870