Synthesis, Redox, and Magnetic Properties of a Neutral, Mixed-Valent Heptanuclear Manganese Wheel with S= 27/2 High-Spin Ground State,
Rolf W. Saalfrank; Andreas Scheurer; Raju Prakash; Frank W. Heinemann; Takayuki Nakajima; Frank Hampel; Roland Leppin; Bernd Pilawa; Holger Rupp; Paul Müller; Inorganic Chemistry 46 (2007) 1586–1592; doi:10.1021/ic0614059

data_4306982
_publ_contact_author
;                                                                               
        Prof. Dr. R. W. SAALFRANK       
        Institut f\"ur Organische Chemie
        Universit\"at Erlangen-N\"urnberg                   
        Henkestr. 42                                     
        D-91054 Erlangen                               
        Bundesrepublik Deutschland                             
;
_publ_contact_author_email       SAALFRANK@CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 852-1165'
_publ_contact_author_phone       '049 9131 852-2554'
_publ_section_title
;
Synthesis, Redox, and Magnetic Properties of a Neutral, Mixed-Valent
Heptanuclear Manganese Wheel with S= 27/2 High-Spin Ground State,
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1586
_journal_page_last               1592
_journal_paper_doi               10.1021/ic0614059
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C48 H102 Cl6 Mn7 N6 O12, 3(C4 H8 O)'
_chemical_formula_sum            'C60 H126 Cl6 Mn7 N6 O15'
_chemical_formula_weight         1768.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.160(7)
_cell_angle_beta                 81.607(4)
_cell_angle_gamma                89.674(6)
_cell_formula_units_Z            1
_cell_length_a                   11.531(1)
_cell_length_b                   13.297(2)
_cell_length_c                   13.464(2)
_cell_measurement_reflns_used    140
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     1918.9(4)
_computing_cell_refinement       'EVALCCD (Bruker-Nonius, 2002)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Bruker-Nonius, 2002)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
 \w-rotations with 2.00 \% and 144 sec per frame
;
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52554
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.385
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-Nonius, 2002'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             925
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         9252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0374P)^2^+1.0209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                6780
_reflns_number_total             9252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0614059si20060727_103444.cif
_cod_data_source_block           rs0414
_cod_database_code               4306982