Mixed Valence Mn(II)/Mn(III) [3 x 3] Grid Complexes: Structural, Electrochemical, Spectroscopic, and Magnetic Properties
Laurence K. Thompson; Timothy L. Kelly; Louise N. Dawe; Hilde Grove; Martin T. Lemaire; Judith A. K. Howard; Elinor C. Spencer; Craig J. Matthews; Stuart T. Onions; Simon J. Coles; Peter N. Horton; Michael B. Hursthouse; Mark E. Light; Inorganic Chemistry 43 (2004) 7605–7616; doi:10.1021/ic040083a

data_4312039
_publ_section_title
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 Mixed Valence Mn(II)/Mn(III) [3 x 3] Grid Complexes: Structural,
 Electrochemical, Spectroscopic, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7605
_journal_page_last               7616
_journal_paper_doi               10.1021/ic040083a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C114 H122 Mn9 N60 O46'
_chemical_formula_weight         3563.18
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 93.820(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3083(19)
_cell_length_b                   23.611(2)
_cell_length_c                   32.178(3)
_cell_measurement_reflns_used    8132
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.732
_cell_measurement_theta_min      2.226
_cell_volume                     16153(2)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w 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  0.0828
_diffrn_reflns_av_sigmaI/netI    0.1065
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            87143
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.7789
_exptl_absorpt_correction_T_min  0.6582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             7276
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.877
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2021
_refine_ls_number_reflns         33083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1891
_refine_ls_R_factor_gt           0.1238
_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^)+(0.1862P)^2^+119.2141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3370
_refine_ls_wR_factor_ref         0.3792
_reflns_number_gt                18513
_reflns_number_total             33083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040083a_1.cif
_cod_data_source_block           shelxl(1)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        16153(3)
_cod_database_code               4312039