Polynuclear Manganese Complexes with the Dicarboxylate Ligand m-Phenylenedipropionate: A Hexanuclear Mixed-Valence (3MnIII, 3MnIV) Complex
Cristina Cañada-Vilalta; William E. Streib; John C. Huffman; Ted A. O'Brien; Ernest R. Davidson; George Christou; Inorganic Chemistry 43 (2004) 101–115; doi:10.1021/ic034973m

data_4310343
_publ_section_title
;
 Polynuclear Manganese Complexes with the Dicarboxylate Ligand
 m-Phenylenedipropionate: A Hexanuclear Mixed-Valence (3MnIII, 3MnIV)
 Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              101
_journal_page_last               115
_journal_paper_doi               10.1021/ic034973m
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
'C66 H60 Mn6 N6 O19 1+, Cl O4 1-, 3.5(C2 H3 N)'
_chemical_formula_sum            'C73 H70.5 Cl Mn6 N9.5 O23'
_chemical_formula_weight         1813.98
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.0280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9056(6)
_cell_length_b                   24.5551(8)
_cell_length_c                   18.9945(7)
_cell_measurement_reflns_used    4512
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.31
_cell_volume                     7885.0(5)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'XTEL (local package)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      112(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
'   0.30 degree frames measured for  30.15 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_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  0.0697
_diffrn_reflns_av_sigmaI/netI    0.1307
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64527
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  640
_diffrn_standards_number         4513
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  .794
_exptl_absorpt_correction_T_min  .679
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. plate'
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .12
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1972
_refine_ls_number_reflns         34959
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
   [\s^2^(Fo^2^)+(0.0908Fo^2^)^2^]^-1^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1847
_reflns_number_gt                23926
_reflns_number_total             34959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034973msi20030818_100625_4.cif
_cod_data_source_block           99101
_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 
;
_cod_original_formula_sum        'C73 H70.50 Cl Mn6 N9.50 O23'
_cod_database_code               4310343