Redetermination of the mixed-valence hexanuclear manganese oxide complex di-μ~4~-oxo-tetra-μ~3~-pivalato-hexa-μ~2~-pivalato-tetrakis(pivalic acid)dimanganese(III)tetramanganese(II) at 100 K
Poyraz, Mehmet; Sarı, Musa; Cevik, Sabri; Büyükgüngör, Orhan; Acta Crystallographica Section E 62 (2006) m1442–m1444; doi:10.1107/S1600536806019155

data_2209171
_publ_section_title
;
 Redetermination of the mixed-valence hexanuclear manganese oxide
 complex
 di-\m~4~-oxo-tetra-\m~3~-pivalato-hexa-\m~2~-pivalato-tetrakis(pivalic
 acid)dimanganese(III)tetramanganese(II) at 100 K
;
_journal_coeditor_code           GK2005
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1442
_journal_page_last               m1444
_journal_paper_doi               10.1107/S1600536806019155
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mn6 (C4 H9 O2)10 O2 (C4 H10 O2)4]'
_chemical_formula_moiety         'C70 H130 Mn6 O30'
_chemical_formula_sum            'C70 H130 Mn6 O30'
_chemical_formula_weight         1781.39
_chemical_name_systematic
;
di-\m~4~-oxo-tetra\m~3~-pivalato-hexa-\m~2~-pivalato-tetrakis(pivalic
acid)dimanganese(III)tetramanganese(II)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.4265(5)
_cell_length_b                   24.8578(5)
_cell_length_c                   28.1714(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      1.45
_cell_volume                     18505.9(7)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16317
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.34
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7520
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.513
_exptl_crystal_size_min          0.440
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.493
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         16317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1086P)^2^+] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                9653
_reflns_number_total             16156
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2005.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2209171
_cod_database_fobs_code          2209171