Rare tetranuclear mixed-valent [MnII2MnIV2] clusters as building blocks for extended networks
Karotsis, Georgios; Jones, Leigh F.; Papaefstathiou, Giannis S.; Collins, Anna; Parsons, Simon; Nguyen, Tuyen D.; Evangelisti, Marco; Brechin, Euan K.; Dalton Transactions  (2008) 4917–4925; doi:10.1039/b804897e

data_7004255
_publ_section_title
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 Rare tetranuclear mixed-valent [MnII2MnIV2] clusters as building
 blocks for extended networks
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              4917
_journal_page_last               4925
_journal_paper_doi               10.1039/b804897e
_journal_year                    2008
_chemical_compound_source        ' G.Karotsis reaction GK3 '
_chemical_formula_moiety
'[Mn4(O)2(C6N2O2H14)2(OH2)2(Cl)4].(C2OH6)2(H2O)'
_chemical_formula_sum            'C16 H46 Cl4 Mn4 N4 O11'
_chemical_formula_weight         832.08
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-05-29
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   23.5608(3)
_cell_length_b                   23.5608(3)
_cell_length_c                   15.5896(6)
_cell_measurement_reflns_used    5589
_cell_measurement_temperature    150
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     7494.6(3)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33942
_diffrn_reflns_theta_full        27.456
_diffrn_reflns_theta_max         29.522
_diffrn_reflns_theta_min         1.644
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.854
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.66
_exptl_crystal_description       square
_exptl_crystal_F_000             3276
_exptl_crystal_recrystallization_method
;
Evaporation of ethanol
;
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
This amounts to 2EtOH and 1H2O per formula unit. The values of f(000),
Dcalc, M and Mu have been calculated on this assumption.
;
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         4268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.000506
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.00P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1062
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1062
_reflns_limit_h_max              16
_reflns_limit_h_min              -32
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                3261
_reflns_number_total             4268
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.49
_oxford_diffrn_Wilson_scale      751.15
_oxford_refine_ls_scale          0.034626(4)
_oxford_structure_analysis_title 'rhomb in R-3'
_cod_data_source_file            b804897e.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C16 H46 N4 O11 Cl4 Mn4'
_cod_database_code               7004255