The highest D value for a Mn(II) ion: investigation of a manganese(II) polyoxometalate complex by high-field electron paramagnetic resonance.
Pichon, Céline; Mialane, Pierre; Rivière, Eric; Blain, Guillaume; Dolbecq, Anne; Marrot, Jérôme; Sécheresse, Francis; Duboc, Carole; Inorganic chemistry 46 (2007) 7710–7712; doi:10.1021/ic701193f

data_4339825
_publ_section_title
;
 The highest D value for a Mn(II) ion: investigation of a manganese(II)
 polyoxometalate complex by high-field electron paramagnetic resonance.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7710
_journal_page_last               7712
_journal_paper_doi               10.1021/ic701193f
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'As2 Mn O86.5 Rb8 W20'
_chemical_formula_weight         5949.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.02380(10)
_cell_length_b                   20.02380(10)
_cell_length_c                   32.8668(3)
_cell_measurement_reflns_used    21724
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.74
_cell_measurement_theta_min      1.33
_cell_volume                     11412.51(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            25207
_diffrn_reflns_theta_full        29.74
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    36.332
_exptl_absorpt_correction_T_max  0.0803
_exptl_absorpt_correction_T_min  0.0380
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    5.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallellepiped
_exptl_crystal_F_000             15354
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.969
_refine_diff_density_min         -4.271
_refine_diff_density_rms         0.464
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0549P)^2^+2159.5691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1898
_reflns_number_gt                5147
_reflns_number_total             6740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701193f-file003.cif
_cod_data_source_block           apc2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        11412.50(13)
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'As2 Mn O86.50 Rb8 W20'
_cod_database_code               4339825