Olmstead, Marilyn; Personal communication to COD  (2017) –; doi:

data_3500073
_journal_name_full               'Personal communication to COD'
_journal_year                    2017
_chemical_formula_moiety         'Mo12 O40 Si, 2(Mn O6), 11(O)'
_chemical_formula_sum            'H46 Mn2 Mo12 O63 Si'
_chemical_formula_weight         2343.62
_chemical_name_common
;
'[Mn(H~2~O)~6~]~2~[SiO~4~(MoO~3~)~12~]^.^11H~2~O
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                80.61(2)
_cell_angle_beta                 71.99(2)
_cell_angle_gamma                71.82(2)
_cell_formula_units_Z            2
_cell_length_a                   13.379(3)
_cell_length_b                   13.929(3)
_cell_length_c                   15.311(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      2.5
_cell_volume                     2571.0(10)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXTL v. 5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Siemens R3m/v'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.001
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14377
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.667
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.456
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'psi-scans (Platon, 1990)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.027
_exptl_crystal_description       prism
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max         1.264
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.271
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         14377
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+6.9750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1533
_refine_special_details          'H atoms were not located due to disorder'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10818
_reflns_number_total             14377
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mn637.cif
_cod_data_source_block           mn637
_cod_database_code               3500073
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.445
_shelx_estimated_absorpt_t_max   0.625
_shelx_res_checksum              33912
_shelx_hkl_checksum              38482