Synthesis and characterization of mixed-valence manganese fluorophosphate and analogues with clathrate-like structures: Mn(III)6F12(PO3(OH))8[Na8(Kx(H3O)4-x(H2O)2)M(IV)(OH)6] (M(IV) = Mn, Ti, Ge).
Ren, Wei-Jian; Wang, Jing-Quan; Huang, Ya-Xi; Sun, Zhi-Mei; Pan, Yuanming; Mi, Jin-Xiao; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7960–7966; doi:10.1039/c5dt00646e

data_7034667
_publ_section_title
;
 Synthesis and characterization of mixed-valence manganese fluorophosphate
 and analogues with clathrate-like structures:
 Mn(III)6F12(PO3(OH))8[Na8(Kx(H3O)4-x(H2O)2)M(IV)(OH)6] (M(IV) = Mn, Ti,
 Ge).
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7960
_journal_page_last               7966
_journal_paper_doi               10.1039/c5dt00646e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'F12 Ge H21.62 K2.79 Mn6 Na8 O41.21 P8'
_chemical_formula_weight         1852.21
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           202
_space_group_name_Hall           '-F 2 2 3'
_space_group_name_H-M_alt        'F m -3'
_symmetry_space_group_name_Hall  '-F 2 2 3'
_symmetry_space_group_name_H-M   'F m -3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.981(7)
_cell_length_b                   15.981(7)
_cell_length_c                   15.981(7)
_cell_measurement_reflns_used    6452
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.754
_cell_measurement_theta_min      2.207
_cell_volume                     4081(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
'DIAMOND (Brandenburg, 2011) & ATOMS (Dowty, 2004)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'Bruker SMART APEX CCD area-detector diffractometer'
_diffrn_measurement_method
'1800 images,\f = 0, 90, 180\%, \c = 54.74\%, \D\w=0.3\%, Exp time: 15 s.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6452
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.754
_diffrn_reflns_theta_min         2.207
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            rosy-red
_exptl_crystal_density_diffrn    3.014
_exptl_crystal_description       Octahedra
_exptl_crystal_F_000             3609
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.820
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.00035(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         493
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+45.4995P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                424
_reflns_number_total             493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00646e1.cif
_cod_data_source_block           RWJGE
_cod_depositor_comments
'Adding full bibliography for 7034667--7034669.cif.'
_cod_original_cell_volume        4082(6)
_cod_database_code               7034667
_shelx_estimated_absorpt_t_min   0.429
_shelx_estimated_absorpt_t_max   0.429
_shelxl_version_number           2013-2
_shelx_res_checksum              29733
_shelx_hkl_checksum              2225