Synthesis, structure and electrochemical characterization of an isopolytungstate (W<sub>4</sub>O<sub>16</sub>) held by Mn<sup>II</sup> anchors within a superlacunary crown heteropolyanion {P<sub>8</sub>W<sub>48</sub>}.
Ibrahim, Masooma; Mbomekallé, Israël M; de Oliveira, Pedro; Kostakis, George E.; Anson, Christopher E.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15545–15552; doi:10.1039/c9dt02478f

data_7700581
_publ_section_title
;
 Synthesis, structure and electrochemical characterization of an
 isopolytungstate (W<sub>4</sub>O<sub>16</sub>) held by Mn<sup>II</sup>
 anchors within a superlacunary crown heteropolyanion
 {P<sub>8</sub>W<sub>48</sub>}.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15545
_journal_page_last               15552
_journal_paper_doi               10.1039/c9dt02478f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'(H120 Li8 Mn2 O60), (H104 Cl2 K13 Li4 Mn10 Na O252 P8 W52)'
_chemical_formula_sum            'Cl2 H224 K13 Li12 Mn12 Na O312 P8 W52'
_chemical_formula_weight         16370.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2019-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-11 deposited with the CCDC.    2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.850(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.2947(14)
_cell_length_b                   30.2573(6)
_cell_length_c                   27.7045(10)
_cell_measurement_reflns_used    62353
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      1.23
_cell_measurement_theta_min      26.05
_cell_volume                     27672.1(16)
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector, \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            95098
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.712
_diffrn_reflns_theta_min         1.234
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    22.436
_exptl_absorpt_correction_T_max  0.216
_exptl_absorpt_correction_T_min  0.134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP (BrukerAXS Inc., 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.929
_exptl_crystal_description       block
_exptl_crystal_F_000             29264
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.323
_refine_diff_density_min         -2.661
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1616
_refine_ls_number_reflns         25538
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0559P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15912
_reflns_number_total             25538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02478f2.cif
_cod_data_source_block           mi42_sq
_cod_depositor_comments          'Adding full bibliography for 7700581.cif.'
_cod_database_code               7700581
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.192
_shelx_estimated_absorpt_t_min   0.107
_olex2_refinement_description
;
1. Restrained distances
 Mn5B-O72 \\sim Mn5A-O72
 with sigma of 0.02
 Mn5A-O113 \\sim Mn5B-O113
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(Mn5B) = Uanis(Mn5A)
3. Rigid body (RIGU) restrains
 K4, O126
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P4, O16, W20, W22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 K6, O123
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Mn5B)=1-FVAR(1)
 Sof(Mn5A)=FVAR(1)
 Fixed Sof: K5A(0.5) K5B(0.5) K7A(0.5) Na1(0.5) O125(0.5) O127(0.5) O209(0.5)
 O210(0.5)
;
_shelx_res_checksum              34655
_shelx_fab_checksum              71535
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'