Syntheses, Crystal Structure, Electrocatalytic, and Magnetic Properties of the Monolanthanide-Containing Germanotungstates [Ln(H<sub>2</sub>O) <i> <sub>n</sub> </i> GeW<sub>11</sub>O<sub>39</sub>]<sup>5-</sup> (Ln = Dy, Er, <i>n</i> = 4,3).
Ibrahim, Masooma; Mbomekallé, Israël M; de Oliveira, Pedro; Baksi, Ananya; Carter, Anthony B.; Peng, Yan; Bergfeldt, Thomas; Malik, Sharali; Anson, Christopher E.; ACS omega 4 (2019) 21873–21882; doi:10.1021/acsomega.9b02846

data_4517194
_publ_section_title
;
 Syntheses, Crystal Structure, Electrocatalytic, and Magnetic Properties
 of the Monolanthanide-Containing Germanotungstates [Ln(H<sub>2</sub>O)
 <i> <sub>n</sub> </i> GeW<sub>11</sub>O<sub>39</sub>]<sup>5-</sup> (Ln =
 Dy, Er, <i>n</i> = 4,3).
;
_journal_issue                   26
_journal_name_full               'ACS omega'
_journal_page_first              21873
_journal_page_last               21882
_journal_paper_doi               10.1021/acsomega.9b02846
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'Er Ge H6 K5 O42 W11'
_chemical_formula_sum            'Er Ge H6 K5 O42 W11'
_chemical_formula_weight         3135.75
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4847(11)
_cell_length_b                   14.4847(11)
_cell_length_c                   12.3555(7)
_cell_measurement_reflns_used    8904
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      1.99
_cell_volume                     2592.3(3)
_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    'Diamond 4 (Crystal Impact, 2018)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector, \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8968
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.602
_diffrn_reflns_theta_min         1.988
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    26.868
_exptl_absorpt_correction_T_max  0.414
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP (BrukerAXS Inc., 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.017
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.132
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.375
_refine_ls_extinction_coef       0.00031(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1285
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0794P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1025
_reflns_number_total             1285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b02846_si_001.cif
_cod_data_source_block           mi-21
_cod_depositor_comments
'Adding full bibliography for 4517194--4517195.cif.'
_cod_original_cell_volume        2592.3(4)
_cod_database_code               4517194
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.222
_shelx_estimated_absorpt_t_min   0.086
_olex2_refinement_description
;
1. Restrained distances
 Er2B-O8B \\sim Er2B-O7B \\sim Er2B-O9B
 with sigma of 0.02
 W2A-O6A \\sim W1-O5
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Er2B \\sim O8B \\sim O7B \\sim O9B: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.02
O3B \\sim O3A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O4A \\sim O4B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: W2A(0.375) Er2B(0.125) O1(0.5) O3A(0.75) O3B(0.25) O4A(0.75)
 O4B(0.25) O6A(0.375) O8B(0.125) O7B(0.125) O9B(0.125)
;
_shelx_res_checksum              59138
_shelx_hkl_checksum              33961
_olex2_submission_special_instructions 'No special instructions were received'