Photochemical and electrochemical hydrogen evolution reactivity of lanthanide-functionalized polyoxotungstates.
Arab Fashapoyeh, Marzieh; Mirzaei, Masoud; Eshtiagh-Hosseini, Hossein; Rajagopal, Ashwene; Lechner, Manuel; Liu, Rongji; Streb, Carsten; Chemical communications (Cambridge, England) 54 (2018) 10427–10430; doi:10.1039/c8cc06334f

data_7122238
_publ_section_title
;
 Photochemical and electrochemical hydrogen evolution reactivity of
 lanthanide-functionalized polyoxotungstates.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10427
_journal_page_last               10430
_journal_paper_doi               10.1039/c8cc06334f
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C13 Dy1.45 K6 N2 O63.75 Si W11'
_chemical_formula_sum            'C13 Dy1.45 K6 N2 O63.75 Si W11'
_chemical_formula_weight         3724.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-24 deposited with the CCDC.
2018-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3465(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6779(5)
_cell_length_b                   20.1665(9)
_cell_length_c                   15.5021(8)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.23
_cell_measurement_theta_min      2.62
_cell_volume                     3248.0(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.98
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            70843
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         3.575
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.561
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.3205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1411 before and 0.0783 after correction.
The Ratio of minimum to maximum transmission is 0.4290.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.809
_exptl_crystal_description       block
_exptl_crystal_F_000             3279
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.843
_refine_diff_density_min         -2.915
_refine_diff_density_rms         0.282
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         12297
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0262
_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^)+52.3712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11532
_reflns_number_total             12297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06334f2.cif
_cod_data_source_block           ma18010_0m
_cod_depositor_comments
'Adding full bibliography for 7122238--7122240.cif.'
_cod_database_code               7122238
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.182
_shelx_estimated_absorpt_t_min   0.099
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(2)
 0.51(2)
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(W11) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(W1) \\sim Ueq, Uanis(W2) \\sim Ueq, Uanis(W3) \\sim Ueq, Uanis(W4) \\sim
Ueq, Uanis(W5) \\sim Ueq, Uanis(W6) \\sim Ueq, Uanis(W7) \\sim Ueq, Uanis(W8)
\\sim Ueq, Uanis(W9) \\sim Ueq, Uanis(W10) \\sim Ueq, Uanis(W11) \\sim Ueq:
with sigma of 0.2 and sigma for terminal atoms of 0.4
3. Others
 Fixed Sof: K4(0.5) K6(0.5) K8(0.5) K0A(0.5) Dy2(0.45) O0AA(0.75)
 Fixed Uiso: O20(0.02) O24(0.02) O33(0.02) O37(0.02) O38(0.02) C1(0.02)
 C2(0.02) C3(0.02) N1(0.02) C4(0.02) C5(0.02) C6(0.02) C7(0.02) O39(0.02)
 K4(0.02) K6(0.02) C8(0.02) O0AA(0.02)
;
_olex2_submission_special_instructions 'No special instructions were received'