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_7122240
_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_formula_moiety         'C14 K4.5 La2 N2 O63.06 Si W11, 0.44(O)'
_chemical_formula_sum            'C14 K4.5 La2 N2 O63.5 Si W11'
_chemical_formula_weight         3716.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.940(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5296(10)
_cell_length_b                   30.702(3)
_cell_length_c                   17.9958(14)
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.221
_cell_measurement_theta_min      2.302
_cell_volume                     6232.4(10)
_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      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0488
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            110257
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.514
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.995
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.4028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1708 before and 0.0669 after correction. The Ratio of minimum to maximum transmission is 0.5392. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    3.961
_exptl_crystal_description       plates
_exptl_crystal_F_000             6534
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.548
_refine_diff_density_min         -2.730
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         12731
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+122.8405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11831
_reflns_number_total             12731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06334f2.cif
_cod_data_source_block           ma18005_0m
_cod_depositor_comments
'Adding full bibliography for 7122238--7122240.cif.'
_cod_original_cell_volume        6232.3(9)
_cod_original_formula_sum        'C14 K4.50 La2 N2 O63.50 Si W11'
_cod_database_code               7122240
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(W5) \\sim Ueq, Uanis(W5) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
2. Others
 Sof(O65)=1-FVAR(1)
 Sof(O63)=FVAR(1)
 Fixed Sof: K4(0.25) O62(0.5) K5(0.5) K6(0.75)
;
_olex2_submission_special_instructions 'No special instructions were received'