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_7122239
_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 N2 O59.75 Pr2 Si W11, 4(O)'
_chemical_formula_sum            'C14 K4 N2 O63.75 Pr2 Si W11'
_chemical_formula_weight         3704.82
_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'
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-17
_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                 101.994(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4529(13)
_cell_length_b                   30.495(3)
_cell_length_c                   17.907(2)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    150(2)
_cell_volume                     6117.6(11)
_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      150.04
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1495
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            102527
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         3.537
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.570
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.2977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1568 before and 0.1134 after correction.
The Ratio of minimum to maximum transmission is 0.3994.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.023
_exptl_crystal_description       plates
_exptl_crystal_F_000             6520
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.265
_refine_diff_density_min         -4.214
_refine_diff_density_rms         0.704
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         11556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+1534.4174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9174
_reflns_number_total             11556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06334f2.cif
_cod_data_source_block           mar18053_0m
_cod_depositor_comments
'Adding full bibliography for 7122238--7122240.cif.'
_cod_original_cell_volume        6117.5(12)
_cod_database_code               7122239
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
: with sigma of 0.2 and sigma for terminal atoms of 0.4
2. Others
 Fixed Sof: O18(0.75)
;
_olex2_submission_special_instructions 'No special instructions were received'