Two isolated Zn-ε-Keggin decorated by pyridine-imidazole with excellent electrocatalytic and third-order NLO properties
Han, Ye-Min; Cheng, Wei-Wei; Cao, Jia-Peng; Yang, Mu-Xiu; Hong, Ya-Lin; Kang, Run-Kun; Xu, Yan; Inorganica Chimica Acta 498 (2019) 119169–; doi:10.1016/j.ica.2019.119169

data_1565812
_publ_section_title
;
 Two isolated Zn-\e-Keggin decorated by pyridine-imidazole with excellent
 electrocatalytic and third-order NLO properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119169
_journal_paper_doi               10.1016/j.ica.2019.119169
_journal_volume                  498
_journal_year                    2019
_chemical_formula_sum            'C32 H37 Mo12 N12 O43 P Zn4'
_chemical_formula_weight         2721.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.179(16)
_cell_length_b                   29.115(14)
_cell_length_c                   19.281(8)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.35
_cell_volume                     15257(13)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49988
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         1.025
_exptl_absorpt_coefficient_mu    3.244
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.370
_exptl_crystal_description       Block
_exptl_crystal_F_000             10368
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.789
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.266
_refine_ls_abs_structure_details
;
 Flack x determined using 4701 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         13252
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1054P)^2^+173.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                11377
_reflns_number_total             13252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           a01_sq
_cod_database_code               1565812
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.642
_shelx_estimated_absorpt_t_max   0.697