A series of metal-organic loops templated by [SiMo12O40]4- and [β-Mo8O26]4- anions by using double chelate ligands: amperometric sensoring and selective photocatalytic properties
Tian, Aixiang; Fu, Yubo; Cui, Hongtao; Ying, Jun; Yang, Mengle; Yang, Yan; Wang, Xiuli; New Journal of Chemistry 43 (2019) 9980–9988; doi:10.1039/C9NJ02224D

data_7058427
_publ_section_title
;
 A series of metal-organic loops templated by [SiMo12O40]4- and
 [\b-Mo8O26]4- anions by using double chelate ligands: amperometric
 sensoring and selective photocatalytic properties
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9980
_journal_page_last               9988
_journal_paper_doi               10.1039/C9NJ02224D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety
'Mo12 O40 Si1, 0.33(C84 H72 Cu6 N24 O6), 2(H2 O)'
_chemical_formula_sum            'C28 H28 Cu2 Mo12 N8 O44 Si'
_chemical_formula_weight         2487.03
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-24 deposited with the CCDC.    2019-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   20.9697(8)
_cell_length_b                   20.9697(8)
_cell_length_c                   22.6321(10)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.030
_cell_measurement_theta_min      2.243
_cell_volume                     8618.7(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47962
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.097
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_min         1.800
_exptl_absorpt_coefficient_mu    3.383
_exptl_absorpt_correction_T_max  0.8915
_exptl_absorpt_correction_T_min  0.4264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7080
_refine_diff_density_max         3.322
_refine_diff_density_min         -2.754
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         5109
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0330P)^2^+195.3615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4179
_reflns_number_total             5109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02224d2.cif
_cod_data_source_block           2_CCDC1
_cod_original_cell_volume        8618.7(8)
_cod_database_code               7058427
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H4A(0.5) H4B(0.5) O23(0.5) O24(0.16667) O25(0.5)
 H25A(0.5) H25B(0.5) O26(0.5) H26A(0.5) H26B(0.5)
4.a Riding coordinates:
 O3(H3A,H3B), O4(H4A,H4B), O25(H25A,H25B), O26(H26A,H26B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14)
;
_shelx_res_checksum              78946
_olex2_submission_special_instructions 'No special instructions were received'