Octamolybdate-based hybrid constructed by flexible bis-triazole ligands: synthesis, photocatalytic and electrochemical properties
Chi, Jiaqi; Fan, Mingyue; Su, Zhongmin; Li, Xiao; Sun, Jing; Zhou, Chen; Hu, Xiaoli; New Journal of Chemistry 44 (2020) 13524–13528; doi:10.1039/D0NJ00169D

data_7059788
_publ_section_title
;
 Octamolybdate-based hybrid constructed by flexible bis-triazole ligands:
 synthesis, photocatalytic and electrochemical properties
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13524
_journal_page_last               13528
_journal_paper_doi               10.1039/D0NJ00169D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C14 H23.7 Co Mo4 N12 O14.85, 1.15(H2 O)'
_chemical_formula_sum            'C14 H26 Co Mo4 N12 O16'
_chemical_formula_weight         1061.16
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-06
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_audit_update_record
;
2020-07-08 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.189(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.734(2)
_cell_length_b                   21.779(4)
_cell_length_c                   12.503(2)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     3097.7(9)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0319
_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       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22832
_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         28.298
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.188
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         7681
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0185P)^2^+1.1736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6644
_reflns_number_total             7681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00169d2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7059788.cif.

 Adding full bibliography for 7059788.cif.
;
_cod_original_cell_volume        3097.6(9)
_cod_database_code               7059788
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.622
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Co1-H16A \\sim Co1-H16B
 with sigma of 0.02
 Co1-H4A \\sim Co1-H4B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N13)
\\sim Ueq, Uanis(O24) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O18) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N12) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C19, N14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Mo3(0.85) Mo4(0.85) Mo5(0.85) Mo6(0.15) O8(0.15) O10(0.85)
 O11(0.85) N3(0.8) O12(0.15) H12C(0.15) H12D(0.15) O13(0.85) O14(0.85)
 O15(0.85) N11(0.8) C8(0.8) H8(0.8) C11(0.8) H11(0.8) C12(0.8) H12A(0.8)
 H12B(0.8) C13(0.8) H13A(0.8) H13B(0.8) C14(0.8) H14A(0.8) H14B(0.8) O16(0.85)
 H16A(0.85) H16B(0.85) C15(0.2) H15A(0.2) H15B(0.2) C16(0.2) H16C(0.2)
 H16D(0.2) C17(0.2) H17A(0.2) H17B(0.2) N12(0.2) C18(0.2) H18(0.2) N13(0.2)
 C19(0.2) H19(0.2) N14(0.2) N15(0.8) Mo7(0.15) Mo8(0.15) O17(0.15) O18(0.15)
 O19(0.15) O20(0.15) H20A(0.15) H20B(0.15) O21(0.85) H21A(0.85) H21B(0.85)
 O23(0.15) O22(0.15) O24(0.85)
6.a Free rotating group:
 O4(H4A,H4B), O12(H12C,H12D), O16(H16A,H16B), O20(H20A,H20B), O21(H21A,H21B)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4C,H4D), C6(H6A,H6B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16C,H16D), C17(H17A,H17B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C18(H18), C19(H19)
6.d Fitted pentagon refined as free rotating group:
 N12(C18,N13,C19,N14)
;
_shelx_res_checksum              377
_olex2_submission_special_instructions 'No special instructions were received'