Various amide-derived ligands induced five octamolybdate-based metal‒organic complexes: synthesis, structure, electrochemical sensing and photocatalytic properties
Wang, Xiuli; Li, Lei; Wang, Xiang; Zhang, Yuqing; CrystEngComm 23 (2021) 5176–5183; doi:10.1039/D1CE00266J

data_7242626
_publ_section_title
;
 Various amide-derived ligands induced five octamolybdate-based
 metal--organic complexes: synthesis, structure, electrochemical sensing
 and photocatalytic properties
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5176
_journal_page_last               5183
_journal_paper_doi               10.1039/D1CE00266J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C16 H16 Co Mo4 N6 O15'
_chemical_formula_sum            'C16 H15 Co Mo4 N6 O15'
_chemical_formula_weight         974.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-25
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2021-01-11 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                106.969(2)
_cell_angle_beta                 108.150(2)
_cell_angle_gamma                105.806(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6083(10)
_cell_length_b                   12.3397(13)
_cell_length_c                   13.1345(14)
_cell_measurement_reflns_used    1164
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      50.000
_cell_measurement_theta_min      1.953
_cell_volume                     1297.4(2)
_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 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7517
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.086
_diffrn_reflns_theta_max         25.086
_diffrn_reflns_theta_min         1.791
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.591
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_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            colorless
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.342
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4603
_refine_ls_number_restraints     398
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0712P)^2^+8.8086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2900
_reflns_number_total             4603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00266j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7242626--7242630.cif.'
_cod_database_code               7242626
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Rigid bond restraints
 C8, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Co1, Co1, Co1, Co1, O2, O2, O2, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 Co1, O2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C17, Mo01, O13, O11, O10, O15, O12, Mo03, Mo02, Mo04, O4, O2, O14, O7, O8, O9,
  O5, O6, Co1, O1, N1, C4, C3, C1, N3, C2, N2, H1, H3, C5, H2A, H2, C6, C10,
 H6A, C7, C9, H10, H7, C8, C11, C12, H11A, H11B, H17A, H17B, N4, H12A, H12B,
 H12C, H12D, H4, C13, O3, C14, N5, C15, C16, N6, H15, H16, H6
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
5. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) C17(0.5) H17A(0.5) H17B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C12(H12C,H12D), C11(H11A,H11B), C17(H17A,H17B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6), N3(H3), N4(H4), C16(H16), C1(H1), C15(H15), C2(H2A), C6(H6A),
 C7(H7), C9(H9), C10(H10)
;
_shelx_res_checksum              86781
_shelx_hkl_checksum              50494
_olex2_submission_special_instructions 'No special instructions were received'