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_7242627
_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         'Mo4 O13, C21 H20 Co N6 O5'
_chemical_formula_sum            'C21 H20 Co Mo4 N6 O18'
_chemical_formula_weight         1087.12
_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             2020-09-25
_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                90
_cell_angle_beta                 110.912(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.892(2)
_cell_length_b                   16.610(2)
_cell_length_c                   16.579(2)
_cell_measurement_reflns_used    6345
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.45
_cell_volume                     4088.0(9)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26539
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.935
_diffrn_reflns_theta_min         1.798
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         8762
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6172
_reflns_number_total             8762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00266j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7242626--7242630.cif.'
_cod_original_cell_volume        4088.0(10)
_cod_database_code               7242627
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 C1, N22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6, N7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6, N22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Rotating group:
 O8(H8A,H8B), O18(H18A,H18B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N4(H4), N7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C6(H6), C20(H20), C21(H21)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3350
_shelx_hkl_checksum              21656
_shelx_fab_checksum              48100
_olex2_submission_special_instructions 'No special instructions were received'