A series of polyoxometalate-based hybrid complexes constructed by a tripodal ligand containing mixed N/O donors
Ying, Jun; Jin, Liang; Yu, Hai-Yan; Tian, Ai-Xiang; Wang, Xiu-Li; CrystEngComm 23 (2021) 7846–7854; doi:10.1039/D1CE01195B

data_7243748
_publ_section_title
;
 A series of polyoxometalate-based hybrid complexes constructed by a
 tripodal ligand containing mixed N/O donors
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7846
_journal_page_last               7854
_journal_paper_doi               10.1039/D1CE01195B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C13 H12 Mo4 N4 O17 Zn'
_chemical_formula_sum            'C13 H12 Mo4 N4 O17 Zn'
_chemical_formula_weight         945.40
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc26rrnd
_audit_creation_date             2020-12-07
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_audit_update_record
;
2020-12-07 deposited with the CCDC.	2021-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                83.4150(10)
_cell_angle_beta                 68.1790(10)
_cell_angle_gamma                73.8600(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6183(3)
_cell_length_b                   11.1742(4)
_cell_length_c                   12.2597(4)
_cell_measurement_reflns_used    4091
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.36
_cell_volume                     1174.92(7)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.397
_diffrn_reflns_theta_min         1.789
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    3.174
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0270 after correction.
The Ratio of minimum to maximum transmission is 0.7891.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.672
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5854
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      10.747
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0197P)^2^+1.4576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5050
_reflns_number_total             5854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01195b2.cif
_cod_data_source_block           2_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7243745--7243750.cif.'
_cod_database_code               7243748
_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) groups, All O(H,H) groups
2. Restrained distances
 O17-O4
 3.5 with sigma of 0.01
3.a Rotating group:
 O15(H15), O14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C12(H12), C9(H9), C5(H5), C1(H1), C11(H11), C13(H13), C2(H2), C3(H3)
;
_shelx_res_checksum              9096
_shelx_fab_checksum              14964
_olex2_submission_special_instructions 'No special instructions were received'