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_7243745
_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         'C26 H26 Co2 Mo8 N8 O34, 0.5(H4 O2)'
_chemical_formula_sum            'C26 H28 Co2 Mo8 N8 O35'
_chemical_formula_weight         1897.94
_chemical_name_systematic        'Compound 3'
_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
_audit_block_doi                 10.5517/ccdc.csd.cc26pfr3
_audit_creation_date             2020-11-23
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_audit_update_record
;
2020-11-25 deposited with the CCDC.	2021-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                83.416(3)
_cell_angle_beta                 68.138(2)
_cell_angle_gamma                73.915(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5767(13)
_cell_length_b                   11.1881(15)
_cell_length_c                   12.2524(17)
_cell_measurement_reflns_used    3689
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.37
_cell_volume                     1170.6(3)
_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 0.989
_diffrn_measured_fraction_theta_max 0.970
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8594
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.428
_diffrn_reflns_theta_min         1.895
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.873
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0685 before and 0.0319 after correction.
The Ratio of minimum to maximum transmission is 0.8414.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.692
_exptl_crystal_description       block
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5718
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0462P)^2^+5.1348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4865
_reflns_number_total             5894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01195b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7243745--7243750.cif.'
_cod_database_code               7243745
_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. Restrained distances
 Co1-H3A \\sim Co1-H3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1W: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within
2A
Uanis(O1W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O1W
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
6.a Free rotating group:
 O3(H3A,H3B), O1W(H1WA,H1WB)
6.b Rotating group:
 O4(H4A,H4B)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C9(H9), C5(H5), C11(H11), C3(H3), C1(H1), C12(H12), C2(H2)
;
_shelx_res_checksum              70205
_olex2_submission_special_instructions 'No special instructions were received'