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_7243750
_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         'Mo12 O40 P, C26 H20 Cd N8 O4, 2(H2 O)'
_chemical_formula_sum            'C26 H24 Cd Mo12 N8 O46 P'
_chemical_formula_weight         2479.18
_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.cc26rg2j
_audit_creation_date             2020-12-04
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_audit_update_record
;
2020-12-04 deposited with the CCDC.	2021-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                87.2800(10)
_cell_angle_beta                 74.4670(10)
_cell_angle_gamma                88.0370(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2622(8)
_cell_length_b                   13.5330(8)
_cell_length_c                   16.2984(10)
_cell_measurement_reflns_used    5048
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.31
_cell_volume                     2814.5(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 0.996
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20643
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.306
_diffrn_reflns_theta_min         1.298
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0455 before and 0.0313 after correction.
The Ratio of minimum to maximum transmission is 0.9134.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.925
_exptl_crystal_description       block
_exptl_crystal_F_000             2342
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.891
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         13838
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.744
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+8.1887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9802
_reflns_number_total             13838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01195b2.cif
_cod_data_source_block           2_CCDC5
_cod_depositor_comments
'Adding full bibliography for 7243745--7243750.cif.'
_cod_database_code               7243750
_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
 O18-O16
 2.1 with sigma of 0.02
3. Rigid bond restraints
 C1, N25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C5(H5), C20(H20), C7(H7), C16(H16), C24(H24), C15(H15), C3(H3A),
 C1(H1), C14(H14), C23(H23), C02F(H02F), C12(H12), C13(H13), C11(H11), C10(H10),
  C9(H9), C8(H8)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O2(H2)
;
_shelx_res_checksum              18299
_olex2_submission_special_instructions 'No special instructions were received'