Three organic-inorganic polyoxoniobate-based compounds modified with Cu(II) amine complexes: synthesis, characterization, and catalytic studies for oxidation of styrene.
Duan, Zhi-Cheng; Li, Guanghua; Li, Ke-Chang; Cui, Xiao-Bing; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17880–17892; doi:10.1039/d4dt02544j

data_7717217
_publ_section_title
;
 Three organic-inorganic polyoxoniobate-based compounds modified with
 Cu(II) amine complexes: synthesis, characterization, and catalytic
 studies for oxidation of styrene.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17880
_journal_page_last               17892
_journal_paper_doi               10.1039/d4dt02544j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'2(K0.5 Nb12 O45 V3), C24 H64 Cu4 K N16, 4(C6 H15 Cu N4), 19(O)'
_chemical_formula_sum            'C48 H214 Cu8 K2 N32 Nb24 O109 V6'
_chemical_formula_weight         6106.50
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-21 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3856(7)
_cell_length_b                   26.3856(7)
_cell_length_c                   27.5212(19)
_cell_measurement_reflns_used    9014
_cell_measurement_temperature    299.00
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.44
_cell_volume                     19160.3(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      299.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            60533
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.362
_diffrn_reflns_theta_min         2.441
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6106
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0699 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.8194.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Brownish-Purple
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             11960
_refine_diff_density_max         4.317
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.637
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4630
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.637
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.1007
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2867
_refine_ls_wR_factor_ref         0.3811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3181
_reflns_number_total             4630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02544j2.cif
_cod_data_source_block           k_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7717215--7717217.cif.'
_cod_original_cell_volume        19160.3(17)
_cod_database_code               7717217
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C3
 2.33 with sigma of 0.04
3. Restrained planarity
 C8, C7, C1, C3
 with sigma of 0.1
4. Rigid bond restraints
 C12, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6. Others
 Fixed Sof: V3(0.5) O23(0.5) K2(0.125) O14(0.25) C1(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) H3C(0.5) O21(0.5) O19(0.125)
7.a Ternary CH refined with riding coordinates:
 C30(H30), C7(H7), C8(H8)
7.b Secondary CH2 refined with riding coordinates:
 N22(H22A,H22B), C25(H25A,H25B), N4(H4A,H4B), N1(H1A,H1B)
7.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              5794
_shelx_hkl_checksum              10557
_olex2_submission_special_instructions 'No special instructions were received'