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_7717215
_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 O45.75 Si V4.25), C24 H64 Cu4 K N16, C24 H72 Cu4 N16, 18(O)'
_chemical_formula_sum            'C48 H199 Cu8 K2 N32 Nb24 O109.5 Si2 V8.5'
_chemical_formula_weight         6282.91
_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                   26.3310(12)
_cell_length_b                   26.3310(12)
_cell_length_c                   27.573(4)
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      63.87
_cell_measurement_theta_min      3.36
_cell_volume                     19117(3)
_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      273.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28531
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        63.965
_diffrn_reflns_theta_max         63.965
_diffrn_reflns_theta_min         2.373
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    16.827
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.2514
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1335 before and 0.0664 after correction.
The Ratio of minimum to maximum transmission is 0.3341.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Brownish-purple
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             12258
_refine_diff_density_max         1.400
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       0.000016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4164
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+543.5092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3295
_reflns_number_total             4164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02544j2.cif
_cod_data_source_block           k
_cod_depositor_comments
'Adding full bibliography for 7717215--7717217.cif.'
_cod_original_formula_sum        'C48 H199 Cu8 K2 N32 Nb24 O109.50 Si2 V8.50'
_cod_database_code               7717215
_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. Rigid bond restraints
 C7, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: K2(0.125) O1(0.25) V3(0.0625) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
 C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) O4(0.0625) O3(0.25) O8(0.125)
5.a Ternary CH refined with riding coordinates:
 C31(H31), C32(H32), C36(H36)
5.b Secondary CH2 refined with riding coordinates:
 N27(H27A,H27B), N28(H28A,H28B), N29(H29A,H29B), C30(H30A,H30B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              33399
_shelx_hkl_checksum              17363
_olex2_submission_special_instructions 'No special instructions were received'