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_7717216
_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(C12 H36 Cu2 K0.5 N8 Nb12 O45 P V2), C24 H64 Cu4 K N16, 19(O)'
_chemical_formula_sum            'C48 H214 Cu8 K2 N32 Nb24 O109 P2 V4'
_chemical_formula_weight         6066.56
_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                   26.3917(6)
_cell_length_b                   26.3917(6)
_cell_length_c                   27.4474(12)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    299.00
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.44
_cell_volume                     19117.7(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36985
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.365
_diffrn_reflns_theta_min         2.440
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.585
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5968
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0655 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.8009.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Brownish-Purple
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             11896
_refine_diff_density_max         4.016
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.00003(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   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1102P)^2^+343.4725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.2061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3734
_reflns_number_total             4613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02544j2.cif
_cod_data_source_block           k_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7717215--7717217.cif.'
_cod_original_cell_volume        19117.7(12)
_cod_database_code               7717216
_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. Others
 Fixed Sof: V8(0.5) O15(0.5) K16(0.125) O18(0.25) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) O19(0.25) O16(0.125)
3.a Ternary CH refined with riding coordinates:
 C16(H16), C6(H6), C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), C11(H11A,H11B), N3(H3A,H3B), N1(H1A,H1B)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              44007
_shelx_hkl_checksum              60436
_olex2_submission_special_instructions 'No special instructions were received'