Two novel telluroniobates with efficient catalytic activity for the imidation/amidation reaction
Cheng, Mengyuan; Liu, Yufeng; Li, Nan; Shi, Jingwen; Du, Weixin; Zhang, Dongdi; Yang, Guoping; Wang, Guan; Niu, Jingyang; Chemical Communications  (2022) –; doi:10.1039/D1CC06781H

data_7129490
_publ_section_title
;
 Two novel telluroniobates with efficient catalytic activity for the
 imidation/amidation reaction
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06781H
_journal_year                    2022
_chemical_formula_moiety
'Na2 Nb14 O63 Te10, 2(C4 H12 Cu N4), 3(C4 H16 Cu N4), 7.5(O)'
_chemical_formula_sum            'C20 H72 Cu5 N20 Na2 Nb14 O70.5 Te10'
_chemical_formula_weight         4661.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-02 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.590(4)
_cell_length_b                   27.526(5)
_cell_length_c                   23.910(4)
_cell_measurement_reflns_used    9340
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.29
_cell_volume                     17500(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0567
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.997
_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       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53472
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.130
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.175
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       block
_exptl_crystal_F_000             8628
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.188
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details
;
 Flack x determined using 4312 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.072(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         15185
_refine_ls_number_restraints     400
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0537
_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^)+(0.1052P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                11573
_reflns_number_total             15185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06781h2.cif
_cod_data_source_block           12213_sq
_cod_original_formula_sum        'C20 H72 Cu5 N20 Na2 Nb14 O70.50 Te10'
_cod_database_code               7129490
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.570
_shelx_estimated_absorpt_t_min   0.450
_exptl_absorpt_special_details   blue
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C18-N10
 1.5 with sigma of 0.02
 C15-C40
 1.43 with sigma of 0.02
 C30-C31
 1.43 with sigma of 0.02
 C18-C21
 1.43 with sigma of 0.02
 N9-C15 = N6-C40 = N3-C30 = N1-C31 = N7-C21 = N10-C18 = N8-C35
 1.35 with sigma of 0.02
 C21-C18
 1.43 with sigma of 0.02
 C35-C33
 1.43 with sigma of 0.02
 N8-C35 = N7-C21 = N10-C18 = N5-C0AA = N11-C13
 1.38 with sigma of 0.02
 C40-C15
 1.45 with sigma of 0.02
 N9-C15 = N6-C40
 1.38 with sigma of 0.02
 Cu1-O34
 2.561 with sigma of 0.02
 O35-Cu1_$1
 2.561 with sigma of 0.02
 Cu3-C35
 2.895 with sigma of 0.02
 C33-Cu3
 2.895 with sigma of 0.02
 N12-C33
 1.43 with sigma of 0.02
3. Restrained planarity
 N8, N12, N7, N10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: Cu3(0.5) N7(0.5) H7A(0.5) H7B(0.5) N8(0.5) H8A(0.5) H8B(0.5)
 C18(0.5) H18A(0.5) H18B(0.5) N10(0.5) H10A(0.5) H10B(0.5) C21(0.5) H21A(0.5)
 H21B(0.5) C33(0.5) H33A(0.5) H33B(0.5) C35(0.5) H35A(0.5) H35B(0.5) O34(0.5)
 O35(0.5) N12(0.5) H12A(0.5) H12B(0.5) O37(0.25)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), N5(H5A,H5B), N6(H6A,H6B), C15(H15A,H15B), N7(H7A,
 H7B), N8(H8A,H8B), N9(H9A,H9B), C18(H18A,H18B), N10(H10A,H10B), C21(H21A,H21B),
  C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C40(H40A,H40B), C13(H13A,
 H13B), C0AA(H0AA,H0AB), C35(H35A,H35B), N11(H11A,H11B), N12(H12A,H12B), C1(H1C,
 H1D), C3(H3C,H3D)
;
_shelx_res_checksum              80282
_shelx_hkl_checksum              77941
_shelx_fab_checksum              91724
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'