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_7129489
_publ_section_title
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 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
'Cu3 Nb21 O96 Te15, 6(C4 H18 Cu N4 O), 1.5(C8 H32 Cu2 N8)'
_chemical_formula_sum            'C36 H106.2 Cu12 N36 Nb21 O111 Te15'
_chemical_formula_weight         7447.35
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-11-17
_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                120
_cell_formula_units_Z            2
_cell_length_a                   24.0801(4)
_cell_length_b                   24.0801(4)
_cell_length_c                   25.4757(4)
_cell_measurement_reflns_used    9392
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.52
_cell_volume                     12793.0(4)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            110906
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.328
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.622
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1007 before and 0.0641 after correction.
The Ratio of minimum to maximum transmission is 0.7955.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_description       block
_exptl_crystal_F_000             6902
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.979
_refine_diff_density_min         -2.836
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         10804
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0453P)^2^+116.6221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8973
_reflns_number_total             10804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06781h2.cif
_cod_data_source_block           te15nb21
_cod_original_cell_volume        12793.0(5)
_cod_original_formula_sum        'C36 H106.20 Cu12 N36 Nb21 O111 Te15'
_cod_database_code               7129489
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.430
_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, All N(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C3AA-C8
 1.65 with sigma of 0.02
 N0AA-C3AA
 1.54 with sigma of 0.02
 N0AA-Cu0A
 1.84 with sigma of 0.02
 C4AA-N1AA
 1.45 with sigma of 0.02
 C4AA-C11
 1.64 with sigma of 0.02
 O11_$1-Te2_$2
 2.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cu0A \\sim N2AA \\sim N1AA \\sim C8 \\sim C11 \\sim N0AA \\sim N5 \\sim C3AA
\\sim C4AA: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C2A)
\\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(N2A)
\\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(N1AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H1AA(0.5) H1AB(0.5) H1BC(0.5) H1BD(0.5) N2(0.5) H2A(0.5) H2B(0.5)
 N2A(0.5) H2AA(0.5) H2AB(0.5) H3AA(0.35) H3AB(0.35) H3BC(0.65) H3BD(0.65)
 N4(0.7) H4A(0.7) H4B(0.7) N4A(0.3) H4AA(0.3) H4AB(0.3) C1(0.5) H1A(0.5)
 H1B(0.5) C1A(0.5) H1AC(0.5) H1AD(0.5) C2(0.5) H2C(0.5) H2D(0.5) C2A(0.5)
 H2AC(0.5) H2AD(0.5) C0AA(0.7) H0AA(0.7) H0AB(0.7) C3A(0.3) H3AC(0.3) H3AD(0.3)
 C4(0.35) H4C(0.35) H4D(0.35) C4A(0.65) H4AC(0.65) H4AD(0.65) H2AE(0.5)
 H2AF(0.5) N1AA(0.5) H1AE(0.5) H1AF(0.5) H8A(0.5) H8B(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) N0AA(0.5) H0AC(0.5) H0AD(0.5) N5(0.5) H5A(0.5) H5B(0.5) C3AA(0.5)
 H3AE(0.5) H3AF(0.5) C4AA(0.5) H4AE(0.5) H4AF(0.5)
5.a Rotating group:
 O19(H19A,H19B)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1AA,H1AB), N1(H1BC,H1BD), N2(H2A,H2B), N2A(H2AA,H2AB), N3(H3AA,H3AB),
 N3(H3BC,H3BD), N4(H4A,H4B), N4A(H4AA,H4AB), C1(H1A,H1B), C1A(H1AC,H1AD),
 C2(H2C,H2D), C2A(H2AC,H2AD), C0AA(H0AA,H0AB), C3A(H3AC,H3AD), C4(H4C,H4D),
 C4A(H4AC,H4AD), N2AA(H2AE,H2AF), N1AA(H1AE,H1AF), C8(H8A,H8B), C11(H11A,H11B),
 N0AA(H0AC,H0AD), N5(H5A,H5B), C3AA(H3AE,H3AF), C4AA(H4AE,H4AF)
;
_shelx_res_checksum              94022
_shelx_hkl_checksum              75843
_shelx_fab_checksum              13249
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'