Novel cyano-activated Cu(ii) complexes of arylhydrazones of active methylene nitriles and their catalytic application for azide–alkyne cycloaddition in water and glycerol
Gurbanov, Atash V.; Mahmoud, Abdallah G.; Aliyeva, Vusala A.; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J. L.; New Journal of Chemistry 47 (2023) 7965–7974; doi:10.1039/D3NJ00512G

data_7062378
_publ_section_title
;
 Novel cyano-activated Cu(ii) complexes of arylhydrazones of active
 methylene nitriles and their catalytic application for azide--alkyne
 cycloaddition in water and glycerol
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7965
_journal_page_last               7974
_journal_paper_doi               10.1039/D3NJ00512G
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C44 H34 Cu3 N12 O10 [+ solvent]'
_chemical_formula_sum            'C44 H34 Cu3 N12 O10'
_chemical_formula_weight         1081.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2023-01-05 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.999(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.947(5)
_cell_length_b                   8.1219(10)
_cell_length_c                   20.211(2)
_cell_measurement_reflns_used    3655
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.31
_cell_measurement_theta_min      2.60
_cell_volume                     4969.0(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Quest PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35267
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.598
_diffrn_reflns_theta_min         3.031
_exptl_absorpt_coefficient_mu    1.338
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       prism
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0856P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2508
_reflns_number_total             4626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00512g2.cif
_cod_data_source_block           AK38
_cod_depositor_comments
'Adding full bibliography for 7062374--7062378.cif.'
_cod_original_cell_volume        4969.1(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7062378
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.814
_shelx_estimated_absorpt_t_max   0.878
_shelx_res_checksum              65984
_shelx_fab_checksum              43252