Heteroleptic Copper Complexes as Catalysts for the CuAAC Reaction: Counter-Ion Influence in Catalyst Efficiency
Viana, Maria S.; Gomes, Clara S. B.; Rosa, Vitor; Catalysts 13 (2023) 386–; doi:10.3390/catal13020386

data_1568585
_publ_section_title
;
 Heteroleptic Copper Complexes as Catalysts for the CuAAC Reaction:
 Counter-Ion Influence in Catalyst Efficiency
;
_journal_issue                   2
_journal_name_full               Catalysts
_journal_page_first              386
_journal_paper_doi               10.3390/catal13020386
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C66 H58 Cu N2 P2, 3(C H Cl3), N O3'
_chemical_formula_sum            'C69 H61 Cl9 Cu N3 O3 P2'
_chemical_formula_weight         1424.73
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2253(4)
_cell_length_b                   13.2253(4)
_cell_length_c                   40.3250(19)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.40
_cell_volume                     7053.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP and Mercury'
_computing_publication_material  'WinGX and enCIFer'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            21487
_diffrn_reflns_point_group_measured_fraction_full 0.784
_diffrn_reflns_point_group_measured_fraction_max 0.766
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.749
_diffrn_reflns_theta_min         2.160
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       prism
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.0048(8)
_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   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         10328
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0611
_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^)+(0.1104P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.556
_reflns_Friedel_fraction_full    0.586
_reflns_Friedel_fraction_max     0.556
_reflns_number_gt                8353
_reflns_number_total             10328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
Ligand-L3_and_complexes_1-BF4_1-OTf_1-NO3_2-NO3_and_3-NO3.cif
_cod_data_source_block           3-NO3
_cod_original_cell_volume        7053.2(5)
_cod_database_code               1568585
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.890
_shelx_res_checksum              6683
_shelx_hkl_checksum              27000