Synthesis, Characterisation and Crystal structure of a New Cu(II)-carboxamide Complex and CuO nanoparticles as New Catalysts in the CuAAC reaction and Investigation of their Antibacterial activity
Kiani, Mahsa; Bagherzadeh, Mojtaba; Meghdadi, Soraia; Fadaei-Tirani, Farzaneh; Babaie, Maryam; Schenk-Joß, Kurt; Inorganica Chimica Acta 506 (2020) 119514–; doi:10.1016/j.ica.2020.119514

data_1565158
_publ_section_title
;
 Synthesis, Characterisation and Crystal structure of a New
 Cu(II)-carboxamide Complex and CuO nanoparticles as New Catalysts in the
 CuAAC reaction and Investigation of their Antibacterial activity
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119514
_journal_paper_doi               10.1016/j.ica.2020.119514
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         'C18 H14 Cu N6 O3 S2, C H Cl3'
_chemical_formula_sum            'C19 H15 Cl3 Cu N6 O3 S2'
_chemical_formula_weight         609.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 92.123(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8921(6)
_cell_length_b                   14.3386(6)
_cell_length_c                   16.9234(11)
_cell_measurement_reflns_used    10151
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      1.86
_cell_volume                     2398.7(2)
_computing_cell_refinement       'X_Area, 1.36 (Stoe, 2006)'
_computing_data_collection       'X_Area, 1.36 (Stoe, 2006)'
_computing_data_reduction        'X_Area, 1.36 (Stoe, 2006)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      292
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      ' 180 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.8 mm diameter'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22878
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.223
_diffrn_reflns_theta_min         1.862
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           43
_diffrn_source_power             2.365
_diffrn_source_voltage           55
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.9526
_exptl_absorpt_correction_T_min  0.6902
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Stoe XRed32 1.31, Stoe (2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       prism
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6476
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0464P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3492
_reflns_number_total             6476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-119514.cif
_cod_data_source_block           sm1
_cod_database_code               1565158
_exptl_absorpt_special_details
;
The habitus consists of a:
{101} prism,
an incomplete {0,-1,2} prism and
a {382} cut face.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Cl1A-C19 \\sim Cl1B-C19 \\sim Cl2A-C19 \\sim Cl2B-C19 \\sim Cl3A-C19 \\sim
Cl3B-C19
 with sigma of 0.02
 Cl1A-Cl2A \\sim Cl2A-Cl3A \\sim Cl3A-Cl1A \\sim Cl1B-Cl2B \\sim Cl2B-Cl3B
\\sim Cl3B-Cl1B
 with sigma of 0.02
 O3-H3A \\sim O3-H3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl1B \\sim Cl2A \\sim Cl2B \\sim Cl3A \\sim Cl3B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=Sof(H19A)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(H19)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C19(H19A)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18)
;
_shelx_res_checksum              4555
_shelx_hkl_checksum              40863
_olex2_submission_special_instructions 'No special instructions were received'