iClick reaction of Cu(II) azido complex having Schiff base ligand
Shrivastav, Akash; Bhattacharya, Subrato; Chemical Communications  (2026) –; doi:10.1039/D6CC00423G

data_7135612
_publ_section_title
;
 iClick reaction of a Cu(II) azido complex having a Schiff base ligand.
;
_journal_issue                   30
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7750
_journal_page_last               7754
_journal_paper_doi               10.1039/d6cc00423g
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C23 H26 Cu F3 N5 O3, C H Cl3'
_chemical_formula_sum            'C24 H27 Cl3 Cu F3 N5 O3'
_chemical_formula_weight         660.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-10 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.76640(10)
_cell_length_b                   14.57750(10)
_cell_length_c                   20.2849(2)
_cell_measurement_reflns_used    23319
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9000
_cell_measurement_theta_min      2.2020
_cell_volume                     2887.96(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -26.00  61.00   0.50    0.23    --   40.83 -54.00   0.00  174
  2  \w    -26.00  40.00   0.50    0.23    --   40.83 -35.00  -2.00  132
  3  \w    -31.00  28.00   0.50    0.23    --   40.83 -21.00-150.00  118
  4  \w    100.00 167.00   0.50    0.91    --   96.04  88.00 -27.00  134
  5  \w     99.00 160.00   0.50    0.91    --   96.04 117.00  60.00  122
  6  \w    -35.00  24.00   0.50    0.23    --   40.83 -11.00 -90.00  118
  7  \w    -22.00  72.00   0.50    0.23    --   40.83 -88.00-143.00  188
  8  \w     26.00 127.00   0.50    0.91    --   96.04 -88.00-143.00  202
  9  \w     50.00 134.00   0.50    0.91    --   96.04-157.00 -15.00  168
 10  \w     41.00 100.00   0.50    0.23    --   40.83-138.00  60.00  118
 11  \w     30.00  85.00   0.50    0.23    --   40.83-119.00 138.00  110
 12  \w     33.00 110.00   0.50    0.91    --   96.04-119.00 138.00  154
 13  \w     28.00  68.00   0.50    0.91    --   96.04 -59.00 150.00   80
 14  \w     28.00  68.00   0.50    0.91    --   96.04 -59.00  90.00   80
 15  \w     28.00  68.00   0.50    0.91    --   96.04 -59.00 120.00   80
 16  \w     28.00  68.00   0.50    0.91    --   96.04 -59.00   0.00   80
 17  \w     29.00  57.00   0.50    0.91    --   96.04 -50.00 -30.00   56
 18  \w     29.00  57.00   0.50    0.91    --   96.04 -50.00 -90.00   56
 19  \w     28.00  68.00   0.50    0.91    --   96.04 -59.00-150.00   80
 20  \w     72.00 110.00   0.50    0.91    --   96.04  68.00 -60.00   76
 21  \w     77.00 163.00   0.50    0.91    --   96.04  50.00 -90.00  172
 22  \w     74.00 163.00   0.50    0.91    --   96.04  59.00-150.00  178
 23  \w     82.00 163.00   0.50    0.91    --   96.04  35.00 154.00  162
 24  \w     14.00 110.00   0.50    0.23    --   40.83  77.00  90.00  192
 25  \w     14.00 110.00   0.50    0.23    --   40.83  77.00  30.00  192
 26  \w     21.00 108.00   0.50    0.23    --   40.83  54.00-120.00  174
 27  \w     18.00 109.00   0.50    0.23    --   40.83  65.00-180.00  182
 28  \w   -108.00 -28.00   0.50    0.91    --  -82.50 157.00  18.00  160
 29  \w    -85.00  -8.00   0.50    0.23    --  -40.83 119.00-136.00  154
 30  \w    -71.00  30.00   0.50    0.23    --  -40.83  88.00 -27.00  202
 31  \w   -113.00 -12.00   0.50    0.91    --  -82.50  88.00 -27.00  202
 32  \w    -57.00 -16.00   0.50    0.91    --  -82.50  50.00 120.00   82
 33  \w    -40.00  26.00   0.50    0.23    --  -40.83  35.00 154.00  132
 34  \w   -108.00 -26.00   0.50    0.23    --  -40.83 -35.00  -2.00  164
 35  \w   -109.00 -14.00   0.50    0.23    --  -40.83 -77.00-120.00  190
 36  \w   -109.00 -14.00   0.50    0.23    --  -40.83 -77.00 -90.00  190
 37  \w   -108.00 -17.00   0.50    0.23    --  -40.83 -65.00 -60.00  182
 38  \w   -108.00 -17.00   0.50    0.23    --  -40.83 -65.00 -30.00  182
 39  \w   -108.00 -21.00   0.50    0.23    --  -40.83 -54.00  90.00  174
 40  \w   -109.00 -14.00   0.50    0.23    --  -40.83 -77.00 150.00  190
 41  \w   -109.00 -14.00   0.50    0.23    --  -40.83 -77.00  60.00  190
 42  \w   -149.00 -68.00   0.50    0.91    --  -82.50 -35.00  -2.00  162
 43  \w   -153.00 -78.00   0.50    0.91    --  -82.50 -88.00-143.00  150
 44  \w   -150.00 -58.00   0.50    0.91    --  -82.50 -68.00  90.00  184
 45  \w   -109.00 -51.00   0.50    0.23    --  -40.83-157.00 -15.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1563967000
_diffrn_orient_matrix_UB_12      0.0110245000
_diffrn_orient_matrix_UB_13      0.0061010000
_diffrn_orient_matrix_UB_21      -0.0042040000
_diffrn_orient_matrix_UB_22      0.0461474000
_diffrn_orient_matrix_UB_23      -0.0682962000
_diffrn_orient_matrix_UB_31      -0.0203332000
_diffrn_orient_matrix_UB_32      -0.0944134000
_diffrn_orient_matrix_UB_33      -0.0326497000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32619
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.093
_diffrn_reflns_theta_min         4.359
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1879 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+0.4137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                4776
_reflns_number_total             5146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00423g2.cif
_cod_data_source_block           akr-79_auto
_cod_depositor_comments
'Adding full bibliography for 7135607--7135612.cif.'
_cod_original_cell_volume        2887.95(5)
_cod_database_code               7135612
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Cu H N O F'
_shelx_estimated_absorpt_t_max   0.661
_shelx_estimated_absorpt_t_min   0.525
_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 C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C20(H20A,H20B), C18(H18A,H18B), C19(H19A,H19B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C17(H17), C14(H14), C9(H9), C13(H13), C12(H12), C11(H11)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              56114
_shelx_hkl_checksum              47609
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.054
_oxdiff_exptl_absorpt_empirical_full_min 0.756