A tetra-nuclear Cu(ii) complex of amide-imine conjugate: highly-selective ESIPT-based probe for OCl−
Das, Jayanta; Ta, Sabyasachi; Das, Debasis; New Journal of Chemistry 47 (2023) 18126–18129; doi:10.1039/D3NJ02743K

data_7062700
_publ_section_title
;
 A tetra-nuclear Cu(ii) complex of amide-imine conjugate: highly-selective
 ESIPT-based probe for OCl&#x2212;
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18126
_journal_page_last               18129
_journal_paper_doi               10.1039/D3NJ02743K
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C64 H56 Cu4 N8 O16'
_chemical_formula_sum            'C64 H56 Cu4 N8 O16'
_chemical_formula_weight         1447.32
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-13
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-13 deposited with the CCDC.	2023-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   27.520(4)
_cell_length_b                   27.520(4)
_cell_length_c                   43.305(7)
_cell_measurement_temperature    150.00
_cell_volume                     28403(7)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            99736
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.458
_diffrn_reflns_theta_min         2.309
_exptl_absorpt_coefficient_mu    1.405
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_F_000             13320
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 3553 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         11175
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0467P)^2^+37.9960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                8421
_reflns_number_total             11175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02743k2.cif
_cod_data_source_block           nj-com-001861(1)
_cod_depositor_comments          'Adding full bibliography for 7062700.cif.'
_cod_original_cell_volume        28402(9)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7062700
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1A-H1A = O1B-H1B = O1C-H1C = O1D-H1D
 0.9 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C15B(H15C,H15D), C15C(H15E,H15F), C15D(H15G,H15H)
3.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C8A(H8A), C12A(H12A), C13A(H13A),
 C14A(H14A), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C8B(H8B), C12B(H12B),
 C13B(H13B), C14B(H14B), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C8C(H8C),
 C12C(H12C), C13C(H13C), C14C(H14C), C2D(H2D), C3D(H3D), C4D(H4D), C5D(H5D),
 C8D(H8D), C12D(H12D), C13D(H13D), C14D(H14D)
3.c Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C16C(H16G,H16H,H16I), C16D(H16J,
 H16K,H16L)
;
_shelx_res_checksum              59390
_olex2_submission_special_instructions 'No special instructions were received'