Highly inert Cu(ii) complexes of C-aryl bifunctional cyclam-picolinates with remarkable 64Cu-labelling and biodistribution
Pineau, Julie; Lima, Luís M. P.; Le Roy, Marie M.; Marionneau-Lambot, Séverine; Cordier, Marie; Le Saëc, Patricia; Zeevaart, Jan Rijn; Driver, Cathryn H. S.; Faivre-Chauvet, Alain; Le Bris, Nathalie; Tripier, Raphaël; Chemical Communications 59 (2023) 888–891; doi:10.1039/D2CC06602E

data_7131162
_publ_section_title
;
 Highly inert Cu(ii) complexes of C-aryl bifunctional cyclam-picolinates
 with remarkable 64Cu-labelling and biodistribution
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              888
_journal_page_last               891
_journal_paper_doi               10.1039/D2CC06602E
_journal_volume                  59
_journal_year                    2023
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H34 Cu N8 O4, 4.75(H2 O)'
_chemical_formula_sum            'C24 H43.5 Cu N8 O8.75'
_chemical_formula_weight         647.70
_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
_audit_update_record
;
2022-09-06 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.393(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.6398(8)
_cell_length_b                   22.4361(9)
_cell_length_c                   30.5104(15)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4624
_cell_measurement_theta_min      2.1952
_cell_measurement_wavelength     0.710730
_cell_volume                     11295.8(9)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_molecular_graphics
;
   'PLATON, A.L.Spek, Acta Cryst. 2009, D65, 148-155'
;
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2021)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      0.0205686
_diffrn_orient_matrix_UB_12      0.0052702
_diffrn_orient_matrix_UB_13      0.0320290
_diffrn_orient_matrix_UB_21      0.0372062
_diffrn_orient_matrix_UB_22      -0.0347411
_diffrn_orient_matrix_UB_23      -0.0014709
_diffrn_orient_matrix_UB_31      0.0431866
_diffrn_orient_matrix_UB_32      0.0274201
_diffrn_orient_matrix_UB_33      -0.0080196
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            85151
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.736
_diffrn_source_current           1.00
_diffrn_source_power             1500.0
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       prism
_exptl_crystal_F_000             5480
_exptl_crystal_size_max          0.640
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.225
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1630
_refine_ls_number_reflns         25753
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      18.666
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+16.2407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                20336
_reflns_number_total             25753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2cc06602e2.cif
_cod_data_source_block           JP288
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H174 Cu4 N32 O35'
_cod_original_formula_weight         2590.82
_cod_original_formula_moiety         '4(C24 H34 Cu N8 O4), 19(H2 O)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7131162
_shelx_res_checksum              51454
_shelx_hkl_checksum              59870