Synthesis,64Cu-labeling and PET imaging of 1,4,7-triazacyclononane derived chelators with pendant azaheterocyclic arms
Gotzmann, Carla; Braun, Friederike; Bartholomä, Mark D; RSC Adv.  (2015) –; doi:10.1039/C5RA21131J

data_7223478
_publ_section_title
;
 Synthesis,64Cu-labeling and PET imaging of 1,4,7-triazacyclononane
 derived chelators with pendant azaheterocyclic arms
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA21131J
_journal_year                    2015
_chemical_formula_moiety         'C18 H24 Cu N6 S3, 2(Cl O4)'
_chemical_formula_sum            'C18 H24 Cl2 Cu N6 O8 S3'
_chemical_formula_weight         683.05
_chemical_name_common            'Copper NOTThia complex perchlorate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2015-01-13 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.627(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6700(12)
_cell_length_b                   15.8947(11)
_cell_length_c                   23.4201(12)
_cell_measurement_temperature    100.0(2)
_cell_volume                     5066.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle fixed chi diffractometer'
_diffrn_measurement_device_type  'Bruker Apex-II Quazar'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51490
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         1.496
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1050 before and 0.0328 after correction.
The Ratio of minimum to maximum transmission is 0.9423.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         11650
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0338P)^2^+3.7717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10186
_reflns_number_total             11650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra21131j2.cif
_cod_data_source_block           mb_cg005_0m
_cod_database_code               7223478
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1-O4 \\sim Cl1-O3 \\sim Cl1-O1 \\sim Cl1-O1A \\sim Cl1-O2A \\sim Cl1-O2
\\sim Cl1-O3A
 with sigma of 0.02
3. Rigid bond restraints
 Cl1, O4, O1A, O2, O3, O3A, O2A, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O3A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O1) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 Cl1, O4, O1A, O2, O3, O3A, O2A, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O1A)=Sof(O3A)=Sof(O2A)=1-FVAR(1)
 Sof(O2)=Sof(O3)=Sof(O1)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C11(H11A,H11B), C15(H15A,H15B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C29(H29A,H29B), C33(H33A,H33B)
7.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C13(H13), C14(H14), C17(H17), C18(H18), C27(H27), C28(H28),
 C31(H31), C32(H32), C35(H35), C36(H36)
;
_shelx_res_checksum              8747
_olex2_submission_special_instructions 'No special instructions were received'