Evaluation of H2CHXdedpa, H2dedpa- and H2CHXdedpa-N,N'-propyl-2-NI ligands for (64)Cu(ii) radiopharmaceuticals.
Ramogida, Caterina F.; Boros, Eszter; Patrick, Brian O.; Zeisler, Stefan K.; Kumlin, Joel; Adam, Michael J.; Schaffer, Paul; Orvig, Chris; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13082–13090; doi:10.1039/c6dt00932h

data_7702071
_publ_section_title
;
 Evaluation of H2CHXdedpa, H2dedpa- and H2CHXdedpa-N,N'-propyl-2-NI
 ligands for (64)Cu(ii) radiopharmaceuticals.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13082
_journal_page_last               13090
_journal_paper_doi               10.1039/c6dt00932h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C28 H29.81 Cu N10 O8, 4.19(H2 O)'
_chemical_formula_sum            'C28 H38.19 Cu N10 O12.19'
_chemical_formula_weight         773.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2013-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2016-03-07 deposited with the CCDC.
2016-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1713(14)
_cell_length_b                   15.9359(16)
_cell_length_c                   31.481(3)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.39
_cell_volume                     6607.8(12)
_computing_data_reduction        'SAINT v8.27B (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55297
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.055
_diffrn_reflns_theta_min         2.016
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0494 before and 0.0449 after correction.
The Ratio of minimum to maximum transmission is 0.9083.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       blade
_exptl_crystal_F_000             3222
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         9684
_refine_ls_number_restraints     1365
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0437P)^2^+2.3837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7216
_reflns_number_total             9684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00932h2.cif
_cod_data_source_block           co455
_cod_database_code               7702071
_shelxl_version_number           2013-3
_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
 N5-C19 \\sim N5A-C19A
 with sigma of 0.01
 C19-C18 \\sim C19A-C18A
 with sigma of 0.01
 C18-C17 \\sim C18A-C17A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
Uanis(C27A) = Uanis(C27)
Uanis(N8A) = Uanis(N8)
Uanis(C28A) = Uanis(C28)
Uanis(O7A) = Uanis(O7)
Uanis(N10A) = Uanis(N10)
Uanis(O8A) = Uanis(O8)
Uanis(C21) = Uanis(C21A)
Uanis(C20) = Uanis(C20A)
Uanis(N6) = Uanis(N6A)
Uanis(C22) = Uanis(C22A)
Uanis(O5) = Uanis(O5A)
Uanis(N7A) = Uanis(N7)
Uanis(C19A) = Uanis(C19A)
Uanis(N5) = Uanis(N5A)
Uanis(C24A) = Uanis(C24)
Uanis(C23A) = Uanis(C23)
Uanis(C19) = Uanis(C19A)
Uanis(C18) = Uanis(C18A)
Uanis(C17A) = Uanis(C17)
Uanis(N9) = Uanis(N9A)
4. Others
 Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=
 Sof(H25C)=Sof(H25D)=Sof(O7A)=Sof(O8A)=Sof(N8A)=Sof(N9A)=Sof(N10A)=Sof(C26A)=
 Sof(H26A)=Sof(C27A)=Sof(C28A)=Sof(O13)=Sof(H13A)=Sof(H13B)=Sof(C18A)=Sof(H18C)=
 Sof(H18D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(O7)=
 Sof(O8)=Sof(N8)=Sof(N9)=Sof(N10)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=
 FVAR(1)
 Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(N7A)=Sof(O5A)=Sof(C22A)=Sof(N6A)=Sof(C21A)=
 Sof(H21A)=Sof(C20A)=Sof(H20A)=Sof(N5A)=Sof(O4A)=1-FVAR(2)
 Sof(O5)=Sof(O6)=Sof(N5)=Sof(N6)=Sof(N7)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=
 Sof(C22)=Sof(C19)=Sof(H19C)=Sof(H19D)=FVAR(2)
5.a Free rotating group:
 O9(H9C,H9D,O10,H10C,H10D,O11,H11A,H11B,O12,H12A,H12B), O13(H13A,H13B)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C17(H17A,H17B),
 C18(H18A,H18B), C19A(H19A,H19B), C23(H23A,H23B), C23A(H23C,H23D), C24(H24A,
 H24B), C24A(H24C,H24D), C25(H25A,H25B), C25A(H25C,H25D), C19(H19C,H19D),
 C18A(H18C,H18D), C17A(H17C,H17D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C20(H20), C21(H21),
 C26(H26), C27(H27), C26A(H26A), C21A(H21A), C20A(H20A)
;
_shelx_res_checksum              55007