Structure and stability of hexadentate complexes of ligands based on AAZTA for efficient PET labelling with gallium-68
Bradley P. Waldron; David Parker; Carsten Burchardt; Dmitry S. Yufit; Melanie Zimny; Frank Roesch; Chem.Commun. 49 (2013) 579–; doi:10.1039/c2cc37544c

data_7108758
_publ_section_title
;
 Structure and stability of hexadentate complexes of ligands based on
 AAZTA for efficient PET labelling with gallium-68
;
_journal_name_full               Chem.Commun.
_journal_page_first              579
_journal_paper_doi               10.1039/c2cc37544c
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C17 H20 Ga N3 O6'
_chemical_formula_sum            'C17 H20 Ga N3 O6'
_chemical_formula_weight         432.08
_chemical_name_systematic
;
?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-09-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2012.08.15 svn.r2450, GUI svn.r4314)
;
_cell_angle_alpha                116.076(9)
_cell_angle_beta                 105.208(7)
_cell_angle_gamma                92.002(7)
_cell_formula_units_Z            4
_cell_length_a                   10.6961(8)
_cell_length_b                   13.0778(12)
_cell_length_c                   13.8414(12)
_cell_measurement_reflns_used    2363
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.6038
_cell_measurement_theta_min      2.5142
_cell_volume                     1652.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9941
_diffrn_measurement_details
;
1 omega -42.00 42.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -26.3429 57.0000 -30.0000 84

2 omega -98.00 18.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -26.3429 -19.0000 150.0000 116

3 omega -38.00 48.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 -57.0000 90.0000 86

4 omega 42.00 92.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 -137.0000 -79.0000 50

5 omega 58.00 85.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 179.0000 -120.0000 27

6 omega 23.00 77.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 19.0000 90.0000 54

7 omega 40.00 90.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 -137.0000 100.0000 50

8 omega -96.00 -14.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -26.3429 -77.0000 -30.0000 82
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      -0.0631794000
_diffrn_orient_matrix_UB_12      -0.0137200000
_diffrn_orient_matrix_UB_13      -0.0399767000
_diffrn_orient_matrix_UB_21      0.0273711000
_diffrn_orient_matrix_UB_22      -0.0266777000
_diffrn_orient_matrix_UB_23      -0.0447314000
_diffrn_orient_matrix_UB_31      -0.0113136000
_diffrn_orient_matrix_UB_32      -0.0534709000
_diffrn_orient_matrix_UB_33      0.0005662000
_diffrn_radiation_collimation    monochromator
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_xray_symbol    Mo
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.1285
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16836
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dull light colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.4732
_exptl_crystal_size_mid          0.1113
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                4908
_reflns_number_total             7571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37544c.txt
_cod_data_source_block           '[Ga.L3]_12srv172'
_cod_original_cell_volume        1652.8(2)
_cod_database_code               7108758
_chemical_oxdiff_formula         'C17 H23 Ga1 N3 O6'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_shelx_res_file_md5              a96b61e39cd56ae4bf144b7c9c8f6f13