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_7108757
_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_absolute_configuration ad
_chemical_formula_moiety         'C15 H24 Ga N3 O6, H2 O'
_chemical_formula_sum            'C15 H26 Ga N3 O7'
_chemical_formula_weight         430.11
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-08-31
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2012.08.15 svn.r2450, GUI svn.r4314)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.735(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.58267(20)
_cell_length_b                   12.6657(3)
_cell_length_c                   9.2185(2)
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.6015
_cell_measurement_theta_min      2.7286
_cell_volume                     869.85(4)
_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 0.9907
_diffrn_measured_fraction_theta_max 0.9934
_diffrn_measurement_details
;
1 omega -48.00 37.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- -26.3429 57.0000 -60.0000 85

2 omega -89.00 -13.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- -26.3429 -57.0000 60.0000 76

3 omega -99.00 17.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- -26.3429 -19.0000 120.0000 116

4 omega 14.00 68.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 -100.0000 -180.0000 54

5 omega -3.00 69.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 -100.0000 30.0000 72

6 omega 38.00 69.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 -100.0000 -90.0000 31

7 omega 56.00 81.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 179.0000 60.0000 25

8 omega -48.00 42.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- -26.3429 57.0000 90.0000 90

9 omega -95.00 -5.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- -26.3429 -57.0000 -60.0000 90

10 omega -45.00 -20.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 -38.0000 150.0000 25
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      0.0632984000
_diffrn_orient_matrix_UB_12      0.0344538000
_diffrn_orient_matrix_UB_13      0.0423972000
_diffrn_orient_matrix_UB_21      0.0119671000
_diffrn_orient_matrix_UB_22      0.0262069000
_diffrn_orient_matrix_UB_23      -0.0654493000
_diffrn_orient_matrix_UB_31      -0.0701211000
_diffrn_orient_matrix_UB_32      0.0355255000
_diffrn_orient_matrix_UB_33      0.0072293000
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12473
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.671
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.1521
_exptl_crystal_size_min          0.0558
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4501
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                4125
_reflns_number_total             4501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37544c.txt
_cod_data_source_block           '[Ga.L2]_12srv170'
_cod_database_code               7108757
_chemical_oxdiff_formula         'C15 H26 Ga1 N3 O7'
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44