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_7108756
_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         'C13 H20 Ga N3 O6, H O0.5'
_chemical_formula_sum            'C13 H21 Ga N3 O6.5'
_chemical_formula_weight         393.05
_chemical_name_systematic
;
?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-08-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2012.08.15 svn.r2450, GUI svn.r4314)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   28.8536(7)
_cell_length_b                   27.2438(7)
_cell_length_c                   7.57981(19)
_cell_measurement_reflns_used    6080
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.3124
_cell_measurement_theta_min      2.8181
_cell_volume                     5958.3(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 0.9981
_diffrn_measured_fraction_theta_max 0.9886
_diffrn_measurement_details
;
1 omega -67.00 14.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.7042 77.0000 0.0000 81

2 omega -108.00 28.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.7042 0.0000 -30.0000 136

3 omega -22.00 34.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.7042 19.0000 0.0000 56

4 omega 6.00 75.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 32.1729 -100.0000 75.0000 69

5 omega 56.00 99.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 32.1729 179.0000 0.0000 43

6 omega 16.00 84.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 32.1729 57.0000 150.0000 68

7 omega 56.00 118.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 32.1729 179.0000 -60.0000 62

8 omega -109.00 -3.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.7042 -38.0000 -150.0000 106
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      0.0054176000
_diffrn_orient_matrix_UB_12      0.0227335000
_diffrn_orient_matrix_UB_13      0.0406596000
_diffrn_orient_matrix_UB_21      0.0021080000
_diffrn_orient_matrix_UB_22      0.0111042000
_diffrn_orient_matrix_UB_23      -0.0842638000
_diffrn_orient_matrix_UB_31      -0.0238917000
_diffrn_orient_matrix_UB_32      0.0061148000
_diffrn_orient_matrix_UB_33      0.0017894000
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18337
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    1.888
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.430
_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    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.5901
_exptl_crystal_size_mid          0.1481
_exptl_crystal_size_min          0.0631
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4319
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0370P)^2^+0.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                4081
_reflns_number_total             4319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37544c.txt
_cod_data_source_block           '[Ga.1]_12srv162'
_cod_original_cell_volume        5958.3(2)
_cod_original_formula_sum        'C13 H21 Ga N3 O6.50'
_cod_database_code               7108756
_chemical_oxdiff_formula         'C13 H21 Ga1 N3 O7'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.93