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_7108760
_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         'C29 H35 N3 O6'
_chemical_formula_sum            'C29 H35 N3 O6'
_chemical_formula_weight         521.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-12-15
_audit_creation_method
;
Olex2 1.1-beta
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.411(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8932(2)
_cell_length_b                   19.1927(5)
_cell_length_c                   15.3402(3)
_cell_measurement_reflns_used    6396
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.3699
_cell_measurement_theta_min      2.5956
_cell_volume                     2616.02(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_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_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
1 omega -70.00 32.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -28.3337 19.0000 30.0000 204

2 omega -104.00 -51.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -28.3337 -179.0000 90.0000 106

3 omega 33.00 79.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- 28.9587 -127.0000 70.0000 92

4 omega 74.00 100.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- 28.9587 -146.0000 -96.0000 52

5 omega -41.00 14.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- 28.9587 -38.0000 60.0000 110

6 omega -97.00 -7.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -28.3337 -57.0000 -150.0000 180

7 omega -98.00 -73.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -28.3337 -77.0000 90.0000 50

8 omega -98.00 2.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -28.3337 -77.0000 0.0000 200
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0347459000
_diffrn_orient_matrix_UB_12      0.0116571000
_diffrn_orient_matrix_UB_13      0.0398369000
_diffrn_orient_matrix_UB_21      -0.0164837000
_diffrn_orient_matrix_UB_22      0.0349846000
_diffrn_orient_matrix_UB_23      -0.0118482000
_diffrn_orient_matrix_UB_31      -0.0699582000
_diffrn_orient_matrix_UB_32      -0.0024582000
_diffrn_orient_matrix_UB_33      0.0203498000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28554
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.60
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0500P)^2^+0.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                5605
_reflns_number_total             7279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37544c.txt
_cod_data_source_block           '[ESI_7]_11srv256'
_cod_original_cell_volume        2616.02(11)
_cod_database_code               7108760
_chemical_oxdiff_formula         'C29 H35 N3 O6'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44