Zirconium tetraazamacrocycle complexes display extraordinary stability and provide a new strategy for zirconium-89-based radiopharmaceutical development.
Pandya, Darpan N.; Bhatt, Nikunj; Yuan, Hong; Day, Cynthia S.; Ehrmann, Brandie M.; Wright, Marcus; Bierbach, Ulrich; Wadas, Thaddeus J.; Chemical science 8 (2017) 2309–2314; doi:10.1039/c6sc04128k

data_1544780
_publ_section_title
;
 Zirconium tetraazamacrocycle complexes display extraordinary stability
 and provide a new strategy for zirconium-89-based radiopharmaceutical
 development.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              2309
_journal_page_last               2314
_journal_paper_doi               10.1039/c6sc04128k
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C16 H32.72 N4 O12.36 Zr'
_chemical_formula_weight         570.16
_space_group_crystal_system      tetragonal
_space_group_IT_number           103
_space_group_name_Hall           'P 4 -2c'
_space_group_name_H-M_alt        'P 4 c c'
_symmetry_space_group_name_Hall  'P 4 -2c'
_symmetry_space_group_name_H-M   'P 4 c c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-26 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0201(18)
_cell_length_b                   13.0201(18)
_cell_length_c                   13.1802(19)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      3.46
_cell_volume                     2234.3(5)
_computing_cell_refinement       'Bruker APEX2 v2014.11-0'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker APEX2 v2014.11-0'
_computing_molecular_graphics    'Bruker APEX2 v2014.11-0'
_computing_publication_material  'Bruker APEX2 v2014.11-0'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39474
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.058
_diffrn_reflns_theta_min         3.465
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for scaling and absorption effects using the
 multi-scan technique (SADABS). The ratio of minimum
 to maximum apparent transmission was 0.929. The
 calculated minimum and maximum transmission
 coefficients (based on crystal size) are 0.797 and 0.962.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       needle
_exptl_crystal_F_000             1182
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.693
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 1231 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+3.3847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2866
_reflns_number_total             3278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04128k2.cif
_cod_data_source_block           a31w
_cod_depositor_comments
;Adding full bibliography for 1544780.cif.

 Adding full bibliography for 1544780.cif.
;
_cod_original_cell_volume        2234.3(7)
_cod_database_code               1544780
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.962
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS)'
_shelx_res_checksum              98663
_shelx_hkl_checksum              94814