Pyclen Tri-n-butylphosphonate Ester as Potential Chelator for Targeted Radiotherapy: From Yttrium(III) Complexation to (90)Y Radiolabeling.
Le Fur, Mariane; Beyler, Maryline; Lepareur, Nicolas; Fougère, Olivier; Platas-Iglesias, Carlos; Rousseaux, Olivier; Tripier, Raphaël; Inorganic chemistry 55 (2016) 8003–8012; doi:10.1021/acs.inorgchem.6b01135

data_4348360
_publ_section_title
;
 Pyclen Tri-n-butylphosphonate Ester as Potential Chelator for Targeted
 Radiotherapy: From Yttrium(III) Complexation to (90)Y Radiolabeling.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8003
_journal_page_last               8012
_journal_paper_doi               10.1021/acs.inorgchem.6b01135
_journal_volume                  55
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C52 H96 N8 O18 P6 Y2), 18(H2 O)'
_chemical_formula_sum            'C104 H228 N16 O54 P12 Y4'
_chemical_formula_weight         3294.33
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2015-01-27T12:32:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                116.1060(10)
_cell_angle_beta                 94.8950(10)
_cell_angle_gamma                104.1750(10)
_cell_formula_units_Z            1
_cell_length_a                   14.2900(4)
_cell_length_b                   16.5673(5)
_cell_length_c                   18.7158(5)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.33
_cell_measurement_wavelength     0.71073
_cell_volume                     3761.66(19)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
          WinGX publication routines (Farrugia, 2012),
          CRYSCALc (T. Roisnel, local program, 2014)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.089
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40870
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.742
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.712
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         17006
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.095
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+5.5547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                11584
_reflns_number_total             17006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01135_si_002.cif
_cod_data_source_block           P04176
_cod_original_cell_volume        3761.65(18)
_cod_database_code               4348360