Syntheses of bifunctional 2,3-diamino propionic acid-based chelators as small and strong tripod ligands for the labelling of biomolecules with (99m)Tc.
Liu, Yu; Oliveira, Bruno L.; Correia, João D G; Santos, Isabel C.; Santos, Isabel; Spingler, Bernhard; Alberto, Roger; Organic & biomolecular chemistry 8 (2010) 2829–2839; doi:10.1039/c002796k

data_7153346
_publ_section_title
;
 Syntheses of bifunctional 2,3-diamino propionic acid-based chelators as
 small and strong tripod ligands for the labelling of biomolecules with
 (99m)Tc.
;
_journal_issue                   12
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2829
_journal_page_last               2839
_journal_paper_doi               10.1039/c002796k
_journal_volume                  8
_journal_year                    2010
_chemical_formula_sum            'C20 H31 N3 O8'
_chemical_formula_weight         441.48
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.2196(7)
_cell_length_b                   27.2811(13)
_cell_length_c                   10.2859(4)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.3
_cell_volume                     4832.0(4)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43838
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.42
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  6
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9843
_exptl_absorpt_correction_T_min  0.9618
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+0.4575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                4011
_reflns_number_total             5312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002796k.txt
_cod_data_source_block           yl250406
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7153346