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_7153348
_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            'C25 H43 N3 O10'
_chemical_formula_weight         545.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.327(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8810(11)
_cell_length_b                   20.9682(19)
_cell_length_c                   16.241(2)
_cell_measurement_reflns_used    25349
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      129.68
_cell_measurement_theta_min      4.21
_cell_volume                     2965.5(6)
_computing_cell_refinement       'X-Area (Stoe, 2005)'
_computing_data_collection       'X-Area (Stoe, 2005)'
_computing_data_reduction        'X-RED32 (Stoe, 2005)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       '\o oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30674
_diffrn_reflns_theta_full        58.99
_diffrn_reflns_theta_max         58.99
_diffrn_reflns_theta_min         3.49
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  7.5
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.9372
_exptl_absorpt_correction_T_min  0.8557
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0049(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4152
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+2.1814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.2198
_reflns_number_gt                2962
_reflns_number_total             4152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002796k.txt
_cod_data_source_block           yl040506
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7153348