Octadentate Cages of Tb(III) 2-Hydroxyisophthalamides: A New Standard for Luminescent Lanthanide Labels
Jide Xu; Todd M. Corneillie; Evan G. Moore; Ga-Lai Law; Nathaniel G. Butlin; Kenneth N. Raymond; Journal of the American Chemical Society 133 (2011) 19900–19910; doi:10.1021/ja2079898

data_4107193
_publ_contact_author             'Kenneth N. Raymond'
_publ_contact_author_email       raymond@socrates.berkeley.edu
_publ_section_title
;
 Octadentate Cages of Tb(III) 2-Hydroxyisophthalamides: A New Standard for
 Luminescent Lanthanide Labels
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19900
_journal_page_last               19910
_journal_paper_doi               10.1021/ja2079898
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C56 H72 N12 O12, C6 H15 N, H Cl, H2 O'
_chemical_formula_sum            'C62 H90 Cl N13 O13'
_chemical_formula_weight         1260.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 122.1540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.4197(11)
_cell_length_b                   13.7261(4)
_cell_length_c                   30.1648(9)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.358
_cell_measurement_theta_min      2.648
_cell_volume                     13818.1(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            59580
_diffrn_reflns_theta_full        68.39
_diffrn_reflns_theta_max         68.39
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  0.9304
_exptl_absorpt_correction_T_min  0.8505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       needle
_exptl_crystal_F_000             5392
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         12464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+22.2082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                11214
_reflns_number_total             12464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2079898_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4107193