Luminescent Cell-Penetrating Pentadecanuclear Lanthanide Clusters
Dominique T. Thielemann; Anna T. Wagner; Esther Rösch; Dominik K. Kölmel; Joachim G. Heck; Birgit Rudat; Marco Neumaier; Claus Feldmann; Ute Schepers; Stefan Bräse; Peter W. Roesky; Journal of the American Chemical Society 135 (2013) 7454–7457; doi:10.1021/ja403539t

data_4119797
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT)
      Institut fuer Anorganische Chemie
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_publ_contact_author_email       roesky@kit.edu
_publ_contact_author_fax         '+49 721 6084854'
_publ_contact_author_phone       '+49 721 6086117'
_publ_section_title
;
 Luminescent Cell-Penetrating Pentadecanuclear Lanthanide Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7454
_journal_page_last               7457
_journal_paper_doi               10.1021/ja403539t
_journal_volume                  135
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C300 H340 Cl5 N20 O80 Tb15, 3(C3 H7 N O), 3(H2 O)'
_chemical_formula_sum            'C309 H367 Cl5 N23 O86 Tb15'
_chemical_formula_weight         8340.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             10-10-20
_audit_creation_method           'STOE X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.264(5)
_cell_length_b                   47.896(10)
_cell_length_c                   31.413(6)
_cell_measurement_reflns_used    67625
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      1.04
_cell_volume                     37179(13)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2.1e/3'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1610
_diffrn_reflns_av_sigmaI/netI    0.1909
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            247534
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         1.04
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.920
_exptl_absorpt_correction_T_max  0.8323
_exptl_absorpt_correction_T_min  0.4292
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       plate
_exptl_crystal_F_000             16520
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2895
_refine_ls_number_reflns         62084
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.1648
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          11.449
_refine_ls_shift/su_mean         0.137
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1620
_reflns_number_gt                24102
_reflns_number_total             62084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja403539t_si_002.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4119797