Highly Luminescent, Visible-Emitting Lanthanide Macrocyclic Chelates Stable in Water and Derived from the Cyclen Framework
Gaël Zucchi; Anne-Claire Ferrand; Rosario Scopelliti; Jean-Claude G. Bünzli; Inorganic Chemistry 41 (2002) 2459–2465; doi:10.1021/ic011121i

data_4317937
_publ_section_title
;
 Highly Luminescent, Visible-Emitting Lanthanide Macrocyclic Chelates
 Stable in Water and Derived from the Cyclen Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2459
_journal_page_last               2465
_journal_paper_doi               10.1021/ic011121i
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C48 H58 N8 O9 Tb, 3(C F3 O3 S), 2(H2 O)'
_chemical_formula_sum            'C51 H62 F9 N8 O20 S3 Tb'
_chemical_formula_weight         1533.19
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                101.37(3)
_cell_angle_beta                 96.16(3)
_cell_angle_gamma                98.60(3)
_cell_formula_units_Z            2
_cell_length_a                   13.308(3)
_cell_length_b                   14.338(3)
_cell_length_c                   16.130(3)
_cell_measurement_reflns_used    '152 spots from first image'
_cell_measurement_temperature    143(2)
_cell_volume                     2953.6(12)
_computing_cell_refinement       'marresearch marHKL, 1.9.1, 1997'
_computing_data_collection       'marresearch mar345, 1.2.11, 1999'
_computing_data_reduction        'marresearch marHKL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'marresearch mar345 IPDS'
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_sigmaI/netI    0.1063
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15797
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.356
_refine_diff_density_min         -2.127
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.0123(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   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         9262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1872
_reflns_number_gt                6503
_reflns_number_total             9262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011121i.cif
_cod_data_source_block           bunz46
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2953.5(10)
_cod_database_code               4317937