Stable Lanthanide Luminescence Agents Highly Emissive in Aqueous Solution: Multidentate 2-Hydroxyisophthalamide Complexes of Sm3+, Eu3+, Tb3+, Dy3+
Stéphane Petoud; Seth M. Cohen; Jean-Claude G. Bünzli; Kenneth N. Raymond; Journal of the American Chemical Society 125 (2003) 13324–13325; doi:10.1021/ja0379363

data_4114327
_publ_contact_author
;
      Kenneth N. Raymond
      Department of Chemistry
      University of California
      Berkeley
      CA 94720-1460
      USA
;
_publ_contact_author_email       raymond@socrates.berkeley.edu
_publ_contact_author_fax         '1 510 4865283'
_publ_contact_author_phone       '1 510 6427219'
_publ_section_title
;
 Stable Lanthanide Luminescence Agents Highly Emissive in Aqueous
 Solution: Multidentate 2-Hydroxyisophthalamide Complexes of Sm3+, Eu3+,
 Tb3+, Dy3+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13324
_journal_page_last               13325
_journal_paper_doi               10.1021/ja0379363
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        synthetic
_chemical_formula_sum            'C36 H41 Br0.25 Cl0.25 Eu0.5 N8 O9'
_chemical_formula_weight         834.59
_chemical_name_common            'Europium Macrobicyclic TRENSAM '
_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
_cell_angle_alpha                78.8210(10)
_cell_angle_beta                 73.0720(10)
_cell_angle_gamma                72.5120(10)
_cell_formula_units_Z            4
_cell_length_a                   14.8309(2)
_cell_length_b                   16.4624(2)
_cell_length_c                   21.0129(2)
_cell_measurement_reflns_used    12883
_cell_measurement_temperature    176(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      1.02
_cell_volume                     4649.28(10)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL XP'
_computing_publication_material  'Siemens SHELXTL XL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      176(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19257
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       'Transparent Blocks'
_exptl_crystal_F_000             1718
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.879
_refine_diff_density_min         -1.853
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.0031(7)
_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_all   1.133
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         12883
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.132
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.1646
_refine_ls_R_factor_obs          0.1348
_refine_ls_shift/esd_max         -1.993
_refine_ls_shift/esd_mean        0.063
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1908P)^2^+68.4753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3893
_refine_ls_wR_factor_obs         0.3411
_reflns_number_observed          10199
_reflns_number_total             12886
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0379363si20030919_103112.cif
_cod_data_source_block           Eu[macrobicyclicTRENSAM]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1908P)^2^+68.4753P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1908P)^2^+68.4753P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4649.29(10)
_cod_original_formula_sum        'C36 H41 Br0.25 Cl0.25 Eu0.50 N8 O9'
_cod_database_code               4114327