Unsymmetrical Tripodal Ligand for Lanthanide Complexation: Structural, Thermodynamic, and Photophysical Studies
Badr El Aroussi; Nathalie Dupont; Gérald Bernardinelli; Josef Hamacek; Inorganic Chemistry 49 (2010) 606–615; doi:10.1021/ic901757u

data_4314546
_publ_contact_author
;
     Dr. Josef Hamacek'
     Department of Inorganic, Analytical 
     and Applied Chemistry
     University of Geneva
     30, quai E. Ansermet
     CH - 1211 Geneva 4
     Switzerland
;
_publ_contact_author_email       Josef.Hamacek@unige.ch
_publ_contact_author_phone       '41 22 379 6413'
_publ_section_title
;
 Unsymmetrical Tripodal Ligand for Lanthanide Complexation: Structural,
 Thermodynamic, and Photophysical Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              606
_journal_page_last               615
_journal_paper_doi               10.1021/ic901757u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C34 H44 N8 O5, O '
_chemical_formula_sum            'C34 H44 N8 O6'
_chemical_formula_weight         660.77
_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
_cell_angle_alpha                83.771(9)
_cell_angle_beta                 84.412(9)
_cell_angle_gamma                73.686(9)
_cell_formula_units_Z            2
_cell_length_a                   9.5730(11)
_cell_length_b                   12.8128(15)
_cell_length_c                   15.5018(18)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1809.6(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR 2004'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Unknown
_diffrn_measurement_device_type  Serial
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37126
_diffrn_reflns_theta_full        27.489
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         2.579
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9802
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         3317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.0001049
_refine_ls_shift/su_mean         2.9821966
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./2F 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1415
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0747
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                3317
_reflns_number_total             8329
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.90
_oxford_diffrn_Wilson_scale      156.54
_oxford_refine_ls_r_factor_ref   0.0709
_oxford_refine_ls_scale          0.7348(16)
_oxford_reflns_number_all        8329
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ic901757u_si_003.cif
_cod_data_source_block           1
_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_sg_symbol_H-M      'P -1 '
_cod_database_code               4314546