Complexation of Trivalent Lanthanides with Planar Tridentate Aromatic Ligands Tuned by Counteranions and Steric Constraints
Aude Escande; Laure Guénée; Kerry-Lee Buchwalder; Claude Piguet; Inorganic Chemistry 48 (2009) 1132–1147; doi:10.1021/ic801908c

data_4301336
_publ_contact_author_address
;Department of Inorganic, Analytical and Applied Chemistry
University of Geneva
30 quai E. Ansermet
CH-1211 Geneva 4
Switzerland
;
_publ_contact_author_email       Laure.Guenee@unige.ch
_publ_contact_author_fax         41(22)3796830
_publ_contact_author_name        'Laure Gu\'en\'ee'
_publ_contact_author_phone       41(22)3796411
_publ_section_title
;
Complexation of Trivalent Lanthanides with Planar Tridentate Aromatic
Ligands Tuned by Counteranions and Steric Constraints
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1132
_journal_page_last               1147
_journal_paper_doi               10.1021/ic801908c
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C25 H35 Lu N5 O7, C N O2, 3(Cl)'
_chemical_formula_sum            'C26 H35 Cl3 Lu N6 O9'
_chemical_formula_weight         856.92
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2589(3)
_cell_length_b                   17.8918(10)
_cell_length_c                   22.0679(9)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      3.9
_cell_volume                     3260.9(3)
_computing_cell_refinement       'CELL (Stoe & Cie, 1999)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1999)'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Stoe Ipds'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23177
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         2.17
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.332
_exptl_absorpt_correction_T_max  0.8543
_exptl_absorpt_correction_T_min  0.7302
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED; Stoe & Cie, 1999'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1708
_exptl_crystal_recrystallization_method 'recrystallised from nitromethane'
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.067(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0392
_reflns_number_gt                5627
_reflns_number_total             6179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801908c_si_001_2.cif
_cod_data_source_block           1
_cod_database_code               4301336