Lower Denticity Leading to Higher Stability: Structural and Solution Studies of Ln(III)-OBETA Complexes.
Negri, Roberto; Baranyai, Zsolt; Tei, Lorenzo; Giovenzana, Giovanni B.; Platas-Iglesias, Carlos; Bényei, Attila C; Bodnár, Judit; Vágner, Adrienn; Botta, Mauro; Inorganic chemistry  (2014) 141111091549002–; doi:10.1021/ic5020225

data_4341585
_publ_section_title
;
 Lower Denticity Leading to Higher Stability: Structural and Solution
 Studies of Ln(III)-OBETA Complexes.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141111091549002
_journal_paper_doi               10.1021/ic5020225
_journal_year                    2014
_chemical_formula_moiety         'C16 H38 Lu1 N11 O14'
_chemical_formula_sum            'C16 H38 Lu N11 O14'
_chemical_formula_weight         783.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-05-23T20:43:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.600(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4880(18)
_cell_length_b                   14.232(5)
_cell_length_c                   20.620(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.1
_cell_measurement_theta_min      6.2
_cell_volume                     2778.9(11)
_computing_cell_refinement       'MACH3/PC (Enraf Nonius, 1996)'
_computing_data_collection       'MACH3/PC (Enraf Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius MACH3'
_diffrn_measurement_method       'non-profiled \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5889
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         2.583
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 196
_diffrn_standards_interval_time  130
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.637
_exptl_absorpt_correction_T_max  0.6902
_exptl_absorpt_correction_T_min  0.2837
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        Fourier smoothing - Window value   5
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.238
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+12.6356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                4631
_reflns_number_total             5098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5020225_si_001.cif
_cod_data_source_block           1432a
_cod_database_code               4341585
_exptl_absorpt_factor_mur        0.364