Terbium(III) and yttrium(III) complexes with pyridine-substituted nitronyl nitroxide radical and different β-diketonate ligands. Crystal structures and magnetic and luminescence properties.
Lannes, Anthony; Intissar, Mourad; Suffren, Yan; Reber, Christian; Luneau, Dominique; Inorganic chemistry 53 (2014) 9548–9560; doi:10.1021/ic500779y

data_4340926
_publ_section_title
;
 Terbium(III) and yttrium(III) complexes with pyridine-substituted
 nitronyl nitroxide radical and different \b-diketonate ligands. Crystal
 structures and magnetic and luminescence properties.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9548
_journal_page_last               9560
_journal_paper_doi               10.1021/ic500779y
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         '2(C27 H37 N3 O8 Tb), C6 H14, H2 O'
_chemical_formula_sum            'C60 H90 N6 O17 Tb2'
_chemical_formula_weight         1485.22
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 115.621(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1941(6)
_cell_length_b                   14.3819(3)
_cell_length_c                   19.1278(4)
_cell_measurement_reflns_used    769
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.90
_cell_measurement_theta_min      3.57
_cell_volume                     6745.4(3)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection       'APEX2  (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL  (Bruker AXS, 2003)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Quazar MX'
_diffrn_radiation_source         'Incoatec I\muS Microsource '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.048
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_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9023
_diffrn_reflns_theta_full        70.74
_diffrn_reflns_theta_max         70.74
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    10.737
_exptl_absorpt_correction_T_max  0.7246
_exptl_absorpt_correction_T_min  0.5314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+19.9904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                5625
_reflns_number_total             6415
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic500779y_si_004.cif
_cod_data_source_block           rebe34
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340923--4340927.cif.
;
_cod_original_cell_volume        6745.4(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4340926