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_4340924
_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_formula_moiety         'C27 H37 N3 O8 Tb, 0.5(H2 O)'
_chemical_formula_sum            'C27 H38 N3 O8.5 Tb'
_chemical_formula_weight         699.54
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 114.947(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.5929(7)
_cell_length_b                   14.5138(3)
_cell_length_c                   19.3570(6)
_cell_measurement_reflns_used    5961
_cell_measurement_temperature    293
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     7028.8(4)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21178
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         29.442
_diffrn_reflns_theta_min         2.923
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.057
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.983
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0608
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5961
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.0191093
_refine_ls_shift/su_mean         0.0000941
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 18.6 -13.1 14.8 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0584
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0410
_reflns_limit_h_max              32
_reflns_limit_h_min              -37
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6445
_reflns_number_total             8397
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0358
_oxford_refine_ls_scale          1.0979(14)
_oxford_reflns_number_all        8381
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic500779y_si_005.cif
_cod_data_source_block           1
_cod_depositor_comments
;
Adding full bibliography for 4340923--4340927.cif.

2021-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_moiety     '2(C27 H37 N3 O8 Tb), H2 O'
_cod_original_formula_sum        'C54 H76 N6 O17 Tb2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1399.08
_cod_database_code               4340924
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE O   (  13,X'S) H   (   1,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 153,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 161,X'S) H   ( 163,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 183,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 193,X'S) H   ( 192,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 262,X'S) H   ( 261,X'S) H   ( 263,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 303,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 313,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 353,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) H   ( 363,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 401,X'S) H   ( 403,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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