New Family of Lanthanide-Based Complexes with Different Scorpionate-Type Ligands: A Rare Case Where Dysprosium and Ytterbium Analogues Display Single-Ion-Magnet Behavior.
Lannes, Anthony; Luneau, Dominique; Inorganic chemistry 54 (2015) 6736–6743; doi:10.1021/acs.inorgchem.5b00432

data_4343507
_publ_section_title
;
 New Family of Lanthanide-Based Complexes with Different Scorpionate-Type
 Ligands: A Rare Case Where Dysprosium and Ytterbium Analogues Display
 Single-Ion-Magnet Behavior.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6736
_journal_page_last               6743
_journal_paper_doi               10.1021/acs.inorgchem.5b00432
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C24 H28 B3 Dy N16), C H2 Cl2'
_chemical_formula_sum            'C49 H58 B6 Cl2 Dy2 N32'
_chemical_formula_weight         1555.98
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.396(5)
_cell_length_b                   17.295(5)
_cell_length_c                   14.667(5)
_cell_measurement_reflns_used    6571
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     3398(2)
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.923
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14698
_diffrn_reflns_theta_full        25.129
_diffrn_reflns_theta_max         29.220
_diffrn_reflns_theta_min         2.734
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.435
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.62
_refine_ls_abs_structure_details 'Flack (1983), 1619 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.031(18)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3065
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.0012825
_refine_ls_shift/su_mean         0.0000232
_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: 
 5.41 -3.53 3.20 0.807 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0439
_refine_ls_wR_factor_gt          0.0378
_refine_ls_wR_factor_ref         0.0360
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -19
_reflns_number_gt                3313
_reflns_number_total             3913
_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   0.0344
_oxford_refine_ls_scale          0.6578(10)
_oxford_reflns_number_all        3900
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic5b00432_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4343504--4343508.cif.'
_cod_original_cell_volume        3398.1(20)
_cod_original_sg_symbol_H-M      'C m c 21 '
_cod_original_formula_sum        ' C49 H58 B6 Cl2 Dy2 N32'
_cod_database_code               4343507
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE B   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1102,X'S) 
RIDE C   ( 202,X'S) H   (2021,X'S) 
RIDE C   ( 203,X'S) H   (2031,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) 
RIDE B   ( 206,X'S) H   (2061,X'S) 
RIDE C   ( 209,X'S) H   (2091,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) 
RIDE C   ( 302,X'S) H   (3021,X'S) 
RIDE C   ( 303,X'S) H   (3031,X'S) 
RIDE C   ( 304,X'S) H   (3041,X'S) 
RIDE B   ( 306,X'S) H   (3061,X'S) H   (3062,X'S) 
RIDE C   ( 208,X'S) H   (2081,X'S) 
RIDE C   ( 401,X'S) H   (4012,X'S) H   (4011,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) 
U(IJ)'S  0.0, 0.010000 = C(209) TO C(208) 
U(IJ)'S  0.0, 0.010000 = CL(403) TO C(401) 
END                                                                             
;