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_4343504
_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 Ho N16), C H2 Cl2'
_chemical_formula_sum            'C49 H58 B6 Cl2 Ho2 N32'
_chemical_formula_weight         1560.84
_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                   13.442(5)
_cell_length_b                   17.306(5)
_cell_length_c                   14.691(5)
_cell_measurement_reflns_used    4164
_cell_measurement_temperature    293
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     3418(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 0.970
_diffrn_measured_fraction_theta_max 0.897
_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  0.037
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8561
_diffrn_reflns_theta_full        25.157
_diffrn_reflns_theta_max         29.252
_diffrn_reflns_theta_min         2.773
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.436
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.58
_refine_ls_abs_structure_details 'Flack (1983), 2083 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         2990
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.0004095
_refine_ls_shift/su_mean         0.0000118
_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: 
 3.35 -1.24 2.86 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0539
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0429
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -17
_reflns_number_gt                3264
_reflns_number_total             3916
_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   0.0370
_oxford_refine_ls_scale          0.2727(6)
_oxford_reflns_number_all        3908
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic5b00432_si_004.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4343504--4343508.cif.'
_cod_original_cell_volume        3417.5(20)
_cod_original_sg_symbol_H-M      'C m c 21 '
_cod_database_code               4343504
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   ( 208,X'S) H   (2081,X'S) 
RIDE C   ( 209,X'S) H   (2091,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) 
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   (1101,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   ( 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   ( 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(11) TO C(40) 
END                                                                             
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