Evidencing under-barrier phenomena in a Yb(iii) SMM: a joint luminescence/neutron diffraction/SQUID study
Guégan, Frédéric; Jung, Julie; Le Guennic, Boris; Riobé, François; Maury, Olivier; Gillon, Béatrice; Jacquot, Jean-François; Guyot, Yannick; Morell, Christophe; Luneau, Dominique; Inorganic Chemistry Frontiers 6 (2019) 3152–; doi:10.1039/C9QI00726A

data_4350089
_publ_section_title
;
 Evidencing under-barrier phenomena in a Yb(iii) SMM: a joint
 luminescence/neutron diffraction/SQUID study
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              3152
_journal_paper_doi               10.1039/C9QI00726A
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C18 H20 B2 N13 O3 Yb1'
_chemical_formula_sum            'C18 H20 B2 N13 O3 Yb'
_chemical_formula_weight         661.10
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2019-06-17 deposited with the CCDC.	2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.876(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7662(4)
_cell_length_b                   9.1066(2)
_cell_length_c                   17.4455(5)
_cell_measurement_reflns_used    13143
_cell_measurement_temperature    293
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     2420.81(11)
_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 0.977
_diffrn_measured_fraction_theta_max 0.901
_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  0.021
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22104
_diffrn_reflns_theta_full        25.132
_diffrn_reflns_theta_max         29.224
_diffrn_reflns_theta_min         3.013
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.914
_exptl_absorpt_correction_T_max  0.19
_exptl_absorpt_correction_T_min  0.08
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            'light white'
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.870
_exptl_crystal_size_mid          0.605
_exptl_crystal_size_min          0.418
_refine_diff_density_max         0.77
_refine_diff_density_min         -1.13
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0746
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5046
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.0016802
_refine_ls_shift/su_mean         0.0000299
_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: 
 12.7 -3.13 8.61 3.56 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0264
_refine_ls_wR_factor_gt          0.0257
_refine_ls_wR_factor_ref         0.0257
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5263
_reflns_number_total             5924
_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   0.0221
_oxford_refine_ls_scale          3.015(3)
_oxford_reflns_number_all        5912
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c9qi00726a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2420.80(12)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C18 H20 B2 N13 O3 Yb1'
_cod_database_code               4350089
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE B   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,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   ( 261,X'S) 
RIDE B   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (   1,X'S) H   (  11,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                                                                             
;