Slow magnetisation relaxation in tetraoxolene-bridged rare-earth complexes
Dunstan, Maja; Rousset, Elodie; Boulon, Marie-Emmanuelle; Gable, Robert William; Sorace, Lorenzo; Boskovic, Colette; Dalton Trans.  (2017) –; doi:10.1039/C7DT02932B

data_7044217
_publ_section_title
;
 Slow magnetisation relaxation in tetraoxolene-bridged rare-earth
 complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02932B
_journal_year                    2017
_chemical_formula_moiety         'C42 H40 B4 Cl2 N24 O4 Y2, 2(C3 H6 O)'
_chemical_formula_sum            'C48 H52 B4 Cl2 N24 O6 Y2'
_chemical_formula_weight         1353.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.072(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2804(4)
_cell_length_b                   15.0832(3)
_cell_length_c                   14.6373(4)
_cell_measurement_reflns_used    10029
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      76.8330
_cell_measurement_theta_min      4.2970
_cell_volume                     2997.25(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -121.00  -1.00   1.00    2.50    --  -40.81 -19.00   0.00  120
  2  \w    -46.00  -2.00   1.00    2.50    --  -40.81  38.00   0.00   44
  3  \w    -49.00  30.00   1.00    2.50    --  -40.81  38.00-180.00   79
  4  \w      2.00  52.00   1.00    2.50    --   40.81 -99.00 -90.00   50
  5  \w     58.00  84.00   1.00    2.50    --   40.81-125.00 150.00   26
  6  \w     23.00  98.00   1.00    2.50    --   40.81-125.00  60.00   75
  7  \w     31.00  89.00   1.00    2.50    --   40.81-125.00 -90.00   58
  8  \w     68.00 125.00   1.00   22.50    --  113.00 -61.00  60.00   57
  9  \w    147.00 173.00   1.00   22.50    --  113.00 111.00  60.00   26
 10  \w    103.00 138.00   1.00   22.50    --  113.00 178.00 -30.00   35
 11  \w    100.00 170.00   1.00   22.50    --  113.00  45.00-150.00   70
 12  \w     36.00  90.00   1.00   22.50    --  113.00 -30.00-180.00   54
 13  \w    136.00 161.00   1.00   22.50    --  113.00 111.00  30.00   25
 14  \w     42.00  67.00   1.00   22.50    --  113.00-111.00  90.00   25
 15  \w     76.00 112.00   1.00   22.50    --  113.00-111.00   0.00   36
 16  \w     45.00  71.00   1.00   22.50    --  113.00-111.00   0.00   26
 17  \w    107.00 133.00   1.00   22.50    --  113.00 111.00  60.00   26
 18  \w     49.00  74.00   1.00   22.50    --  113.00-111.00-120.00   25
 19  \w     87.00 114.00   1.00   22.50    --  113.00-111.00-120.00   27
 20  \w     49.00 141.00   1.00   22.50    --  113.00 -61.00 -30.00   92
 21  \w     57.00  82.00   1.00   22.50    --  113.00 -30.00-150.00   25
 22  \w     29.00  55.00   1.00   22.50    --  113.00 -94.00 120.00   26
 23  \w     74.00 109.00   1.00   22.50    --  113.00 -94.00 120.00   35
 24  \w     67.00  92.00   1.00   22.50    --  113.00 178.00  30.00   25
 25  \w    120.00 175.00   1.00   22.50    --  113.00  45.00-180.00   55
 26  \w     30.00  80.00   1.00   22.50    --  113.00 -94.00 -30.00   50
 27  \w     89.00 177.00   1.00   22.50    --  113.00  61.00 150.00   88
 28  \w    102.00 157.00   1.00   22.50    --  113.00  77.00  60.00   55
 29  \w     62.00 108.00   1.00   22.50    --  113.00 -94.00 -90.00   46
 30  \w     33.00  58.00   1.00   22.50    --  113.00 -94.00  60.00   25
 31  \w     43.00  69.00   1.00   22.50    --  113.00 -94.00   0.00   26
 32  \w     73.00 102.00   1.00   22.50    --  113.00-111.00-150.00   29
 33  \w     91.00 116.00   1.00   22.50    --  113.00-111.00  90.00   25
 34  \w     78.00 107.00   1.00   22.50    --  113.00 -94.00  60.00   29
 35  \w     39.00  74.00   1.00   22.50    --  113.00 -45.00 -30.00   35
 36  \w     61.00  87.00   1.00   22.50    --  113.00 178.00 -30.00   26
 37  \w     54.00  98.00   1.00   22.50    --  113.00 -45.00 120.00   44
 38  \w     78.00 111.00   1.00   22.50    --  113.00-111.00  30.00   33
 39  \w     89.00 175.00   1.00   22.50    --  113.00  61.00 120.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0601299000
_diffrn_orient_matrix_UB_12      -0.0056487000
_diffrn_orient_matrix_UB_13      -0.1072506000
_diffrn_orient_matrix_UB_21      -0.0961174000
_diffrn_orient_matrix_UB_22      -0.0019862000
_diffrn_orient_matrix_UB_23      0.0268136000
_diffrn_orient_matrix_UB_31      -0.0052721000
_diffrn_orient_matrix_UB_32      0.1019742000
_diffrn_orient_matrix_UB_33      -0.0054859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30166
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.185
_diffrn_reflns_theta_min         3.778
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light purple'
_exptl_crystal_colour_lustre     light
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.9334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5362
_reflns_number_total             6302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02932b2.cif
_cod_data_source_block           1-y-2me2co
_cod_original_cell_volume        2997.25(13)
_cod_database_code               7044217
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         Y2Cl2N24H4O4C42B4
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A), B2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              33374
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.443
_oxdiff_exptl_absorpt_empirical_full_min 0.724