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_7044214
_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         'C36 H58 B4 N12 O14 Y2, 4.5(C H4 O)'
_chemical_formula_sum            'C40.5 H76 B4 N12 O18.5 Y2'
_chemical_formula_weight         1248.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-19
_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                71.183(6)
_cell_angle_beta                 81.824(6)
_cell_angle_gamma                87.703(6)
_cell_formula_units_Z            1
_cell_length_a                   10.3026(8)
_cell_length_b                   11.8817(7)
_cell_length_c                   13.8646(11)
_cell_measurement_reflns_used    4537
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      73.0170
_cell_measurement_theta_min      4.2600
_cell_volume                     1590.1(2)
_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    'ShelXT (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 0.997
_diffrn_measured_fraction_theta_max 0.967
_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   -130.00 -20.00   1.00    1.00    --  -40.81   0.00 -90.00  110
  2  \w    -50.00   9.00   1.00    1.00    --  -40.81  38.00 -90.00   59
  3  \w    -43.00  35.00   1.00    1.00    --  -40.81  38.00  90.00   78
  4  \w     32.00  81.00   1.00    1.00    --   40.81-125.00-180.00   49
  5  \w     27.00  89.00   1.00    1.00    --   40.81-125.00   0.00   62
  6  \w     61.00  87.00   1.00   15.00    --  106.63 -45.00 120.00   26
  7  \w     27.00 108.00   1.00   15.00    --  106.63 -94.00  30.00   81
  8  \w     56.00  87.00   1.00   15.00    --  106.63 -45.00 -90.00   31
  9  \w    144.00 170.00   1.00   15.00    --  106.63 125.00 -90.00   26
 10  \w     29.00  82.00   1.00   15.00    --  106.63 -30.00  90.00   53
 11  \w     94.00 127.00   1.00   15.00    --  106.63 125.00  60.00   33
 12  \w     29.00  91.00   1.00   15.00    --  106.63 -30.00  30.00   62
 13  \w     34.00  99.00   1.00   15.00    --  106.63 -45.00-150.00   65
 14  \w     46.00 107.00   1.00   15.00    --  106.63 -94.00 120.00   61
 15  \w     59.00 104.00   1.00   15.00    --  106.63 -94.00 -60.00   45
 16  \w     76.00 178.00   1.00   15.00    --  106.63  30.00   0.00  102
 17  \w    100.00 128.00   1.00   15.00    --  106.63 125.00-180.00   28
 18  \w    139.00 167.00   1.00   15.00    --  106.63 125.00-180.00   28
 19  \w     87.00 166.00   1.00   15.00    --  106.63  45.00  60.00   79
 20  \w     32.00 117.00   1.00   15.00    --  106.63-125.00 -90.00   85
;
_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      -0.0611545000
_diffrn_orient_matrix_UB_12      -0.0013313000
_diffrn_orient_matrix_UB_13      -0.0947698000
_diffrn_orient_matrix_UB_21      0.1330966000
_diffrn_orient_matrix_UB_22      -0.0363439000
_diffrn_orient_matrix_UB_23      -0.0471224000
_diffrn_orient_matrix_UB_31      -0.0369809000
_diffrn_orient_matrix_UB_32      -0.1320660000
_diffrn_orient_matrix_UB_33      0.0532986000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11043
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.915
_diffrn_reflns_theta_min         3.931
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.028
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             649
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.546
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6215
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0562
_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^)+(0.1070P)^2^+0.6110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5445
_reflns_number_total             6215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02932b2.cif
_cod_data_source_block           4-y-meoh
_cod_original_formula_sum        'C40.50 H76 B4 N12 O18.50 Y2'
_cod_database_code               7044214
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C41 H77 B4 N12 O19 Y2'
_chemical_oxdiff_usercomment     'Owens mix *(Nd, Cs, S, N O Mn)'
_reflns_odcompleteness_completeness 99.86
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7A
 0.85 with sigma of 0.01
 O7-H7B
 0.85 with sigma of 0.01
 C18-H7A
 1.873734 with sigma of 0.02
 Y1-H7A
 2.911315 with sigma of 0.02
 C19-H7B
 1.932896 with sigma of 0.02
 Y1-H7B
 2.879394 with sigma of 0.02
3. Others
 Fixed Sof: H7A(0.5) H7B(0.5) O11(0.5) H11(0.5) O12(0.5) H12(0.5) C24(0.5)
 H24A(0.5) H24B(0.5) H24C(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C18(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) O9(0.5) H9A(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) O8(0.5) H8A(0.5) C20(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5) O10(0.25) H10(0.25) C22(0.25) H22A(0.25)
 H22B(0.25) H22C(0.25)
4.a Ternary CH refined with riding coordinates:
 B1(H1A)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C8(H8), C7(H7), C6(H6), C5(H5), C9(H9), C4(H4), C3(H3)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C),
 C22(H22A,H22B,H22C)
4.d Idealised tetrahedral OH refined as rotating group:
 O11(H11), O12(H12), O9(H9A), O8(H8A), O10(H10)
;
_shelx_res_checksum              42856
_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 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.778