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_7044218
_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
'C63.34 H90.69 B6 N24 O20 Y4, 10(C H4 O), 2(Cl)'
_chemical_formula_sum            'C73.35 H130.69 B6 Cl2 N24 O30 Y4'
_chemical_formula_weight         2320.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.2134(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1868(3)
_cell_length_b                   21.4815(4)
_cell_length_c                   19.6434(4)
_cell_measurement_reflns_used    23979
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      77.2420
_cell_measurement_theta_min      3.9600
_cell_volume                     5458.2(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 0.999
_diffrn_measured_fraction_theta_max 0.989
_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    -43.00 -13.00   1.00    1.45    --  -40.81 -57.00 -30.00   30
  2  \w    -50.00  35.00   1.00    1.45    --  -40.81  38.00-150.00   85
  3  \w    -36.00  70.00   1.00    1.45    --   40.81 -77.00-120.00  106
  4  \w     36.00  98.00   1.00    1.45    --   40.81-125.00-180.00   62
  5  \w     54.00  90.00   1.00   12.50    --  113.00 -30.00-150.00   36
  6  \w    103.00 133.00   1.00   12.50    --  113.00  15.00-120.00   30
  7  \w    140.00 173.00   1.00   12.50    --  113.00  15.00-120.00   33
  8  \w    143.00 178.00   1.00   12.50    --  113.00  45.00 -30.00   35
  9  \w    152.00 177.00   1.00   12.50    --  113.00 111.00 -30.00   25
 10  \w    105.00 156.00   1.00   12.50    --  113.00  30.00 120.00   51
 11  \w    110.00 136.00   1.00   12.50    --  113.00 -77.00 150.00   26
 12  \w     88.00 116.00   1.00   12.50    --  113.00-111.00 150.00   28
 13  \w     75.00 142.00   1.00   12.50    --  113.00 -77.00  60.00   67
 14  \w    112.00 138.00   1.00   12.50    --  113.00 -61.00 -30.00   26
 15  \w     96.00 121.00   1.00   12.50    --  113.00 -77.00 -60.00   25
 16  \w     82.00 114.00   1.00   12.50    --  113.00-111.00 -60.00   32
 17  \w     79.00 115.00   1.00   12.50    --  113.00-111.00-120.00   36
 18  \w     89.00 114.00   1.00   12.50    --  113.00-111.00-180.00   25
 19  \w     63.00  97.00   1.00   12.50    --  113.00-111.00 -90.00   34
 20  \w     58.00 112.00   1.00   12.50    --  113.00-111.00   0.00   54
 21  \w     71.00  97.00   1.00   12.50    --  113.00 -45.00  30.00   26
 22  \w     58.00 116.00   1.00   12.50    --  113.00-111.00  60.00   58
 23  \w     56.00  93.00   1.00   12.50    --  113.00 -77.00 150.00   37
 24  \w     48.00  96.00   1.00   12.50    --  113.00 -94.00  60.00   48
 25  \w     52.00  78.00   1.00   12.50    --  113.00 -61.00 -30.00   26
 26  \w     45.00  97.00   1.00   12.50    --  113.00 -45.00 -60.00   52
 27  \w     85.00 155.00   1.00   12.50    --  113.00  30.00 -90.00   70
 28  \w     89.00 176.00   1.00   12.50    --  113.00  77.00 -60.00   87
 29  \w     48.00  74.00   1.00   12.50    --  113.00 -77.00  60.00   26
 30  \w     41.00  91.00   1.00   12.50    --  113.00 -30.00   0.00   50
 31  \w     42.00  68.00   1.00   12.50    --  113.00-111.00-120.00   26
 32  \w     35.00  67.00   1.00   12.50    --  113.00-111.00-180.00   32
 33  \w     39.00 132.00   1.00   12.50    --  113.00 -61.00-120.00   93
 34  \w     36.00  71.00   1.00   12.50    --  113.00 -30.00 -30.00   35
 35  \w     35.00 172.00   1.00   12.50    --  113.00 -15.00-120.00  137
 36  \w     47.00  74.00   1.00   12.50    --  113.00-111.00 150.00   27
 37  \w     36.00  74.00   1.00   12.50    --  113.00 -94.00 150.00   38
 38  \w     43.00  99.00   1.00   12.50    --  113.00 -45.00 150.00   56
 39  \w    -50.00  32.00   1.00    1.45    --  -40.81  38.00 120.00   82
 40  \w   -105.00 -16.00   1.00    1.45    --  -40.81 -57.00 -60.00   89
;
_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      -0.0472401000
_diffrn_orient_matrix_UB_12      0.0610054000
_diffrn_orient_matrix_UB_13      0.0207786000
_diffrn_orient_matrix_UB_21      0.0616245000
_diffrn_orient_matrix_UB_22      0.0370946000
_diffrn_orient_matrix_UB_23      -0.0454396000
_diffrn_orient_matrix_UB_31      -0.0904242000
_diffrn_orient_matrix_UB_32      -0.0066666000
_diffrn_orient_matrix_UB_33      -0.0623633000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.592
_diffrn_reflns_theta_min         3.417
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.880
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.681
_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            'intense purple'
_exptl_crystal_colour_modifier   intense
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             2398
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.371
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         11486
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+8.2208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10142
_reflns_number_total             11486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02932b2.cif
_cod_data_source_block           5-y-meoh
_cod_original_cell_volume        5458.21(19)
_cod_database_code               7044218
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.97
_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. Shared sites
{O10A, O10B}
3. Restrained distances
 O10A-H10C
 0.85 with sigma of 0.01
 O10B-H10B
 0.82 with sigma of 0.001
 H10A-H10B
 1.34 with sigma of 0.001
 Y2-H10B
 2.85 with sigma of 0.001
 O9-H9
 0.85 with sigma of 0.01
 O15A-C37A
 1.46 with sigma of 0.02
 C37B-O15B
 1.4 with sigma of 0.001
 Y2-H10C
 2.902118 with sigma of 0.02
 C32-H10C
 1.891083 with sigma of 0.02
 C31-H9
 1.872335 with sigma of 0.02
 Y1-H9
 2.858143 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O10A) = Uanis(O10B)
Uanis(C37A) = Uanis(O15B)
Uanis(O15A) = Uanis(C37A)
Uanis(O11) = Uanis(O15B) = Uanis(O15A)
Uanis(O15B) = Uanis(C37B)
Uanis(C33) = Uanis(C37A) = Uanis(C37B)
5. Others
 1*[Sof(Cl1A)]+1*[Sof(Cl1B)]+1*[Sof(Cl1C)]=1 with esd of 0.001
 Sof(O10B)=Sof(H10A)=Sof(H10B)=Sof(O12A)=Sof(H12A)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=1-FVAR(1)
 Sof(O12B)=Sof(H12B)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(O10A)=
 Sof(H10C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(O15B)=Sof(H15B)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(2)
 Sof(O15A)=Sof(H15A)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(2)
 Fixed X: H10A(0.8348)
 Fixed Y: H10A(0.68752)
 Fixed Z: H10A(0.34091)
6.a Ternary CH refined with riding coordinates:
 B1(H1A), B2(H2A)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C9(H9A), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18)
6.c Idealised Me refined with riding coordinates:
 C37B(H37D,H37E,H37F)
6.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C34A(H34A,H34B,H34C), C33(H33A,H33B,H33C), C37A(H37A,H37B,H37C), C36(H36A,H36B,
 H36C), C35(H35A,H35B,H35C), C34B(H34D,H34E,H34F), C32(H32A,H32B,H32C)
6.e Idealised tetrahedral OH refined as rotating group:
 O12A(H12A), O11(H11A), O15A(H15A), O14(H14A), O13(H13A), O12B(H12B),
 O10A(H10C), O15B(H15B)
;
_shelx_res_checksum              11190
_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 1.756
_oxdiff_exptl_absorpt_empirical_full_min 0.543