Mechanism of Magnetization Relaxation in {MIII2DyIII2} (M = Cr, Mn, Fe, Al) “Butterfly” Complexes: How Important Are the Transition Metal Ions Here?
Peng, Yan; Singh, Mukesh Kumar; Mereacre, Valeriu; Anson, Christopher; Rajaraman, Gopalan; Powell, Annie K.; Chemical Science  (2019) –; doi:10.1039/C8SC05362F

data_1550899
_publ_section_title
;
 Mechanism of Magnetization Relaxation in {MIII2DyIII2} (M = Cr, Mn, Fe,
 Al) &#x201C;Butterfly&#x201D; Complexes: How Important Are the Transition
 Metal Ions Here?
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05362F
_journal_year                    2019
_chemical_formula_moiety         'C68 H72 Al2 Dy0.18 N4 O18 Y1.82, 2(C2 H3 N)'
_chemical_formula_sum            'C72 H78 Al2 Dy0.18 N6 O18 Y1.82'
_chemical_formula_weight         1560.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-21 deposited with the CCDC.    2019-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.202(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5982(3)
_cell_length_b                   10.6800(2)
_cell_length_c                   24.4179(3)
_cell_measurement_reflns_used    12012
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.8260
_cell_measurement_theta_min      4.4290
_cell_volume                     7177.80(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0534
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -43.00   18.00   1.0000    1.1300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  102.0000  -46.4319 61

  2 omega  -30.00   70.00   1.0000    1.1300
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -180.0000 100

  3 omega   28.00  126.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000   30.0000 98

  4 omega   23.00  111.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -120.0000 88

  5 omega  -15.00   75.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  120.0000 90

  6 omega   33.00  123.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -90.0000 90

  7 omega   33.00  123.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -60.0000 90

  8 omega   36.00   93.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -150.0000 57

  9 omega   74.00  178.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000   30.0000 104

 10 omega  100.00  178.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 78

 11 omega   38.00  104.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -60.0000 66

 12 omega   36.00   93.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000    0.0000 57

 13 omega   36.00  116.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 80

 14 omega   35.00   94.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 59

 15 omega   35.00   94.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 59

 16 omega   36.00   93.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -120.0000 57

 17 omega   38.00  104.00   1.0000    4.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  120.0000 66

 18 omega  -69.00   21.00   1.0000    1.1300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 90

 19 omega  -72.00   26.00   1.0000    1.1300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000    0.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0099299000
_diffrn_orient_matrix_UB_12      0.0075639000
_diffrn_orient_matrix_UB_13      -0.0628417000
_diffrn_orient_matrix_UB_21      -0.0535309000
_diffrn_orient_matrix_UB_22      0.0327463000
_diffrn_orient_matrix_UB_23      0.0072152000
_diffrn_orient_matrix_UB_31      0.0130087000
_diffrn_orient_matrix_UB_32      0.1402264000
_diffrn_orient_matrix_UB_33      0.0017220000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.068
_diffrn_reflns_theta_min         4.441
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.810
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             3219
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+5.6915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6259
_reflns_number_total             6811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05362f3.cif
_cod_data_source_block           p1506121
_cod_database_code               1550899
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.726
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Y1, Dy1}
3. Restrained distances
 O1-H1
 0.88 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(Y1) = Uanis(Dy1)
5. Others
 Sof(Dy1)=1-FVAR(1)
 Sof(Y1)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17),
 C21(H21), C22(H22), C24(H24), C25(H25), C29(H29), C30(H30), C32(H32), C33(H33)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C), C42(H42A,H42B,
 H42C)
;
_shelx_res_checksum              21469
_olex2_submission_special_instructions 'No special instructions were received'