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_1550898
_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 Dy2 Mn2 N4 O18, 2(C H4 O), C2 H3 N'
_chemical_formula_sum            'C72 H83 Dy2 Mn2 N5 O20'
_chemical_formula_weight         1773.31
_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     '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                111.771(2)
_cell_angle_beta                 93.386(2)
_cell_angle_gamma                110.092(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1952(2)
_cell_length_b                   13.2472(3)
_cell_length_c                   14.6071(3)
_cell_measurement_reflns_used    14388
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      70.7190
_cell_measurement_theta_min      3.9010
_cell_volume                     1845.67(8)
_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      180.01(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 0.986
_diffrn_measurement_details
;
  1 omega  -70.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -60.0000 100

  2 omega  -36.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   88.0000   84.0000 69

  3 omega  -21.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 90

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

  5 omega  -19.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -19.0000  -90.0000 117

  6 omega   33.00  123.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -120.0000 90

  7 omega   23.00  111.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   60.0000 88

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

  9 omega  -16.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -120.0000 100

 10 omega   23.00  111.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 88

 11 omega   36.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 80

 12 omega   99.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   88.0000   84.0000 79

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

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

 15 omega   38.00  138.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 100

 16 omega   35.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 59

 17 omega   86.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -120.0000 92

 18 omega   36.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   60.0000 57

 19 omega   57.00  151.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   60.0000 94

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

 21 omega   36.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 57

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

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

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

 25 omega   35.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000   60.0000 143

 26 omega   40.00  130.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000 -180.0000 90

 27 omega  -26.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 98

 28 omega  -44.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000 -150.0000 117

 29 omega   24.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 100

 30 omega   28.00  126.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000    0.0000 98

 31 omega   24.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 100

 32 omega   24.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 100

 33 omega   24.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 100

 34 omega   24.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 100

 35 omega   82.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 96

 36 omega   78.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 100

 37 omega   82.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  120.0000 96

 38 omega   78.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 100

 39 omega   82.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -180.0000 96
;
_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      0.0581744000
_diffrn_orient_matrix_UB_12      -0.0072214000
_diffrn_orient_matrix_UB_13      0.0945014000
_diffrn_orient_matrix_UB_21      -0.1175585000
_diffrn_orient_matrix_UB_22      0.0117953000
_diffrn_orient_matrix_UB_23      0.0458741000
_diffrn_orient_matrix_UB_31      -0.0727616000
_diffrn_orient_matrix_UB_32      -0.1355548000
_diffrn_orient_matrix_UB_33      -0.0498048000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26827
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.895
_diffrn_reflns_theta_min         3.335
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.983
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_correction_T_min  0.304
_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            brown
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7030
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.6127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6602
_reflns_number_total             7030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05362f3.cif
_cod_data_source_block           pmn32dy2
_cod_original_cell_volume        1845.67(7)
_cod_database_code               1550898
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H80Mn2Dy2N16O30
_shelx_estimated_absorpt_t_max   0.542
_shelx_estimated_absorpt_t_min   0.308
_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 C(H) groups, H1 of O1, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H41A of O41A, H42A of O42A
2. Restrained distances
 H41A-O42A
 1.98 with sigma of 0.04
 H42A-O9
 1.92 with sigma of 0.04
 O1-H1
 0.88 with sigma of 0.04
 O41A-C41A \\sim O42A-C42A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C41B \\sim N41B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Rigid body (RIGU) restrains
 O41A, C41A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O42A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N41B, C41B, C42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O41A(0.5) H41A(0.5) C41A(0.5) H41B(0.5) H41C(0.5) H41D(0.5)
 O42A(0.5) H42A(0.5) C42A(0.5) H42B(0.5) H42C(0.5) H42D(0.5) N41B(0.5)
 C41B(0.5) C42B(0.5) H42E(0.5) H42F(0.5) H42G(0.5)
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), C41A(H41B,H41C,
 H41D), C42A(H42B,H42C,H42D), C42B(H42E,H42F,H42G)
6.d Idealised tetrahedral OH refined as rotating group:
 O41A(H41A), O42A(H42A)
;
_shelx_res_checksum              97784
_olex2_submission_special_instructions 'No special instructions were received'