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_1550900
_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 Cr2 N4 O18 Y2, 2(C2 H3 N)'
_chemical_formula_sum            'C72 H78 Cr2 N6 O18 Y2'
_chemical_formula_weight         1597.22
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-11 deposited with the CCDC.    2019-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.794(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.1143(3)
_cell_length_b                   10.5198(2)
_cell_length_c                   24.3898(3)
_cell_measurement_reflns_used    12406
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      70.7550
_cell_measurement_theta_min      3.1580
_cell_volume                     7188.21(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1067
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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    -33.00  40.00   1.00    4.38    --    0.00  83.00  93.00   73
  2  \w    -18.00  33.00   1.00    4.38    --    0.00 -83.00 -26.00   51
  3  \w    -17.00  87.00   1.00   17.55    --   54.00 -83.00 -26.00  104
  4  \w     97.00 178.00   1.00   17.55    --  108.00  83.00  93.00   81
  5  \w     37.00 141.00   1.00   17.55    --  108.00 -83.00 -26.00  104
  6  \w    -21.00  69.00   1.00    4.38    --    0.00  57.00 -30.00   90
  7  \w    -21.00  69.00   1.00    4.38    --    0.00  57.00-180.00   90
  8  \w     33.00 123.00   1.00   17.55    --   54.00  57.00 -60.00   90
  9  \w     23.00 111.00   1.00   17.55    --   54.00-125.00-180.00   88
 10  \w     24.00 124.00   1.00   17.55    --   54.00  77.00-120.00  100
 11  \w      1.00  96.00   1.00   17.55    --   54.00 -99.00 120.00   95
 12  \w     36.00 113.00   1.00   17.55    --  108.00-111.00 120.00   77
 13  \w     86.00 178.00   1.00   17.55    --  108.00  50.00 150.00   92
 14  \w     36.00 113.00   1.00   17.55    --  108.00-111.00-180.00   77
 15  \w     40.00 130.00   1.00   17.55    --  108.00 -63.00   0.00   90
 16  \w     86.00 176.00   1.00   17.55    --  108.00  63.00   0.00   90
 17  \w     86.00 178.00   1.00   17.55    --  108.00  50.00-150.00   92
 18  \w     86.00 178.00   1.00   17.55    --  108.00  50.00  30.00   92
 19  \w    -73.00  44.00   1.00    4.38    --    0.00 -19.00 -90.00  117
 20  \w    -72.00  26.00   1.00    4.38    --    0.00 -38.00   0.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0186488000
_diffrn_orient_matrix_UB_12      -0.1071008000
_diffrn_orient_matrix_UB_13      0.0355778000
_diffrn_orient_matrix_UB_21      0.0478269000
_diffrn_orient_matrix_UB_22      -0.0707605000
_diffrn_orient_matrix_UB_23      -0.0016446000
_diffrn_orient_matrix_UB_31      0.0196612000
_diffrn_orient_matrix_UB_32      0.0705258000
_diffrn_orient_matrix_UB_33      0.0524466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23208
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.065
_diffrn_reflns_theta_min         3.155
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.133
_exptl_absorpt_correction_T_max  0.555
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+6.6202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6110
_reflns_number_total             6828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05362f3.cif
_cod_data_source_block           cr2y21
_cod_database_code               1550900
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.494
_reflns_odcompleteness_completeness 99.75
_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 C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.88 with sigma of 0.02
3. Others
 Fixed Sof: H1AA(0.5) H1AB(0.5) H1BC(0.5) H1BD(0.5) C2A(0.5) H2AA(0.5)
 H2AB(0.5) C2B(0.5) H2BA(0.5) H2BB(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B)
4.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)
4.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              99480
_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 1.140
_oxdiff_exptl_absorpt_empirical_full_min 0.908