A double-dysprosocenium single-molecule magnet bound together with neutral ligands.
Evans, Peter; Reta, Daniel; Goodwin, Conrad A. P.; Ortu, Fabrizio; Chilton, Nicholas F.; Mills, David P.; Chemical communications (Cambridge, England) 56 (2020) 5677–5680; doi:10.1039/c9cc08945d

data_7126388
_publ_section_title
;
 A double-dysprosocenium single-molecule magnet bound together with
 neutral ligands.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5677
_journal_page_last               5680
_journal_paper_doi               10.1039/c9cc08945d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C48 H84 Al2 Dy2, 4(C7 H8)'
_chemical_formula_sum            'C76 H116 Al2 Dy2'
_chemical_formula_weight         1408.725
_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_Int_Tables_number      2
_audit_creation_date             2020-04-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-15 deposited with the CCDC.	2020-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                104.043(4)
_cell_angle_beta                 100.205(3)
_cell_angle_gamma                111.785(4)
_cell_formula_units_Z            1
_cell_length_a                   11.1938(3)
_cell_length_b                   12.4457(7)
_cell_length_c                   14.8073(5)
_cell_measurement_reflns_used    7795
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      26.3280
_cell_measurement_theta_min      2.5400
_cell_volume                     1774.66(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_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    -83.00 -39.00   0.50    3.00    --    5.00 -76.00  30.00   88
  2  \w    -20.00   7.00   0.50    3.00    --    5.00 -76.00  30.00   54
  3  \w    -94.00  22.00   0.50    3.00    --   -7.40 -57.00  60.00  232
  4  \w    -10.00  17.00   0.50    3.00    --   -7.40 -76.00-150.00   54
  5  \w    -96.00 -39.00   0.50    3.00    --   -7.40 -76.00-150.00  114
  6  \w    -69.00 -19.00   0.50    3.00    --   -7.40 -57.00 -30.00  100
  7  \w    -96.00  82.00   0.50    3.00    --   -7.40 -19.00 150.00  356
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0598062000
_diffrn_orient_matrix_UB_12      0.0048949000
_diffrn_orient_matrix_UB_13      0.0050175000
_diffrn_orient_matrix_UB_21      -0.0305890000
_diffrn_orient_matrix_UB_22      -0.0294866000
_diffrn_orient_matrix_UB_23      -0.0510166000
_diffrn_orient_matrix_UB_31      -0.0243601000
_diffrn_orient_matrix_UB_32      -0.0579447000
_diffrn_orient_matrix_UB_33      0.0067510000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11216
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9991
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.55
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             730.357
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.6062
_refine_diff_density_min         -2.3814
_refine_diff_density_rms         0.2450
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             7.9775
_refine_ls_goodness_of_fit_ref   1.0363
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    86
_refine_ls_number_parameters     378
_refine_ls_number_reflns         11216
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.0343
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0941
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+52.3852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2336
_refine_ls_wR_factor_ref         0.2574
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                8687
_reflns_number_total             11216
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc08945d2.cif
_cod_data_source_block           Dy_Cpstar_Me4Al
_cod_depositor_comments
'Adding full bibliography for 7126383--7126388.cif.'
_cod_original_cell_volume        1774.64(15)
_cod_database_code               7126388
_manchester_internal_coll_name   rdpm15
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 3s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   08/05/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 9/05/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 10/05/17
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 14/04/20
_manchester_internal_validation_user FO
_manchester_internal_validation_date 14/04/20
_manchester_internal_archive_date 14/04/20
_chemical_oxdiff_formula         (Dy(C5(CH3)5)2Al(CH3)4)2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80(8)
 0.20(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C33-C32
 1.52 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C18(H18a,H18b,H18c)
6.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38)
6.c Fitted hexagon refined as free rotating group:
 C31(C26,C27,C28,C29,C30), C33(C34,C35,C36,C37,C38)
6.d Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C19(H19a,H19b,H19c),
 C20(H20a,H20b,H20c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C25(H25a,H25b,
 H25c), C32(H32a,H32b,H32c), C22(H22a,H22b,H22c), C21(H21a,H21b,H21c)
;
_olex2_exptl_crystal_mounting_method 'in fomblin oil on micromount'
_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 1.373
_oxdiff_exptl_absorpt_empirical_full_min 0.674