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_7126387
_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 Y2, 2(C14 H16)'
_chemical_formula_sum            'C76 H116 Al2 Y2'
_chemical_formula_weight         1261.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-25
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2019-11-06 deposited with the CCDC.	2020-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                103.8942(17)
_cell_angle_beta                 100.2987(17)
_cell_angle_gamma                111.860(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2354(3)
_cell_length_b                   12.4540(3)
_cell_length_c                   14.8193(2)
_cell_measurement_reflns_used    19332
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.0560
_cell_measurement_theta_min      4.0700
_cell_volume                     1783.50(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_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   -118.00 -71.00   0.50    0.50    --  -46.60 -50.00 -34.75   94
  2  \w   -127.00 -96.00   0.50    0.50    --  -46.60 -38.00   0.00   62
  3  \w    -33.00  -7.00   0.50    0.50    --  -46.60  57.00-120.00   52
  4  \w    -64.00 -15.00   0.50    0.50    --  -46.60 -50.00 -34.75   98
  5  \w   -122.00 -10.00   0.50    0.50    --  -46.60 -76.00 -90.00  224
  6  \w   -108.00 -14.00   0.50    0.50    --  -46.60 -45.00 117.44  188
  7  \w    -89.00 -10.00   0.50    0.50    --  -46.60 -38.00   0.00  158
  8  \w     11.00  39.00   0.50    0.50    --  -46.60  57.00-120.00   56
  9  \w   -169.00-102.00   0.50    0.50    -- -107.20 -62.00 -85.97  134
 10  \w   -146.00-121.00   0.50    0.50    -- -107.20  76.00-150.00   50
 11  \w    -52.00 -26.00   0.50    0.50    -- -107.20  38.00 150.00   52
 12  \w    -75.00 -49.00   0.50    0.50    -- -107.20  76.00-150.00   52
 13  \w   -105.00 -68.00   0.50    0.50    -- -107.20  57.00  60.00   74
 14  \w   -146.00 -24.00   0.50    0.50    -- -107.20  76.00 -90.00  244
 15  \w   -146.00 -19.00   0.50    0.50    -- -107.20  76.00 -30.00  254
 16  \w   -141.00 -18.00   0.50    0.50    -- -107.20  76.00  30.00  246
 17  \w   -134.00 -73.00   0.50    0.50    -- -107.20  38.00 150.00  122
 18  \w   -189.00 -75.00   0.50    0.50    -- -107.20 -47.00-139.73  228
 19  \w   -195.00 -74.00   0.50    0.50    -- -107.20 -60.00 165.16  242
 20  \w   -104.00 -52.00   0.50    0.50    -- -107.20  76.00 120.00  104
 21  \w   -191.00-152.00   0.50    0.50    -- -107.20 -44.00 152.07   78
 22  \w   -103.00 -77.00   0.50    0.50    -- -107.20  76.00   0.00   52
 23  \w   -145.00 -52.00   0.50    0.50    -- -107.20  76.00-120.00  186
 24  \w   -197.00 -76.00   0.50    0.50    -- -107.20 -54.00 -59.51  242
 25  \w   -188.00-132.00   0.50    0.50    -- -107.20 -57.00   0.00  112
 26  \w   -181.00-147.00   0.50    0.50    -- -107.20 -42.00  92.17   68
 27  \w   -162.00-136.00   0.50    0.50    -- -107.20 -50.00-113.50   52
 28  \w   -130.00 -83.00   0.50    0.50    -- -107.20  76.00-180.00   94
 29  \w    -73.00 -35.00   0.50    0.50    -- -107.20  76.00-180.00   76
 30  \w   -101.00 -64.00   0.50    0.50    -- -107.20  76.00  60.00   74
 31  \w   -112.00 -19.00   0.50    0.50    -- -107.20  76.00  90.00  186
 32  \w   -129.00 -74.00   0.50    0.50    -- -107.20 -73.00 111.77  110
 33  \w   -197.00 -68.00   0.50    0.50    -- -107.20 -31.00-173.57  258
;
_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      0.0778622000
_diffrn_orient_matrix_UB_12      -0.0791377000
_diffrn_orient_matrix_UB_13      -0.0076017000
_diffrn_orient_matrix_UB_21      0.0057021000
_diffrn_orient_matrix_UB_22      0.0019030000
_diffrn_orient_matrix_UB_23      0.1050422000
_diffrn_orient_matrix_UB_31      -0.1336187000
_diffrn_orient_matrix_UB_32      -0.1172890000
_diffrn_orient_matrix_UB_33      -0.0386206000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24477
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.240
_diffrn_reflns_theta_min         3.218
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.373
_exptl_crystal_size_min          0.339
_refine_diff_density_max         1.854
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6466
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0627P)^2^+3.7614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6370
_reflns_number_total             6466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08945d2.cif
_cod_data_source_block           YCpMe5_Me4Al
_cod_depositor_comments
'Adding full bibliography for 7126383--7126388.cif.'
_cod_original_cell_volume        1783.51(7)
_cod_database_code               7126387
_manchester_internal_coll_name   rdpm12
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 0.5s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   2/05/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 2/05/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 2/05/17
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 25/10/19
_manchester_internal_validation_user FO
_manchester_internal_validation_date 25/10/19
_manchester_internal_archive_date 25/10/19
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 Y Al'
_chemical_oxdiff_usercomment     FO/CAPG/DPM
_reflns_odcompleteness_completeness 98.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32A-C33A \\sim C32B-C33B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C38A \\sim C33A \\sim C36A \\sim C37A \\sim C32A \\sim C33B \\sim C38B \\sim
C37B \\sim C36B \\sim C35B \\sim C34A \\sim C35A \\sim C32B \\sim C34B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=Sof(C38B)=Sof(H38B)=
 Sof(C37B)=Sof(H37B)=Sof(C36B)=Sof(H36B)=Sof(C35B)=Sof(H35B)=Sof(C34B)=
 Sof(H34B)=1-FVAR(1)
 Sof(C38A)=Sof(H38A)=Sof(C33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C27(H27), C30(H30), C28(H28), C29(H29), C38A(H38A), C34A(H34A),
 C35A(H35A), C36A(H36A), C37A(H37A), C38B(H38B), C37B(H37B), C36B(H36B),
 C35B(H35B), C34B(H34B)
5.b Fitted hexagon refined as free rotating group:
 C38A(C33A,C34A,C35A,C36A,C37A), C33B(C38B,C37B,C36B,C35B,C34B)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C9(H9A,H9B,H9C),
  C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C25(H25A,H25B,H25C), C32A(H32A,H32B,H32C), C32B(H32D,H32E,H32F),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              47670
_shelx_hkl_checksum              20533
_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 13.659
_oxdiff_exptl_absorpt_empirical_full_min 0.604