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_7126384
_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         'C6 H14 Li O Y, 2(C10 H15)'
_chemical_formula_sum            'C26 H44 Li O Y'
_chemical_formula_weight         468.46
_chemical_name_systematic        '[Y(Cp*)2(Me)2Li(THF)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 94.016(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2530(13)
_cell_length_b                   15.4572(12)
_cell_length_c                   18.3771(16)
_cell_measurement_reflns_used    2262
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      19.3710
_cell_measurement_theta_min      3.2810
_cell_volume                     2621.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_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      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -97.00 -70.00   1.00   12.50    --  -18.77-178.00  60.00   27
  2  \w    -17.00  23.00   1.00   12.50    --  -18.77 -99.00-120.00   40
  3  \w    -18.00  25.00   1.00   12.50    --  -18.77 -99.00-180.00   43
  4  \w    -20.00  15.00   1.00   12.50    --  -18.77 -99.00  60.00   35
  5  \w     40.00  72.00   1.00   12.50    --   20.02-178.00 -30.00   32
  6  \w     -7.00  93.00   1.00   12.50    --   20.02  38.00  90.00  100
  7  \w    -41.00  45.00   1.00   12.50    --   20.02 -38.00 120.00   86
  8  \w    -48.00  45.00   1.00   12.50    --   20.02 -38.00 -90.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0480730000
_diffrn_orient_matrix_UB_12      -0.0263954000
_diffrn_orient_matrix_UB_13      -0.0186019000
_diffrn_orient_matrix_UB_21      -0.0599185000
_diffrn_orient_matrix_UB_22      -0.0216268000
_diffrn_orient_matrix_UB_23      -0.0180533000
_diffrn_orient_matrix_UB_31      -0.0007463000
_diffrn_orient_matrix_UB_32      0.0306964000
_diffrn_orient_matrix_UB_33      -0.0287282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1413
_diffrn_reflns_av_unetI/netI     0.1581
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19670
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.738
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.7b (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         4797
_refine_ls_number_restraints     1092
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1760
_refine_ls_R_factor_gt           0.0954
_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^)+(0.0336P)^2^+16.7462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2680
_reflns_number_total             4797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08945d2.cif
_cod_data_source_block           YCpMe5_Me2Li
_cod_depositor_comments
'Adding full bibliography for 7126383--7126388.cif.'
_cod_database_code               7126384
_manchester_internal_coll_name   adpm592
_manchester_internal_coll_client PE
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 12.5s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   PE
_manchester_internal_coll_date   8/5/2019
_manchester_internal_process_user PE
_manchester_internal_process_date 9/5/2019
_manchester_internal_solution_user PE
_manchester_internal_solution_date 6/8/2019
_manchester_internal_refinement_user PE/FO
_manchester_internal_refinement_date 25/10/2019
_manchester_internal_validation_user FO
_manchester_internal_validation_date 25/10/2019
_manchester_internal_archive_date 25/10/2019
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C26H44LiOY
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.702
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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
 C24-C25 = C24A-C25
 1.54 with sigma of 0.02
 C24-C23 = C24A-C23
 1.5 with sigma of 0.02
 C2-C3 \\sim C2A-C3A \\sim C4-C3 \\sim C3A-C4A \\sim C4-C5 \\sim C5-C1 \\sim
C5A-C1A \\sim C5A-C4A \\sim C2-C1
 \\sim C2A-C1A \\sim C13-C14 \\sim C13A-C14A \\sim C14-C15 \\sim C15A-C14A
\\sim C15A-C11A \\sim C11-C15 ~
 C11A-C12A \\sim C12-C11 \\sim C13-C12 \\sim C13A-C12A
 with sigma of 0.02
 C18A-C13A \\sim C18-C13 \\sim C17A-C12A \\sim C17-C12 \\sim C11A-C16A \\sim
C16-C11 \\sim C20A-C15A ~
 C20-C15 \\sim C19A-C14A \\sim C19-C14 \\sim C10-C5 \\sim C9A-C4A \\sim
C10A-C5A \\sim C6-C1 \\sim C6A-C1A
 \\sim C7A-C2A \\sim C7-C2 \\sim C8-C3 \\sim C8A-C3A \\sim C9-C4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A
\\sim C8A \\sim C9A \\sim C10A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O1 \\sim C23 \\sim C25 \\sim C26 \\sim C24 \\sim C24A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim
C19 \\sim C20 \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A
\\sim C17A \\sim C18A \\sim C19A \\sim C20A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=Sof(C15A)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=
 Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=
 Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 FVAR(1)
 Sof(H23C)=Sof(H23D)=Sof(H25C)=Sof(H25D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(2)
 Sof(H23A)=Sof(H23B)=Sof(H25A)=Sof(H25B)=Sof(C24)=Sof(H24A)=Sof(H24B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C23(H23C,H23D), C25(H25A,H25B), C25(H25C,H25D), C26(H26A,
 H26B), C24(H24A,H24B), C24A(H24C,H24D)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), 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), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F),
 C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,
 H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              20315
_shelx_hkl_checksum              14000
_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 2.120
_oxdiff_exptl_absorpt_empirical_full_min 0.631