Synthesis and single-molecule magnet properties of a trimetallic dysprosium metallocene cation.
He, Mian; Guo, Fu-Sheng; Tang, Jinkui; Mansikkamäki, Akseli; Layfield, Richard A.; Chemical communications (Cambridge, England) 57 (2021) 6396–6399; doi:10.1039/d1cc02139g

data_7128395
_publ_section_title
;
 Synthesis and single-molecule magnet properties of a trimetallic
 dysprosium metallocene cation.
;
_journal_issue                   52
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6396
_journal_page_last               6399
_journal_paper_doi               10.1039/d1cc02139g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C72 H122 B3 Dy3, 2(C3 H7)'
_chemical_formula_sum            'C78 H136 B3 Dy3'
_chemical_formula_weight         1593.79
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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   mixed
_audit_creation_date             2020-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-13 deposited with the CCDC.	2021-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.3090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.14480(10)
_cell_length_b                   21.92880(10)
_cell_length_c                   26.0721(2)
_cell_measurement_reflns_used    22591
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.0270
_cell_measurement_theta_min      3.7940
_cell_volume                     8002.12(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_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    -98.00 -59.00   1.00   12.00    --  -36.63-178.00 -60.00   39
  2  \w    -85.00 -38.00   1.00   12.00    --  -36.63 126.00  77.00   47
  3  \w   -101.00 -53.00   1.00   12.00    --  -36.63 145.00-114.00   48
  4  \w     78.00 106.00   1.00   12.00    --   36.63  38.00  30.00   28
  5  \w    -33.00  56.00   1.00   12.00    --   36.63 -38.00-150.00   89
  6  \w     11.00  66.00   1.00   12.00    --   36.63  19.00-150.00   55
  7  \w     81.00 108.00   1.00   12.00    --   36.63-178.00 -30.00   27
  8  \w     17.00  46.00   1.00   12.00    --   36.63 -38.00 120.00   29
  9  \w     20.00  95.00   1.00   12.00    --   36.63  57.00   0.00   75
 10  \w     33.00  75.00   1.00   12.00    --   36.63-178.00-180.00   42
 11  \w     40.00 121.00   1.00   50.00    --  107.00 -45.00 -90.00   81
 12  \w     91.00 122.00   1.00   50.00    --  107.00  45.00   0.00   31
 13  \w    147.00 173.00   1.00   50.00    --  107.00  45.00   0.00   26
 14  \w     41.00 123.00   1.00   50.00    --  107.00 -45.00  30.00   82
 15  \w     41.00 108.00   1.00   50.00    --  107.00 -45.00 120.00   67
 16  \w     90.00 147.00   1.00   50.00    --  107.00  45.00  60.00   57
 17  \w     38.00 142.00   1.00   50.00    --  107.00 -91.00 -61.44  104
 18  \w     43.00 112.00   1.00   50.00    --  107.00 -91.00-119.98   69
 19  \w     38.00 138.00   1.00   50.00    --  107.00 -91.00  73.92  100
 20  \w     38.00 117.00   1.00   50.00    --  107.00 -30.00-180.00   79
 21  \w    122.00 148.00   1.00   50.00    --  107.00  61.00 -60.00   26
 22  \w     83.00 109.00   1.00   50.00    --  107.00 -91.00 -11.91   26
 23  \w    113.00 138.00   1.00   50.00    --  107.00  45.00  90.00   25
 24  \w     70.00 171.00   1.00   50.00    --  107.00  15.00-180.00  101
 25  \w     73.00 101.00   1.00   50.00    --  107.00 -90.00 124.89   28
 26  \w     81.00 106.00   1.00   50.00    --  107.00 -91.00-149.79   25
 27  \w     82.00 107.00   1.00   50.00    --  107.00 -91.00 176.27   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0804535000
_diffrn_orient_matrix_UB_12      0.0059818000
_diffrn_orient_matrix_UB_13      0.0463281000
_diffrn_orient_matrix_UB_21      -0.0717174000
_diffrn_orient_matrix_UB_22      -0.0146885000
_diffrn_orient_matrix_UB_23      0.0374804000
_diffrn_orient_matrix_UB_31      0.0224259000
_diffrn_orient_matrix_UB_32      -0.0684197000
_diffrn_orient_matrix_UB_33      -0.0039620000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            55554
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.257
_diffrn_reflns_theta_min         3.426
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.012
_exptl_absorpt_correction_type   none
_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    1.323
_exptl_crystal_description       block
_exptl_crystal_F_000             3268
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.758
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         15365
_refine_ls_number_restraints     2213
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+4.3708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13632
_reflns_number_total             15365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02139g2.cif
_cod_data_source_block           exp_1947_sq
_cod_depositor_comments
'Adding full bibliography for 7128395--7128396.cif.'
_cod_original_cell_volume        8002.11(9)
_cod_database_code               7128395
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.315
_shelx_estimated_absorpt_t_min   0.315
_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, All C(H,H) groups
 At 1.5 times of:
  All B(H,H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C75-C74 = C74-C73
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C41 \\sim C8 \\sim C37 \\sim C1 \\sim C42 \\sim C5 \\sim C9 \\sim C43 \\sim C40
\\sim C38 \\sim C44 \\sim C39 \\sim C7 \\sim C45 \\sim C4 \\sim C2 \\sim C55
\\sim C10 \\sim C70 \\sim C47 \\sim C6 \\sim C63 \\sim C11 \\sim C65 \\sim C59
\\sim C67 \\sim C3 \\sim C19 \\sim C46 \\sim C62 \\sim C66 \\sim C23 \\sim C64
\\sim C15 \\sim C14 \\sim C20 \\sim C22 \\sim C49 \\sim C28 \\sim C60 \\sim C71
\\sim C69 \\sim C61 \\sim C13 \\sim C72 \\sim C21 \\sim C12 \\sim C27 \\sim C78
\\sim C48 \\sim C50 \\sim C51 \\sim C57 \\sim C29 \\sim C68 \\sim C31 \\sim C58
\\sim C18 \\sim C30 \\sim C77 \\sim C56 \\sim C16 \\sim C33 \\sim C17 \\sim C32
\\sim C34 \\sim C36 \\sim C35 \\sim C76 \\sim C25 \\sim C24 \\sim C26 \\sim
C24A \\sim C26A \\sim C25A \\sim C54 \\sim C53 \\sim C52 \\sim C74 \\sim C73
\\sim C75: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C53) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C73, C74, C75
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
6.a Riding coordinates:
 B3(H3A,H3B,H3C,H3D)
6.b Secondary CH2 refined with riding coordinates:
 C78(H78A,H78B), C77(H77A,H77B), C74(H74A,H74B), C73(H73A,H73B)
6.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C5(H5), C9(H9), C43(H43), C39(H39), C7(H7), C45(H45), C3(H3)
6.d Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C62(H62A,H62B,H62C), C14(H14A,H14B,H14C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C49(H49A,H49B,H49C), C60(H60A,H60B,H60C), C71(H71A,
 H71B,H71C), C69(H69A,H69B,H69C), C61(H61A,H61B,H61C), C13(H13A,H13B,H13C),
 C72(H72A,H72B,H72C), C21(H21A,H21B,H21C), C12(H12A,H12B,H12C), C48(H48A,H48B,
 H48C), C50(H50A,H50B,H50C), C57(H57A,H57B,H57C), C68(H68A,H68B,H68C), C58(H58A,
 H58B,H58C), C18(H18A,H18B,H18C), C56(H56A,H56B,H56C), C16(H16A,H16B,H16C),
 C33(H33A,H33B,H33C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C76(H76A,H76B,H76C), C25(H25A,
 H25B,H25C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C24A(H24D,H24E,H24F),
 C26A(H26D,H26E,H26F), C25A(H25D,H25E,H25F), C54(H54A,H54B,H54C), C53(H53A,H53B,
 H53C), C52(H52A,H52B,H52C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              12080
_shelx_fab_checksum              37256
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.782