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_7128396
_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 H118 B2 Dy3, B C24 F20, C6 H14'
_chemical_formula_sum            'C102 H132 B3 Dy3 F20'
_chemical_formula_weight         2258.00
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-13 deposited with the CCDC.	2021-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                80.945(3)
_cell_angle_beta                 88.122(3)
_cell_angle_gamma                88.861(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2955(5)
_cell_length_b                   17.6222(7)
_cell_length_c                   19.9866(6)
_cell_measurement_reflns_used    12860
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      70.9080
_cell_measurement_theta_min      3.9680
_cell_volume                     4969.0(3)
_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 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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -101.00 -74.00   1.00   10.00    --  -36.75 -57.00-150.00   27
  2  \w     35.00 104.00   1.00   10.00    --   36.75 178.00  60.00   69
  3  \w     39.00  97.00   1.00   10.00    --   36.75  77.00 150.00   58
  4  \w     21.00  99.00   1.00   10.00    --   36.75  57.00 120.00   78
  5  \w     10.00 104.00   1.00   10.00    --   36.75  77.00-120.00   94
  6  \w     46.00  76.00   1.00   10.00    --   36.75 -99.00 120.00   30
  7  \w     36.00 109.00   1.00   10.00    --   36.75 178.00 120.00   73
  8  \w     41.00  74.00   1.00   10.00    --   36.75 -99.00 -30.00   33
  9  \w     90.00 129.00   1.00   50.00    --  107.00  45.00 -90.00   39
 10  \w     43.00 135.00   1.00   50.00    --  107.00 -91.00 -15.05   92
 11  \w     39.00  65.00   1.00   50.00    --  107.00 -91.00 -84.02   26
 12  \w     91.00 116.00   1.00   50.00    --  107.00 -91.00 -84.02   25
 13  \w     79.00 105.00   1.00   50.00    --  107.00 -90.00 -64.13   26
 14  \w     40.00  65.00   1.00   50.00    --  107.00 -84.00 123.87   25
 15  \w     37.00 128.00   1.00   50.00    --  107.00 -30.00 -90.00   91
 16  \w     37.00  87.00   1.00   50.00    --  107.00-111.00 -30.00   50
 17  \w     43.00 136.00   1.00   50.00    --  107.00 -91.00 150.20   93
 18  \w     43.00 122.00   1.00   50.00    --  107.00 -45.00 120.00   79
 19  \w     76.00 101.00   1.00   50.00    --  107.00 -91.00  51.93   25
 20  \w     40.00 116.00   1.00   50.00    --  107.00 -45.00   0.00   76
 21  \w     51.00  77.00   1.00   50.00    --  107.00 178.00 -30.00   26
 22  \w    109.00 134.00   1.00   50.00    --  107.00 178.00 -30.00   25
 23  \w    149.00 175.00   1.00   50.00    --  107.00  45.00 -90.00   26
 24  \w     85.00 122.00   1.00   50.00    --  107.00 -91.00-154.50   37
 25  \w     82.00 107.00   1.00   50.00    --  107.00 -91.00  87.12   25
 26  \w     69.00 177.00   1.00   50.00    --  107.00  15.00-150.00  108
 27  \w     84.00 111.00   1.00   50.00    --  107.00 -61.00 -60.00   27
 28  \w     93.00 174.00   1.00   50.00    --  107.00  45.00  90.00   81
;
_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      -0.0071610000
_diffrn_orient_matrix_UB_12      0.0870133000
_diffrn_orient_matrix_UB_13      0.0017514000
_diffrn_orient_matrix_UB_21      -0.1063899000
_diffrn_orient_matrix_UB_22      -0.0020691000
_diffrn_orient_matrix_UB_23      -0.0094494000
_diffrn_orient_matrix_UB_31      -0.0160729000
_diffrn_orient_matrix_UB_32      -0.0162114000
_diffrn_orient_matrix_UB_33      0.0774940000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34352
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.641
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.576
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             2274
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.916
_refine_diff_density_min         -1.709
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1221
_refine_ls_number_reflns         17677
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0598P)^2^+6.8249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14469
_reflns_number_total             17677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02139g2.cif
_cod_data_source_block           exp_2012
_cod_depositor_comments
'Adding full bibliography for 7128395--7128396.cif.'
_cod_database_code               7128396
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.254
_reflns_odcompleteness_completeness 99.73
_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 C(H,H,H) groups
2. Restrained distances
 C101-C102
 1.55 with sigma of 0.02
 C101-C100
 1.55 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C99, C100, C101, C98, C102, C97
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C98(H98A,H98B), C99(H99A,H99B), C101(H10F,H10G)
4.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C3(H3), C45(H45), C9(H9), C43(H43), C7(H7), C5(H5), C39(H39)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C61(H61A,H61B,H61C), C68(H68A,H68B,H68C), C13(H13A,H13B,
 H13C), C50(H50A,H50B,H50C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C35(H35A,
 H35B,H35C), C14(H14A,H14B,H14C), C72(H72A,H72B,H72C), C62(H62A,H62B,H62C),
 C48(H48A,H48B,H48C), C36(H36A,H36B,H36C), C60(H60A,H60B,H60C), C32(H32A,H32B,
 H32C), C54(H54A,H54B,H54C), C20(H20A,H20B,H20C), C53(H53A,H53B,H53C), C70(H70A,
 H70B,H70C), C18(H18A,H18B,H18C), C69(H69A,H69B,H69C), C12(H12A,H12B,H12C),
 C49(H49A,H49B,H49C), C71(H71A,H71B,H71C), C33(H33A,H33B,H33C), C52(H52A,H52B,
 H52C), C22(H22A,H22B,H22C), C34(H34A,H34B,H34C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C56(H56A,H56B,H56C), C97(H97A,H97B,H97C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C102(H10C,H10D,H10E)
;
_shelx_res_checksum              90385
_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 1.479
_oxdiff_exptl_absorpt_empirical_full_min 0.804