Enhanced single-molecule magnetism in dysprosium complexes of a pristine cyclobutadienyl ligand.
Durrant, James P.; Tang, Jinkui; Mansikkamäki, Akseli; Layfield, Richard A.; Chemical communications (Cambridge, England) 56 (2020) 4708–4711; doi:10.1039/d0cc01722a

data_7126242
_publ_section_title
;
 Enhanced single-molecule magnetism in dysprosium complexes of a pristine
 cyclobutadienyl ligand.
;
_journal_issue                   34
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4708
_journal_page_last               4711
_journal_paper_doi               10.1039/d0cc01722a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C40 H104 B4 Na2 O2 Si8 Y2'
_chemical_formula_sum            'C40 H104 B4 Na2 O2 Si8 Y2'
_chemical_formula_weight         1108.99
_chemical_properties_physical    Air-sensitive,Moisture-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
_audit_creation_date             2020-02-27
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-02-28 deposited with the CCDC.	2020-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.747(10)
_cell_angle_beta                 90.198(11)
_cell_angle_gamma                92.00(2)
_cell_formula_units_Z            2
_cell_length_a                   10.929(2)
_cell_length_b                   16.497(4)
_cell_length_c                   17.2819(10)
_cell_measurement_reflns_used    1993
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.5190
_cell_measurement_theta_min      4.0760
_cell_volume                     3113.7(10)
_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 (Sheldrick, 2015)'
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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    -72.00  29.00   1.00    5.00    --    0.00 -38.00 120.00  101
  2  \w   -114.00 -27.00   1.00   20.00    --  -54.75 125.00-180.00   87
  3  \w    -89.00 -47.00   1.00   20.00    --  -54.75 125.00 -60.00   42
  4  \w    -17.00 121.00   1.00   20.00    --   54.75 -19.00  90.00  138
  5  \w    -13.00  78.00   1.00   20.00    --   54.75 -57.00  60.00   91
  6  \w     33.00 101.00   1.00   20.00    --   54.75  57.00 -60.00   68
  7  \w     -7.00  77.00   1.00   20.00    --   54.75 -57.00 -30.00   84
  8  \w    142.00 178.00   1.00   30.00    --  109.50  64.00 -60.00   36
  9  \w    111.00 178.00   1.00   30.00    --  109.50  50.00 -90.00   67
 10  \w     94.00 131.00   1.00   30.00    --  109.50  64.00 -60.00   37
 11  \w    120.00 147.00   1.00   30.00    --  109.50 -91.00-105.49   27
 12  \w     51.00 113.00   1.00   30.00    --  109.50 -91.00-105.49   62
 13  \w     40.00 135.00   1.00   30.00    --  109.50 -50.00-120.00   95
 14  \w     37.00  68.00   1.00   30.00    --  109.50 -92.00 150.00   31
 15  \w     36.00 118.00   1.00   30.00    --  109.50 -38.00 150.00   82
 16  \w     36.00  72.00   1.00   30.00    --  109.50 -91.00 117.46   36
 17  \w     77.00 149.00   1.00   30.00    --  109.50 -91.00 -44.15   72
 18  \w     37.00 133.00   1.00   30.00    --  109.50 -38.00 -30.00   96
 19  \w     74.00 134.00   1.00   30.00    --  109.50 -91.00 117.46   60
 20  \w     76.00 105.00   1.00   30.00    --  109.50 -91.00  60.59   29
 21  \w    123.00 150.00   1.00   30.00    --  109.50 -91.00  60.59   27
 22  \w     51.00 178.00   1.00   30.00    --  109.50   0.00-120.00  127
;
_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      0.0213235000
_diffrn_orient_matrix_UB_12      0.0920595000
_diffrn_orient_matrix_UB_13      0.0123864000
_diffrn_orient_matrix_UB_21      -0.0090384000
_diffrn_orient_matrix_UB_22      -0.0111278000
_diffrn_orient_matrix_UB_23      0.0881909000
_diffrn_orient_matrix_UB_31      0.1391493000
_diffrn_orient_matrix_UB_32      -0.0113576000
_diffrn_orient_matrix_UB_33      0.0042009000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24473
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.681
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95517
_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_density_diffrn    1.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method Benzene
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.789
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         24473
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1085P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14492
_reflns_number_total             24473
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 2.1193\% 
 around [0.01 -0.10 1.00] (reciprocal) or [0.03 -0.09 1.00] (direct)
Component 3 rotated by -179.9282\% 
 around [1.00 -0.04 -0.01] (reciprocal) or [1.00 0.01 0.00] (direct)
;
_cod_data_source_file            d0cc01722a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7126242--7126245.cif.'
_cod_original_cell_volume        3113.7(11)
_cod_database_code               7126242
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H88 B4 O2 Na2 Si8 Y2'
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.564
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.1822(18)
 0.4899(14) 0.3279(12)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 B4-H4A = B4-H4B = B4-H4D = B3-H3A = B3-H3D = B3-H3C = B1-H1A = B1-H1B = B1-
 H1C = B2-H2A = B2-H2D = B2-H2B
 1.2 with sigma of 0.02
 B1-H1D = B2-H2C = B4-H4C = B3-H3B
 1.05 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C40(H40A,H40B), C37(H37A,H37B), C18(H18A,H18B), C17(H17A,
 H17B), C19(H19A,H19B), C39(H39A,H39B), C38(H38A,H38B)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C36(H36A,H36B,H36C), C16(H16A,H16B,
 H16C), C35(H35A,H35B,H35C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C10(H10A,
 H10B,H10C), C28(H28A,H28B,H28C), C15(H15A,H15B,H15C), C27(H27A,H27B,H27C),
 C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C),
 C31(H31A,H31B,H31C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C26(H26A,H26B,H26C),
 C13(H13A,H13B,H13C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              89683
_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 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.859
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3