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_7126245
_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         'C20 H52 B2 K O Si4 Y'
_chemical_formula_sum            'C20 H52 B2 K O Si4 Y'
_chemical_formula_weight         570.60
_chemical_properties_physical    Air-sensitive,Moisture-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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-28 deposited with the CCDC.	2020-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.955(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7817(4)
_cell_length_b                   17.5986(5)
_cell_length_c                   16.9013(6)
_cell_measurement_reflns_used    5757
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.7650
_cell_measurement_theta_min      4.7920
_cell_volume                     3205.03(19)
_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 (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 0.998
_diffrn_measured_fraction_theta_max 0.987
_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    -25.00  45.00   1.00    5.00    --    0.00 -99.00 -30.00   70
  2  \w     32.00  82.00   1.00    5.00    --    0.00-178.00-150.00   50
  3  \w     32.00  82.00   1.00    5.00    --    0.00-178.00 120.00   50
  4  \w    -25.00  45.00   1.00    5.00    --    0.00 -99.00-120.00   70
  5  \w   -115.00 -18.00   1.00   20.00    --  -54.75 125.00 150.00   97
  6  \w     31.00 125.00   1.00   20.00    --   54.75  57.00 150.00   94
  7  \w     73.00 127.00   1.00   20.00    --   54.75 125.00 -30.00   54
  8  \w     73.00 127.00   1.00   20.00    --   54.75 125.00  30.00   54
  9  \w     31.00 125.00   1.00   20.00    --   54.75  57.00  90.00   94
 10  \w     31.00 125.00   1.00   20.00    --   54.75  57.00  60.00   94
 11  \w     73.00 127.00   1.00   20.00    --   54.75 125.00  90.00   54
 12  \w     83.00 178.00   1.00   40.00    --  109.50  64.00 -60.00   95
 13  \w     36.00  87.00   1.00   40.00    --  109.50-111.00 150.00   51
 14  \w     36.00  84.00   1.00   40.00    --  109.50 -92.00  60.00   48
 15  \w     36.00  84.00   1.00   40.00    --  109.50 -92.00 150.00   48
 16  \w     65.00 178.00   1.00   40.00    --  109.50  25.00-120.00  113
 17  \w     36.00  84.00   1.00   40.00    --  109.50 -92.00   0.00   48
 18  \w     36.00  84.00   1.00   40.00    --  109.50 -92.00  90.00   48
 19  \w     38.00 135.00   1.00   40.00    --  109.50 -50.00-180.00   97
 20  \w     36.00  84.00   1.00   40.00    --  109.50 -92.00-180.00   48
 21  \w     34.00 154.00   1.00   40.00    --  109.50 -25.00   0.00  120
 22  \w    -24.00  71.00   1.00    5.00    --    0.00  57.00  60.00   95
;
_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      -0.0869711000
_diffrn_orient_matrix_UB_12      0.0147269000
_diffrn_orient_matrix_UB_13      -0.0726319000
_diffrn_orient_matrix_UB_21      -0.0929433000
_diffrn_orient_matrix_UB_22      0.0398246000
_diffrn_orient_matrix_UB_23      0.0534001000
_diffrn_orient_matrix_UB_31      0.0650386000
_diffrn_orient_matrix_UB_32      0.0765418000
_diffrn_orient_matrix_UB_33      -0.0139475000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11390
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         3.627
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.217
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91764
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF / Hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         11390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.855
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0389P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8247
_reflns_number_total             11390
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9887\% 
 around [-0.02 0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct)
;
_cod_data_source_file            d0cc01722a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7126242--7126245.cif.'
_cod_database_code               7126245
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H40 Y1 B2 O1 Si4 K1'
_shelx_estimated_absorpt_t_max   0.780
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4578(6)
 0.5422(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              6954
_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 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.817
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2