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_7126243
_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 Dy2 Na2 O2 Si8'
_chemical_formula_sum            'C40 H104 B4 Dy2 Na2 O2 Si8'
_chemical_formula_weight         1256.17
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-29
_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                90.676(4)
_cell_angle_beta                 90.257(3)
_cell_angle_gamma                92.791(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9592(4)
_cell_length_b                   16.5329(8)
_cell_length_c                   17.2892(7)
_cell_measurement_reflns_used    5823
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      69.6560
_cell_measurement_theta_min      4.0380
_cell_volume                     3128.6(2)
_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      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.966
_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     39.00  82.00   1.00    7.50    --    0.00-178.00  90.00   43
  2  \w    -68.00  -6.00   1.00    7.50    --    0.00 -77.00-180.00   62
  3  \w     -4.00  32.00   1.00    7.50    --    0.00 -77.00-180.00   36
  4  \w    -78.00  15.00   1.00   20.00    --  -54.75  57.00 120.00   93
  5  \w   -125.00 -31.00   1.00   20.00    --  -54.75 -57.00 -30.00   94
  6  \w   -111.00 -25.00   1.00   20.00    --  -54.75 -77.00-150.00   86
  7  \w   -109.00 -18.00   1.00   20.00    --  -54.75 125.00  90.00   91
  8  \w     -3.00  78.00   1.00   20.00    --   54.75-125.00 -30.00   81
  9  \w     55.00 126.00   1.00   20.00    --   54.75  77.00  30.00   71
 10  \w     84.00 178.00   1.00   65.00    --  109.50  64.00  30.00   94
 11  \w    117.00 145.00   1.00   65.00    --  109.50 -91.00   3.41   28
 12  \w     38.00 138.00   1.00   65.00    --  109.50 -38.00   0.00  100
 13  \w     68.00 107.00   1.00   65.00    --  109.50  25.00-120.00   39
 14  \w    136.00 172.00   1.00   65.00    --  109.50  25.00-120.00   36
 15  \w    121.00 176.00   1.00   65.00    --  109.50  50.00  90.00   55
 16  \w     39.00 101.00   1.00   65.00    --  109.50 -50.00-120.00   62
 17  \w     36.00  84.00   1.00   65.00    --  109.50 -92.00-120.00   48
 18  \w     74.00 115.00   1.00   65.00    --  109.50 -91.00 161.12   41
 19  \w     36.00  63.00   1.00   65.00    --  109.50 -91.00 161.12   27
 20  \w    107.00 165.00   1.00   65.00    --  109.50  77.00 -60.00   58
 21  \w     46.00 150.00   1.00   65.00    --  109.50 -91.00  65.18  104
 22  \w     73.00 106.00   1.00   65.00    --  109.50 -91.00   3.41   33
 23  \w     85.00 174.00   1.00   65.00    --  109.50  50.00   0.00   89
 24  \w     69.00 150.00   1.00   65.00    --  109.50 -91.00-103.28   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      -0.0453214000
_diffrn_orient_matrix_UB_12      -0.0834447000
_diffrn_orient_matrix_UB_13      0.0300792000
_diffrn_orient_matrix_UB_21      0.1320026000
_diffrn_orient_matrix_UB_22      -0.0185583000
_diffrn_orient_matrix_UB_23      0.0221742000
_diffrn_orient_matrix_UB_31      -0.0185270000
_diffrn_orient_matrix_UB_32      0.0374116000
_diffrn_orient_matrix_UB_33      0.0808459000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17751
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.329
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66965
_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    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method Benzene
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.619
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         17751
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0932P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12298
_reflns_number_total             17751
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9959\% 
 around [1.00 -0.07 -0.01] (reciprocal) or [1.00 0.00 0.00] (direct)
;
_cod_data_source_file            d0cc01722a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7126242--7126245.cif.'
_cod_database_code               7126243
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H50 Dy1 Si4 B2 O1 Na1'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5526(9)
 0.4474(9)
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
 B3-H3D = B4-H4C = B2-H2D = B1-H1D
 1.05 with sigma of 0.02
 B3-H3C = B3-H3A = B3-H3B = B4-H4B = B4-H4D = B4-H4A = B2-H2B = B2-H2A = B2-
 H2C = B1-H1B = B1-H1C = B1-H1A
 1.2 with sigma of 0.02
4.a Riding coordinates:
 B3(H3A), B4(H4A), B1(H1A)
4.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C37(H37A,H37B), C20(H20A,H20B), C19(H19A,H19B), C38(H38A,
 H38B), C40(H40A,H40B), C39(H39A,H39B), C17(H17A,H17B)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C28(H28A,H28B,H28C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C),
 C33(H33A,H33B,H33C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C30(H30A,H30B,
 H30C), C8(H8A,H8B,H8C), C32(H32A,H32B,H32C), C11(H11A,H11B,H11C), C27(H27A,
 H27B,H27C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), C29(H29A,
 H29B,H29C), C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C),
 C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C31(H31A,H31B,H31C), C36(H36A,H36B,
 H36C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              81037
_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 2.794
_oxdiff_exptl_absorpt_empirical_full_min 0.626
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2