Influence of pressure on a dysprosocenium single-molecule magnet.
Parmar, Vijay S.; Thiel, Andreas M.; Nabi, Rizwan; Gransbury, Gemma K.; Norre, Marie S.; Evans, Peter; Corner, Sophie C.; Skelton, Jonathan M.; Chilton, Nicholas F.; Mills, David P.; Overgaard, Jacob; Chemical communications (Cambridge, England) 59 (2023) 2656–2659; doi:10.1039/d2cc06722f

data_7131351
_publ_section_title
;
 Influence of pressure on a dysprosocenium single-molecule magnet.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2656
_journal_page_last               2659
_journal_paper_doi               10.1039/d2cc06722f
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C34 H58 Dy, B C24 F20'
_chemical_formula_sum            'C58 H58 B Dy F20'
_chemical_formula_weight         1308.35
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-30 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                107.27(5)
_cell_angle_beta                 95.31(4)
_cell_angle_gamma                100.58(3)
_cell_formula_units_Z            2
_cell_length_a                   11.287(3)
_cell_length_b                   11.804(4)
_cell_length_c                   18.747(14)
_cell_measurement_reflns_used    775
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.7480
_cell_measurement_theta_min      2.0270
_cell_volume                     2316(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      air
_diffrn_ambient_pressure         3520000
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.379
_diffrn_measured_fraction_theta_max 0.379
_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    -31.00   9.00   1.00   30.00    --   12.55  81.00 151.00   40
  2  \w     13.00  56.00   1.00   30.00    --   12.55 -77.00-150.00   43
  3  \w    -13.00  34.00   1.00   30.00    --   12.55 -38.00-150.00   47
  4  \w    -32.00  25.00   1.00   30.00    --   12.55  39.00 -12.00   57
  5  \w     72.00 108.00   1.00   30.00    --   12.55 178.00  90.00   36
  6  \w    -28.00  20.00   1.00   30.00    --   12.55  53.00 162.00   48
  7  \w     58.00 109.00   1.00   30.00    --   12.55-178.00 -90.00   51
  8  \w    -35.00 -12.00   1.00   30.00    --  -13.41  77.00 -30.00   23
  9  \w      2.00  37.00   1.00   30.00    --  -13.41 -99.00-150.00   35
 10  \w     -8.00  31.00   1.00   30.00    --  -13.41 -81.00  29.00   39
 11  \w    -42.00  33.00   1.00   30.00    --  -13.41  13.00  -3.00   75
 12  \w     12.00  35.00   1.00   30.00    --   12.55 -77.00  60.00   23
 13  \w     12.00  35.00   1.00   30.00    --   12.55 -77.00  30.00   23
 14  \w     34.00  61.00   1.00   30.00    --   12.55 -99.00  60.00   27
 15  \w     34.00  61.00   1.00   30.00    --   12.55 -99.00  30.00   27
 16  \w    -14.00  33.00   1.00   30.00    --  -13.41 -38.00-180.00   47
 17  \w    -35.00 -12.00   1.00   30.00    --  -13.41  77.00 120.00   23
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0150647000
_diffrn_orient_matrix_UB_12      -0.0165615000
_diffrn_orient_matrix_UB_13      -0.0398604000
_diffrn_orient_matrix_UB_21      -0.0300776000
_diffrn_orient_matrix_UB_22      -0.0591172000
_diffrn_orient_matrix_UB_23      -0.0014318000
_diffrn_orient_matrix_UB_31      -0.0553001000
_diffrn_orient_matrix_UB_32      0.0198973000
_diffrn_orient_matrix_UB_33      0.0042861000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2422
_diffrn_reflns_av_unetI/netI     0.1896
_diffrn_reflns_Laue_measured_fraction_full 0.379
_diffrn_reflns_Laue_measured_fraction_max 0.379
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12789
_diffrn_reflns_point_group_measured_fraction_full 0.379
_diffrn_reflns_point_group_measured_fraction_max 0.379
_diffrn_reflns_theta_full        20.814
_diffrn_reflns_theta_max         20.814
_diffrn_reflns_theta_min         1.842
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43641
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       plate
_exptl_crystal_F_000             1314
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.568
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         1834
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.2501
_refine_ls_R_factor_gt           0.1524
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3403
_refine_ls_wR_factor_ref         0.3967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                886
_reflns_number_total             1834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06722f2.cif
_cod_data_source_block           dy60_hp7
_cod_database_code               7131351
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C58H58BDyF20
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.690
_reflns_odcompleteness_completeness 38.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     20.77
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C19
 1.55 with sigma of 0.1
 C7-C6 \\sim C8-C6 \\sim C9-C6
 with sigma of 0.02
 C13-C10 \\sim C11-C10 \\sim C12-C10
 with sigma of 0.02
 C17-C14 \\sim C15-C14 \\sim C16-C14
 with sigma of 0.02
 C26-C23 \\sim C25-C23 \\sim C24-C23
 with sigma of 0.02
 C33-C31 \\sim C34-C31 \\sim C32-C31
 with sigma of 0.02
 C30-C27 \\sim C29-C27 \\sim C28-C27
 with sigma of 0.02
 C7-C8 \\sim C7-C9 \\sim C8-C9
 with sigma of 0.02
 C13-C11 \\sim C13-C12 \\sim C11-C12
 with sigma of 0.02
 C17-C15 \\sim C17-C16 \\sim C16-C15
 with sigma of 0.02
 C26-C25 \\sim C25-C24 \\sim C25-C24
 with sigma of 0.02
 C33-C34 \\sim C33-C32 \\sim C34-C32
 with sigma of 0.02
 C30-C29 \\sim C30-C28 \\sim C29-C28
 with sigma of 0.02
 C7-C1 \\sim C8-C1 \\sim C9-C1
 with sigma of 0.02
 C13-C2 \\sim C11-C2 \\sim C12-C2
 with sigma of 0.02
 C17-C4 \\sim C15-C4 \\sim C16-C4
 with sigma of 0.02
 C26-C18 \\sim C25-C18 \\sim C24-C18
 with sigma of 0.02
 C33-C21 \\sim C34-C21 \\sim C32-C21
 with sigma of 0.02
 C30-C19 \\sim C29-C19 \\sim C28-C19
 with sigma of 0.02
3. Restrained planarity
 C54, C55, C56, C57, C58, F16, F17, F18, F19, F20, B1, C53
 with sigma of 0.1
 C47, C52, C51, C50, C49, C48, F15, F14, F13, F12, F11, B1
 with sigma of 0.1
 C35, C36, C37, C38, C39, C40, F1, F2, F3, F4, F5, B1
 with sigma of 0.1
 C41, C46, C45, C44, C43, C42, F10, F9, F8, F7, F6, B1
 with sigma of 0.1
4.a Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
4.c Fitted pentagon refined as free rotating group:
 C1(C2,C3,C4,C5), C21(C20,C19,C18,C22)
4.d Fitted hexagon refined as free rotating group:
 C35(C40,C39,C38,C37,C36), C41(C42,C43,C44,C45,C46), C47(C48,C49,C50,C51,C52),
 C53(C58,C57,C56,C55,C54)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              16214
_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 1.630
_oxdiff_exptl_absorpt_empirical_full_min 0.642