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_7131346
_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             2020-02-27
_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                106.90(3)
_cell_angle_beta                 95.05(3)
_cell_angle_gamma                100.716(14)
_cell_formula_units_Z            2
_cell_length_a                   11.5239(18)
_cell_length_b                   12.176(2)
_cell_length_c                   19.539(8)
_cell_measurement_reflns_used    2011
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.2030
_cell_measurement_theta_min      1.7940
_cell_volume                     2547.9(13)
_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_pressure         1010000
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.371
_diffrn_measured_fraction_theta_max 0.371
_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     34.00  58.00   1.00   30.00    --    7.60 -99.00  30.00   24
  2  \w    -33.00  20.00   1.00   30.00    --    7.60  53.00 -17.00   53
  3  \w    -36.00   9.00   1.00   30.00    --    7.60  81.00 -29.00   45
  4  \w    -35.00  14.00   1.00   30.00    --    7.60  67.00 157.00   49
  5  \w    -14.00  35.00   1.00   30.00    --   -8.46 -67.00-157.00   49
  6  \w    -42.00  33.00   1.00   30.00    --   -8.46  13.00  -3.00   75
  7  \w    -35.00 -12.00   1.00   30.00    --   -8.46  77.00 150.00   23
  8  \w     -9.00  36.00   1.00   30.00    --   -8.46 -81.00  29.00   45
  9  \w     12.00  35.00   1.00   30.00    --    7.60 -77.00  60.00   23
 10  \w     34.00  58.00   1.00   30.00    --    7.60 -99.00-150.00   24
 11  \w     34.00  58.00   1.00   30.00    --    7.60 -99.00   0.00   24
 12  \w     34.00  58.00   1.00   30.00    --    7.60 -99.00  60.00   24
 13  \w     12.00  51.00   1.00   30.00    --    7.60 -77.00-150.00   39
 14  \w     12.00  35.00   1.00   30.00    --    7.60 -77.00  30.00   23
 15  \w    -35.00 -12.00   1.00   30.00    --   -8.46  77.00 120.00   23
 16  \w     20.00  80.00   1.00   30.00    --    7.60-135.00  57.00   60
 17  \w     -1.00  48.00   1.00   30.00    --    7.60 -57.00-150.00   49
 18  \w    -20.00   5.00   1.00   30.00    --   -8.46 -53.00  17.00   25
 19  \w    -50.00  20.00   1.00   30.00    --   -8.46  53.00 162.00   70
;
_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      -0.0145240000
_diffrn_orient_matrix_UB_12      -0.0156853000
_diffrn_orient_matrix_UB_13      -0.0381353000
_diffrn_orient_matrix_UB_21      -0.0316065000
_diffrn_orient_matrix_UB_22      -0.0565095000
_diffrn_orient_matrix_UB_23      -0.0011300000
_diffrn_orient_matrix_UB_31      -0.0529706000
_diffrn_orient_matrix_UB_32      0.0214396000
_diffrn_orient_matrix_UB_33      0.0041917000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2160
_diffrn_reflns_av_unetI/netI     0.1698
_diffrn_reflns_Laue_measured_fraction_full 0.371
_diffrn_reflns_Laue_measured_fraction_max 0.371
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12263
_diffrn_reflns_point_group_measured_fraction_full 0.371
_diffrn_reflns_point_group_measured_fraction_max 0.371
_diffrn_reflns_theta_full        20.807
_diffrn_reflns_theta_max         20.807
_diffrn_reflns_theta_min         1.786
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25046
_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    1.705
_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         1.158
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         1981
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.1243
_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          0.2842
_refine_ls_wR_factor_ref         0.3322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1210
_reflns_number_total             1981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06722f2.cif
_cod_data_source_block           dy60_hp3
_cod_original_cell_volume        2547.8(13)
_cod_database_code               7131346
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C58H58BDyF20
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.713
_reflns_odcompleteness_completeness 37.35
_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 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
3.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
3.c Fitted pentagon refined as free rotating group:
 C1(C2,C3,C4,C5), C21(C20,C19,C18,C22)
3.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)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              94013
_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 2.577
_oxdiff_exptl_absorpt_empirical_full_min 0.549