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_7131344
_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             2020-02-26
_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                107.031(3)
_cell_angle_beta                 96.387(3)
_cell_angle_gamma                99.377(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6278(3)
_cell_length_b                   12.6173(5)
_cell_length_c                   20.3029(7)
_cell_measurement_reflns_used    8547
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.2720
_cell_measurement_theta_min      1.7250
_cell_volume                     2769.80(17)
_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_pressure         0
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     44.00  69.00   1.00   30.00    --   22.61-157.00-132.00   25
  2  \w     21.00  46.00   1.00   30.00    --   22.61-119.00  23.00   25
  3  \w     56.00 109.00   1.00   30.00    --   22.61 157.00 -96.00   53
  4  \w    -94.00 -60.00   1.00   30.00    --  -23.39-157.00-132.00   34
  5  \w    -93.00 -68.00   1.00   30.00    --  -23.39 157.00 -96.00   25
  6  \w    -57.00 -30.00   1.00   30.00    --  -23.39 119.00 108.00   27
  7  \w     88.00 128.00   1.00   30.00    --   22.61  77.00-120.00   40
  8  \w     82.00 128.00   1.00   30.00    --   22.61  77.00-150.00   46
  9  \w    -26.00  41.00   1.00   30.00    --   22.61  77.00  60.00   67
 10  \w     82.00 128.00   1.00   30.00    --   22.61  77.00  90.00   46
 11  \w    -25.00  42.00   1.00   30.00    --   22.61  77.00 -60.00   67
 12  \w   -131.00 -93.00   1.00   30.00    --  -23.39 -77.00-120.00   38
 13  \w   -128.00 -82.00   1.00   30.00    --  -23.39 -77.00  30.00   46
 14  \w      8.00  33.00   1.00   30.00    --  -23.39 -99.00 120.00   25
 15  \w   -131.00-102.00   1.00   30.00    --  -23.39 -77.00  60.00   29
 16  \w    -12.00  29.00   1.00   30.00    --  -23.39 -99.00  30.00   41
 17  \w   -130.00 -82.00   1.00   30.00    --  -23.39 -77.00  90.00   48
;
_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      0.0514630000
_diffrn_orient_matrix_UB_12      0.0428399000
_diffrn_orient_matrix_UB_13      0.0157040000
_diffrn_orient_matrix_UB_21      -0.0075283000
_diffrn_orient_matrix_UB_22      -0.0049516000
_diffrn_orient_matrix_UB_23      0.0332411000
_diffrn_orient_matrix_UB_31      0.0350585000
_diffrn_orient_matrix_UB_32      -0.0418317000
_diffrn_orient_matrix_UB_33      -0.0047393000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27269
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.716
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75583
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       irregular
_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         1.228
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+2.6137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8367
_reflns_number_total             10122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06722f2.cif
_cod_data_source_block           dy60_hp0
_cod_original_cell_volume        2769.81(18)
_cod_database_code               7131344
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C58H58BDyF20
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.731
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
2.b 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), C15(H15A,H15B,H15C), 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              61688
_olex2_date_sample_data_collection 2019-11-12
_olex2_exptl_crystal_mounting_method 'In paratone oil on a Kapton loop'
_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 1.513
_oxdiff_exptl_absorpt_empirical_full_min 0.728