Correlating axial and equatorial ligand field effects to the single-molecule magnet performances of a family of dysprosium bis-methanediide complexes
Thomas-Hargreaves, Lewis R.; Giansiracusa, Marcus J.; Gregson, Matthew; Zanda, Emanuele; O'Donnell, Felix; Wooles, Ashley J.; Chilton, Nicholas F.; Liddle, Stephen T.; Chemical Science 12 (2021) 3911–3920; doi:10.1039/D1SC00238D

data_1560751
_publ_section_title
;
 Correlating axial and equatorial ligand field effects to the
 single-molecule magnet performances of a family of dysprosium
 bis-methanediide complexes
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              3911
_journal_page_last               3920
_journal_paper_doi               10.1039/D1SC00238D
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C50 H40 Dy P4 S4, C66 H80 Dy K2 O8 P4 S4'
_chemical_formula_sum            'C116 H120 Dy2 K2 O8 P8 S8'
_chemical_formula_weight         2549.55
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-18 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                71.6450(10)
_cell_angle_beta                 79.4080(10)
_cell_angle_gamma                84.3730(10)
_cell_formula_units_Z            2
_cell_length_a                   13.5210(2)
_cell_length_b                   20.9074(3)
_cell_length_c                   22.2017(3)
_cell_measurement_reflns_used    45773
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.6470
_cell_measurement_theta_min      2.1260
_cell_volume                     5849.94(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.967
_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   -104.29  83.70   1.00   10.00    --  -75.00  73.87-115.79  188
  2  \w     80.71 268.71   1.00   20.00    --  110.00  73.87  74.21  188
  3  \f   -200.44 152.84   1.00   20.00 118.36 105.50  73.87    --   353
  4  \w     83.21 269.21   1.00   20.00    --  113.00  73.87-165.79  186
  5  \f    -93.60 151.59   1.00   10.00 145.57  20.50  73.87    --   245
  6  \f    -25.79 334.49   1.00   20.00 174.21 113.00  73.87    --   360
  7  \f    134.21 332.40   1.00   10.00  63.23 -60.00  73.87    --   198
  8  \w    -83.98  -4.99   1.00   10.00    --  -55.00  73.87 -10.79   79
  9  \w     82.21 269.21   1.00   20.00    --  112.00  73.87 124.21  187
 10  \w    256.66 327.66   1.00   10.00    --  -75.00  73.87 124.21   71
 11  \f    -25.79 334.43   1.00   20.00-140.79 110.00  73.87    --   360
 12  \f    -25.79 170.33   1.00   10.00  37.12 -45.00  73.87    --   196
 13  \w     60.80 148.80   1.00   10.00    --   35.50  73.87  11.71   88
 14  \f    -25.79  63.27   1.00   10.00  12.05  25.00  73.87    --    89
 15  \f    -62.49  37.59   1.00   10.00  66.87  25.50  73.87    --   100
 16  \w     54.21 153.21   1.00   10.00    --   23.00  73.87 176.71   99
 17  \f    -15.30  92.77   1.00   10.00-151.64  75.00  73.87    --   108
 18  \w     -7.01 120.99   1.00   10.00    --   20.50  73.87 111.71  128
 19  \w    -65.29 112.71   1.00   10.00    --  -45.00  73.87-110.79  178
 20  \f    -45.29  77.58   1.00   10.00 113.73 -42.00  73.87    --   123
 21  \w    -79.23  57.77   1.00   10.00    --  -50.00  73.87 -85.79  137
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1136196000
_diffrn_orient_matrix_UB_12      -0.0186962000
_diffrn_orient_matrix_UB_13      -0.0098785000
_diffrn_orient_matrix_UB_21      0.0230506000
_diffrn_orient_matrix_UB_22      0.0754219000
_diffrn_orient_matrix_UB_23      -0.0251248000
_diffrn_orient_matrix_UB_31      0.0044902000
_diffrn_orient_matrix_UB_32      -0.0005346000
_diffrn_orient_matrix_UB_33      0.0689924000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66763
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.125
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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    1.447
_exptl_crystal_description       plate
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         6.105
_refine_diff_density_min         -3.214
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1305
_refine_ls_number_reflns         20731
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1596P)^2^+34.4212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17211
_reflns_number_total             20731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00238d2.cif
_cod_data_source_block           2Dy
_cod_depositor_comments
'Adding full bibliography for 1560749--1560758.cif.'
_cod_database_code               1560751
_manchester_internal_diff_code   xstl7
_manchester_internal_stl_name    DYLTH1
_manchester_internal_stl_number  403
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   26/05/2017
_manchester_internal_process_date 07/05/2017
_manchester_internal_process_user LTH
_manchester_internal_solution_date 07/05/2017
_manchester_internal_solution_user LTH
_manchester_internal_refinement_date 27/06/2018
_manchester_internal_refinement_user LTH
_manchester_internal_validation_date 27/06/2018
_manchester_internal_validation_user LTH
_manchester_internal_archive_date 27/06/2018
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Dy2S8P8K2C100H100O8
_shelx_estimated_absorpt_t_max   0.429
_shelx_estimated_absorpt_t_min   0.235
_reflns_odcompleteness_completeness 96.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
P5 \\sim C51 \\sim P6 \\sim Dy2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 P5, C51, P6, C51, C106, C107
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C102(H10D,H10E), C103(H10F,H10G), C106(H10N,H10O), C107(H10P,H10Q), C110(H11A,
 H11B), C111(H11C,H11D), C114(H11K,H11L), C115(H11M,H11N)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
 C50(H50), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60),
  C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C68(H68),
 C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C78(H78), C79(H79),
  C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87),
 C88(H88), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
  C98(H98), C99(H99), C100(H100)
4.c Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C104(H10H,H10I,H10J), C105(H10K,H10L,H10M), C108(H10R,
 H10S,H10T), C109(H10U,H10V,H10W), C112(H11E,H11F,H11G), C113(H11H,H11I,H11J),
 C116(H11O,H11P,H11Q)
;
_shelx_res_checksum              36768
_shelx_hkl_checksum              89854
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.406
_oxdiff_exptl_absorpt_empirical_full_min 0.358