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_1560753
_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 P4 S4 Y, C66 H80 K2 O8 P4 S4 Y'
_chemical_formula_sum            'C116 H120 K2 O8 P8 S8 Y2'
_chemical_formula_weight         2402.37
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2020-12-18 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                71.523(2)
_cell_angle_beta                 79.315(2)
_cell_angle_gamma                84.386(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4728(4)
_cell_length_b                   20.8633(5)
_cell_length_c                   22.1735(4)
_cell_measurement_reflns_used    22240
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1840
_cell_measurement_theta_min      3.5630
_cell_volume                     5803.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.21a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.21a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.21a (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_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.843
_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    -29.00   9.00   0.50    2.50    --    5.00 -38.00 -90.00   76
  2  \w    -77.00 -52.00   0.50    2.50    --    5.00 -38.00-180.00   50
  3  \w    -96.00   4.00   0.50    2.50    --   -7.30 -38.00   0.00  200
  4  \w    -46.00  50.00   0.50    2.50    --   -7.30  38.00 -90.00  192
  5  \w    -34.00  25.00   0.50    2.50    --   -7.30  76.00 120.00  118
  6  \w     38.00  81.00   0.50    2.50    --   -7.30  76.00 120.00   86
  7  \w    -73.00  24.00   0.50    2.50    --   -7.30 -76.00 120.00  194
  8  \w    -94.00   1.00   0.50    2.50    --   -7.30 -57.00 -90.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0126579000
_diffrn_orient_matrix_UB_12      0.0004174000
_diffrn_orient_matrix_UB_13      -0.0326274000
_diffrn_orient_matrix_UB_21      -0.0083211000
_diffrn_orient_matrix_UB_22      0.0356399000
_diffrn_orient_matrix_UB_23      -0.0101958000
_diffrn_orient_matrix_UB_31      0.0514387000
_diffrn_orient_matrix_UB_32      0.0040953000
_diffrn_orient_matrix_UB_33      0.0005493000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            98260
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.024
_diffrn_reflns_theta_min         3.396
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.21a (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.609
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1305
_refine_ls_number_reflns         28623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0626P)^2^+8.8348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20852
_reflns_number_total             28623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00238d2.cif
_cod_data_source_block           2Y
_cod_depositor_comments
'Adding full bibliography for 1560749--1560758.cif.'
_cod_database_code               1560753
_manchester_internal_diff_code   rstl33
_manchester_internal_stl_name    YLTH5
_manchester_internal_stl_number  380
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   11/04/2017
_manchester_internal_process_date 12/04/2017
_manchester_internal_process_user LTH/AW
_manchester_internal_solution_date 12/04/2017
_manchester_internal_solution_user LTH/AW
_manchester_internal_refinement_date 12/04/2017
_manchester_internal_refinement_user LTH/AW
_manchester_internal_validation_date 12/04/2017
_manchester_internal_validation_user LTH/AW
_manchester_internal_archive_date 13/04/2017
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Y2 S8 P8 K2 C116 H120'
_chemical_oxdiff_usercomment     'LTH/STL YLTH5 '
_diffrn_oxdiff_ac3_digest_frames
;
013b10fe118c7af15fa518209d6f61668101106cb84
;
_diffrn_oxdiff_ac3_digest_hkl
;
0150e05d587a703ce643be22e55c9158fd25ad
;
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.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)
2.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)
2.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              60830
_shelx_hkl_checksum              29346
_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 1.253
_oxdiff_exptl_absorpt_empirical_full_min 0.859