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_1560757
_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, C4 H8 O, C18 H36 K N2 O6'
_chemical_formula_sum            'C72 H84 Dy K N2 O7 P4 S4'
_chemical_formula_weight         1543.13
_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             2017-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-12-18 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                97.435(2)
_cell_angle_beta                 91.979(2)
_cell_angle_gamma                116.190(2)
_cell_formula_units_Z            2
_cell_length_a                   15.0677(3)
_cell_length_b                   15.8625(4)
_cell_length_c                   17.3285(3)
_cell_measurement_reflns_used    29658
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6690
_cell_measurement_theta_min      1.8170
_cell_volume                     3665.66(15)
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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    -66.00 -41.00   1.00    2.00    --   19.90  11.00 153.00   25
  2  \w    -69.00 -27.00   1.00    2.00    --   19.90  60.00-120.00   42
  3  \w     40.00  67.00   1.00    2.00    --   19.90  60.00-120.00   27
  4  \w    -70.00  10.00   1.00    2.00    --   19.90  43.00-150.00   80
  5  \w    -70.00 109.00   1.00    2.00    --   19.90  60.00  60.00  179
  6  \w    -34.00  -8.00   1.00    2.00    --   19.90  57.00 150.00   26
  7  \w      1.00  60.00   1.00    2.00    --   19.90  57.00 150.00   59
  8  \w     70.00  95.00   1.00    2.00    --   19.90  57.00 150.00   25
  9  \w     22.00  48.00   1.00    2.00    --   19.90  60.00-150.00   26
 10  \w    -69.00 109.00   1.00    2.00    --   19.90  60.00  90.00  178
 11  \w     -5.00  84.00   1.00    2.00    --   19.90  11.00 153.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0456533000
_diffrn_orient_matrix_UB_12      -0.0023509000
_diffrn_orient_matrix_UB_13      -0.0034645000
_diffrn_orient_matrix_UB_21      0.0227540000
_diffrn_orient_matrix_UB_22      0.0476810000
_diffrn_orient_matrix_UB_23      -0.0071338000
_diffrn_orient_matrix_UB_31      0.0134013000
_diffrn_orient_matrix_UB_32      0.0164467000
_diffrn_orient_matrix_UB_33      0.0407355000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47182
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_min         1.828
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.309
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       plate
_exptl_crystal_F_000             1590
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.703
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         15484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0441P)^2^+9.3611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14161
_reflns_number_total             15484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00238d2.cif
_cod_data_source_block           4Dy
_cod_depositor_comments
'Adding full bibliography for 1560749--1560758.cif.'
_cod_original_cell_volume        3665.65(15)
_cod_database_code               1560757
_manchester_internal_diff_code   LSTL36
_manchester_internal_stl_name    DYLTH4
_manchester_internal_stl_number  587
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   24/10/2017
_manchester_internal_process_date 26/10/2017
_manchester_internal_process_user LTH
_manchester_internal_solution_date 26/10/2017
_manchester_internal_solution_user LTH/AW
_manchester_internal_refinement_date 26/10/2017
_manchester_internal_refinement_user LTH/AW
_manchester_internal_validation_date 26/10/2017
_manchester_internal_validation_user LTH/AW
_manchester_internal_archive_date 30/10/2017
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C72H84DyKN2O7P4S4
_chemical_oxdiff_usercomment     lth
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.592
_reflns_odcompleteness_completeness 99.93
_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
2.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B),
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B),
  C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,
 H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B)
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)
;
_shelx_res_checksum              34329
_shelx_hkl_checksum              24272
_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 1.780
_oxdiff_exptl_absorpt_empirical_full_min 0.561