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_1560749
_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         'C54 H49 Dy O P4 S4, 2(C7 H8)'
_chemical_formula_sum            'C68 H65 Dy O P4 S4'
_chemical_formula_weight         1312.82
_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             2016-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2020-12-18 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                89.265(3)
_cell_angle_beta                 88.319(4)
_cell_angle_gamma                83.122(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2686(6)
_cell_length_b                   12.7447(3)
_cell_length_c                   21.7296(12)
_cell_measurement_reflns_used    8001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4170
_cell_measurement_theta_min      3.6890
_cell_volume                     3096.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.809
_diffrn_measurement_details
;
  1 omega   35.00  101.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3799  178.0000   60.0000 66

  2 omega  -82.00   15.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8486  -57.0000   60.0000 97

  3 omega  -41.00   57.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8486   57.0000 -150.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0009724000
_diffrn_orient_matrix_UB_12      0.0007124000
_diffrn_orient_matrix_UB_13      -0.0326549000
_diffrn_orient_matrix_UB_21      0.0030329000
_diffrn_orient_matrix_UB_22      -0.0559100000
_diffrn_orient_matrix_UB_23      -0.0000794000
_diffrn_orient_matrix_UB_31      -0.0633460000
_diffrn_orient_matrix_UB_32      0.0040387000
_diffrn_orient_matrix_UB_33      0.0004107000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22189
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.495
_diffrn_reflns_theta_min         3.572
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.658
_exptl_absorpt_correction_T_min  0.322
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.6875
_exptl_crystal_size_mid          0.2462
_exptl_crystal_size_min          0.1786
_refine_diff_density_max         2.073
_refine_diff_density_min         -2.144
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         13948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0481P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10859
_reflns_number_total             13948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00238d2.cif
_cod_data_source_block           1Dy
_cod_depositor_comments
'Adding full bibliography for 1560749--1560758.cif.'
_cod_database_code               1560749
_manchester_internal_diff_code   ostl8
_manchester_internal_stl_number  38
_manchester_internal_stl_name    DYEZ1
_manchester_internal_coll_client MG/EZ
_manchester_internal_coll_user   MG
_manchester_internal_coll_date   04/02/2016
_manchester_internal_process_user MG
_manchester_internal_process_date 04/02/2016
_manchester_internal_solution_user MG
_manchester_internal_solution_date 04/02/2016
_manchester_internal_refinement_user MG
_manchester_internal_refinement_date 04/02/2016
_manchester_internal_validation_user MG
_manchester_internal_validation_date 04/02/2016
_manchester_internal_archive_user AW
_manchester_internal_archive_date 05/02/2016
_chemical_oxdiff_formula         'Dy C54 H49 S4 P4 O'
_chemical_oxdiff_usercomment     'DYEZ1 for EZ/MG'
_reflns_odcompleteness_completeness 98.48
_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 Ternary CH refined with riding coordinates:
 C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
2.c 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), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68)
2.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              70803
_shelx_hkl_checksum              3689
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'