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_1560754
_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         'C62 H76 Dy N4 P4 Si4, C31 H40 K O7'
_chemical_formula_sum            'C93 H116 Dy K N4 O7 P4 Si4'
_chemical_formula_weight         1839.73
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                90
_cell_angle_beta                 97.5329(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.23949(14)
_cell_length_b                   23.5137(3)
_cell_length_c                   30.0645(4)
_cell_measurement_reflns_used    20482
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.8670
_cell_measurement_theta_min      3.9580
_cell_volume                     9278.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2207
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -27.00   24.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.0601   38.0000   60.0000 51

  2 omega  -50.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.0601   38.0000  150.0000 76

  3 omega  -66.00  -21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.0601   57.0000   30.0000 45

  4 omega  -35.00   24.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.0601   38.0000 -150.0000 59

  5 omega   88.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      103.6263    0.0000 -150.0000 89

  6 omega   81.00  172.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      103.6263   45.0000   60.0000 91

  7 omega   57.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      103.6263  -45.0000  120.0000 31

  8 omega   57.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      103.6263  -45.0000   60.0000 26

  9 omega   41.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      103.6263  -45.0000  -60.0000 46

 10 omega   50.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      103.6263    0.0000 -150.0000 26

 11 omega   36.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      103.6263  -45.0000 -120.0000 54

 12 omega   27.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      103.6263  -94.0000 -120.0000 56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0511333000
_diffrn_orient_matrix_UB_12      0.0427151000
_diffrn_orient_matrix_UB_13      -0.0347219000
_diffrn_orient_matrix_UB_21      0.1015770000
_diffrn_orient_matrix_UB_22      0.0075261000
_diffrn_orient_matrix_UB_23      -0.0191501000
_diffrn_orient_matrix_UB_31      -0.0288744000
_diffrn_orient_matrix_UB_32      -0.0491421000
_diffrn_orient_matrix_UB_33      -0.0331388000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39163
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.984
_diffrn_reflns_theta_min         3.971
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.284
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_correction_T_min  0.343
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             3836
_exptl_crystal_size_max          0.2776
_exptl_crystal_size_mid          0.1959
_exptl_crystal_size_min          0.1158
_refine_diff_density_max         1.094
_refine_diff_density_min         -1.496
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         18298
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.8015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16808
_reflns_number_total             18298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00238d2.cif
_cod_data_source_block           5Dy
_cod_depositor_comments
'Adding full bibliography for 1560749--1560758.cif.'
_cod_database_code               1560754
_nottingham_internal_coll_name   DYMGLG
_nottingham_internal_coll_number 15052
_nottingham_internal_coll_client MG/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '5.0000, 20.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxmjg
_nottingham_internal_coll_date   09/08/2015
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_process_date 10/08/2015
_nottingham_internal_process_user pczmjg1
_nottingham_internal_solution_date 10/08/2015
_nottingham_internal_solution_user pczmjg1
_nottingham_internal_refinement_date 10/08/2015
_nottingham_internal_refinement_user pczmjg1
_nottingham_internal_self_archive_date 10/08/2015
_nottingham_internal_self_validation_date 10/08/2015
_nottingham_internal_self_validation_user pczmjg1
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C90 H116 Dy K N4 O8 P4 Si4'
_chemical_oxdiff_usercomment
'DYMGLG #15052 GVA675 FOR MG/STL IN FOMBLIN FILM ON MICROMOUNT'
_reflns_odcompleteness_completeness 99.87
_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. Restrained distances
 C90-C89 \\sim C93-C92
 with sigma of 0.01
 C89-C88 \\sim C93-C88
 with sigma of 0.01
 C91-C90 \\sim C92-C91
 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C79(H79A,
 H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B)
3.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), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58),
 C59(H59), C64(H64), C65(H65), C66(H66), C67(H67), C74(H74), C75(H75), C76(H76),
  C77(H77), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C87(H87A,H87B,H87C)
;
_shelx_res_checksum              14095
_shelx_hkl_checksum              84945
_olex2_submission_special_instructions 'No special instructions were received'