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_1560752
_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 H48 O P4 S4 Y, C18 H36 K N2 O6, C4 H8 O'
_chemical_formula_sum            'C76 H92 K N2 O8 P4 S4 Y'
_chemical_formula_weight         1541.64
_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             2017-09-14
_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                81.430(3)
_cell_angle_beta                 83.556(3)
_cell_angle_gamma                84.318(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9072(4)
_cell_length_b                   12.5346(5)
_cell_length_c                   26.2160(11)
_cell_measurement_reflns_used    8139
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.6880
_cell_measurement_theta_min      3.4600
_cell_volume                     3831.2(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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1428
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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    -40.00  54.00   1.00    2.02    --  -18.77  37.00 -60.00   94
  2  \w      8.00  34.00   1.00    2.02    --  -18.77   0.00-180.00   26
  3  \w    -18.00   8.00   1.00    2.02    --  -18.77 -99.00  30.00   26
  4  \w    -16.00  25.00   1.00    2.02    --  -18.77 -99.00 150.00   41
  5  \w    -68.00 -36.00   1.00    2.02    --  -18.77-178.00 -90.00   32
  6  \w     -8.00  25.00   1.00    2.02    --  -18.77 -99.00-120.00   33
  7  \w    -61.00 -35.00   1.00    2.02    --  -18.77   0.00-180.00   26
  8  \w    -46.00  43.00   1.00    2.02    --  -18.77  37.00-150.00   89
  9  \w     36.00  97.00   1.00    2.02    --   20.02 178.00-180.00   61
 10  \w     63.00  97.00   1.00    2.02    --   20.02 178.00  90.00   34
 11  \w    -90.00 -64.00   1.00    2.02    --  -18.77   0.00-180.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0282741000
_diffrn_orient_matrix_UB_12      -0.0039345000
_diffrn_orient_matrix_UB_13      -0.0219797000
_diffrn_orient_matrix_UB_21      0.0102309000
_diffrn_orient_matrix_UB_22      -0.0571835000
_diffrn_orient_matrix_UB_23      0.0043773000
_diffrn_orient_matrix_UB_31      -0.0521056000
_diffrn_orient_matrix_UB_32      -0.0035402000
_diffrn_orient_matrix_UB_33      0.0159313000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.1273
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29249
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.283
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.148
_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    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.959
_exptl_crystal_size_mid          0.732
_exptl_crystal_size_min          0.53
_refine_diff_density_max         1.506
_refine_diff_density_min         -2.107
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         12993
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1571P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9096
_reflns_number_total             12993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00238d2.cif
_cod_data_source_block           4Y
_cod_depositor_comments
'Adding full bibliography for 1560749--1560758.cif.'
_cod_database_code               1560752
_manchester_internal_diff_code   astl199
_manchester_internal_stl_name    YLTH14
_manchester_internal_stl_number  475
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   07/08/2017
_manchester_internal_process_date 08/08/2017
_manchester_internal_process_user LTH
_manchester_internal_solution_date 12/09/2017
_manchester_internal_solution_user LTH/AW
_manchester_internal_refinement_date 12/09/2017
_manchester_internal_refinement_user LTH/AW
_manchester_internal_validation_date 12/09/2017
_manchester_internal_validation_user LTH/AW
_manchester_internal_archive_date 15/09/2017
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Y S4 P4 C75 H80 O6 N2 K'
_chemical_oxdiff_usercomment     LTH
_shelx_estimated_absorpt_t_max   0.603
_shelx_estimated_absorpt_t_min   0.429
_reflns_odcompleteness_completeness 95.86
_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. Restrained distances
 C52-C51 = C53-C52 = C54-C53
 1.55 with sigma of 0.01
 C76-C75 = C75-C74 = C74-C73 = C76A-C75A = C74A-C75A = C74A-C73A
 1.55 with sigma of 0.01
 C58-C57 = C70-C69 = C64-C63
 1.55 with sigma of 0.01
 O8-C73 \\sim O8-C76 \\sim O8A-C76A \\sim O8A-C73A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O8A \\sim C73A \\sim C74A \\sim C75A \\sim C76A \\sim O8 \\sim C73 \\sim C74
\\sim C75 \\sim C76: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
4. Rigid body (RIGU) restrains
 C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23,
 C24, C25, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39, C40,
  C41, C42, C43, C44, C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8A, C73A, C74A, C75A, C76A, O8, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O8)=Sof(C73)=Sof(H73C)=Sof(H73D)=Sof(C74)=Sof(H74C)=Sof(H74D)=Sof(C75)=
 Sof(H75C)=Sof(H75D)=Sof(C76)=Sof(H76C)=Sof(H76D)=1-FVAR(1)
 Sof(O8A)=Sof(C73A)=Sof(H73A)=Sof(H73B)=Sof(C74A)=Sof(H74A)=Sof(H74B)=
 Sof(C75A)=Sof(H75A)=Sof(H75B)=Sof(C76A)=Sof(H76A)=Sof(H76B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 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), C69(H69A,
 H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73A(H73A,H73B),
 C74A(H74A,H74B), C75A(H75A,H75B), C76A(H76A,H76B), C73(H73C,H73D), C74(H74C,
 H74D), C75(H75C,H75D), C76(H76C,H76D)
6.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              50464
_shelx_hkl_checksum              51050
_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 98.549
_oxdiff_exptl_absorpt_empirical_full_min 0.541