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_1560750
_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 O P4 S4 Y'
_chemical_formula_sum            'C54 H49 O P4 S4 Y'
_chemical_formula_weight         1054.96
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-14
_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                90
_cell_angle_beta                 99.013(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8536(6)
_cell_length_b                   22.5853(10)
_cell_length_c                   21.0093(11)
_cell_measurement_reflns_used    3028
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.0320
_cell_measurement_theta_min      3.6660
_cell_volume                     5086.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     12.00  85.00   1.00   25.00    --   18.70  37.00 -90.00   73
  2  \w    -18.00  86.00   1.00   25.00    --   18.70  19.00  30.00  104
  3  \w     51.00  87.00   1.00   25.00    --   18.70-178.00-150.00   36
  4  \w    -83.00 -45.00   1.00   25.00    --  -17.77-178.00  60.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0255695000
_diffrn_orient_matrix_UB_12      0.0072966000
_diffrn_orient_matrix_UB_13      0.0322263000
_diffrn_orient_matrix_UB_21      -0.0510633000
_diffrn_orient_matrix_UB_22      -0.0140884000
_diffrn_orient_matrix_UB_23      0.0110549000
_diffrn_orient_matrix_UB_31      0.0334190000
_diffrn_orient_matrix_UB_32      -0.0270987000
_diffrn_orient_matrix_UB_33      0.0029168000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.1411
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22004
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.343
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.475
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0705
_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^)+(0.0220P)^2^+0.4376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5840
_reflns_number_total             8952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00238d2.cif
_cod_data_source_block           1Y
_cod_depositor_comments
'Adding full bibliography for 1560749--1560758.cif.'
_cod_database_code               1560750
_manchester_internal_diff_code   astl1
_manchester_internal_stl_number  2
_manchester_internal_stl_name    YEZ2
_manchester_internal_coll_client MG/STL
_manchester_internal_coll_user   MG
_manchester_internal_coll_date   30/11/2015
_manchester_internal_process_user MG
_manchester_internal_process_date 30/11/2015
_manchester_internal_solution_user MG
_manchester_internal_solution_date 30/11/2015
_manchester_internal_refinement_user MG
_manchester_internal_refinement_date 14/12/2015
_manchester_internal_validation_user MG
_manchester_internal_validation_date 14/12/2015
_manchester_internal_archive_user AW
_manchester_internal_archive_date 18/12/2020
_chemical_oxdiff_formula         C54H49Y1P4S4O1
_chemical_oxdiff_usercomment     'astl1 s/n YEZ2 for MG/EZ'
_reflns_odcompleteness_completeness 99.71
_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 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)
;
_shelx_res_checksum              34219
_shelx_hkl_checksum              57949
_shelx_shelxl_version_number     2014/7
_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 1.106
_oxdiff_exptl_absorpt_empirical_full_min 0.813