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_1560756
_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 Gd P4 S4, C12 H30 Na O6'
_chemical_formula_sum            'C62 H70 Gd Na O6 P4 S4'
_chemical_formula_weight         1343.54
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-02-26
_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                90
_cell_angle_beta                 110.508(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1998(4)
_cell_length_b                   30.9404(6)
_cell_length_c                   15.6211(5)
_cell_measurement_reflns_used    15465
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.1940
_cell_measurement_theta_min      2.7430
_cell_volume                     6428.1(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -20.00  25.00   1.00   17.50    --  -18.62 -99.00   0.00   45
  2  \w    -46.00  54.00   1.00   17.50    --  -18.62  37.00-120.00  100
  3  \w    -96.00 -35.00   1.00   17.50    --  -18.62-178.00  60.00   61
  4  \w    -49.00  42.00   1.00   17.50    --   20.02 -57.00 -30.00   91
  5  \w     -2.00  89.00   1.00   17.50    --   20.02  57.00 -30.00   91
  6  \w    -12.00  91.00   1.00   17.50    --   20.02  77.00-150.00  103
  7  \w     35.00  98.00   1.00   17.50    --   20.02 178.00 -60.00   63
  8  \w    -12.00  91.00   1.00   17.50    --   20.02  77.00  90.00  103
  9  \w    -92.00  55.00   1.00   17.50    --  -18.62   0.00  90.00  147
 10  \w    -93.00  31.00   1.00   17.50    --  -18.62 -19.00-120.00  124
 11  \w    -20.00  64.00   1.00   17.50    --   20.02 -99.00  90.00   84
 12  \w    -20.00  64.00   1.00   17.50    --   20.02 -99.00-180.00   84
 13  \w    -20.00  64.00   1.00   17.50    --   20.02 -99.00 -60.00   84
 14  \w     35.00  98.00   1.00   17.50    --   20.02 178.00-180.00   63
 15  \w    -20.00  20.00   1.00   17.50    --  -18.62 -99.00 -30.00   40
;
_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      0.0127613000
_diffrn_orient_matrix_UB_12      -0.0150808000
_diffrn_orient_matrix_UB_13      0.0364710000
_diffrn_orient_matrix_UB_21      -0.0089858000
_diffrn_orient_matrix_UB_22      0.0159621000
_diffrn_orient_matrix_UB_23      0.0288244000
_diffrn_orient_matrix_UB_31      -0.0509978000
_diffrn_orient_matrix_UB_32      -0.0066002000
_diffrn_orient_matrix_UB_33      -0.0136900000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1779
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            156285
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.666
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.718
_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    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.867
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         14169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0633P)^2^+2.4810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9013
_reflns_number_total             14169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00238d2.cif
_cod_data_source_block           3Gd
_cod_depositor_comments
'Adding full bibliography for 1560749--1560758.cif.'
_cod_database_code               1560756
_manchester_internal_diff_code   astl312
_manchester_internal_stl_name    GDFO2
_manchester_internal_coll_client FO
_manchester_internal_coll_date   14/02/2018
_manchester_internal_process_date 26/02/2018
_manchester_internal_process_user LTH
_manchester_internal_solution_date 26/02/2018
_manchester_internal_solution_user LTH
_manchester_internal_refinement_date 26/02/2018
_manchester_internal_refinement_user LTH/AW
_manchester_internal_validation_date 26/02/2018
_manchester_internal_validation_user LTH/AW
_manchester_internal_archive_date 12/03/2018
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Gd P4 S4 C60 H60 O6 Na'
_chemical_oxdiff_usercomment     FO/STL
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.744
_reflns_odcompleteness_completeness 99.87
_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 Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C56(H56A,H56B), C57(H57A,H57B), C60(H60A,
 H60B), C61(H61A,H61B)
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)
2.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              6956
_shelx_hkl_checksum              68555
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.919
_oxdiff_exptl_absorpt_empirical_full_min 0.599