Peripheral site modification in a family of dinuclear [Dy2(hynad)2-6(NO3)0-6(sol)0-2]0/2- single-molecule magnets bearing a {Dy2(μ-OR)2}4+ diamond-shaped core and exhibiting dissimilar magnetic dynamics
Armenis, Alexandros; Alexandropoulos, Dimitris; Worrell, Anne; Cunha-Silva, Luis; Dunbar, Kim R.; Stamatatos, Theocharis; Dalton Transactions  (2023) –; doi:10.1039/D3DT02596A

data_7713931
_publ_section_title
;
 Peripheral site modification in a family of dinuclear
 [Dy2(hynad)2-6(NO3)0-6(sol)0-2]0/2- single-molecule magnets bearing a
 {Dy2(\m-OR)2}4+ diamond-shaped core and exhibiting dissimilar magnetic
 dynamics
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02596A
_journal_year                    2023
_chemical_formula_moiety         'C24 H12 Dy2 N8 O24, 2(C2 H3 N), 2(C4 H12 N)'
_chemical_formula_sum            'C36 H42 Dy2 N12 O24'
_chemical_formula_weight         1351.81
_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
_audit_creation_date             2018-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-06-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                115.252(3)
_cell_angle_beta                 109.857(3)
_cell_angle_gamma                96.441(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9643(3)
_cell_length_b                   11.4838(3)
_cell_length_c                   11.7527(5)
_cell_measurement_reflns_used    7372
_cell_measurement_temperature    293.0(1)
_cell_measurement_theta_max      76.4880
_cell_measurement_theta_min      4.4380
_cell_volume                     1199.95(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.988
_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    -90.00 -45.00   1.00    0.10    --  -48.45 -49.00 147.00   45
  2  \w     47.00 121.00   1.00    0.10    --   48.45  49.00 -64.00   74
  3  \w     -7.00  58.00   1.00    0.10    --   48.45 -49.00 147.00   65
  4  \w   -159.00 -73.00   1.00    0.20    --  -86.25 -49.00 147.00   86
  5  \w    -48.00 -14.00   1.00    0.20    --  -86.25  49.00 -64.00   34
  6  \w     86.00 118.00   1.00    0.20    --  107.75 -49.00 147.00   32
  7  \w     37.00  63.00   1.00    0.20    --  107.75 -49.00 147.00   26
  8  \w     95.00 177.00   1.00    0.20    --  107.75  49.00 -64.00   82
  9  \w   -120.00 -71.00   1.00    0.10    --  -48.45-125.00  90.00   49
 10  \w    -61.00 -32.00   1.00    0.10    --  -48.45  49.00 -64.00   29
 11  \w   -119.00 -75.00   1.00    0.10    --  -48.45-125.00-150.00   44
 12  \w    -24.00  15.00   1.00    0.10    --  -48.45  49.00 -64.00   39
 13  \w     39.00  96.00   1.00    0.10    --   48.45-125.00-180.00   57
 14  \w    -58.00 -13.00   1.00    0.20    --  -86.25 125.00  30.00   45
 15  \w    -90.00 -63.00   1.00    0.20    --  -86.25 125.00  30.00   27
 16  \w     40.00  95.00   1.00    0.20    --  107.75 -99.00  60.00   55
 17  \w     35.00 125.00   1.00    0.20    --  107.75 -77.00 120.00   90
 18  \w     35.00 116.00   1.00    0.20    --  107.75-125.00  30.00   81
 19  \w     95.00 172.00   1.00    0.20    --  107.75  57.00-150.00   77
 20  \w     93.00 177.00   1.00    0.20    --  107.75  57.00-180.00   84
 21  \w    110.00 178.00   1.00    0.20    --  107.75 125.00  90.00   68
 22  \w     44.00 115.00   1.00    0.20    --  107.75-125.00 -60.00   71
 23  \w     35.00 109.00   1.00    0.20    --  107.75 -99.00 120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0978183000
_diffrn_orient_matrix_UB_12      0.0708067000
_diffrn_orient_matrix_UB_13      0.0500285000
_diffrn_orient_matrix_UB_21      0.1053846000
_diffrn_orient_matrix_UB_22      0.0625108000
_diffrn_orient_matrix_UB_23      0.1525524000
_diffrn_orient_matrix_UB_31      0.0623373000
_diffrn_orient_matrix_UB_32      0.1236551000
_diffrn_orient_matrix_UB_33      -0.0052616000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10900
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         4.466
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0268P)^2^+0.8884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3823
_reflns_number_total             4225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02596a2.cif
_cod_data_source_block           aw823c
_cod_original_cell_volume        1199.95(8)
_cod_database_code               7713931
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         DyCNO
_shelx_estimated_absorpt_t_max   0.478
_shelx_estimated_absorpt_t_min   0.338
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              60678
_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 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.727