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_7713930
_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         'C30 H26 Dy2 N8 O20'
_chemical_formula_sum            'C30 H26 Dy2 N8 O20'
_chemical_formula_weight         1143.59
_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
_audit_creation_date             2018-06-07
_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                91.834(2)
_cell_angle_beta                 112.263(2)
_cell_angle_gamma                112.030(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7495(3)
_cell_length_b                   10.3059(3)
_cell_length_c                   10.8266(2)
_cell_measurement_reflns_used    6878
_cell_measurement_temperature    293.0(1)
_cell_measurement_theta_max      76.6690
_cell_measurement_theta_min      4.5000
_cell_volume                     913.81(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      293.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.986
_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    -61.00 -24.00   0.50    0.05    --  -48.45  11.00 -93.00   74
  2  \w   -116.00 -50.00   0.50    0.05    --  -48.45 -11.00  93.00  132
  3  \w     65.00 119.00   0.50    0.05    --   48.45  11.00 -93.00  108
  4  \w   -102.00 -74.00   0.50    0.20    --  -86.25  11.00 -93.00   56
  5  \w   -158.00 -99.00   0.50    0.20    --  -86.25 -11.00  93.00  118
  6  \w    -67.00 -41.00   0.50    0.20    --  -86.25  11.00 -93.00   52
  7  \w    151.00 177.00   0.50    0.20    --  107.75  11.00 -93.00   52
  8  \w    114.00 146.00   0.50    0.20    --  107.75  11.00 -93.00   64
  9  \w     -8.00  20.00   0.50    0.05    --  -48.45  11.00 -93.00   56
 10  \w    -63.00  19.00   0.50    0.05    --  -48.45  57.00 -90.00  164
 11  \w     -5.00  20.00   0.50    0.05    --   48.45 -11.00  93.00   50
 12  \w   -105.00 -17.00   0.50    0.20    --  -86.25  77.00 120.00  176
 13  \w    -99.00 -16.00   0.50    0.20    --  -86.25  37.00 -90.00  166
 14  \w     36.00 120.00   0.50    0.20    --  107.75 -37.00 -90.00  168
 15  \w     95.00 176.00   0.50    0.20    --  107.75  19.00 120.00  162
 16  \w     95.00 124.00   0.50    0.20    --  107.75 -11.00  93.00   58
 17  \w     92.00 117.00   0.50    0.20    --  107.75-125.00 120.00   50
 18  \w     44.00  85.00   0.50    0.20    --  107.75-125.00 120.00   82
 19  \w     50.00  87.00   0.50    0.20    --  107.75 -99.00-150.00   74
 20  \w     37.00 108.00   0.50    0.20    --  107.75 -77.00 -90.00  142
 21  \w     51.00 108.00   0.50    0.20    --  107.75 -99.00 150.00  114
 22  \w     41.00 119.00   0.50    0.20    --  107.75 -57.00 -60.00  156
 23  \w     37.00 108.00   0.50    0.20    --  107.75 -99.00 -90.00  142
 24  \w     49.00  92.00   0.50    0.20    --  107.75 -11.00  93.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1676846000
_diffrn_orient_matrix_UB_12      -0.1157469000
_diffrn_orient_matrix_UB_13      -0.0223152000
_diffrn_orient_matrix_UB_21      -0.0639685000
_diffrn_orient_matrix_UB_22      0.1158742000
_diffrn_orient_matrix_UB_23      -0.0000976000
_diffrn_orient_matrix_UB_31      -0.0560124000
_diffrn_orient_matrix_UB_32      -0.0172191000
_diffrn_orient_matrix_UB_33      -0.1554298000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8071
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         4.507
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    22.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_description       block
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.100
_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     273
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0309P)^2^+0.4383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3037
_reflns_number_total             3221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02596a2.cif
_cod_data_source_block           180607a
_cod_database_code               7713930
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         DyNOC
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.399
_reflns_odcompleteness_completeness 99.11
_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), C8(H8), C9(H9), C10(H10), C13(H13)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              92144
_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 1.798
_oxdiff_exptl_absorpt_empirical_full_min 0.719