Tetraoxolene-bridged rare-earth complexes: a radical-bridged dinuclear Dy single-molecule magnet.
Reed, William R.; Dunstan, Maja A.; Gable, Robert W.; Phonsri, Wasinee; Murray, Keith S.; Mole, Richard A.; Boskovic, Colette; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15635–15645; doi:10.1039/c9dt01320b

data_7700911
_publ_section_title
;
 Tetraoxolene-bridged rare-earth complexes: a radical-bridged dinuclear Dy
 single-molecule magnet.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15635
_journal_page_last               15645
_journal_paper_doi               10.1039/c9dt01320b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C42 H40 B4 Br2 Dy2 N24 O4, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H44 B4 Br2 Cl4 Dy2 N24 O4'
_chemical_formula_weight         1642.89
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-27 deposited with the CCDC.    2019-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.024(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1280(4)
_cell_length_b                   15.0635(4)
_cell_length_c                   14.8028(4)
_cell_measurement_reflns_used    11056
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.9420
_cell_measurement_theta_min      4.2780
_cell_volume                     2995.70(15)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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    -35.00  23.00   0.50    0.50    --  -48.30  91.00  38.00  116
  2  \w    -76.00 -41.00   0.50    0.50    --  -48.30  91.00  38.00   70
  3  \w     20.00  50.00   0.50    0.50    --   48.30 -91.00 -74.00   60
  4  \w   -158.00-131.00   0.50    1.75    --  -86.25 -91.00 -74.00   54
  5  \w    118.00 151.00   0.50    1.75    --  107.75  91.00  38.00   66
  6  \w     36.00 134.00   0.50    1.75    --  107.75 -91.00 -74.00  196
  7  \w    -54.00  24.00   0.50    0.50    --  -48.30  38.00 150.00  156
  8  \w   -118.00 -86.00   0.50    0.50    --  -48.30-125.00-180.00   64
  9  \w    -57.00  18.00   0.50    0.50    --  -48.30  38.00-150.00  150
 10  \w    -71.00 -46.00   0.50    1.75    --  -86.25  91.00  38.00   50
 11  \w     35.00  61.00   0.50    1.75    --  107.75 -30.00-120.00   52
 12  \w     35.00  71.00   0.50    1.75    --  107.75 -30.00 -30.00   72
 13  \w     38.00  64.00   0.50    1.75    --  107.75 -30.00 -90.00   52
 14  \w     42.00  73.00   0.50    1.75    --  107.75 -45.00 -90.00   62
 15  \w     35.00  70.00   0.50    1.75    --  107.75 -30.00  30.00   70
 16  \w     37.00  68.00   0.50    1.75    --  107.75 -30.00  90.00   62
 17  \w     42.00  76.00   0.50    1.75    --  107.75 -45.00 -30.00   68
 18  \w     39.00  70.00   0.50    1.75    --  107.75 -45.00  60.00   62
 19  \w     38.00  77.00   0.50    1.75    --  107.75 -45.00-180.00   78
 20  \w     44.00  71.00   0.50    1.75    --  107.75 -45.00 -60.00   54
 21  \w    149.00 175.00   0.50    1.75    --  107.75  30.00 -30.00   52
 22  \w     98.00 123.00   0.50    1.75    --  107.75  30.00 -30.00   50
 23  \w     36.00  62.00   0.50    1.75    --  107.75 -30.00 -60.00   52
 24  \w     93.00 118.00   0.50    1.75    --  107.75 125.00  90.00   50
 25  \w    153.00 178.00   0.50    1.75    --  107.75 125.00  90.00   50
 26  \w     39.00  70.00   0.50    1.75    --  107.75 -30.00   0.00   62
 27  \w     40.00  71.00   0.50    1.75    --  107.75 -30.00 120.00   62
 28  \w     46.00  71.00   0.50    1.75    --  107.75 -30.00  60.00   50
;
_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      0.0494685000
_diffrn_orient_matrix_UB_12      0.0893624000
_diffrn_orient_matrix_UB_13      -0.0086186000
_diffrn_orient_matrix_UB_21      0.0942643000
_diffrn_orient_matrix_UB_22      -0.0285141000
_diffrn_orient_matrix_UB_23      0.0795329000
_diffrn_orient_matrix_UB_31      0.0426523000
_diffrn_orient_matrix_UB_32      -0.0407386000
_diffrn_orient_matrix_UB_33      -0.0746854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.463
_diffrn_reflns_theta_min         3.781
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.923
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            purple
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       plate
_exptl_crystal_F_000             1596
_exptl_crystal_recrystallization_method
'crystallized by slow evaporation of dichloromethane/ethanol'
_exptl_crystal_size_max          0.043
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0247P)^2^+5.1914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5513
_reflns_number_total             6046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01320b2.cif
_cod_data_source_block           2-Dy
_cod_depositor_comments
'Adding full bibliography for 7700911--7700914.cif.'
_cod_original_cell_volume        2995.68(14)
_cod_database_code               7700911
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H44 B4 Br2 Cl4 N24 O4 Dy2'
_chemical_oxdiff_usercomment     'Mg O-Bipy HBA'
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.530
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A), B2(H2A)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18)
;
_shelx_res_checksum              37050
_shelx_fab_checksum              70826
_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 1.633
_oxdiff_exptl_absorpt_empirical_full_min 0.518