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_7700912
_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 N24 O4 Y2, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H44 B4 Br2 Cl4 N24 O4 Y2'
_chemical_formula_weight         1495.71
_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                 107.921(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0880(4)
_cell_length_b                   15.0798(3)
_cell_length_c                   14.8048(3)
_cell_measurement_reflns_used    12234
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.8060
_cell_measurement_theta_min      2.6990
_cell_volume                     2992.59(13)
_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 0.994
_diffrn_measured_fraction_theta_max 0.942
_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    -77.00  -7.00   0.50   38.65    --   -5.27 -55.00 -48.00  140
  2  \w    -26.00  16.00   0.50   38.65    --   -5.27 -99.00   0.00   84
  3  \w    -26.00  27.00   0.50   38.65    --   -5.27 -99.00-180.00  106
  4  \w     -7.00  63.00   0.50   38.65    --   -5.27  55.00  94.00  140
;
_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      0.0406597000
_diffrn_orient_matrix_UB_12      0.0283756000
_diffrn_orient_matrix_UB_13      0.0016048000
_diffrn_orient_matrix_UB_21      0.0032646000
_diffrn_orient_matrix_UB_22      0.0125259000
_diffrn_orient_matrix_UB_23      0.0470281000
_diffrn_orient_matrix_UB_31      0.0337095000
_diffrn_orient_matrix_UB_32      -0.0353784000
_diffrn_orient_matrix_UB_33      0.0179425000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23599
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.398
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.507
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.620
_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    1.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method
'crystallized by slow evaporation of dichloromethane/ethanol'
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.1812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6101
_reflns_number_total             7000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01320b2.cif
_cod_data_source_block           2-Y
_cod_depositor_comments
'Adding full bibliography for 7700911--7700914.cif.'
_cod_original_cell_volume        2992.60(13)
_cod_database_code               7700912
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H44 B4 Br2 Cl4 N24 O4 Y2'
_chemical_oxdiff_usercomment     'Purple plate xtal - Will'
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.442
_reflns_odcompleteness_completeness 73.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.70
_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              84806
_shelx_fab_checksum              35002
_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 3.764
_oxdiff_exptl_absorpt_empirical_full_min 0.578