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_7700913
_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 Y2 F2 N24 O4),(H2 O)'
_chemical_formula_sum            'C42 H42 B4 F2 N24 O5 Y2'
_chemical_formula_weight         1222.05
_chemical_name_systematic
'bis(bis(tri(1H-pyrazol-1-yl)hydroborate)u-2,5difluoro-3,6-dihydroxy-1,4-benzoquinone diyttrium'
_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                 104.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.780(2)
_cell_length_b                   18.470(4)
_cell_length_c                   12.240(2)
_cell_measurement_reflns_used    92744
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.78
_cell_measurement_theta_min      1.10
_cell_volume                     2582.6(9)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEQUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       synchrotron
_diffrn_measurement_device_type  'ADSC Qantum 210r'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.710900
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            84085
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         2.040
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    2.313
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1236
_exptl_crystal_preparation       'Reaction in DCM/EtOH'
_exptl_crystal_recrystallization_method
'crystallized by slow evaporation of dichloromethane/ethanol'
_exptl_crystal_size_max          0.026
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.009
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0193(11)
_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   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0811P)^2^+0.7173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4896
_reflns_number_total             6410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01320b2.cif
_cod_data_source_block           1-Y
_cod_depositor_comments
'Adding full bibliography for 7700911--7700914.cif.'
_cod_original_cell_volume        2582.5(10)
_cod_database_code               7700913
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.942
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A), B2(H2A)
2.b 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              17108
_shelx_fab_checksum              3146
_olex2_exptl_crystal_mounting_method 'mounted on a cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'