Slow magnetisation relaxation in tetraoxolene-bridged rare-earth complexes
Dunstan, Maja; Rousset, Elodie; Boulon, Marie-Emmanuelle; Gable, Robert William; Sorace, Lorenzo; Boskovic, Colette; Dalton Trans.  (2017) –; doi:10.1039/C7DT02932B

data_7044219
_publ_section_title
;
 Slow magnetisation relaxation in tetraoxolene-bridged rare-earth
 complexes
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_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02932B
_journal_year                    2017
_chemical_formula_moiety         'C44 H46 B4 N24 O4 Y2'
_chemical_formula_sum            'C44 H46 B4 N24 O4 Y2'
_chemical_formula_weight         1196.11
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   49.226(7)
_cell_length_b                   49.226(7)
_cell_length_c                   13.220(3)
_cell_measurement_reflns_used    2714
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.089
_cell_measurement_theta_min      0.407
_cell_volume                     27743(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1746
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       72
_diffrn_reflns_limit_h_min       -72
_diffrn_reflns_limit_k_max       70
_diffrn_reflns_limit_k_min       -71
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            260816
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.854
_diffrn_reflns_theta_min         0.827
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.931
_exptl_absorpt_correction_T_max  0.4342
_exptl_absorpt_correction_T_min  0.2940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1181 before and 0.0897 after correction.
The Ratio of minimum to maximum transmission is 0.6771.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       needle
_exptl_crystal_F_000             10944
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.433
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         19276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+15.6478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11662
_reflns_number_total             19276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02932b2.cif
_cod_data_source_block           3-ydcm
_cod_original_cell_volume        27743(10)
_cod_database_code               7044219
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 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), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
2.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              9343
_shelx_fab_checksum              38513
_olex2_submission_special_instructions 'No special instructions were received'