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_7044215
_publ_section_title
;
 Slow magnetisation relaxation in tetraoxolene-bridged rare-earth
 complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02932B
_journal_year                    2017
_chemical_formula_moiety         'C42 H40 B4 Cl2 N24 O4 Y2, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H44 B4 Cl6 N24 O4 Y2'
_chemical_formula_weight         1406.79
_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
_audit_creation_date             2017-06-16
_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                 107.57(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.940(3)
_cell_length_b                   15.052(3)
_cell_length_c                   14.280(3)
_cell_measurement_reflns_used    2162
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.089
_cell_measurement_theta_min      0.407
_cell_volume                     2856.5(11)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.720
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55283
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.720
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.849
_diffrn_reflns_theta_min         1.789
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  0.4343
_exptl_absorpt_correction_T_min  0.3098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1245 before and 0.0842 after correction.
The Ratio of minimum to maximum transmission is 0.7133.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light purple'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.146
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.0185(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0658P)^2^+3.6926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6344
_reflns_number_total             7662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02932b2.cif
_cod_data_source_block           1-y-2ch2cl2
_cod_original_cell_volume        2856.4(11)
_cod_database_code               7044215
_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, 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:
 C9(H9), C7(H7), C8(H8), C12(H12), C10(H10), C6(H6), C11(H11), C3(H3), C5(H5),
 C13(H13), C1(H1), C18(H18), C2(H2), C4(H4), C15(H15), C17(H17), C14(H14),
 C16(H16)
;
_shelx_res_checksum              38762
_olex2_submission_special_instructions 'No special instructions were received'