Radical-cation salts of BEDT-TTF with tris-coordinated racemic dysprosium(III) and terbium(III) anions.
Howarth, Emily; Lopez, Jordan; Ogar, Joseph O.; Blundell, Toby J.; Akutsu, Hiroki; Nakazawa, Yasuhiro; Imajo, Shusaku; Ihara, Yoshihiko; Coles, Simon J.; Horton, Peter N.; Christensen, Jeppe; Martin, Lee; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3207–3215; doi:10.1039/d4dt03484h

data_7717832
_publ_section_title
;
 Radical-cation salts of BEDT-TTF with tris-coordinated racemic
 dysprosium(III) and terbium(III) anions.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3207
_journal_page_last               3215
_journal_paper_doi               10.1039/d4dt03484h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C21 H6 Dy O18, 5(C10 H8 S8), C2 H6 O, 2(H2 O)'
_chemical_formula_sum            'C73 H56 Dy O21 S40'
_chemical_formula_weight         2714.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-05-23 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.191(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   44.9281(9)
_cell_length_b                   11.0132(2)
_cell_length_c                   20.9971(4)
_cell_measurement_reflns_used    7916
_cell_measurement_temperature    30(2)
_cell_measurement_theta_max      33.1688230732
_cell_measurement_theta_min      1.91935545588
_cell_volume                     9549.9(3)
_computing_cell_refinement
'XIA2 0.4.0.438-g4431aaa, Winter, G. (2010) J. Appl. Cryst. 43'
_computing_data_collection       'GDA 8.44; generic data acquisition software'
_computing_data_reduction
'XIA2 0.4.0.438-g4431aaa, Winter, G. (2010) J. Appl. Cryst. 43'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT Acta Cryst. (2015). A71, 3-8'
_diffrn_ambient_temperature      30(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_dtime           0.004
_diffrn_detector_type            'Dectris, PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;Data collection strategy using shutter-less operation of detector. 
Three omega scans -170 to 25 with phi 0, 120 and 240 respectively.
0.1 degree images with 0.5 sec exposure
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_details 'custom build fixed Chi diffractometer'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_radiation_collimation    'focusing mirrors and 0.100 mm pinhole'
_diffrn_radiation_monochromator  'Si 111, double crystal monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_wavelength_details 'Zr absorption edge'
_diffrn_radiation_wavelength_determination estimated
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_av_unetI/netI     0.1293
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30702
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.573
_diffrn_reflns_theta_min         1.855
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19, undulator'
_exptl_absorpt_coefficient_mu    1.723
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.048: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, 
absorption correction using spherical harmonics
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_description       plate
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.776
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         10815
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0502
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8708
_reflns_number_total             10815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03484h2.cif
_cod_data_source_block           2018NCS0045
_cod_depositor_comments
'Adding full bibliography for 7717832--7717833.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7717832
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              35189