A New Organic Conductor of Tetramethyltetraselenafulvalene (TMTSF) with a Magnetic Dy(III) Complex
Wan, Qingyun; Wakizaka, Masanori; Zhang, Haitao; Shen, Yongbing; Funakoshi, Nobuto; Che, Chi-Ming; Takaishi, Shinya; Yamashita, Masahiro; Magnetochemistry 9 (2023) 77–; doi:10.3390/magnetochemistry9030077

data_1568785
_publ_section_title
;
 A New Organic Conductor of Tetramethyltetraselenafulvalene (TMTSF) with a
 Magnetic Dy(III) Complex
;
_journal_issue                   3
_journal_name_full               Magnetochemistry
_journal_page_first              77
_journal_paper_doi               10.3390/magnetochemistry9030077
_journal_volume                  9
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C4 Dy N6 O6 S4, 4(C10 H12 Se4), C10 Se4, C H Cl3'
_chemical_formula_sum            'C55 H49 Cl3 Dy N6 O6 S4 Se20'
_chemical_formula_weight         2866.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-11
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-01-29 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9823(6)
_cell_length_b                   13.8784(5)
_cell_length_c                   29.3863(9)
_cell_measurement_reflns_used    11918
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.3380
_cell_measurement_theta_min      2.8130
_cell_volume                     8149.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_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      120
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.893
_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    -37.00  -4.00   0.50  160.00    --   -0.90  45.00  72.90   66
  2  \w     24.00  51.00   0.50  160.00    --   -0.90  45.00  72.90   54
  3  \w    -88.00  59.00   0.50  160.00    --   -0.90  45.00 120.00  294
  4  \w     27.00  53.00   0.50  160.00    --   -0.90  45.00  60.00   52
  5  \w    -88.00 -63.00   0.50  160.00    --   -0.90  45.00  72.90   50
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0285246000
_diffrn_orient_matrix_UB_12      0.0051597000
_diffrn_orient_matrix_UB_13      0.0141481000
_diffrn_orient_matrix_UB_21      0.0200433000
_diffrn_orient_matrix_UB_22      0.0091827000
_diffrn_orient_matrix_UB_23      -0.0194347000
_diffrn_orient_matrix_UB_31      -0.0067708000
_diffrn_orient_matrix_UB_32      0.0500163000
_diffrn_orient_matrix_UB_33      0.0020329000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            49327
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.948
_diffrn_reflns_theta_min         2.742
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    10.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_description       needle
_exptl_crystal_F_000             5320
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.618
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details
;
 Flack x determined using 3767 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.089(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         12224
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0314P)^2^+35.2197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.798
_reflns_number_gt                9589
_reflns_number_total             12224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2238596.cif
_cod_data_source_block           b_120k
_cod_database_code               1568785
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N4 S4 Se4 Dy'
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.432
_diffrn_oxdiff_digest_frames
;
01c72e955d02ad4b29ca9df92e14e15331000255355
;
_diffrn_oxdiff_digest_hkl
;
015d676f7ac2e69e6b1d08363168d891a5c055
;
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C34(H34)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              45477
_shelx_hkl_checksum              78905
_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 2.435
_oxdiff_exptl_absorpt_empirical_full_min 0.709