Single-Ion Magnetism in a Three-Dimensional Thiocyanate-Bridged Dysprosium(III) Framework
Wan, Qingyun; Arczyński, Mirosław; Wakizaka, Masanori; Gupta, Shraddha; Funakoshi, Nobuto; Yamashita, Masahiro; Chemistry 5 (2023) 987–995; doi:10.3390/chemistry5020067

data_1569030
_publ_section_title
;
 Single-Ion Magnetism in a Three-Dimensional Thiocyanate-Bridged
 Dysprosium(III) Framework
;
_journal_issue                   2
_journal_name_full               Chemistry
_journal_page_first              987
_journal_page_last               995
_journal_paper_doi               10.3390/chemistry5020067
_journal_volume                  5
_journal_year                    2023
_chemical_formula_moiety         '0.25(C28 H16 Gd4 K16 N28 O24 S28)'
_chemical_formula_sum            'C7 H4 Gd K4 N7 O6 S7'
_chemical_formula_weight         820.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-26
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.245(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0701(4)
_cell_length_b                   6.46040(10)
_cell_length_c                   22.2814(5)
_cell_measurement_reflns_used    13091
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.3910
_cell_measurement_theta_min      3.3520
_cell_volume                     2759.15(10)
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.856
_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     23.00  72.00   0.50    1.00    --   -0.90  45.00  90.00   98
  2  \w    -90.00 -42.00   0.50    1.00    --   -0.90  45.00   0.00   96
  3  \w    -22.00  87.00   0.50    1.00    --   -0.90  45.00   0.00  218
  4  \w    -24.00   1.00   0.50    1.00    --   -0.90  45.00  30.00   50
  5  \w     42.00  73.00   0.50    1.00    --   -0.90  45.00 168.35   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0230238000
_diffrn_orient_matrix_UB_12      0.0203065000
_diffrn_orient_matrix_UB_13      -0.0180278000
_diffrn_orient_matrix_UB_21      -0.0079228000
_diffrn_orient_matrix_UB_22      0.1070657000
_diffrn_orient_matrix_UB_23      -0.0001370000
_diffrn_orient_matrix_UB_31      0.0278288000
_diffrn_orient_matrix_UB_32      0.0139131000
_diffrn_orient_matrix_UB_33      0.0280539000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14860
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.166
_diffrn_reflns_theta_min         3.296
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66543
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.00100(9)
_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   1.122
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3825
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0162
_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^)+(0.0187P)^2^+7.1348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3749
_reflns_number_total             3825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3-Gd.cif
_cod_data_source_block           a_120k
_cod_database_code               1569030
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N10 S10 O10 Gd K5'
_chemical_oxdiff_usercomment     'broken thin plate'
_shelx_estimated_absorpt_t_max   0.535
_shelx_estimated_absorpt_t_min   0.535
_diffrn_oxdiff_digest_frames
;
01b13dcf4a3d6eae5f09735f417afae9b600037ee4a
;
_diffrn_oxdiff_digest_hkl
;
01bda921cb321c77ee722b77accaa6149df306
;
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
 H1A-H1B
 1.34 with sigma of 0.04
 Gd1-H1A \\sim Gd1-H1B
 with sigma of 0.02
3. Others
 Fixed Sof: S4(0.5) N4(0.5)
;
_shelx_res_checksum              89574
_shelx_hkl_checksum              43913
_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 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.873