Effect of coordinated anions on ferromagnetically coupled Dy<sub>2</sub> zero-field single-molecule magnets.
Liu, Cai-Ming; Hao, Xiang; Zhu, Dong-Mei; Zhang, Yi-Quan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6120–6127; doi:10.1039/d4dt00293h

data_7715404
_publ_section_title
;
 Effect of coordinated anions on ferromagnetically coupled Dy<sub>2</sub>
 zero-field single-molecule magnets.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6120
_journal_page_last               6127
_journal_paper_doi               10.1039/d4dt00293h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H34 Dy2 N12 O14'
_chemical_formula_sum            'C32 H34 Dy2 N12 O14'
_chemical_formula_weight         1135.71
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-01-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-04 deposited with the CCDC.	2024-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.221(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8836(2)
_cell_length_b                   15.5639(3)
_cell_length_c                   12.5827(3)
_cell_measurement_reflns_used    19228
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      31.1150
_cell_measurement_theta_min      2.0750
_cell_volume                     1924.17(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.882
_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     19.00  66.00   0.50    4.00    --    5.00  45.00 179.38   94
  2  \w    -81.00  -6.00   0.50    4.00    --  -10.80  45.00 120.00  150
  3  \w   -100.00 -34.00   0.50    4.00    --  -10.80  45.00 -16.50  132
  4  \w   -100.00  78.00   0.50    4.00    --  -10.80  45.00  60.00  356
  5  \w    -97.00  36.00   0.50    4.00    --  -10.80  45.00   0.00  266
;
_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      0.0608854000
_diffrn_orient_matrix_UB_12      0.0169525000
_diffrn_orient_matrix_UB_13      0.0271281000
_diffrn_orient_matrix_UB_21      0.0378501000
_diffrn_orient_matrix_UB_22      -0.0184713000
_diffrn_orient_matrix_UB_23      -0.0390135000
_diffrn_orient_matrix_UB_31      -0.0086679000
_diffrn_orient_matrix_UB_32      0.0380786000
_diffrn_orient_matrix_UB_33      -0.0308663000
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.992
_diffrn_reflns_theta_min         2.089
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0159
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+1.0858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4925
_reflns_number_total             5414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00293h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715404--7715405.cif.'
_cod_database_code               7715404
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNODy
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              90426
_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 1.383
_oxdiff_exptl_absorpt_empirical_full_min 0.702