Anion-dependent dysprosium(iii) cluster single-molecule magnets
Liu, Cai-Ming; Hao, Xiang; New Journal of Chemistry 47 (2023) 18849–18855; doi:10.1039/D3NJ03610C

data_7062779
_publ_section_title
;
 Anion-dependent dysprosium(iii) cluster single-molecule magnets
;
_journal_issue                   40
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18849
_journal_page_last               18855
_journal_paper_doi               10.1039/D3NJ03610C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C48 H40 Dy4 F4 N18 O19, 4(C2 H3 N), C H4 O'
_chemical_formula_sum            'C57 H56 Dy4 F4 N22 O20'
_chemical_formula_weight         2095.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-20 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                75.6740(10)
_cell_angle_beta                 80.4120(10)
_cell_angle_gamma                86.0850(10)
_cell_formula_units_Z            2
_cell_length_a                   12.74600(10)
_cell_length_b                   13.98880(10)
_cell_length_c                   20.3905(2)
_cell_measurement_reflns_used    87561
_cell_measurement_temperature    170.07(11)
_cell_measurement_theta_max      40.9110
_cell_measurement_theta_min      1.5640
_cell_volume                     3471.99(5)
_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      170.07(11)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -105.00  65.00   0.50    1.00    --  -20.00  45.00   0.00  340
  2  \w   -105.00  65.00   0.50    1.00    --  -20.00  45.00  90.00  340
  3  \w   -105.00  65.00   0.50    1.00    --  -20.00  45.00 180.00  340
  4  \w    -97.00  73.00   0.50    1.00    --   -8.00  45.00 270.00  340
  5  \w   -125.00  45.00   0.50    1.00    --  -40.00  45.00   0.00  340
  6  \w   -125.00  45.00   0.50    1.00    --  -40.00  45.00  45.00  340
  7  \w   -125.00  45.00   0.50    1.00    --  -40.00  45.00 135.00  340
  8  \w   -125.00  45.00   0.50    1.00    --  -40.00  45.00 205.00  340
;
_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      -0.0389060000
_diffrn_orient_matrix_UB_12      0.0201102000
_diffrn_orient_matrix_UB_13      0.0224196000
_diffrn_orient_matrix_UB_21      0.0273018000
_diffrn_orient_matrix_UB_22      -0.0222853000
_diffrn_orient_matrix_UB_23      0.0278022000
_diffrn_orient_matrix_UB_31      0.0304736000
_diffrn_orient_matrix_UB_32      0.0428926000
_diffrn_orient_matrix_UB_33      -0.0067101000
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            89284
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.030
_diffrn_reflns_theta_min         1.503
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66409
_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    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.443
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.00015(2)
_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   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         12281
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      2.038
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0230P)^2^+10.0145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11779
_reflns_number_total             12281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03610c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7062779--7062780.cif.'
_cod_original_cell_volume        3472.00(5)
_cod_database_code               7062779
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFDy
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H10 of O10, H9 of O9, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H18 of O18, H17A of O17, All O(H,H) groups
2. Restrained distances
 O17-C57 = O17-C58
 1.41 with sigma of 0.01
 Dy2-O16 \\sim Dy2-O3W
 with sigma of 0.02
 Dy1-H1WA \\sim Dy1-H1WB
 with sigma of 0.02
3. Others
 Fixed Sof: C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) O17(0.5) H17A(0.5) C58(0.5)
 H58A(0.5) H58B(0.5) H58C(0.5) O18(0.5) H18(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O9(H9), O10(H10), O17(H17A),
 O18(H18)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6), N10(H10A), N14(H14), C2(H2A), C3(H3), C5(H5), C7(H7),
 C10(H10B), C11(H11), C12(H12), C14(H14A), C15(H15), C17(H17), C19(H19),
 C22(H22), C59(H59), C24(H24), C26(H26), C27(H27), C29(H29), C31(H31), C34(H34),
  C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C43(H43), C46(H46),
 C47(H47), C48(H48)
4.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              42351
_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 1.427
_oxdiff_exptl_absorpt_empirical_full_min 0.601