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_7062780
_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         'C75 H51 Cl2 Dy6 F6 N24 O22, 5(C H4 O)'
_chemical_formula_sum            'C80 H71 Cl2 Dy6 F6 N24 O27'
_chemical_formula_weight         2960.50
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-20
_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                90
_cell_angle_beta                 101.5751(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2124(2)
_cell_length_b                   26.5826(4)
_cell_length_c                   26.3977(5)
_cell_measurement_reflns_used    40449
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      27.6720
_cell_measurement_theta_min      1.6400
_cell_volume                     9770.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_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    -36.00 -10.00   0.50    7.00    --    5.00  45.00 166.54   52
  2  \w      0.00  56.00   0.50    7.00    --  -10.70  45.00  60.00  112
  3  \w   -100.00  77.00   0.50    7.00    --  -10.70  45.00 173.73  354
  4  \w     -7.00  78.00   0.50    7.00    --  -10.70  45.00 -19.55  170
  5  \w   -100.00 -22.00   0.50    7.00    --  -10.70  45.00  60.00  156
  6  \w    -69.00  61.00   0.50    7.00    --  -10.70  45.00 120.00  260
;
_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      -0.0256091000
_diffrn_orient_matrix_UB_12      0.0218487000
_diffrn_orient_matrix_UB_13      -0.0101740000
_diffrn_orient_matrix_UB_21      0.0298719000
_diffrn_orient_matrix_UB_22      0.0148386000
_diffrn_orient_matrix_UB_23      0.0190048000
_diffrn_orient_matrix_UB_31      0.0322924000
_diffrn_orient_matrix_UB_32      0.0036117000
_diffrn_orient_matrix_UB_33      -0.0169305000
_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  0.1183
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            147127
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_min         1.532
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
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    2.013
_exptl_crystal_description       block
_exptl_crystal_F_000             5676
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.393
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         22402
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0644P)^2^+256.1199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18558
_reflns_number_total             22402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03610c2.cif
_cod_data_source_block           n
_cod_depositor_comments
'Adding full bibliography for 7062779--7062780.cif.'
_cod_database_code               7062780
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOClDy
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O24-C77 = O22-C76 = O23-C73 = O21-C75 = O20-C74
 1.43 with sigma of 0.02
 O20-C74
 1.43 with sigma of 0.02
 F6-C64 \\sim F6A-C64A
 with sigma of 0.02
 O7-C61 \\sim O7-C61A
 with sigma of 0.02
 C61-C62 \\sim C61A-C62A
 with sigma of 0.02
 C61-C66 \\sim C61A-C66A
 with sigma of 0.02
 C62-C63 \\sim C62A-C63A
 with sigma of 0.02
 C63-C64 \\sim C63A-C64A
 with sigma of 0.02
 C64-C65 \\sim C64A-C65A
 with sigma of 0.02
 C65-C66 \\sim C65A-C66A
 with sigma of 0.02
 C66-C67 \\sim C66A-C67
 with sigma of 0.02
 F6-C63 \\sim F6A-C63A
 with sigma of 0.04
 F6-C65 \\sim F6A-C65A
 with sigma of 0.04
 O7-C62 \\sim O7-C62A
 with sigma of 0.04
 O7-C66 \\sim O7-C66A
 with sigma of 0.04
 C61-C63 \\sim C61A-C63A
 with sigma of 0.04
 C61-C65 \\sim C61A-C65A
 with sigma of 0.04
 C61-C67 \\sim C61A-C67
 with sigma of 0.04
 C62-C64 \\sim C62A-C64A
 with sigma of 0.04
 C62-C66 \\sim C62A-C66A
 with sigma of 0.04
 C63-C65 \\sim C63A-C65A
 with sigma of 0.04
 C64-C66 \\sim C64A-C66A
 with sigma of 0.04
 C65-C67 \\sim C65A-C67
 with sigma of 0.04
 O7-C61A \\sim O7-C61
 with sigma of 0.02
 C67-C66 \\sim C67-C66A
 with sigma of 0.02
3. Restrained planarity
 F6, C61, C62, C63, C64, C65, C66
 with sigma of 0.02
 F6A, C61A, C62A, C63A, C64A, C65A, C66A
 with sigma of 0.02
4. Rigid bond restraints
 O20, C74
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O23, C73
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O22, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O24, C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
F6 \\sim F6A \\sim C61 \\sim C61A \\sim C62 \\sim C62A \\sim C63 \\sim C63A
\\sim C64 \\sim C64A \\sim C65 \\sim C65A \\sim C66 \\sim C66A: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Dy4 \\sim Dy4A \\sim Dy4B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
Dy5 \\sim Dy5A \\sim Dy5B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
Dy1 \\sim Dy1A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Dy2 \\sim Dy2A \\sim Dy2B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
Dy3 \\sim Dy3A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Dy6 \\sim Dy6A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Uanis(F6A) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
Uanis(C78) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(Dy1A) \\sim Ueq, Uanis(Dy2A) \\sim Ueq, Uanis(Dy3A) \\sim Ueq,
Uanis(Dy4A) \\sim Ueq, Uanis(Dy5A) \\sim Ueq, Uanis(Dy6A) \\sim Ueq,
Uanis(Dy2B) \\sim Ueq, Uanis(Dy4B) \\sim Ueq, Uanis(Dy5B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Sof(F6A)=Sof(C61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=
 Sof(C65A)=Sof(H65A)=Sof(C66A)=1-FVAR(1)
 Sof(F6)=Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(C65)=
 Sof(H65)=Sof(C66)=FVAR(1)
 Fixed Sof: Dy1(0.94) Dy1A(0.06) Dy2(0.91) Dy2A(0.05) Dy2B(0.04) Dy3(0.97)
 Dy3A(0.03) Dy4(0.91) Dy4A(0.05) Dy4B(0.04) Dy5(0.91) Dy5A(0.05) Dy5B(0.04)
 Dy6(0.97) Dy6A(0.03)
 Fixed X: Dy1A(0.628601) Dy2A(0.956499) Dy2B(0.9587) Dy3A(0.734799)
 Dy4A(0.5485) Dy4B(0.555301) Dy5A(0.8804) Dy5B(0.8705) Dy6A(0.655201)
 Fixed Y: Dy1A(0.2708) Dy2A(0.3176) Dy2B(0.2976) Dy3A(0.4248) Dy4A(0.3096)
 Dy4B(0.2887) Dy5A(0.3604) Dy5B(0.343301) Dy6A(0.4668)
 Fixed Z: Dy1A(0.5858) Dy2A(0.6534) Dy2B(0.6814) Dy3A(0.5525) Dy4A(0.7138)
 Dy4B(0.736499) Dy5A(0.777699) Dy5B(0.8097) Dy6A(0.6776)
7.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O19(H19), O23(H23A), C73(H73A,
 H73B,H73C), O22(H22A), C76(H76A,H76B,H76C), O20(H20), C74(H74A,H74B,H74C),
 O24(H24A), C77(H77A,H77B,H77C), O21(H21), C75(H75A,H75B,H75C)
7.b Me refined with riding coordinates:
 C78(H78A,H78B,H78C)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C19(H19A), C22(H22), C23(H23), 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), C50(H50), C51(H51),
 C53(H53), C55(H55), C58(H58), C59(H59), C60(H60), C62(H62), C62A(H62A),
 C63(H63), C63A(H63A), C65(H65), C65A(H65A), C70(H70), C71(H71), C72(H72)
;
_shelx_res_checksum              99677
_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 1.481
_oxdiff_exptl_absorpt_empirical_full_min 0.603