Regulating the magnetic dynamics of mononuclear β-diketone Dy(iii) single-molecule magnets through the substitution effect on capping N-donor coligands.
Xi, Jing; Ma, Xiufang; Cen, Peipei; Wu, Yuewei; Zhang, Yi-Quan; Guo, Yan; Yang, Jinhui; Chen, Lei; Liu, Xiangyu; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2102–2111; doi:10.1039/d0dt03780j

data_7706393
_publ_section_title
;
 Regulating the magnetic dynamics of mononuclear \b-diketone Dy(iii)
 single-molecule magnets through the substitution effect on capping
 N-donor coligands.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2102
_journal_page_last               2111
_journal_paper_doi               10.1039/d0dt03780j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C60 H48 Dy F9 N2 O6'
_chemical_formula_sum            'C60 H48 Dy F9 N2 O6'
_chemical_formula_weight         1226.50
_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   geom
_audit_creation_date             2019-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                81.837(7)
_cell_angle_beta                 73.573(8)
_cell_angle_gamma                66.289(9)
_cell_formula_units_Z            2
_cell_length_a                   12.6768(13)
_cell_length_b                   15.0227(14)
_cell_length_c                   16.5274(14)
_cell_measurement_reflns_used    2044
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      66.1880
_cell_measurement_theta_min      3.9020
_cell_volume                     2762.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -67.00  32.00   1.00    5.00    --  -39.95  57.00 -30.00   99
  2  \w    -64.00  34.00   1.00    5.00    --  -39.95  38.00-120.00   98
  3  \w    -35.00  73.00   1.00    5.00    --   39.95 -77.00  60.00  108
  4  \w     35.00  60.00   1.00    8.00    --  105.48 -30.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0625354000
_diffrn_orient_matrix_UB_12      -0.0552851000
_diffrn_orient_matrix_UB_13      0.0700762000
_diffrn_orient_matrix_UB_21      -0.0054819000
_diffrn_orient_matrix_UB_22      0.0960768000
_diffrn_orient_matrix_UB_23      0.0267834000
_diffrn_orient_matrix_UB_31      -0.1219241000
_diffrn_orient_matrix_UB_32      0.0152972000
_diffrn_orient_matrix_UB_33      0.0621351000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15207
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.589
_diffrn_reflns_theta_max         66.589
_diffrn_reflns_theta_min         3.932
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1234
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.123
_refine_diff_density_min         -1.854
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         9615
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0759P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7609
_reflns_number_total             9615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03780j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7706390--7706394.cif.'
_cod_database_code               7706393
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.475
_shelx_estimated_absorpt_t_min   0.363
_reflns_odcompleteness_completeness 35.14
_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. Uiso/Uaniso restraints and constraints
Uanis(C57) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C59A) \\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(C60A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59A)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28),
  C31(H31), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
 C42(H42), C43(H43), C44(H44), C46(H46), C49(H49), C51(H51), C52(H52)
4.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C58A(H58D,H58E,H58F),
 C59A(H59D,H59E,H59F), C60A(H60D,H60E,H60F)
;
_shelx_res_checksum              2411
_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 1.816
_oxdiff_exptl_absorpt_empirical_full_min 0.641