Modulating the slow magnetic relaxation of a mononuclear Dy(iii) single-molecule magnet via a magnetic field and dilution effects
Cen, Peipei; He, Zixin; Ding, Runmei; Yang, Huifang; Li, Li; Zhang, Yi-Quan; Li, Yonghong; Tian, Danian; Liu, Xiangyu; CrystEngComm 23 (2021) 5443–5450; doi:10.1039/D1CE00682G

data_7243116
_publ_section_title
;
 Modulating the slow magnetic relaxation of a mononuclear Dy(iii)
 single-molecule magnet via a magnetic field and dilution effects
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              5443
_journal_page_last               5450
_journal_paper_doi               10.1039/D1CE00682G
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C44 H26 F9 N4 O6 Y'
_chemical_formula_sum            'C44 H26 F9 N4 O6 Y'
_chemical_formula_weight         966.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-23 deposited with the CCDC.	2021-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.53(2)
_cell_length_b                   10.926(10)
_cell_length_c                   18.350(16)
_cell_measurement_reflns_used    5187
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      19.84
_cell_measurement_theta_min      2.19
_cell_volume                     4317(7)
_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      296.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_unetI/netI     0.1601
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22036
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.596
_diffrn_reflns_theta_min         1.891
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 1264 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         9327
_refine_ls_number_restraints     475
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1948
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0701P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1953
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.922
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                3964
_reflns_number_total             9327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00682g2.cif
_cod_data_source_block           mxf611
_cod_depositor_comments
'Adding full bibliography for 7243116--7243117.cif.'
_cod_database_code               7243116
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.846
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-C21
 1.45 with sigma of 0.01
 C23-C22
 1.38 with sigma of 0.01
 Y1-N2 \\sim Y1-N2A
 with sigma of 0.02
 Y1-N1 \\sim Y1-N1A
 with sigma of 0.02
 C36A-C35A \\sim C36-C35
 with sigma of 0.02
 C41A-C34A \\sim C41-C34
 with sigma of 0.02
 C42A-C37A \\sim C42-C37
 with sigma of 0.02
 F3A-C1 \\sim F2-C1 \\sim F2A-C1 \\sim F1-C1 \\sim F1A-C1 \\sim F3-C1
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F2-F3
 with sigma of 0.02
 F1A-F2A \\sim F1A-F3A \\sim F2A-F3A
 with sigma of 0.02
 F8-C21 \\sim F9-C21 \\sim F7-C21
 with sigma of 0.02
 F7-F9 \\sim F7-F8 \\sim F9-F8
 with sigma of 0.02
3. Rigid bond restraints
 C17, C18, C14, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
F4 \\sim F5 \\sim F6 \\sim C11 \\sim C21 \\sim F9 \\sim F8 \\sim F7: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Y1, N1, N2, N3, N4, C31, C33, C34, C35, C36, C37, C38, C39, C40, C41, C42,
 C43, C44, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Y1, N1A, N2A, N3A, N4A, C31A, C32A, C33A, C34A, C35A, C36A, C37A, C38A, C39A,
 C40A, C41A, C42A, C43A, C44A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1, F2A, F3A, F1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1, F1, F2, F3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C21, F9, F8, F7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(N1A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=
 Sof(C34A)=Sof(C35A)=Sof(N2A)=Sof(C36A)=Sof(C37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=
 Sof(H39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(C42A)=Sof(N4A)=Sof(C44A)=Sof(H44A)=
 Sof(C43A)=Sof(H43A)=Sof(N3A)=1-FVAR(1)
 Sof(N1)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=
 Sof(C35)=Sof(N2)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(C42)=Sof(N4)=Sof(C44)=Sof(H44)=Sof(C43)=
 Sof(H43)=Sof(N3)=FVAR(1)
 Sof(F2A)=Sof(F1A)=Sof(F3A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C38(H38), C39(H39), C40(H40), C3(H3), C6(H6),
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C44(H44), C43(H43), C31A(H31A), C32A(H32A), C33A(H33A), C38A(H38A),
 C39A(H39A), C40A(H40A), C44A(H44A), C43A(H43A)
7.b Fitted hexagon refined as free rotating group:
 N1(C31,C32,C33,C34,C35), N2(C36,C37,C38,C39,C40), C5(C6,C7,C8,C9,C10),
 C15(C16,C17,C18,C19,C20), C25(C26,C27,C28,C29,C30), C41(C42,N4,C44,C43,N3),
 N1A(C31A,C32A,C33A,C34A,C35A), N2A(C36A,C37A,C38A,C39A,C40A), C41A(C42A,N4A,
 C44A,C43A,N3A)
;
_shelx_res_checksum              91312
_shelx_hkl_checksum              816
_olex2_submission_special_instructions 'No special instructions were received'