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_7706390
_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         'C52 H30 Br2 Dy F9 N2 O6'
_chemical_formula_sum            'C52 H30 Br2 Dy F9 N2 O6'
_chemical_formula_weight         1272.10
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-01-06 deposited with the CCDC.	2021-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.322(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.614(5)
_cell_length_b                   11.155(3)
_cell_length_c                   23.874(6)
_cell_measurement_reflns_used    8730
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.276
_cell_measurement_theta_min      2.883
_cell_volume                     4861(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1325
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            91273
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.916
_diffrn_reflns_theta_min         2.883
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.268
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1309 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.7639.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         11113
_refine_ls_number_restraints     358
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0404P)^2^+1.1830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6488
_reflns_number_total             11113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03780j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7706390--7706394.cif.'
_cod_database_code               7706390
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C33-C32 \\sim C33A-C32
 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
 F3-F2 \\sim F2-F1 \\sim F3-F1
 with sigma of 0.02
 F3A-F2A \\sim F2A-F1A \\sim F3A-F1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.012
Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F9) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5)
\\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(F3A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F1A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C33A) = Uanis(C33)
4. Rigid body (RIGU) restrains
 C32, C33, C42, C41, C40, C35, C34, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C32, C33A, C42A, C41A, C40A, C35A, C34A, C36A, C37A, C38A, C39A
 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, F2, F3, F1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(H41A)=
 Sof(C40A)=Sof(C35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=
 Sof(H38A)=Sof(C39A)=Sof(H39A)=1-FVAR(1)
 Sof(C34)=Sof(H34)=Sof(C33)=Sof(C42)=Sof(H42)=Sof(C41)=Sof(H41)=Sof(C40)=
 Sof(C35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=
 Sof(H39)=FVAR(1)
 Sof(F2A)=Sof(F1A)=Sof(F3A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
6.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), C42(H42), C41(H41), C36(H36), C37(H37), C38(H38),
 C39(H39), C43(H43), C44(H44), C46(H46), C49(H49), C51(H51), C52(H52),
 C34A(H34A), C42A(H42A), C41A(H41A), C36A(H36A), C37A(H37A), C38A(H38A),
 C39A(H39A)
6.b Naphthalene refined as free rotating group:
 C34(C33,C42,C41,C40,C35,C36,C37,C38,C39), C34A(C33A,C42A,C41A,C40A,C35A,C36A,
 C37A,C38A,C39A)
;
_shelx_res_checksum              89065
_olex2_submission_special_instructions 'No special instructions were received'