[2 + 2] Photochemical modulation of the Dy(iii) single-molecule magnet: opposite influence on the energy barrier and relaxation time
Wang, Long-Fei; Qiu, Jiang-Zhen; Chen, Yan-Cong; Liu, Jun-Liang; Li, Quan-Wen; Jia, Jian-Hua; Tong, Ming-Liang; Inorganic Chemistry Frontiers 4 (2017) 1311–; doi:10.1039/C7QI00221A

data_4349726
_publ_section_title
;
 [2 + 2] Photochemical modulation of the Dy(iii) single-molecule magnet:
 opposite influence on the energy barrier and relaxation time
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1311
_journal_paper_doi               10.1039/C7QI00221A
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C20 H17 Dy N7 O5 S3, C N S, 2(C12 H11 N2)'
_chemical_formula_sum            'C45 H39 Dy N12 O5 S4'
_chemical_formula_weight         1118.62
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-17 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                92.846(2)
_cell_angle_beta                 98.463(2)
_cell_angle_gamma                109.273(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4132(7)
_cell_length_b                   12.4976(7)
_cell_length_c                   19.8741(12)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.50
_cell_volume                     2401.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0672
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46586
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.50
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.788
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1668 before and 0.0748 after correction.
The Ratio of minimum to maximum transmission is 0.6499.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1126
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         11081
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+5.5809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                9971
_reflns_number_total             11081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qi00221a2.cif
_cod_data_source_block           a
_cod_database_code               4349726
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H,H) groups
2. Shared sites
{N7A, N7B}
{N8A, N8B}
3. Uiso/Uaniso restraints and constraints
Uanis(C10A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C14A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C21B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(N7A) = Uanis(N7B)
Uanis(N8A) = Uanis(N8B)
Uanis(C10A) = Uanis(C10B)
Uanis(C11A) = Uanis(C11B)
Uanis(C12A) = Uanis(C12B)
Uanis(C13A) = Uanis(C13B)
Uanis(C14A) = Uanis(C14B)
Uanis(C15A) = Uanis(C15B)
Uanis(C16A) = Uanis(C16B)
Uanis(C17A) = Uanis(C17B)
Uanis(C18A) = Uanis(C18B)
Uanis(C19A) = Uanis(C19B)
Uanis(C20A) = Uanis(C20B)
Uanis(C21A) = Uanis(C21B)
4. Others
 Sof(N7B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(C13B)=
 Sof(H13B)=Sof(C14B)=Sof(H14B)=Sof(N8B)=Sof(C19B)=Sof(H19B)=Sof(C18B)=Sof(H18B)=
 Sof(C17B)=Sof(C21B)=Sof(H21B)=Sof(C20B)=Sof(H20B)=Sof(C15B)=Sof(H15B)=
 Sof(C16B)=Sof(H16B)=1-FVAR(1)
 Sof(N7A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(C13A)=
 Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(N8A)=Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=
 Sof(C17A)=Sof(C21A)=Sof(H21A)=Sof(C20A)=Sof(H20A)=Sof(C15A)=Sof(H15A)=
 Sof(C16A)=Sof(H16A)=FVAR(1)
5.a Riding coordinates:
 O1W(H1WA,H1WB), N12(H12)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N9(H9A), C6(H6), C7(H7), C8(H8), C11A(H11A), C13A(H13A), C14A(H14A),
 C19A(H19A), C18A(H18A), C21A(H21A), C20A(H20A), C15A(H15A), C16A(H16A),
 C10B(H10B), C11B(H11B), C13B(H13B), C14B(H14B), C19B(H19B), C18B(H18B),
 C21B(H21B), C20B(H20B), C15B(H15B), C16B(H16B), C9(H9), C22(H22), C23(H23),
 C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
 C43(H43), C44(H44), C45(H45)
;
_olex2_submission_special_instructions 'No special instructions were received'