Cyclic OFF/Part/ON switching of single-molecule magnet behaviours via multistep single-crystal-to-single-crystal transformation between discrete Fe(ii)-Dy(iii) complexes.
Chen, Wen-Bin; Chen, Yan-Cong; Huang, Guo-Zhang; Liu, Jun-Liang; Jia, Jian-Hua; Tong, Ming-Liang; Chemical communications (Cambridge, England) 54 (2018) 10886–10889; doi:10.1039/c8cc04989k

data_7122310
_publ_section_title
;
 Cyclic OFF/Part/ON switching of single-molecule magnet behaviours via
 multistep single-crystal-to-single-crystal transformation between
 discrete Fe(ii)-Dy(iii) complexes.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10886
_journal_page_last               10889
_journal_paper_doi               10.1039/c8cc04989k
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '2(C30 H29 Dy Fe N10 O4 S2)'
_chemical_formula_sum            'C60 H58 Dy2 Fe2 N20 O8 S4'
_chemical_formula_weight         1752.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                89.095(3)
_cell_angle_beta                 83.157(3)
_cell_angle_gamma                85.417(3)
_cell_formula_units_Z            2
_cell_length_a                   14.4632(12)
_cell_length_b                   15.3659(13)
_cell_length_c                   15.8216(13)
_cell_measurement_reflns_used    9711
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.552
_cell_measurement_theta_min      2.487
_cell_volume                     3479.9(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      120.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_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  0.0634
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62874
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.553
_diffrn_reflns_theta_min         2.374
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1093 before and 0.0721 after correction. The Ratio of minimum to maximum transmission is 0.8649. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.091
_platon_squeeze_details
;
TITL C_a.res in P-1
CELL   14.4632   15.3659   15.8216     89.10     83.16     85.42
SPGR P-1
Q101 0.621 0.042 0.348 !       4.53 eA-3
Q102 0.594 0.089 0.390 !       4.51 eA-3
Q103 0.891 0.984 0.422 !       4.45 eA-3
Q104 0.650 0.438 0.020 !       4.02 eA-3
Q105 0.891 0.417 0.141 !       3.82 eA-3
Q106 0.864 0.463 0.190 !       3.34 eA-3
Q107 0.865 0.026 0.469 !       3.27 eA-3
Q108 0.624 0.482 0.069 !       3.20 eA-3
Q109 0.692 0.719 0.098 !       2.97 eA-3
Q110 0.560 0.202 0.028 !       2.64 eA-3
Q111 0.856 0.100 0.453 !       2.63 eA-3
Q112 0.606 0.543 0.064 !       2.32 eA-3
Q113 0.807 0.839 0.329 !       2.29 eA-3
Q114 0.068 0.841 0.401 !       2.25 eA-3
Q115 0.674 0.663 0.206 !       2.07 eA-3
Q116 0.057 0.204 0.234 !       1.98 eA-3
Q117 0.546 0.315 0.036 !       1.97 eA-3
Q118 0.935 0.273 0.483 !       1.88 eA-3
Q119 0.658 0.783 0.143 !       1.85 eA-3
Q120 0.609 0.486 0.109 !       1.79 eA-3
Q121 0.628 0.420 0.061 !       1.61 eA-3
Q122 0.094 0.774 0.363 !       1.58 eA-3
Q123 0.435 0.727 0.039 !       1.57 eA-3
Q124 0.683 0.238 0.465 !       1.45 eA-3
Q125 0.347 0.714 0.478 !       1.43 eA-3
Q126 0.154 0.412 0.202 !       1.42 eA-3
Q127 0.939 0.031 0.456 !       1.42 eA-3
Q128 0.721 0.682 0.028 !       1.41 eA-3
C129 0.468 0.499 0.361 !       1.41 eA-3
Q130 0.081 0.705 0.410 !       1.41 eA-3
Q131 0.065 0.703 0.046 !       1.39 eA-3
Q132 0.562 0.417 0.028 !       1.39 eA-3
Q133 0.326 0.206 0.296 !       1.38 eA-3
Q134 0.532 0.249 0.083 !       1.36 eA-3
Q135 0.600 0.994 0.387 !       1.33 eA-3
Q136 0.814 0.173 0.111 !       1.31 eA-3
Q137 0.638 0.266 0.030 !       1.28 eA-3
Q138 0.888 0.565 0.424 !       1.28 eA-3
Q139 0.672 0.079 0.373 !       1.27 eA-3
Q140 0.265 0.945 0.154 !       1.25 eA-3
Q141 0.398 0.473 0.325 !       1.25 eA-3
Q142 0.331 0.062 0.309 !       1.24 eA-3
Q143 0.128 0.363 0.244 !       1.24 eA-3
Q144 0.391 0.720 0.139 !       1.24 eA-3
Q145 0.684 0.450 0.113 !       1.24 eA-3
Q146 0.265 0.111 0.308 !       1.23 eA-3
Q147 0.091 0.698 0.472 !       1.21 eA-3
Q148 0.825 0.248 0.008 !       1.21 eA-3
Q149 0.592 0.641 0.360 !       1.21 eA-3
Q150 0.329 0.824 0.184 !       1.20 eA-3
Q151 0.151 0.831 0.236 !       1.19 eA-3
Q152 0.091 0.131 0.175 !       1.19 eA-3
Q153 0.142 0.460 0.266 !       1.19 eA-3
Q154 0.610 0.933 0.096 !       1.18 eA-3
Q155 0.692 0.512 0.013 !       1.18 eA-3
Q156 0.908 0.492 0.090 !       1.18 eA-3
C157 0.014 0.027 0.014 !       1.17 eA-3
Q158 0.738 0.529 0.073 !       1.17 eA-3
Q159 0.123 0.970 0.487 !       1.17 eA-3
Q160 0.923 0.228 0.419 !       1.17 eA-3
Q161 0.218 0.051 0.046 !       1.16 eA-3
Q162 0.832 0.032 0.405 !       1.16 eA-3
C163 0.988 0.060 0.079 !       1.15 eA-3
Q164 0.781 0.377 0.265 !       1.15 eA-3
Q165 0.862 0.473 0.111 !       1.14 eA-3
Q166 0.666 0.296 0.362 !       1.14 eA-3
Q167 1.000 0.500 0.000 !       1.13 eA-3
Q168 0.357 0.016 0.268 !       1.12 eA-3
Q169 0.733 0.997 0.132 !       1.12 eA-3
Q170 0.812 0.155 0.499 !       1.12 eA-3
Q171 0.716 0.475 0.033 !       1.12 eA-3
Q172 0.190 0.358 0.174 !       1.12 eA-3
Q173 0.809 0.750 0.080 !       1.12 eA-3
C174 0.420 0.379 0.450 !       1.11 eA-3
Q175 0.799 0.247 0.088 !       1.11 eA-3
Q176 0.097 0.677 0.208 !       1.11 eA-3
Q177 0.611 0.878 0.219 !       1.11 eA-3
Q178 0.627 0.162 0.487 !       1.11 eA-3
Q179 0.325 0.503 0.011 !       1.10 eA-3
C180 0.950 0.078 0.033 !       1.10 eA-3
Q181 0.379 0.395 0.390 !       1.10 eA-3
Q182 0.159 0.015 0.050 !       1.10 eA-3
Q183 0.669 0.220 0.348 !       1.10 eA-3
Q184 0.797 0.797 0.430 !       1.09 eA-3
Q185 0.296 0.420 0.094 !       1.09 eA-3
Q186 0.236 0.170 0.108 !       1.09 eA-3
Q187 0.466 0.982 0.217 !       1.09 eA-3
C188 0.087 0.985 0.019 !       1.08 eA-3
Q189 0.438 0.050 0.221 !       1.08 eA-3
Q190 0.580 0.577 0.135 !       1.08 eA-3
Q191 0.404 0.779 0.160 !       1.07 eA-3
Q192 0.787 0.308 0.155 !       1.07 eA-3
Q193 0.483 0.032 0.010 !       1.06 eA-3
Q194 0.466 0.422 0.022 !       1.06 eA-3
Q195 0.707 0.892 0.012 !       1.06 eA-3
Q196 0.203 0.558 0.455 !       1.06 eA-3
Q197 0.204 0.017 0.466 !       1.05 eA-3
Q198 0.763 0.404 0.077 !       1.05 eA-3
Q199 0.673 1.000 0.377 !       1.05 eA-3
;
_refine_diff_density_max         4.343
_refine_diff_density_min         -2.230
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         14276
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0772
_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^)+88.8541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10136
_reflns_number_total             14276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04989k2.cif
_cod_data_source_block           c_sq
_cod_depositor_comments
'Adding full bibliography for 7122308--7122310.cif.'
_cod_database_code               7122310
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.660
_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
2. Rigid bond restraints
 C56, N17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N9, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C39(H39), C40(H40), C41(H41), C45(H45), C46(H46), C47(H47),
 C48(H48), C31(H31), C32(H32), C33(H33), C34(H34), C52(H52), C53(H53), C54(H54),
  C55(H55), C8(H8A), C9(H9), C10(H10), C11(H11), C1(H1), C2(H2), C3(H3),
 C4(H4A), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
 C25(H25)
3.b Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C51(H51A,H51B,H51C), C37(H37A,H37B,H37C), C58(H58A,H58B,
 H58C), C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C28(H28A,
 H28B,H28C)
3.c Idealised tetrahedral OH refined as rotating group:
 O8(H8), O4(H4)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'