Reversible structural transformation induced switchable single-molecule magnet behavior in lanthanide metal-organic frameworks.
Wang, Mengmeng; Meng, Xixi; Song, Fen; He, Yanfei; Shi, Wei; Gao, Hongling; Tang, Jinkui; Peng, Cheng; Chemical communications (Cambridge, England) 54 (2018) 10183–10186; doi:10.1039/c8cc06058d

data_7122138
_publ_section_title
;
 Reversible structural transformation induced switchable single-molecule
 magnet behavior in lanthanide metal-organic frameworks.
;
_journal_issue                   72
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10183
_journal_page_last               10186
_journal_paper_doi               10.1039/c8cc06058d
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.25(C240 H140 Dy12 N4 O96)'
_chemical_formula_sum            'C60 H35 Dy3 N O24'
_chemical_formula_weight         1641.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2022sz
_audit_creation_date             2018-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-13 deposited with the CCDC.
2018-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.7738(15)
_cell_length_b                   10.6809(5)
_cell_length_c                   19.1423(8)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.7050
_cell_measurement_theta_min      3.5870
_cell_volume                     5678.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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      1.00  80.00   1.00   16.00    --   18.55  57.00-180.00   79
  2  \w    -12.00  45.00   1.00   16.00    --   18.55  77.00 -90.00   57
  3  \w     22.00  60.00   1.00   16.00    --   18.55 -99.00  60.00   38
  4  \w    -44.00  35.00   1.00   16.00    --   18.55 -57.00 -60.00   79
  5  \w     14.00  41.00   1.00   16.00    --   18.55  57.00 -90.00   27
  6  \w    -26.00  91.00   1.00   16.00    --   18.55  19.00 120.00  117
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0160568000
_diffrn_orient_matrix_UB_12      -0.0441180000
_diffrn_orient_matrix_UB_13      0.0148742000
_diffrn_orient_matrix_UB_21      0.0012431000
_diffrn_orient_matrix_UB_22      0.0322186000
_diffrn_orient_matrix_UB_23      0.0324636000
_diffrn_orient_matrix_UB_31      -0.0198421000
_diffrn_orient_matrix_UB_32      0.0376851000
_diffrn_orient_matrix_UB_33      -0.0100233000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18237
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.10
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.712
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.265(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5030
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0300P)^2^+28.0720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                4858
_reflns_number_total             5030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc06058d2.cif
_cod_data_source_block           Ln-MOF1
_cod_depositor_comments
'Adding full bibliography for 7122138--7122139.cif.'
_cod_database_code               7122138
_chemical_oxdiff_formula         'Dy C H O N'
_chemical_oxdiff_usercomment     k1
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O11) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N0AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C18) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C19) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C1AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: C0AA(0.5) C1AA(0.5) C2AA(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C14(H14), C24(H24), C13(H13), C16(H16), C6(H6), C3(H3), C2(H2),
 C20(H20), C28(H28), C5(H5), C27(H27), C10(H10A), C19(H19), C25(H25), C17(H17),
 C11(H11)
;
_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 1.797
_oxdiff_exptl_absorpt_empirical_full_min 0.456