A series of dysprosium-based hydrogen-bonded organic frameworks (Dy‒HOFs): thermally triggered off →on conversion of a single-ion magnet
Wang, Hai-Ling; Ma, Xiong-Feng; Zhu, Zhong-Hong; Zhang, Yi-Quan; Zou, Hua-Hong; Liang, Fu-Pei; Inorganic Chemistry Frontiers 6 (2019) 2906–; doi:10.1039/C9QI00582J

data_4350060
_publ_section_title
;
 A series of dysprosium-based hydrogen-bonded organic frameworks
 (Dy--HOFs): thermally triggered off \\rightarrow on conversion of a
 single-ion magnet
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2906
_journal_paper_doi               10.1039/C9QI00582J
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C30 H18 Br6 Cl Dy N3 O3, C10 H10 N'
_chemical_formula_sum            'C40 H28 Br6 Cl Dy N4 O3'
_chemical_formula_weight         1290.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-12 deposited with the CCDC.	2019-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.014(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7059(6)
_cell_length_b                   18.3642(4)
_cell_length_c                   13.6199(4)
_cell_measurement_reflns_used    11779
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7860
_cell_measurement_theta_min      3.7050
_cell_volume                     4134.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -61.00  39.00   1.00   10.00    --   10.68 -57.00-180.00  100
  2  \w    -72.00  78.00   1.00   10.00    --   10.68   0.00-180.00  150
  3  \w    -17.00  11.00   1.00   10.00    --  -11.93 -99.00 -90.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0248840000
_diffrn_orient_matrix_UB_12      -0.0292820000
_diffrn_orient_matrix_UB_13      -0.0272161000
_diffrn_orient_matrix_UB_21      0.0348931000
_diffrn_orient_matrix_UB_22      -0.0218407000
_diffrn_orient_matrix_UB_23      0.0089033000
_diffrn_orient_matrix_UB_31      -0.0026232000
_diffrn_orient_matrix_UB_32      -0.0125572000
_diffrn_orient_matrix_UB_33      0.0478765000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28403
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.27
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2452
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+1.1480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                6139
_reflns_number_total             7701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9qi00582j2.cif
_cod_data_source_block           20180525_lfp_whl_1340aaa
_cod_database_code               4350060
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C14(H14), C23(H23), N4(H4a), C3(H3), C13(H13), C4(H4), C7(H7),
 C17(H17), C24(H24), C36(H36), C37(H37), C39(H39), C33(H33), C38(H38), C34(H34)
2.b Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C1(H1a,H1b,H1c), C11(H11a,H11b,H11c), C31(H31a,H31b,H31c)
;
_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 2.334
_oxdiff_exptl_absorpt_empirical_full_min 0.736