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_4350059
_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
'C11 H10 Br2 Dy N4 O11, C14 H12 N2, C14 H13 N2'
_chemical_formula_sum            'C39 H35 Br2 Dy N8 O11'
_chemical_formula_weight         1114.07
_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
_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                 99.618(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3824(5)
_cell_length_b                   18.8386(11)
_cell_length_c                   21.0988(13)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    150(2)
_cell_volume                     4068.7(4)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55058
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.872
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0856 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.8051.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.629
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0489P)^2^+9.1093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                5997
_reflns_number_total             7991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9qi00582j2.cif
_cod_data_source_block           mo_1212_6_0m
_cod_database_code               4350059
_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. Restrained distances
 O13-H13
 0.87 with sigma of 0.01
 C11-H13
 1.926775 with sigma of 0.02
 Dy1-H13
 2.898999 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O5) \\sim Ueq,
Uanis(O3) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O7) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O3(0.5) O8(0.5) O7(0.5) O4(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C4(H4), C18(H18), C17(H17), C28(H28), C14(H14), C35(H35),
 C31(H31), C15(H15), C32(H32), C29(H29), C20(H20), C34(H34), C21(H21)
5.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C12(H12a,H12b,H12c), C37(H37a,H37b,H37c), C26(H26a,H26b,
 H26c), C11(H11a,H11b,H11c), C23(H23a,H23b,H23c)
;
_olex2_submission_special_instructions 'No special instructions were received'