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_4350058
_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         'C31 H23 Br6 Dy N3 O4, C14 H12 N2'
_chemical_formula_sum            'C45 H35 Br6 Dy N5 O4'
_chemical_formula_weight         1351.74
_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             2018-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-01 deposited with the CCDC.	2019-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.39(4)
_cell_length_b                   11.17(2)
_cell_length_c                   25.90(5)
_cell_measurement_reflns_used    4487
_cell_measurement_temperature    296(2)
_cell_volume                     5040(17)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0704
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38101
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.17
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.287
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         8866
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                6481
_reflns_number_total             8866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9qi00582j2.cif
_cod_data_source_block           bbbb
_cod_original_cell_volume        5037(17)
_cod_database_code               4350058
_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
 O1-H1
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 C9-H1
 1.84705 with sigma of 0.02
 Dy1-H1
 2.831307 with sigma of 0.02
 C31-H4
 1.94076 with sigma of 0.02
 Dy1-H4
 2.960227 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C23(H23), C24(H24), C4(H4a), C3(H3), C37(H37), C7(H7), C13(H13),
 C14(H14), C17(H17), C40(H40), C41(H41), C35(H35), C38(H38), C34(H34)
4.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C1(H1a,H1b,H1c), C21(H21a,H21b,H21c), C43(H43a,H43b,
 H43c), C32(H32a,H32b,H32c), C31(H31a,H31b,H31c)
;
_olex2_submission_special_instructions 'No special instructions were received'