A rare chloride-bridged dysprosium chain with slow magnetic relaxation: a thermally activated mechanism via a second-excited state promoted by magnetic interactions
Ji, Xiao-Qin; Ma, Fang; Xiong, Jin; Yang, Jing; Sun, Hao-Ling; Zhang, Yi-Quan; Gao, Song; Inorganic Chemistry Frontiers 6 (2019) 786–; doi:10.1039/C8QI01331D

data_4349979
_publ_section_title
;
 A rare chloride-bridged dysprosium chain with slow magnetic relaxation: a
 thermally activated mechanism via a second-excited state promoted by
 magnetic interactions
;
_journal_issue                   3
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              786
_journal_paper_doi               10.1039/C8QI01331D
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C13 H12 Br Cl Dy N4 O4'
_chemical_formula_sum            'C13 H12 Br Cl Dy N4 O4'
_chemical_formula_weight         566.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-25 deposited with the CCDC.
2019-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                99.133(6)
_cell_angle_beta                 92.117(6)
_cell_angle_gamma                104.301(7)
_cell_formula_units_Z            2
_cell_length_a                   6.9739(6)
_cell_length_b                   9.0675(7)
_cell_length_c                   13.0622(9)
_cell_measurement_reflns_used    1394
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      24.8440
_cell_measurement_theta_min      3.5180
_cell_volume                     787.75(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_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    -18.00  94.00   1.00    1.50    --   23.13  57.00   0.00  112
  2  \w     99.00 125.00   1.00    1.50    --   23.13 178.00   0.00   26
  3  \w    -14.00 107.00   1.00    1.50    --   23.13  57.00 120.00  121
  4  \w    -13.00 103.00   1.00    1.50    --   23.13  77.00-150.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.1211
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5233
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    2.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.226
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3429
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0134P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                2654
_reflns_number_total             3429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qi01331d2.cif
_cod_data_source_block           20161116l
_cod_database_code               4349979
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H4 of O4, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H11 of O4
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N1) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C8) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C12(H12), C7(H7), C3(H3), C2(H2A), C10(H10), C5(H5), O4(H4)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_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
;