Effect of a bromo-substituent on the magnetization dynamics of dysprosium coordination polymers constructed using a hybrid-ligand concept.
Ma, Fang; Zhang, Lei; Yang, Chan; Huang, Zhen-Na; Huang, XiaoXiao; Sun, Hao-Ling; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15529–15536; doi:10.1039/d5dt01924a

data_7719462
_publ_section_title
;
 Effect of a bromo-substituent on the magnetization dynamics of dysprosium
 coordination polymers constructed using a hybrid-ligand concept.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15529
_journal_page_last               15536
_journal_paper_doi               10.1039/d5dt01924a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C32 H28 Br Dy N6 O7, 2(Cl O4), 3(C H4 O)'
_chemical_formula_sum            'C35 H40 Br Cl2 Dy N6 O18'
_chemical_formula_weight         1146.04
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-07-19
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-08-11 deposited with the CCDC.	2025-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                105.931(5)
_cell_angle_beta                 95.444(4)
_cell_angle_gamma                107.157(4)
_cell_formula_units_Z            2
_cell_length_a                   11.5744(6)
_cell_length_b                   13.3322(6)
_cell_length_c                   15.1448(9)
_cell_measurement_reflns_used    4698
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.0060
_cell_measurement_theta_min      3.3520
_cell_volume                     2107.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.864
_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    -69.00 113.00   1.00    2.50    --   23.29 -19.00 120.00  182
  2  \w     45.00 125.00   1.00    2.50    --   23.29-178.00 150.00   80
  3  \w     67.00  93.00   1.00    2.50    --   23.29-178.00-120.00   26
  4  \w     27.00  53.00   1.00    2.50    --   23.29 -99.00-150.00   26
  5  \w   -114.00 -68.00   1.00    2.50    --  -21.96-178.00-180.00   46
  6  \w     42.00  72.00   1.00    2.50    --   23.29 178.00  90.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0625811000
_diffrn_orient_matrix_UB_12      -0.0344280000
_diffrn_orient_matrix_UB_13      -0.0100383000
_diffrn_orient_matrix_UB_21      0.0057128000
_diffrn_orient_matrix_UB_22      -0.0250492000
_diffrn_orient_matrix_UB_23      -0.0464197000
_diffrn_orient_matrix_UB_31      0.0179088000
_diffrn_orient_matrix_UB_32      -0.0404504000
_diffrn_orient_matrix_UB_33      0.0143807000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.1044
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14727
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.810
_diffrn_reflns_theta_min         3.218
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.931
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       block
_exptl_crystal_F_000             1142
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.143
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9508
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7675
_reflns_number_total             9508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01924a2.cif
_cod_data_source_block           20170911c
_cod_depositor_comments
'Adding full bibliography for 7719461--7719462.cif.'
_cod_database_code               7719462
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 O10 N10 Dy2 Cl2 Br2'
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.758
_reflns_odcompleteness_completeness 99.81
_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, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 C35-H6
 1.901942 with sigma of 0.02
 Dy1-H6
 2.883962 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C29(H29), C21(H21), C28(H28), C22(H22), C18(H18), C14(H14),
 C13(H13), C20(H20), C30(H30), C2(H2a), C15(H15), C31(H31), C25(H25), C5(H5),
 C17(H17), C23(H23), C26(H26), C3(H3), C12(H12), C10(H10), C19(H19), C11(H11)
4.b Idealised Me refined as rotating group:
 C35(H35a,H35b,H35c), C32(H32a,H32b,H32c), C34(H34a,H34b,H34c), C33(H33a,H33b,
 H33c)
4.c Idealised tetrahedral OH refined as rotating group:
 O18(H18a), O16(H16), O17(H17a)
;
_shelx_res_checksum              92327
_olex2_date_sample_data_collection 2017-09-11
_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 3.021
_oxdiff_exptl_absorpt_empirical_full_min 0.583