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_7719461
_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         'C25 H20 Cl Dy N5 O9, Cl O4, C H4 O'
_chemical_formula_sum            'C26 H24 Cl2 Dy N5 O14'
_chemical_formula_weight         863.90
_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
_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                109.623(5)
_cell_angle_beta                 104.315(4)
_cell_angle_gamma                97.684(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5480(5)
_cell_length_b                   11.2040(8)
_cell_length_c                   15.0999(7)
_cell_measurement_reflns_used    4728
_cell_measurement_temperature    124(30)
_cell_measurement_theta_max      27.5640
_cell_measurement_theta_min      3.8670
_cell_volume                     1582.08(17)
_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    'Bourhis et al., 2015'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      124(30)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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    -14.00 106.00   1.00   10.00    --   23.29  77.00  30.00  120
  2  \w     41.00  68.00   1.00   10.00    --   23.29  77.00 -30.00   27
  3  \w    -13.00 104.00   1.00   10.00    --   23.29  77.00 150.00  117
  4  \w    -21.00 106.00   1.00   10.00    --   23.29  77.00 -90.00  127
;
_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      -0.0268041000
_diffrn_orient_matrix_UB_12      -0.0078388000
_diffrn_orient_matrix_UB_13      0.0369440000
_diffrn_orient_matrix_UB_21      0.0641056000
_diffrn_orient_matrix_UB_22      0.0309508000
_diffrn_orient_matrix_UB_23      0.0361545000
_diffrn_orient_matrix_UB_31      -0.0166209000
_diffrn_orient_matrix_UB_32      0.0613843000
_diffrn_orient_matrix_UB_33      0.0092256000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0996
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8974
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.177
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32907
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       needle
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.704
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         5465
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0473P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4561
_reflns_number_total             5465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01924a2.cif
_cod_data_source_block           20170801a
_cod_depositor_comments
'Adding full bibliography for 7719461--7719462.cif.'
_cod_original_cell_volume        1582.08(16)
_cod_database_code               7719461
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C10 H10 O10 N10 Dy2 Cl2'
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.855
_reflns_odcompleteness_completeness 99.72
_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
 C27-O11
 1.4 with sigma of 0.02
 H11a-H2_$1
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C27)
\\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2a), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12),
  C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25)
4.b Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c)
4.c Idealised tetrahedral OH refined as rotating group:
 O11(H11a)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98469
_shelx_fab_checksum              31907
_olex2_date_sample_data_collection 2017-08-01
_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 3.029
_oxdiff_exptl_absorpt_empirical_full_min 0.567