Asymmetric triply bridged lanthanide binuclear clusters with distinctly different magnetic behaviors.
Yang, Yue; Wang, Yu-Xia; Lei, Yu-Zhe; Cheng, Peng; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19097–19101; doi:10.1039/d4dt02652g

data_7717482
_publ_section_title
;
 Asymmetric triply bridged lanthanide binuclear clusters with distinctly
 different magnetic behaviors.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19097
_journal_page_last               19101
_journal_paper_doi               10.1039/d4dt02652g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C31 H38 Dy2 N4 O16, 2(C2 H6 O)'
_chemical_formula_sum            'C35 H50 Dy2 N4 O18'
_chemical_formula_weight         1139.79
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-09-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-09-11 deposited with the CCDC.	2024-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.8520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.27550(10)
_cell_length_b                   26.0316(2)
_cell_length_c                   16.4282(2)
_cell_measurement_reflns_used    18988
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.2490
_cell_measurement_theta_min      3.2330
_cell_volume                     4227.23(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_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     45.00  90.00   0.50    0.06    --  105.29 -95.00-150.00   90
  2  \w     34.00  59.00   0.50    0.06    --  105.29 -61.00 -90.00   50
  3  \w     37.00 109.00   0.50    0.06    --  105.29 -77.00 120.00  144
  4  \w     59.00 107.00   0.50    0.06    --  105.29-103.00 128.00   96
  5  \w     17.00  42.00   0.50    0.05    --   47.14-103.00 128.00   50
  6  \w    -15.00  15.00   0.50    0.05    --   47.14 -19.00 -90.00   60
  7  \w     91.00 162.00   0.50    0.06    --  105.29 103.00-130.00  142
  8  \w    130.00 170.00   0.50    0.06    --  105.29  45.00  30.00   80
  9  \w     93.00 118.00   0.50    0.06    --  105.29  45.00  30.00   50
 10  \w    106.00 135.00   0.50    0.06    --  105.29  15.00 150.00   58
 11  \w    140.00 172.00   0.50    0.06    --  105.29  15.00 150.00   64
 12  \w    -22.00  26.00   0.50    0.05    --  -47.14  38.00   0.00   96
 13  \w    -23.00  21.00   0.50    0.05    --  -47.14  19.00-120.00   88
 14  \w    -17.00  28.00   0.50    0.05    --  -47.14  19.00-180.00   90
 15  \w     -9.00  28.00   0.50    0.05    --  -47.14  19.00 -30.00   74
 16  \w    -23.00  15.00   0.50    0.05    --  -47.14  19.00 150.00   76
 17  \w    -60.00 -35.00   0.50    0.06    -- -104.50 125.00 -90.00   50
 18  \w    -81.00   7.00   0.50    0.05    --  -47.14 103.00-130.00  176
 19  \w   -110.00 -74.00   0.50    0.06    -- -104.50 125.00 -90.00   72
 20  \w    -95.00 -70.00   0.50    0.06    -- -104.50 103.00-130.00   50
 21  \w    -90.00 -42.00   0.50    0.06    -- -104.50  77.00 -90.00   96
 22  \w    -61.00 -33.00   0.50    0.06    -- -104.50  61.00-180.00   56
 23  \w    -68.00 -42.00   0.50    0.06    -- -104.50  61.00  30.00   52
 24  \w    -68.00 -32.00   0.50    0.06    -- -104.50  61.00  90.00   72
 25  \w    -58.00 -32.00   0.50    0.06    -- -104.50  61.00  60.00   52
 26  \w    -67.00 -42.00   0.50    0.06    -- -104.50  61.00   0.00   50
 27  \w    -66.00 -39.00   0.50    0.06    -- -104.50  61.00-150.00   54
 28  \w   -173.00-110.00   0.50    0.06    -- -104.50 -30.00-150.00  126
 29  \w   -141.00-116.00   0.50    0.06    -- -104.50-103.00 128.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0409398000
_diffrn_orient_matrix_UB_12      -0.0568092000
_diffrn_orient_matrix_UB_13      0.0022006000
_diffrn_orient_matrix_UB_21      -0.0627777000
_diffrn_orient_matrix_UB_22      0.0009338000
_diffrn_orient_matrix_UB_23      -0.0965882000
_diffrn_orient_matrix_UB_31      0.1366454000
_diffrn_orient_matrix_UB_32      -0.0165441000
_diffrn_orient_matrix_UB_33      -0.0132378000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31635
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.215
_diffrn_reflns_theta_min         3.272
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.99a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.350
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.000060(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         8562
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0263P)^2^+28.5424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7766
_reflns_number_total             8562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02652g2.cif
_cod_data_source_block           Dy
_cod_depositor_comments
'Adding full bibliography for 7717482--7717483.cif.'
_cod_database_code               7717482
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6
 0.87 with sigma of 0.01
 O8-H8
 0.87 with sigma of 0.01
 O7-H7
 0.87 with sigma of 0.01
 C22-H8
 1.905248 with sigma of 0.02
 C25-H7
 1.913958 with sigma of 0.02
 Dy1-H8
 3.012778 with sigma of 0.02
 Dy1-H7
 3.042631 with sigma of 0.02
 C29-H6
 1.907152 with sigma of 0.02
 Dy1-H6
 3.057053 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C30(H30A,H30B), C25(H25A,H25B), C31(H31A,H31B), C23(H23A,
 H23B), C29(H29A,H29B), C27(H27A,H27B), C28(H28A,H28B), C24(H24A,H24B),
 C26(H26A,H26B), C33(H33A,H33B), C34(H34A,H34B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C7(H7A), C17(H17), C21(H21), C13(H13), C18(H18), C3(H3),
 C20(H20), C19(H19), C6(H6A), C12(H12), C4(H4), C5(H5), C11(H11)
3.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C35(H35A,H35B,H35C)
3.d Idealised tetrahedral OH refined as rotating group:
 O17(H17A), O18(H18A)
;
_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 5.423
_oxdiff_exptl_absorpt_empirical_full_min 0.647