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_7717483
_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 Gd2 N4 O16, 2(C2 H6 O)'
_chemical_formula_sum            'C35 H50 Gd2 N4 O18'
_chemical_formula_weight         1129.29
_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                 105.754(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3156(2)
_cell_length_b                   26.0237(4)
_cell_length_c                   16.4697(2)
_cell_measurement_reflns_used    17999
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.5060
_cell_measurement_theta_min      3.2490
_cell_volume                     4255.21(12)
_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 0.969
_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     49.00  75.00   0.50    0.05    --   47.14-101.00 165.00   52
  2  \w     81.00 106.00   0.50    0.17    --  105.29-101.00 165.00   50
  3  \w     36.00  77.00   0.50    0.17    --  105.29-101.00 165.00   82
  4  \w     33.00  62.00   0.50    0.17    --  105.29 -61.00  60.00   58
  5  \w     80.00 105.00   0.50    0.17    --  105.29 -77.00 -30.00   50
  6  \w     39.00  65.00   0.50    0.17    --  105.29 -77.00 -30.00   52
  7  \w     38.00  70.00   0.50    0.17    --  105.29 -61.00 150.00   64
  8  \w    -25.00  46.00   0.50    0.05    --   47.14 -38.00   0.00  142
  9  \w     37.00  73.00   0.50    0.17    --  105.29 -61.00-150.00   72
 10  \w     34.00  71.00   0.50    0.17    --  105.29 -61.00-180.00   74
 11  \w    122.00 170.00   0.50    0.17    --  105.29  30.00 -90.00   96
 12  \w    110.00 136.00   0.50    0.17    --  105.29 101.00 -90.00   52
 13  \w     96.00 123.00   0.50    0.17    --  105.29  30.00-120.00   54
 14  \w     25.00 117.00   0.50    0.05    --   47.14  77.00  60.00  184
 15  \w    -10.00  25.00   0.50    0.05    --  -47.14  19.00-180.00   70
 16  \w   -102.00 -38.00   0.50    0.17    -- -104.50  77.00-120.00  128
 17  \w   -100.00 -38.00   0.50    0.17    -- -104.50  77.00  30.00  124
 18  \w    -62.00 -33.00   0.50    0.17    -- -104.50  61.00  30.00   58
 19  \w    -58.00 -32.00   0.50    0.17    -- -104.50  61.00  60.00   52
 20  \w    -68.00 -32.00   0.50    0.17    -- -104.50  61.00  90.00   72
 21  \w    -67.00 -36.00   0.50    0.17    -- -104.50  61.00 120.00   62
 22  \w   -163.00 -96.00   0.50    0.17    -- -104.50 -45.00 150.00  134
 23  \w   -138.00-113.00   0.50    0.17    -- -104.50-101.00 165.00   50
 24  \w   -158.00-102.00   0.50    0.17    -- -104.50 -45.00   0.00  112
 25  \w    -97.00 -35.00   0.50    0.17    -- -104.50 101.00 -90.00  124
 26  \w    -78.00  12.00   0.50    0.05    --  -47.14 101.00 -90.00  180
;
_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      -0.0278462000
_diffrn_orient_matrix_UB_12      -0.0448496000
_diffrn_orient_matrix_UB_13      -0.0634491000
_diffrn_orient_matrix_UB_21      0.0973913000
_diffrn_orient_matrix_UB_22      -0.0343539000
_diffrn_orient_matrix_UB_23      0.0651231000
_diffrn_orient_matrix_UB_31      -0.1175544000
_diffrn_orient_matrix_UB_32      -0.0177783000
_diffrn_orient_matrix_UB_33      0.0341884000
_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  0.0547
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31890
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.218
_diffrn_reflns_theta_min         3.265
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49230
_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    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.118
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.000083(16)
_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   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         8630
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0377P)^2^+17.9935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7659
_reflns_number_total             8630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02652g2.cif
_cod_data_source_block           Gd
_cod_depositor_comments
'Adding full bibliography for 7717482--7717483.cif.'
_cod_database_code               7717483
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 100.00
_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
 O8-H8
 0.87 with sigma of 0.01
 O6-H6
 0.87 with sigma of 0.01
 O7-H7
 0.87 with sigma of 0.01
 C22-H8
 1.910927 with sigma of 0.02
 C25-H6
 1.907068 with sigma of 0.02
 Gd1-H8
 3.024874 with sigma of 0.02
 C29-H7
 1.901184 with sigma of 0.02
 Gd1-H6
 3.076647 with sigma of 0.02
 Gd1-H7
 3.087238 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C23(H23A,H23B), C22(H22A,H22B), C31(H31A,H31B), C25(H25A,
 H25B), C29(H29A,H29B), C28(H28A,H28B), C27(H27A,H27B), C24(H24A,H24B),
 C26(H26A,H26B), C32(H32A,H32B), C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7A), C10(H10), C14(H14), C17(H17), C13(H13), C21(H21), C3(H3), C20(H20),
 C18(H18), C12(H12), C6(H6A), C19(H19), C5(H5), C11(H11), C4(H4)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
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 1.927
_oxdiff_exptl_absorpt_empirical_full_min 0.703