Redox, spectroscopic and magnetic properties of <i>C</i><sub>3</sub>-symmetric rare earth complexes featuring atypical <i>ortho</i>-dioxolene binding.
Bagio, Stanley; González, Jonay; Gable, Robert W.; Hall, Christopher R.; Boskovic, Colette; Giansiracusa, Marcus J.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5061–5074; doi:10.1039/d4dt03474k

data_7718069
_publ_section_title
;
 Redox, spectroscopic and magnetic properties of
 <i>C</i><sub>3</sub>-symmetric rare earth complexes featuring atypical
 <i>ortho</i>-dioxolene binding.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5061
_journal_page_last               5074
_journal_paper_doi               10.1039/d4dt03474k
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H21 Br12 N4 O6 Tb'
_chemical_formula_sum            'C36 H21 Br12 N4 O6 Tb'
_chemical_formula_weight         1723.41
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.11280(10)
_cell_length_b                   13.11280(10)
_cell_length_c                   46.3988(7)
_cell_measurement_reflns_used    17954
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      78.4390
_cell_measurement_theta_min      3.9970
_cell_volume                     6909.21(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -64.00 -36.00   0.50    0.05    --  -47.51  77.00-180.00   56
  2  \w    -33.00  24.00   0.50    0.05    --  -47.51  77.00-180.00  114
  3  \w    -37.00  15.00   0.50    0.05    --  -47.51  38.00 -30.00  104
  4  \w    -61.00  13.00   0.50    0.05    --  -47.51  57.00  90.00  148
  5  \w    -25.00   1.00   0.50    0.05    --   47.51 -19.00 -90.00   52
  6  \w     -4.00  23.00   0.50    0.05    --   47.51 -19.00-120.00   54
  7  \w    -27.00  30.00   0.50    0.05    --   47.51 -19.00  30.00  114
  8  \w    -21.00  27.00   0.50    0.05    --   47.51 -19.00 150.00   96
  9  \w     98.00 124.00   0.50    0.05    --  113.25 125.00 120.00   52
 10  \w    151.00 176.00   0.50    0.05    --  113.25 125.00 120.00   50
 11  \w     63.00 106.00   0.50    0.05    --  113.25 -94.00  90.00   86
 12  \w     46.00  81.00   0.50    0.05    --  113.25-132.00 124.47   70
 13  \w     86.00 117.00   0.50    0.05    --  113.25-132.00 124.47   62
 14  \w     86.00 111.00   0.50    0.05    --  113.25-125.00   0.00   50
 15  \w     44.00  75.00   0.50    0.05    --  113.25-125.00   0.00   62
 16  \w     81.00 111.00   0.50    0.05    --  113.25-125.00  30.00   60
 17  \w     66.00 106.00   0.50    0.05    --  113.25-125.00  90.00   80
 18  \w     63.00 101.00   0.50    0.05    --  113.25-125.00  60.00   76
 19  \w     69.00 105.00   0.50    0.05    --  113.25-102.00 -80.70   72
 20  \w     58.00  96.00   0.50    0.05    --  113.25 -94.00 -60.00   76
 21  \w     45.00  89.00   0.50    0.05    --  113.25-125.00 -90.00   88
 22  \w     48.00  78.00   0.50    0.05    --  113.25-125.00-150.00   60
 23  \w     46.00 107.00   0.50    0.05    --  113.25-125.00-180.00  122
 24  \w     76.00 106.00   0.50    0.05    --  113.25 -94.00-180.00   60
 25  \w     61.00 103.00   0.50    0.05    --  113.25 -94.00-150.00   84
 26  \w     79.00 104.00   0.50    0.05    --  113.25 -94.00 150.00   50
 27  \w     44.00  70.00   0.50    0.05    --  113.25 -61.00   0.00   52
 28  \w     44.00  69.00   0.50    0.05    --  113.25 -61.00  90.00   50
 29  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00  30.00   50
 30  \w     45.00  70.00   0.50    0.05    --  113.25 -61.00 120.00   50
 31  \w     45.00  70.00   0.50    0.05    --  113.25 -61.00 -30.00   50
 32  \w     44.00  70.00   0.50    0.05    --  113.25 -61.00 -60.00   52
 33  \w     53.00  94.00   0.50    0.05    --  113.25 -77.00-120.00   82
 34  \w     45.00  70.00   0.50    0.05    --  113.25 -61.00-180.00   50
 35  \w    111.00 175.00   0.50    0.05    --  113.25  15.00 -90.00  128
 36  \w    153.00 178.00   0.50    0.05    --  113.25  77.00  30.00   50
 37  \w     96.00 140.00   0.50    0.05    --  113.25  77.00  30.00   88
 38  \w    105.00 175.00   0.50    0.05    --  113.25  45.00   0.00  140
 39  \w    146.00 176.00   0.50    0.05    --  113.25  45.00 -30.00   60
 40  \w    101.00 142.00   0.50    0.05    --  113.25  45.00 -30.00   82
 41  \w    102.00 134.00   0.50    0.05    --  113.25  61.00-180.00   64
 42  \w    140.00 166.00   0.50    0.05    --  113.25  61.00-180.00   52
 43  \w    102.00 154.00   0.50    0.05    --  113.25  45.00-120.00  104
 44  \w    101.00 177.00   0.50    0.05    --  113.25  45.00 -60.00  152
 45  \w    101.00 145.00   0.50    0.05    --  113.25  45.00 120.00   88
 46  \w    103.00 143.00   0.50    0.05    --  113.25  30.00 120.00   80
 47  \w   -111.00 -47.00   0.50    0.05    --  -47.51 -57.00  30.00  128
 48  \w    -50.00 -20.00   0.50    0.05    --  -91.75  45.00  30.00   60
 49  \w    -80.00 -36.00   0.50    0.05    --  -91.75 125.00-120.00   88
 50  \w    -48.00 -23.00   0.50    0.05    --  -91.75  45.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0039137000
_diffrn_orient_matrix_UB_12      -0.1110330000
_diffrn_orient_matrix_UB_13      -0.0122494000
_diffrn_orient_matrix_UB_21      -0.0136315000
_diffrn_orient_matrix_UB_22      -0.0496287000
_diffrn_orient_matrix_UB_23      0.0307536000
_diffrn_orient_matrix_UB_31      -0.1349336000
_diffrn_orient_matrix_UB_32      -0.0599599000
_diffrn_orient_matrix_UB_33      -0.0027519000
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            28311
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.418
_diffrn_reflns_theta_min         4.335
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.153
_exptl_absorpt_correction_T_max  0.369
_exptl_absorpt_correction_T_min  0.150
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    2.485
_exptl_crystal_description       block
_exptl_crystal_F_000             4788
_exptl_crystal_recrystallization_method 'From reaction'
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Flack x determined using 1572 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3324
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+74.5090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                3276
_reflns_number_total             3324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03474k2.cif
_cod_data_source_block           sb01-05-tb2-xrd-100k_abs
_cod_depositor_comments
'Adding full bibliography for 7718068--7718078.cif.'
_cod_original_cell_volume        6909.21(15)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7718069
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Gd C36 Br12 O6 N4'
_chemical_oxdiff_usercomment     'clear cube in oil at 100K'
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
1.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_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 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.698