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_7718078
_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 Lu N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Lu N4 O6'
_chemical_formula_weight         1739.46
_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                   13.09510(10)
_cell_length_b                   13.09510(10)
_cell_length_c                   45.9594(6)
_cell_measurement_reflns_used    23109
_cell_measurement_temperature    99.97(12)
_cell_measurement_theta_max      79.3430
_cell_measurement_theta_min      4.3340
_cell_volume                     6825.31(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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      99.97(12)
_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 0.996
_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    -59.00  22.00   0.50    0.33    --  -47.26  57.00 -30.00  162
  2  \w    -23.00   6.00   0.50    0.33    --  -47.26  19.00  90.00   58
  3  \w    -56.00  25.00   0.50    0.33    --  -47.26  57.00-150.00  162
  4  \w    -30.00  27.00   0.50    0.33    --  -47.26  19.00 120.00  114
  5  \w    -70.00  16.00   0.50    0.33    --  -47.26  77.00  90.00  172
  6  \w    -22.00   8.00   0.50    0.33    --   47.26 -19.00 -90.00   60
  7  \w    -13.00  13.00   0.50    0.33    --   47.26 -19.00 150.00   52
  8  \w   -152.00-126.00   0.50    1.31    --  -91.75 -15.00-120.00   52
  9  \w    -60.00 -31.00   0.50    1.31    --  -91.75 125.00-180.00   58
 10  \w   -111.00 -79.00   0.50    1.31    --  -91.75 -30.00 -30.00   64
 11  \w    -46.00 -20.00   0.50    1.31    --  -91.75  45.00  60.00   52
 12  \w   -146.00-120.00   0.50    1.31    --  -91.75 -30.00 -30.00   52
 13  \w     42.00  67.00   0.50    1.31    --  113.25 -61.00  90.00   50
 14  \w     42.00  71.00   0.50    1.31    --  113.25 -61.00  60.00   58
 15  \w    102.00 148.00   0.50    1.31    --  113.25  30.00   0.00   92
 16  \w     44.00  92.00   0.50    1.31    --  113.25-125.00 -90.00   96
 17  \w     60.00 101.00   0.50    1.31    --  113.25-125.00 -60.00   82
 18  \w     42.00  67.00   0.50    1.31    --  113.25 -61.00 120.00   50
 19  \w     74.00 105.00   0.50    1.31    --  113.25 -94.00 150.00   62
 20  \w    137.00 163.00   0.50    1.31    --  113.25  30.00-150.00   52
 21  \w    105.00 132.00   0.50    1.31    --  113.25  30.00-150.00   54
 22  \w    108.00 176.00   0.50    1.31    --  113.25  61.00 -60.00  136
 23  \w     48.00 105.00   0.50    1.31    --  113.25 -94.00   0.00  114
 24  \w     72.00 106.00   0.50    1.31    --  113.25 -94.00  30.00   68
 25  \w     53.00 107.00   0.50    1.31    --  113.25-125.00-180.00  108
 26  \w    102.00 149.00   0.50    1.31    --  113.25  45.00  60.00   94
 27  \w     47.00 103.00   0.50    1.31    --  113.25 -94.00 -60.00  112
 28  \w     42.00  68.00   0.50    1.31    --  113.25 -61.00   0.00   52
 29  \w     44.00  92.00   0.50    1.31    --  113.25 -77.00-120.00   96
 30  \w    106.00 161.00   0.50    1.31    --  113.25  77.00-180.00  110
 31  \w     45.00 106.00   0.50    1.31    --  113.25 -94.00  90.00  122
 32  \w     42.00  68.00   0.50    1.31    --  113.25 -94.00  30.00   52
 33  \w     51.00  98.00   0.50    1.31    --  113.25 -94.00  60.00   94
 34  \w     44.00 106.00   0.50    1.31    --  113.25 -94.00 -30.00  124
 35  \w    113.00 149.00   0.50    1.31    --  113.25  45.00   0.00   72
 36  \w    105.00 154.00   0.50    1.31    --  113.25  30.00 -90.00   98
 37  \w     71.00 103.00   0.50    1.31    --  113.25 -94.00-180.00   64
 38  \w    105.00 155.00   0.50    1.31    --  113.25  30.00 -60.00  100
 39  \w    103.00 162.00   0.50    1.31    --  113.25  45.00 120.00  118
 40  \w     79.00 104.00   0.50    1.31    --  113.25 -94.00 -90.00   50
 41  \w     47.00  73.00   0.50    1.31    --  113.25 -94.00-150.00   52
 42  \w     81.00 106.00   0.50    1.31    --  113.25 -94.00-150.00   50
 43  \w    111.00 170.00   0.50    1.31    --  113.25  30.00  90.00  118
 44  \w     47.00  83.00   0.50    1.31    --  113.25-125.00-150.00   72
;
_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      0.0840202000
_diffrn_orient_matrix_UB_12      0.1317682000
_diffrn_orient_matrix_UB_13      0.0062417000
_diffrn_orient_matrix_UB_21      -0.0725724000
_diffrn_orient_matrix_UB_22      -0.0086844000
_diffrn_orient_matrix_UB_23      0.0272362000
_diffrn_orient_matrix_UB_31      0.0782795000
_diffrn_orient_matrix_UB_32      -0.0316516000
_diffrn_orient_matrix_UB_33      0.0185368000
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            27160
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.223
_diffrn_reflns_theta_min         4.348
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.911
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    2.539
_exptl_crystal_description       block
_exptl_crystal_F_000             4824
_exptl_crystal_recrystallization_method 'From reaction'
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.981
_refine_diff_density_min         -1.949
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 1493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0536P)^2^+55.3523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                3181
_reflns_number_total             3234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03474k2.cif
_cod_data_source_block           sb01-05-lu3-xrd5-100k_abs
_cod_depositor_comments
'Adding full bibliography for 7718068--7718078.cif.'
_cod_original_cell_volume        6825.31(14)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7718078
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Lu Br8 C36 H21 O6 N4'
_chemical_oxdiff_usercomment     'colourless block in oil 100K'
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.425
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              28414
_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 1.565
_oxdiff_exptl_absorpt_empirical_full_min 0.582