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_7718076
_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 Gd N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Gd N4 O6'
_chemical_formula_weight         1721.74
_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                   13.14520(10)
_cell_length_b                   13.14520(10)
_cell_length_c                   46.4914(7)
_cell_measurement_reflns_used    24018
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.1920
_cell_measurement_theta_min      4.3240
_cell_volume                     6957.25(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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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     46.00  71.00   0.50    0.19    --  113.25-125.00 150.00   50
  2  \w     84.00 110.00   0.50    0.19    --  113.25-125.00 150.00   52
  3  \w     47.00  92.00   0.50    0.19    --  113.25-125.00   0.00   90
  4  \w     76.00 111.00   0.50    0.19    --  113.25-125.00 -90.00   70
  5  \w     48.00 104.00   0.50    0.19    --  113.25 -96.00-127.11  112
  6  \w     76.00 101.00   0.50    0.19    --  113.25 -94.00 -90.00   50
  7  \w     45.00  70.00   0.50    0.19    --  113.25 -94.00 -90.00   50
  8  \w     69.00 101.00   0.50    0.19    --  113.25 -94.00-120.00   64
  9  \w     73.00 104.00   0.50    0.19    --  113.25 -94.00   0.00   62
 10  \w     78.00 106.00   0.50    0.19    --  113.25 -94.00 -30.00   56
 11  \w     44.00  75.00   0.50    0.19    --  113.25 -94.00  30.00   62
 12  \w     79.00 106.00   0.50    0.19    --  113.25 -94.00  60.00   54
 13  \w     43.00  97.00   0.50    0.19    --  113.25 -94.00  90.00  108
 14  \w     43.00  69.00   0.50    0.19    --  113.25 -94.00 120.00   52
 15  \w     74.00 100.00   0.50    0.19    --  113.25 -94.00 150.00   52
 16  \w     78.00 103.00   0.50    0.19    --  113.25 -94.00 120.00   50
 17  \w     46.00  72.00   0.50    0.19    --  113.25 -94.00 150.00   52
 18  \w     77.00 103.00   0.50    0.19    --  113.25 -94.00  30.00   52
 19  \w     76.00 103.00   0.50    0.19    --  113.25 -94.00 -60.00   54
 20  \w     45.00  98.00   0.50    0.19    --  113.25 -94.00-180.00  106
 21  \w    -23.00  30.00   0.50    0.05    --   47.26 -19.00-180.00  106
 22  \w     42.00  71.00   0.50    0.19    --  113.25 -61.00-180.00   58
 23  \w     42.00  70.00   0.50    0.19    --  113.25 -61.00 -90.00   56
 24  \w     42.00  71.00   0.50    0.19    --  113.25 -61.00-150.00   58
 25  \w     45.00  71.00   0.50    0.19    --  113.25 -61.00-120.00   52
 26  \w     44.00  83.00   0.50    0.19    --  113.25 -77.00 -30.00   78
 27  \w     46.00  71.00   0.50    0.19    --  113.25 -61.00  30.00   50
 28  \w     46.00  71.00   0.50    0.19    --  113.25 -61.00  90.00   50
 29  \w    150.00 176.00   0.50    0.19    --  113.25   0.00  30.00   52
 30  \w    145.00 171.00   0.50    0.19    --  113.25  77.00 150.00   52
 31  \w     91.00 130.00   0.50    0.19    --  113.25  77.00 150.00   78
 32  \w    101.00 151.00   0.50    0.19    --  113.25  45.00  60.00  100
 33  \w    133.00 158.00   0.50    0.19    --  113.25  45.00  30.00   50
 34  \w    107.00 169.00   0.50    0.19    --  113.25  30.00 150.00  124
 35  \w    102.00 149.00   0.50    0.19    --  113.25  45.00   0.00   94
 36  \w    101.00 155.00   0.50    0.19    --  113.25  45.00 -60.00  108
 37  \w    106.00 178.00   0.50    0.19    --  113.25  30.00-150.00  144
 38  \w    112.00 178.00   0.50    0.19    --  113.25  15.00 -90.00  132
 39  \w     84.00 109.00   0.50    0.19    --  113.25   0.00  30.00   50
 40  \w    112.00 138.00   0.50    0.19    --  113.25  15.00 120.00   52
 41  \w    141.00 166.00   0.50    0.19    --  113.25  15.00 120.00   50
 42  \w    -69.00  21.00   0.50    0.05    --  -47.26  77.00-120.00  180
 43  \w    -21.00  15.00   0.50    0.05    --  -47.26  38.00  30.00   72
 44  \w     -7.00  20.00   0.50    0.05    --  -47.26  57.00  30.00   54
 45  \w    -61.00 -26.00   0.50    0.05    --  -47.26  57.00  30.00   70
 46  \w    -29.00  27.00   0.50    0.05    --  -47.26  19.00 150.00  112
 47  \w    -67.00 -20.00   0.50    0.19    --  -91.75  61.00 150.00   94
 48  \w    -48.00 -22.00   0.50    0.19    --  -91.75  45.00  90.00   52
 49  \w    -51.00 -22.00   0.50    0.19    --  -91.75  45.00  60.00   58
 50  \w    -53.00 -19.00   0.50    0.19    --  -91.75  61.00-150.00   68
 51  \w   -162.00-124.00   0.50    0.19    --  -91.75 -61.00-180.00   76
 52  \w   -120.00 -49.00   0.50    0.05    --  -47.26 -77.00-180.00  142
;
_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      0.0868745000
_diffrn_orient_matrix_UB_12      0.0503864000
_diffrn_orient_matrix_UB_13      0.0253402000
_diffrn_orient_matrix_UB_21      0.1016955000
_diffrn_orient_matrix_UB_22      0.0683491000
_diffrn_orient_matrix_UB_23      -0.0212906000
_diffrn_orient_matrix_UB_31      -0.0206219000
_diffrn_orient_matrix_UB_32      0.1053422000
_diffrn_orient_matrix_UB_33      0.0016949000
_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  0.0473
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            28668
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.972
_diffrn_reflns_theta_min         4.324
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.764
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.144
_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    2.466
_exptl_crystal_description       block
_exptl_crystal_F_000             4782
_exptl_crystal_recrystallization_method 'From reaction'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.612
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 1595 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3342
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0627P)^2^+38.0844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.974
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                3308
_reflns_number_total             3342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03474k2.cif
_cod_data_source_block           sb01-05-gd2-xrd-100k_abs
_cod_depositor_comments
'Adding full bibliography for 7718068--7718078.cif.'
_cod_original_cell_volume        6957.25(15)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7718076
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Gd C36 Br12 O6 N4'
_chemical_oxdiff_usercomment     'clear cube in oil at 100K'
_shelx_estimated_absorpt_t_max   0.311
_shelx_estimated_absorpt_t_min   0.151
_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              81276
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.822