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_7718070
_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 Dy N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Dy N4 O6'
_chemical_formula_weight         1726.99
_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                   13.11740(10)
_cell_length_b                   13.11740(10)
_cell_length_c                   46.3156(6)
_cell_measurement_reflns_used    22606
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      79.3170
_cell_measurement_theta_min      4.0670
_cell_volume                     6901.66(12)
_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      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -51.00 -26.00   0.50    0.20    --  -47.51  57.00  90.00   50
  2  \w    -22.00  25.00   0.50    0.20    --  -47.51  57.00  90.00   94
  3  \w    -18.00  26.00   0.50    0.20    --  -47.51  19.00  90.00   88
  4  \w    106.00 149.00   0.50    0.80    --  113.25  45.00   0.00   86
  5  \w    101.00 151.00   0.50    0.80    --  113.25  61.00 -30.00  100
  6  \w    140.00 176.00   0.50    0.80    --  113.25  45.00  30.00   72
  7  \w    101.00 173.00   0.50    0.80    --  113.25  45.00 120.00  144
  8  \w    106.00 172.00   0.50    0.80    --  113.25  30.00  60.00  132
  9  \w    107.00 133.00   0.50    0.80    --  113.25  45.00  30.00   52
 10  \w    126.00 173.00   0.50    0.80    --  113.25  15.00 -60.00   94
 11  \w    107.00 174.00   0.50    0.80    --  113.25  30.00 -90.00  134
 12  \w    108.00 157.00   0.50    0.80    --  113.25  30.00-150.00   98
 13  \w      6.00  44.00   0.50    0.20    --   47.51 -38.00-120.00   76
 14  \w     43.00  75.00   0.50    0.80    --  113.25 -77.00 -60.00   64
 15  \w     42.00  90.00   0.50    0.80    --  113.25 -77.00 -30.00   96
 16  \w     52.00  80.00   0.50    0.80    --  113.25 -77.00  30.00   56
 17  \w     54.00  79.00   0.50    0.80    --  113.25 -77.00   0.00   50
 18  \w     42.00  68.00   0.50    0.80    --  113.25 -61.00  60.00   52
 19  \w     42.00  67.00   0.50    0.80    --  113.25 -61.00 120.00   50
 20  \w     43.00  68.00   0.50    0.80    --  113.25 -61.00  30.00   50
 21  \w    116.00 165.00   0.50    0.80    --  113.25 125.00  30.00   98
 22  \w    122.00 170.00   0.50    0.80    --  113.25 125.00 -90.00   96
 23  \w     52.00  84.00   0.50    0.80    --  113.25 -77.00-180.00   64
 24  \w     46.00  73.00   0.50    0.80    --  113.25-125.00-150.00   54
 25  \w     78.00 103.00   0.50    0.80    --  113.25-125.00-150.00   50
 26  \w     63.00 111.00   0.50    0.80    --  113.25-125.00-120.00   96
 27  \w     45.00 111.00   0.50    0.80    --  113.25-125.00 -90.00  132
 28  \w     45.00  82.00   0.50    0.80    --  113.25-125.00 -30.00   74
 29  \w     44.00  70.00   0.50    0.80    --  113.25-125.00 120.00   52
 30  \w     80.00 107.00   0.50    0.80    --  113.25-125.00 120.00   54
 31  \w     86.00 111.00   0.50    0.80    --  113.25-125.00 150.00   50
 32  \w     54.00 106.00   0.50    0.80    --  113.25 -94.00 120.00  104
 33  \w     43.00 100.00   0.50    0.80    --  113.25 -94.00  90.00  114
 34  \w     74.00 106.00   0.50    0.80    --  113.25 -94.00 -30.00   64
 35  \w     71.00 106.00   0.50    0.80    --  113.25 -94.00   0.00   70
 36  \w     71.00 104.00   0.50    0.80    --  113.25 -94.00 -60.00   66
 37  \w     81.00 106.00   0.50    0.80    --  113.25 -94.00 -90.00   50
 38  \w     51.00  76.00   0.50    0.80    --  113.25 -94.00 -90.00   50
 39  \w     81.00 106.00   0.50    0.80    --  113.25 -94.00-120.00   50
 40  \w    -83.00 -14.00   0.50    0.20    --  -47.51 125.00-180.00  138
 41  \w    -85.00 -13.00   0.50    0.20    --  -47.51 125.00   0.00  144
 42  \w    -76.00 -29.00   0.50    0.80    --  -91.75 125.00 150.00   94
 43  \w   -115.00 -79.00   0.50    0.80    --  -91.75 -45.00   0.00   72
 44  \w   -163.00-120.00   0.50    0.80    --  -91.75 -45.00   0.00   86
 45  \w   -119.00 -28.00   0.50    0.20    --  -47.51 -77.00 -30.00  182
;
_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      -0.0591708000
_diffrn_orient_matrix_UB_12      0.0714759000
_diffrn_orient_matrix_UB_13      -0.0087253000
_diffrn_orient_matrix_UB_21      0.1133760000
_diffrn_orient_matrix_UB_22      0.0895209000
_diffrn_orient_matrix_UB_23      -0.0157013000
_diffrn_orient_matrix_UB_31      -0.0451556000
_diffrn_orient_matrix_UB_32      -0.0724465000
_diffrn_orient_matrix_UB_33      -0.0280124000
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            27533
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.217
_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    21.305
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.451
_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    2.493
_exptl_crystal_description       block
_exptl_crystal_F_000             4794
_exptl_crystal_recrystallization_method 'From reaction'
_exptl_crystal_size_max          0.056
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 1337 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3084
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0259P)^2^+67.0449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.848
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                3046
_reflns_number_total             3084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03474k2.cif
_cod_data_source_block           sb01-05-dy2-xrd-100k_abs
_cod_depositor_comments
'Adding full bibliography for 7718068--7718078.cif.'
_cod_original_cell_volume        6901.66(14)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7718070
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Dy Br12 O6 N4 C36'
_chemical_oxdiff_usercomment     'colourless cube in oil 100K'
_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              95491
_olex2_exptl_crystal_mounting_method mounted
_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 1.355
_oxdiff_exptl_absorpt_empirical_full_min 0.826