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_7718075
_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 Er N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Er N4 O6'
_chemical_formula_weight         1731.75
_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
;
2025-01-23 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                   13.1015(2)
_cell_length_b                   13.1015(2)
_cell_length_c                   46.1778(5)
_cell_measurement_reflns_used    10493
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      79.9090
_cell_measurement_theta_min      4.1460
_cell_volume                     6864.45(17)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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     34.00  76.00   0.50    0.08    --   47.51-125.00 -90.00   84
  2  \w     51.00  95.00   0.50    0.32    --  113.25-125.00-150.00   88
  3  \w     86.00 111.00   0.50    0.32    --  113.25-125.00-120.00   50
  4  \w     47.00  72.00   0.50    0.32    --  113.25-125.00-180.00   50
  5  \w     55.00  81.00   0.50    0.32    --  113.25-125.00-120.00   52
  6  \w     59.00 106.00   0.50    0.32    --  113.25-108.00-127.96   94
  7  \w     52.00  78.00   0.50    0.32    --  113.25-125.00 -30.00   52
  8  \w     82.00 107.00   0.50    0.32    --  113.25-103.00 -18.05   50
  9  \w     44.00  76.00   0.50    0.32    --  113.25-103.00 -18.05   64
 10  \w     48.00 111.00   0.50    0.32    --  113.25-125.00  90.00  126
 11  \w     47.00 107.00   0.50    0.32    --  113.25-125.00 120.00  120
 12  \w     57.00 103.00   0.50    0.32    --  113.25 -94.00 120.00   92
 13  \w     71.00 105.00   0.50    0.32    --  113.25 -94.00  90.00   68
 14  \w     46.00 100.00   0.50    0.32    --  113.25 -94.00   0.00  108
 15  \w     80.00 106.00   0.50    0.32    --  113.25 -94.00 -60.00   52
 16  \w     77.00 104.00   0.50    0.32    --  113.25 -94.00-120.00   54
 17  \w     79.00 105.00   0.50    0.32    --  113.25 -94.00 -90.00   52
 18  \w     43.00  76.00   0.50    0.32    --  113.25 -77.00   0.00   66
 19  \w     44.00  71.00   0.50    0.32    --  113.25 -61.00  60.00   54
 20  \w     45.00  70.00   0.50    0.32    --  113.25 -77.00 -60.00   50
 21  \w     42.00  70.00   0.50    0.32    --  113.25 -77.00 -90.00   56
 22  \w     44.00  78.00   0.50    0.32    --  113.25 -77.00-150.00   68
 23  \w     -6.00  30.00   0.50    0.08    --   47.51 -19.00 150.00   72
 24  \w    -18.00  29.00   0.50    0.08    --   47.51 -19.00  90.00   94
 25  \w     42.00  68.00   0.50    0.32    --  113.25 -61.00 120.00   52
 26  \w     42.00  67.00   0.50    0.32    --  113.25 -61.00  30.00   50
 27  \w     44.00  69.00   0.50    0.32    --  113.25 -77.00-120.00   50
 28  \w    103.00 178.00   0.50    0.32    --  113.25  15.00 -60.00  150
 29  \w    148.00 173.00   0.50    0.32    --  113.25  45.00-120.00   50
 30  \w    105.00 131.00   0.50    0.32    --  113.25  45.00-120.00   52
 31  \w    107.00 143.00   0.50    0.32    --  113.25  30.00-150.00   72
 32  \w    111.00 178.00   0.50    0.32    --  113.25  45.00  30.00  134
 33  \w    122.00 162.00   0.50    0.32    --  113.25  45.00  90.00   80
 34  \w    103.00 176.00   0.50    0.32    --  113.25  45.00 120.00  146
 35  \w    148.00 178.00   0.50    0.32    --  113.25  15.00 150.00   60
 36  \w    103.00 141.00   0.50    0.32    --  113.25  15.00  60.00   76
 37  \w    146.00 174.00   0.50    0.32    --  113.25  15.00  60.00   56
 38  \w    112.00 178.00   0.50    0.32    --  113.25  30.00   0.00  132
 39  \w     50.00 105.00   0.50    0.08    --   47.51  19.00  90.00  110
 40  \w    -22.00  20.00   0.50    0.08    --  -47.51  77.00  60.00   84
 41  \w    -63.00 -26.00   0.50    0.08    --  -47.51  77.00  60.00   74
 42  \w    -50.00 -25.00   0.50    0.32    --  -91.75  45.00  90.00   50
 43  \w    -30.00  26.00   0.50    0.08    --  -47.51  19.00  60.00  112
 44  \w    -55.00  22.00   0.50    0.08    --  -47.51  57.00 -30.00  154
 45  \w    -82.00 -55.00   0.50    0.32    --  -91.75 125.00-120.00   54
 46  \w    -67.00 -37.00   0.50    0.08    --  -47.51 -38.00 -90.00   60
 47  \w   -118.00 -85.00   0.50    0.08    --  -47.51 -38.00 -90.00   66
 48  \w   -109.00 -80.00   0.50    0.32    --  -91.75 -30.00 150.00   58
;
_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      -0.1123868000
_diffrn_orient_matrix_UB_12      -0.0211165000
_diffrn_orient_matrix_UB_13      0.0158599000
_diffrn_orient_matrix_UB_21      -0.0636859000
_diffrn_orient_matrix_UB_22      -0.1296700000
_diffrn_orient_matrix_UB_23      -0.0098388000
_diffrn_orient_matrix_UB_31      0.0418330000
_diffrn_orient_matrix_UB_32      -0.0340103000
_diffrn_orient_matrix_UB_33      0.0276640000
_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  0.0831
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       58
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            26953
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.198
_diffrn_reflns_theta_min         4.342
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.089
_exptl_absorpt_correction_T_max  0.576
_exptl_absorpt_correction_T_min  0.416
_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    2.514
_exptl_crystal_description       block
_exptl_crystal_F_000             4806
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.486
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Flack x determined using 1251 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3133
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0673P)^2^+43.0451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.905
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                2929
_reflns_number_total             3133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03474k2.cif
_cod_data_source_block           sb01-05-er2-xrd-100k_abs
_cod_depositor_comments
'Adding full bibliography for 7718068--7718078.cif.'
_cod_original_cell_volume        6864.5(2)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7718075
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C36 Er Br12 O6 N4'
_chemical_oxdiff_usercomment     'Small 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. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              76541
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.789