Taming 2,2'-biimidazole ligands in trivalent chromium complexes.
Chong, Julien; Benchohra, Amina; Besnard, Céline; Guénée, Laure; Rosspeintner, Arnulf; Cruz, Carlos M.; Jiménez, Juan-Ramón; Piguet, Claude; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15801–15814; doi:10.1039/d4dt01608d

data_7716546
_publ_section_title
;
 Taming 2,2'-biimidazole ligands in trivalent chromium complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15801
_journal_page_last               15814
_journal_paper_doi               10.1039/d4dt01608d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H18 Cr1 N12, 3(N O3)'
_chemical_formula_sum            'C18 H18 Cr N15 O9'
_chemical_formula_weight         640.47
_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_date             2023-02-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.2169(3)
_cell_length_b                   17.2169(3)
_cell_length_c                   15.7297(4)
_cell_measurement_reflns_used    16392
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      74.9690
_cell_measurement_theta_min      4.1420
_cell_volume                     4037.95(14)
_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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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      4.00  30.00   0.50    1.50    --    2.00  33.00 -74.14   52
  2  \w      4.00  29.00   0.50    1.50    --    2.00  33.00  -8.05   50
  3  \w     -1.00  24.00   0.50    1.50    --   -6.00  36.00 -49.49   50
  4  \w     -1.00  24.00   0.50    1.50    --   -6.00  36.00 -89.80   50
  5  \w     -1.00  24.00   0.50    1.50    --   -6.00  36.00 -33.25   50
  6  \w      5.00  30.00   0.50    1.50    --    6.00  31.00  -4.62   50
  7  \w     -3.00  22.00   0.50    1.50    --  -10.00  38.00 -83.69   50
  8  \w     -8.00  17.00   0.50    1.50    --  -14.00  37.00-140.14   50
  9  \w     11.00  36.00   0.50    1.50    --   18.00  28.00 -88.28   50
 10  \w    -11.00  14.00   0.50    1.50    --  -18.00  45.00 -20.30   50
 11  \w     13.00  40.00   0.50    1.50    --   18.00  28.00 -47.34   54
 12  \w    -16.00   9.00   0.50    1.50    --  -22.00  47.00 -47.03   50
 13  \w    -15.00  10.00   0.50    1.50    --  -22.00  49.00 -78.27   50
 14  \w    -48.00 -23.00   0.50    1.50    --  -34.00 -26.00 108.62   50
 15  \w    -51.00 -26.00   0.50    1.50    --  -42.00 -25.00  71.23   50
 16  \w    -51.00 -25.00   0.50    1.50    --  -42.00 -25.00 128.23   52
 17  \w    -56.00 -31.00   0.50    1.50    --  -50.00 -24.00  85.35   50
 18  \w    -56.00 -31.00   0.50    1.50    --  -50.00 -24.00 161.09   50
 19  \w    -61.00 -35.00   0.50    1.50    --  -58.00 -23.00 109.85   52
 20  \w   -101.00 -76.00   0.50    1.50    --  -59.39   0.00  30.00   50
 21  \w    -99.00 -71.00   0.50    1.50    --  -59.39-151.00  34.00   56
 22  \w   -101.00 -76.00   0.50    1.50    --  -59.39   0.00 -60.00   50
 23  \w     25.00  61.00   0.50    1.50    --   59.71 -94.00 -30.00   72
 24  \w    -71.00 -44.00   0.50    1.50    --  -66.50 -22.00 167.02   54
 25  \w     43.00  81.00   0.50    1.50    --   66.73  21.00-133.98   76
 26  \w     50.00  91.00   0.50    1.50    --   66.73  21.00-112.53   82
 27  \w     41.00  70.00   0.50    1.50    --   66.73  22.00 -47.19   58
 28  \w     41.00  66.00   0.50    1.50    --   66.73  22.00 -60.82   50
 29  \w     35.00  72.00   0.50    1.50    --   73.75 -94.00  30.00   74
 30  \w     37.00 117.00   0.50    1.50    --   73.75  10.00 107.00  160
 31  \w     40.00  95.00   0.50    1.50    --   73.75-125.00-120.00  110
 32  \w     33.00  60.00   0.50    1.50    --   74.46 -94.00   0.00   54
 33  \w     68.00 109.00   0.50    1.50    --   83.95-125.00-150.00   82
 34  \w     39.00  65.00   0.50    1.50    --   83.95-125.00-150.00   52
 35  \w     44.00 111.00   0.50    1.50    --   83.95   0.00  90.00  134
 36  \w     81.00 110.00   0.50    1.50    --   83.95 154.00  15.00   58
 37  \w     51.00  78.00   0.50    1.50    --   83.95  15.00 -90.00   54
 38  \w     42.00  67.00   0.50    1.50    --   83.95 -94.00 -60.00   50
 39  \w     42.00  92.00   0.50    1.50    --   83.95-119.00 152.00  100
 40  \w     67.00  94.00   0.50    1.50    --   83.95  15.00 -60.00   54
 41  \w    103.00 130.00   0.50    1.50    --   83.95  15.00-120.00   54
 42  \w     52.00  79.00   0.50    1.50    --   83.95  15.00-120.00   54
 43  \w      2.00  29.00   0.50    1.50    --   -2.00  34.00-144.73   54
 44  \w      6.00  32.00   0.50    1.50    --    2.00  32.00 117.22   52
 45  \w     10.00  37.00   0.50    1.50    --   10.00  30.00 158.13   54
 46  \w     -3.00  22.00   0.50    1.50    --  -10.00  38.00 106.97   50
 47  \w     12.00  39.00   0.50    1.50    --   14.00  29.00  47.11   54
 48  \w    -12.00  14.00   0.50    1.50    --  -18.00  46.00 160.31   52
 49  \w    -11.00  14.00   0.50    1.50    --  -18.00  45.00  28.90   50
 50  \w     15.00  41.00   0.50    1.50    --   18.00  28.00   8.50   52
 51  \w    -41.00 -15.00   0.50    1.50    --  -22.00 -28.00  10.30   52
 52  \w    -44.00 -19.00   0.50    1.50    --  -26.00 -27.00  42.66   50
 53  \w    -44.00 -19.00   0.50    1.50    --  -26.00 -27.00 174.80   50
 54  \w    -48.00 -20.00   0.50    1.50    --  -34.00 -26.00-120.90   56
 55  \w    -56.00 -31.00   0.50    1.50    --  -50.00 -24.00-155.43   50
 56  \w    -56.00 -30.00   0.50    1.50    --  -50.00 -24.00 -76.67   52
 57  \w    -56.00 -30.00   0.50    1.50    --  -50.00 -24.00 -13.83   52
 58  \w    -61.00 -35.00   0.50    1.50    --  -58.00 -23.00 -34.32   52
 59  \w    -77.00 -35.00   0.50    1.50    --  -59.39 125.00  60.00   84
 60  \w    -78.00 -28.00   0.50    1.50    --  -59.39   0.00  30.00  100
 61  \w    -85.00 -18.00   0.50    1.50    --  -59.39   0.00  90.00  134
 62  \w   -100.00 -18.00   0.50    1.50    --  -59.39   0.00-180.00  164
 63  \w     18.00  60.00   0.50    1.50    --   59.71 -94.00-180.00   84
 64  \w     18.00  43.00   0.50    1.50    --   59.71 -94.00   0.00   50
 65  \w     20.00  46.00   0.50    1.50    --   59.71 -94.00-150.00   52
 66  \w     18.00  49.00   0.50    1.50    --   59.71 -94.00  60.00   62
 67  \w    -59.00 -28.00   0.50    1.50    --  -66.50  83.00-126.10   62
 68  \w     41.00  67.00   0.50    1.50    --   66.73  22.00  60.33   52
 69  \w     48.00  84.00   0.50    1.50    --   66.73  21.00-160.32   72
 70  \w     41.00  68.00   0.50    1.50    --   66.73  22.00  85.45   54
 71  \w     41.00  69.00   0.50    1.50    --   66.73  22.00 179.58   56
 72  \w     43.00  71.00   0.50    1.50    --   66.73  22.00 109.34   56
 73  \w     41.00  71.00   0.50    1.50    --   66.73  22.00  28.29   60
 74  \w     42.00  71.00   0.50    1.50    --   66.73  22.00 -17.04   58
 75  \w     44.00  69.00   0.50    1.50    --   70.00  22.00-135.21   50
 76  \w     35.00 100.00   0.50    1.50    --   73.75-125.00 -90.00  130
 77  \w     36.00 102.00   0.50    1.50    --   73.75-125.00   0.00  132
 78  \w     36.00 105.00   0.50    1.50    --   73.75-125.00 120.00  138
 79  \w     35.00  82.00   0.50    1.50    --   74.46-125.00 -60.00   94
 80  \w     44.00 122.00   0.50    1.50    --   79.20  18.00 141.83  156
 81  \w     46.00 114.00   0.50    1.50    --   79.20  21.00   7.28  136
 82  \w     78.00 111.00   0.50    1.50    --   83.95-125.00 -30.00   66
 83  \w     38.00  64.00   0.50    1.50    --   83.95-125.00 -30.00   52
 84  \w     85.00 111.00   0.50    1.50    --   83.95-125.00-180.00   52
 85  \w     39.00  79.00   0.50    1.50    --   83.95-125.00-180.00   80
 86  \w     38.00 111.00   0.50    1.50    --   83.95-125.00  90.00  146
 87  \w     56.00 102.00   0.50    1.50    --   83.95   0.00 -90.00   92
 88  \w     43.00 118.00   0.50    1.50    --   83.95   0.00-150.00  150
 89  \w     38.00 111.00   0.50    1.50    --   83.95-125.00  30.00  146
 90  \w     43.00 122.00   0.50    1.50    --   83.95   0.00 -30.00  158
 91  \w     60.00 117.00   0.50    1.50    --   83.95   0.00  30.00  114
 92  \w     86.00 111.00   0.50    1.50    --   83.95-125.00  60.00   50
 93  \w     86.00 111.00   0.50    1.50    --   83.95-125.00 150.00   50
 94  \w     38.00  64.00   0.50    1.50    --   83.95-125.00 150.00   52
 95  \w     38.00  64.00   0.50    1.50    --   83.95-125.00  60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0567687000
_diffrn_orient_matrix_UB_12      -0.1023991000
_diffrn_orient_matrix_UB_13      0.0115982000
_diffrn_orient_matrix_UB_21      -0.0857348000
_diffrn_orient_matrix_UB_22      0.0069678000
_diffrn_orient_matrix_UB_23      0.0042452000
_diffrn_orient_matrix_UB_31      -0.0104831000
_diffrn_orient_matrix_UB_32      -0.0118895000
_diffrn_orient_matrix_UB_33      -0.0971270000
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33096
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.426
_diffrn_reflns_theta_min         5.138
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.199
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.289
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       needle
_exptl_crystal_F_000             1962
_exptl_crystal_size_max          0.604
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
The structure is almost centrosymmetric and could be refine in the space
 group R-3c, at the expense of larger ellipsoids, especially for O2 and the position 
 corresponding to N3/N4. The model is R3c was then preferred. The Flack parameter refined
 to 0.42(2) which different enough from 0.5 to privilege this twinned model. The space group contains 
 element of the second king so that the inversion twinning is equivalent to an orientation ambiguity.

;
_refine_ls_abs_structure_Flack   0.419(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1612
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0979P)^2^+3.1098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    0.776
_reflns_Friedel_fraction_max     0.725
_reflns_number_gt                1474
_reflns_number_total             1612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_original_cell_volume        4037.95(17)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7716546
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C18 H18 Cr1 N15 O9'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.581(19)
 0.419(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C1(H1), C2(H2), C5(H5), C6(H6)
;
_shelx_res_checksum              55113
_shelx_hkl_checksum              42081
_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 1.467
_oxdiff_exptl_absorpt_empirical_full_min 0.706