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_7716551
_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         'C30 H21 Cr N8, 2(C F3 O3 S), 0.5(H2 O)'
_chemical_formula_sum            'C32 H22 Cr F6 N8 O6.5 S2'
_chemical_formula_weight         852.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-01-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                79.588(3)
_cell_angle_beta                 68.575(4)
_cell_angle_gamma                68.511(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6371(4)
_cell_length_b                   13.6703(5)
_cell_length_c                   14.0130(6)
_cell_measurement_reflns_used    17475
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.9710
_cell_measurement_theta_min      3.3780
_cell_volume                     1762.41(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/3 (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 0.962
_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    5.00    --    0.00  32.00 175.67   52
  2  \w      5.00  30.00   0.50    5.00    --    0.00  31.00 -70.16   50
  3  \w      7.00  37.00   0.50    5.00    --    4.00  30.00  65.37   60
  4  \w     13.00  39.00   0.50    5.00    --    8.00  29.00-153.62   52
  5  \w     -1.00  26.00   0.50    5.00    --   -8.00  36.00 -12.30   54
  6  \w      9.00  35.00   0.50    5.00    --    8.00  30.00 147.68   52
  7  \w     -1.00  27.00   0.50    5.00    --   -8.00  35.00 -96.16   56
  8  \w     10.00  37.00   0.50    5.00    --    8.00  30.00 104.53   54
  9  \w    -15.00  10.00   0.50    5.00    --  -24.00  49.00 -51.83   50
 10  \w     18.00  51.00   0.50    5.00    --   24.00  25.00 -50.35   66
 11  \w    -15.00  11.00   0.50    5.00    --  -24.00  49.00-143.15   52
 12  \w     20.00  47.00   0.50    5.00    --   28.00  26.00-121.75   54
 13  \w    -25.00   1.00   0.50    5.00    --  -36.00  62.00 125.45   52
 14  \w    -51.00 -26.00   0.50    5.00    --  -36.00 -25.00   4.28   50
 15  \w    -32.00   3.00   0.50    5.00    --  -40.00  60.00  50.90   70
 16  \w    -55.00 -29.00   0.50    5.00    --  -44.00 -24.00 -46.59   52
 17  \w    -55.00 -30.00   0.50    5.00    --  -44.00 -24.00-109.28   50
 18  \w    -56.00 -31.00   0.50    5.00    --  -44.00 -24.00 115.67   50
 19  \w    -55.00 -29.00   0.50    5.00    --  -44.00 -24.00  33.14   52
 20  \w    -61.00 -35.00   0.50    5.00    --  -52.00 -23.00-177.54   52
 21  \w    -62.00 -37.00   0.50    5.00    --  -52.00 -23.00-149.76   50
 22  \w    -61.00 -36.00   0.50    5.00    --  -52.00 -23.00-125.75   50
 23  \w    -55.00 -29.00   0.50    5.00    --  -57.24   0.00  90.00   52
 24  \w    -87.00 -21.00   0.50    5.00    --  -57.24   0.00  30.00  132
 25  \w    -96.00 -36.00   0.50    5.00    --  -57.24   0.00 -30.00  120
 26  \w    -97.00 -45.00   0.50    5.00    --  -57.24   0.00 -90.00  104
 27  \w    -82.00 -19.00   0.50    5.00    --  -57.24   0.00-180.00  126
 28  \w    -82.00 -56.00   0.50    5.00    --  -57.24   0.00  90.00   52
 29  \w     24.00  64.00   0.50    5.00    --   60.11 -94.00 120.00   80
 30  \w     23.00  65.00   0.50    5.00    --   60.11 -94.00-150.00   84
 31  \w     21.00  64.00   0.50    5.00    --   60.11 -94.00-180.00   86
 32  \w     26.00  66.00   0.50    5.00    --   60.11 -94.00   0.00   80
 33  \w     22.00  62.00   0.50    5.00    --   60.11 -94.00  60.00   80
 34  \w     22.00  70.00   0.50    5.00    --   60.11 -94.00 -90.00   96
 35  \w     21.00  68.00   0.50    5.00    --   60.11 -94.00 -30.00   94
 36  \w    -70.00 -44.00   0.50    5.00    --  -64.50 -22.00  94.74   52
 37  \w    -70.00 -45.00   0.50    5.00    --  -64.50 -22.00  -1.68   50
 38  \w    -71.00 -45.00   0.50    5.00    --  -64.50 -22.00-133.80   52
 39  \w    -71.00 -46.00   0.50    5.00    --  -64.50 -22.00  23.79   50
 40  \w     47.00  92.00   0.50    5.00    --   67.34  21.00 126.44   90
 41  \w     76.00 103.00   0.50    5.00    --   67.34  21.00-148.28   54
 42  \w     44.00  73.00   0.50    5.00    --   67.34  21.00-148.28   58
 43  \w     51.00  85.00   0.50    5.00    --   67.34  21.00  71.44   68
 44  \w     47.00  84.00   0.50    5.00    --   67.34  21.00 -46.62   74
 45  \w     78.00 104.00   0.50    5.00    --   74.58-125.00 120.00   52
 46  \w     78.00 103.00   0.50    5.00    --   74.58-125.00 -90.00   50
 47  \w     36.00  61.00   0.50    5.00    --   74.58-125.00 -90.00   50
 48  \w     35.00  65.00   0.50    5.00    --   74.58-125.00 120.00   60
 49  \w     53.00  91.00   0.50    5.00    --   76.00  21.00 -79.41   76
 50  \w     36.00 109.00   0.50    5.00    --   79.88-125.00-180.00  146
 51  \w     72.00 108.00   0.50    5.00    --   79.88-125.00-120.00   72
 52  \w     55.00 114.00   0.50    5.00    --   79.88   0.00  90.00  118
 53  \w     40.00  69.00   0.50    5.00    --   79.88-125.00-120.00   58
 54  \w     38.00  65.00   0.50    5.00    --   79.88-125.00  30.00   54
 55  \w     38.00 108.00   0.50    5.00    --   79.88-125.00 150.00  140
 56  \w     36.00  94.00   0.50    5.00    --   79.88-125.00  60.00  116
 57  \w     38.00  90.00   0.50    5.00    --   79.88-125.00-150.00  104
 58  \w     40.00  96.00   0.50    5.00    --   79.88-125.00 120.00  112
 59  \w     38.00  98.00   0.50    5.00    --   79.88-125.00 -30.00  120
 60  \w     36.00  76.00   0.50    5.00    --   79.88-125.00   0.00   80
 61  \w     42.00 112.00   0.50    5.00    --   79.88   0.00 -30.00  140
 62  \w     41.00 116.00   0.50    5.00    --   79.88   0.00-120.00  150
 63  \w     38.00 108.00   0.50    5.00    --   79.88-125.00  90.00  140
 64  \w     39.00 108.00   0.50    5.00    --   79.88-125.00 -60.00  138
 65  \w     54.00 116.00   0.50    5.00    --   79.88   0.00  30.00  124
 66  \w     43.00  92.00   0.50    5.00    --   79.88-125.00 -90.00   98
 67  \w     54.00 117.00   0.50    5.00    --   79.88   0.00 150.00  126
 68  \w    102.00 127.00   0.50    5.00    --   80.00  20.00-124.63   50
 69  \w     51.00  87.00   0.50    5.00    --   80.00  20.00-124.63   72
 70  \w     41.00  66.00   0.50    5.00    --   83.50-131.00  21.12   50
 71  \w     48.00 124.00   0.50    5.00    --   83.50  19.00 -83.10  152
 72  \w     50.00 109.00   0.50    5.00    --   83.50  17.00  -6.25  118
 73  \w     52.00 113.00   0.50    5.00    --   83.50  17.00 177.64  122
 74  \w     48.00 108.00   0.50    5.00    --   83.50  19.00  53.57  120
 75  \w     48.00 112.00   0.50    5.00    --   83.50  19.00 114.71  128
 76  \w     69.00 116.00   0.50    5.00    --   83.50-131.00  21.12   94
;
_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      -0.0483470000
_diffrn_orient_matrix_UB_12      -0.0182893000
_diffrn_orient_matrix_UB_13      -0.0844537000
_diffrn_orient_matrix_UB_21      0.1032168000
_diffrn_orient_matrix_UB_22      -0.1141856000
_diffrn_orient_matrix_UB_23      -0.0061271000
_diffrn_orient_matrix_UB_31      -0.1188783000
_diffrn_orient_matrix_UB_32      -0.0365880000
_diffrn_orient_matrix_UB_33      0.0825738000
_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  0.0623
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.272
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.594
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         7102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0872P)^2^+1.2795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5922
_reflns_number_total             7102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_original_cell_volume        1762.42(13)
_cod_original_formula_sum        'C32 H22 Cr F6 N8 O6.50 S2'
_cod_database_code               7716551
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H22 Cr F6 N8 O6.5 S2'
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.527
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(C32B)=Sof(F6B)=Sof(S2B)=Sof(O6B)=1-FVAR(1)
 Sof(C32A)=Sof(F6A)=Sof(S2A)=Sof(O6A)=FVAR(1)
 Fixed Sof: O8(0.5) H8A(0.5) H8B(0.5)
3.a Free rotating group:
 O8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 N7(H7), C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C25(H25), C26(H26), C29(H29), C30(H30)
;
_shelx_res_checksum              55258
_shelx_hkl_checksum              70087
_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 2.108
_oxdiff_exptl_absorpt_empirical_full_min 0.207