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_7716549
_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         'C24 H30 Cr N12, 3(C F3 O3 S)'
_chemical_formula_sum            'C27 H30 Cr F9 N12 O9 S3'
_chemical_formula_weight         985.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-10
_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                90
_cell_angle_beta                 108.113(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6274(3)
_cell_length_b                   19.7662(3)
_cell_length_c                   12.2436(2)
_cell_measurement_reflns_used    17115
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      71.3210
_cell_measurement_theta_min      3.5460
_cell_volume                     3824.58(12)
_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  (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 1.000
_diffrn_measured_fraction_theta_max 0.971
_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    -68.00 -18.00   0.50    1.00    --  -59.38   0.00-150.00  100
  2  \w   -103.00 -24.00   0.50    1.00    --  -59.38 -15.00 -60.00  158
  3  \w   -100.00 -24.00   0.50    1.00    --  -59.38   0.00   0.00  152
  4  \w    -80.00 -21.00   0.50    1.00    --  -59.38   0.00  60.00  118
  5  \w   -101.00 -75.00   0.50    1.00    --  -59.38   0.00-180.00   52
  6  \w    -92.00 -57.00   0.50    1.00    --  -59.38 -15.00-150.00   70
  7  \w     27.00  62.00   0.50    1.00    --   59.54  15.00 150.00   70
  8  \w     21.00  77.00   0.50    1.00    --   59.54-104.00-104.00  112
  9  \w     18.00  43.00   0.50    1.00    --   59.54 -94.00 -60.00   50
 10  \w     39.00  93.00   0.50    1.00    --   59.54-125.00  90.00  108
 11  \w     62.00  93.00   0.50    1.00    --   59.54-125.00-180.00   62
 12  \w     80.00 108.00   0.50    1.00    --   59.54  15.00 150.00   56
 13  \w     35.00  93.00   0.50    1.00    --   59.54-125.00   0.00  116
 14  \w    -55.00 -20.00   0.50    1.00    --  -66.50  57.00  18.91   70
 15  \w    -63.00 -29.00   0.50    1.00    --  -66.50  66.00 -57.70   68
 16  \w    -67.00 -40.00   0.50    1.00    --  -66.50  82.00 -35.18   54
 17  \w     67.00  95.00   0.50    1.00    --   73.61  15.00-120.00   56
 18  \w     71.00 107.00   0.50    1.00    --   73.61-125.00 -30.00   72
 19  \w     35.00  69.00   0.50    1.00    --   73.61-125.00 -30.00   68
 20  \w     85.00 122.00   0.50    1.00    --   73.61  15.00 120.00   74
 21  \w     40.00  65.00   0.50    1.00    --   73.61  15.00 120.00   50
 22  \w     35.00  65.00   0.50    1.00    --   73.61-125.00  30.00   60
 23  \w     55.00  82.00   0.50    1.00    --   73.61-125.00-120.00   54
 24  \w     47.00  74.00   0.50    1.00    --   73.61 -94.00   0.00   54
 25  \w     50.00  77.00   0.50    1.00    --   73.61 -94.00  60.00   54
 26  \w     38.00  66.00   0.50    1.00    --   73.61-125.00  60.00   56
 27  \w     35.00  72.00   0.50    1.00    --   73.61-125.00 -60.00   74
 28  \w     38.00 120.00   0.50    1.00    --   73.61  15.00 -60.00  164
 29  \w     36.00 101.00   0.50    1.00    --   73.61-125.00-180.00  130
 30  \w     34.00  85.00   0.50    1.00    --   73.61 -94.00 -30.00  102
 31  \w     76.00 115.00   0.50    1.00    --   74.34   0.00  30.00   78
 32  \w     34.00  59.00   0.50    1.00    --   74.34   0.00  30.00   50
 33  \w     36.00 104.00   0.50    1.00    --   74.34   0.00 -60.00  136
 34  \w     34.00  87.00   0.50    1.00    --   74.34 -94.00  90.00  106
 35  \w     33.00 116.00   0.50    1.00    --   74.34   0.00-150.00  166
 36  \w     50.00 109.00   0.50    1.00    --   79.11-118.00 -87.96  118
 37  \w     42.00 117.00   0.50    1.00    --   79.11-133.00  86.96  150
 38  \w     86.00 111.00   0.50    1.00    --   79.11-124.00 106.30   50
 39  \w     35.00  60.00   0.50    1.00    --   79.11-124.00 106.30   50
 40  \w     68.00 110.00   0.50    1.00    --   79.11-120.00-148.75   84
 41  \w     85.00 110.00   0.50    1.00    --   79.11-124.00 -14.16   50
 42  \w     35.00  60.00   0.50    1.00    --   79.11-124.00 -14.16   50
 43  \w     32.00  59.00   0.50    1.00    --   79.11-120.00-148.75   54
;
_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      0.0224551000
_diffrn_orient_matrix_UB_12      -0.0448826000
_diffrn_orient_matrix_UB_13      -0.0891551000
_diffrn_orient_matrix_UB_21      -0.0168997000
_diffrn_orient_matrix_UB_22      0.0599591000
_diffrn_orient_matrix_UB_23      -0.0846328000
_diffrn_orient_matrix_UB_31      0.0933233000
_diffrn_orient_matrix_UB_32      0.0216552000
_diffrn_orient_matrix_UB_33      0.0490650000
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.162
_diffrn_reflns_theta_min         3.581
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.015
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0483P)^2^+3.7879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3598
_reflns_number_total             3723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_original_cell_volume        3824.58(13)
_cod_database_code               7716549
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H30 Cr1 F9 N12 O9 S3'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: S2(0.5) F5(0.5) O4(0.5) O5(0.5) O6(0.5) C14(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C8(H8), C9(H9), C10(H10)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              87678
_shelx_hkl_checksum              5926
_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 1.649
_oxdiff_exptl_absorpt_empirical_full_min 0.782