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_7716554
_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         'C16 H20 Cl2 Cr N8, Cl, 3(C H4 O)'
_chemical_formula_sum            'C19 H32 Cl3 Cr N8 O3'
_chemical_formula_weight         578.87
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-27
_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                99.106(2)
_cell_angle_beta                 95.598(2)
_cell_angle_gamma                104.370(2)
_cell_formula_units_Z            2
_cell_length_a                   6.8363(2)
_cell_length_b                   13.7717(3)
_cell_length_c                   14.7817(3)
_cell_measurement_reflns_used    7172
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      72.5010
_cell_measurement_theta_min      3.3810
_cell_volume                     1317.44(6)
_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 2018/2 (Sheldrick, 2018)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.955
_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    -84.00 -58.00   0.50   10.00    --  -57.33   0.00 -30.00   52
  2  \w   -101.00 -75.00   0.50   10.00    --  -57.33 -15.00 150.00   52
  3  \w    -55.00 -19.00   0.50   10.00    --  -57.33   0.00 -30.00   72
  4  \w     22.00  47.00   0.50   10.00    --   60.24 -94.00  30.00   50
  5  \w     27.00  77.00   0.50   10.00    --   60.24  15.00 150.00  100
  6  \w     21.00  66.00   0.50   10.00    --   60.24 -94.00 -60.00   90
  7  \w     22.00  70.00   0.50   10.00    --   60.24 -94.00 -90.00   96
  8  \w     45.00  85.00   0.50   10.00    --   60.24-125.00-180.00   80
  9  \w     40.00  70.00   0.50   10.00    --   60.24 -94.00  60.00   60
 10  \w     26.00  59.00   0.50   10.00    --   60.24 -94.00 -30.00   66
 11  \w     36.00  89.00   0.50   10.00    --   60.24-125.00-120.00  106
 12  \w     47.00 118.00   0.50   10.00    --   74.64  15.00-180.00  142
 13  \w     58.00  84.00   0.50   10.00    --   74.64 -94.00  30.00   52
 14  \w     41.00 119.00   0.50   10.00    --   74.64  15.00  30.00  156
 15  \w     45.00  81.00   0.50   10.00    --   79.80 -94.00-150.00   72
 16  \w     57.00 120.00   0.50   10.00    --   79.80  15.00 120.00  126
 17  \w     43.00  96.00   0.50   10.00    --   79.80-107.00 -16.00  106
 18  \w     51.00 102.00   0.50   10.00    --   79.80-125.00 -60.00  102
 19  \w     40.00  74.00   0.50   10.00    --   79.80   0.00 120.00   68
 20  \w     44.00  69.00   0.50   10.00    --   79.80 -94.00  30.00   50
 21  \w     73.00 105.00   0.50   10.00    --   79.80-125.00 -90.00   64
 22  \w     59.00 108.00   0.50   10.00    --   79.80-125.00  90.00   98
 23  \w     43.00  70.00   0.50   10.00    --   79.80-125.00 -90.00   54
 24  \w     44.00  72.00   0.50   10.00    --   79.80 -94.00 150.00   56
 25  \w     47.00  76.00   0.50   10.00    --   79.80-125.00 120.00   58
 26  \w     61.00 108.00   0.50   10.00    --   79.80-125.00-150.00   94
 27  \w     41.00  90.00   0.50   10.00    --   79.80 -94.00 120.00   98
 28  \w     50.00 124.00   0.50   10.00    --   79.80  15.00 -30.00  148
 29  \w     61.00  87.00   0.50   10.00    --   79.80 -94.00  60.00   52
 30  \w     46.00  88.00   0.50   10.00    --   79.80 -94.00   0.00   84
 31  \w     40.00  80.00   0.50   10.00    --   79.80 -94.00 -60.00   80
 32  \w     83.00 108.00   0.50   10.00    --   79.80-125.00 120.00   50
 33  \w    104.00 131.00   0.50   10.00    --   83.50  18.00-114.25   54
 34  \w     53.00  83.00   0.50   10.00    --   83.50  18.00-114.25   60
 35  \w     49.00 127.00   0.50   10.00    --   83.50  17.00-178.39  156
 36  \w     60.00 106.00   0.50   10.00    --   83.50  16.00  63.19   92
 37  \w     98.00 123.00   0.50   10.00    --   83.50 152.00 -66.90   50
 38  \w     97.00 122.00   0.50   10.00    --   83.50-139.00  32.80   50
 39  \w     44.00  74.00   0.50   10.00    --   83.50-139.00  32.80   60
;
_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      -0.0077072000
_diffrn_orient_matrix_UB_12      -0.0800474000
_diffrn_orient_matrix_UB_13      -0.0867636000
_diffrn_orient_matrix_UB_21      0.0508045000
_diffrn_orient_matrix_UB_22      0.0854887000
_diffrn_orient_matrix_UB_23      -0.0566361000
_diffrn_orient_matrix_UB_31      0.2293593000
_diffrn_orient_matrix_UB_32      0.0107053000
_diffrn_orient_matrix_UB_33      0.0252646000
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17103
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.776
_diffrn_reflns_theta_min         3.059
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.686
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.531
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       needle
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0704
_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^)+(0.1191P)^2^+1.3207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4337
_reflns_number_total             5256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_database_code               7716554
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H32 Cl3 Cr N8 O3'
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.334
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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, All O(H) groups, All O(H,H) groups
2. Others
 Sof(H3BB)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(H19C)=1-FVAR(1)
 Sof(H3AA)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C9(H9), C10(H10), C14(H14), C15(H15)
3.b Tetrahedral OH refined with riding coordinates:
 O3(H3BB), O3(H3AA)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19B(H19A,H19B,H19C), C19A(H19D,H19E,
 H19F)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2A)
;
_shelx_res_checksum              2802
_shelx_hkl_checksum              9951
_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 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.614