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_7716547
_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 H15 Cr1 N12, 10[CH3OH]'
_chemical_formula_sum            'C28 H55 Cr N12 O10'
_chemical_formula_weight         771.84
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-11-07
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.8046(3)
_cell_length_b                   17.8046(3)
_cell_length_c                   22.4548(4)
_cell_measurement_reflns_used    10506
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      72.6790
_cell_measurement_theta_min      3.4550
_cell_volume                     6164.59(18)
_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      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_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    -89.00 -63.00   0.50   10.00    --  -57.32   0.00 -90.00   52
  2  \w    -61.00 -25.00   0.50   10.00    --  -57.32   0.00  30.00   72
  3  \w    -55.00 -20.00   0.50   10.00    --  -57.32   0.00 -90.00   70
  4  \w    -95.00 -68.00   0.50   10.00    --  -57.32   0.00  30.00   54
  5  \w    -50.00 -24.00   0.50   10.00    --  -57.32 -15.00  30.00   52
  6  \w     21.00  53.00   0.50   10.00    --   60.32 -94.00-180.00   64
  7  \w     26.00  59.00   0.50   10.00    --   60.32 -94.00-120.00   66
  8  \w     21.00  57.00   0.50   10.00    --   60.32 -94.00   0.00   72
  9  \w     22.00  50.00   0.50   10.00    --   60.32 -94.00  30.00   56
 10  \w     22.00  48.00   0.50   10.00    --   60.32 -94.00 -30.00   52
 11  \w     91.00 117.00   0.50   10.00    --   74.75  15.00 150.00   52
 12  \w     43.00  68.00   0.50   10.00    --   74.75  15.00 150.00   50
 13  \w     78.00 105.00   0.50   10.00    --   74.75-125.00 -60.00   54
 14  \w     41.00  74.00   0.50   10.00    --   74.75-125.00 -60.00   66
 15  \w     50.00  76.00   0.50   10.00    --   74.75 -94.00 -30.00   52
 16  \w     95.00 122.00   0.50   10.00    --   74.75  15.00 120.00   54
 17  \w     47.00  73.00   0.50   10.00    --   74.75  15.00 120.00   52
 18  \w     52.00  81.00   0.50   10.00    --   77.03 -94.00 -90.00   58
 19  \w     62.00 109.00   0.50   10.00    --   77.03   0.00   0.00   94
 20  \w     36.00  86.00   0.50   10.00    --   77.03-125.00  60.00  100
 21  \w     67.00 106.00   0.50   10.00    --   77.03-125.00 -90.00   78
 22  \w     77.00 117.00   0.50   10.00    --   77.03   0.00  90.00   80
 23  \w     45.00  71.00   0.50   10.00    --   77.03   0.00  90.00   52
 24  \w     37.00  62.00   0.50   10.00    --   77.03 -94.00 150.00   50
 25  \w     49.00  76.00   0.50   10.00    --   77.03 -94.00-180.00   54
 26  \w     73.00 104.00   0.50   10.00    --   77.03   0.00-120.00   62
 27  \w     38.00  66.00   0.50   10.00    --   77.03   0.00-120.00   56
 28  \w     79.00 105.00   0.50   10.00    --   77.03   0.00 -90.00   52
 29  \w     76.00 102.00   0.50   10.00    --   77.03-125.00 120.00   52
 30  \w     39.00  71.00   0.50   10.00    --   77.03 -94.00-150.00   64
 31  \w     99.00 125.00   0.50   10.00    --   81.25  19.00 -66.16   52
 32  \w     57.00 118.00   0.50   10.00    --   81.25  19.00-132.77  122
 33  \w     52.00  80.00   0.50   10.00    --   81.25  19.00 -66.16   56
 34  \w     44.00  85.00   0.50   10.00    --   81.25-102.00  61.66   82
 35  \w     94.00 120.00   0.50   10.00    --   81.25-141.00  15.67   52
 36  \w     51.00  81.00   0.50   10.00    --   81.25-141.00  15.67   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      0.0595126000
_diffrn_orient_matrix_UB_12      -0.0113583000
_diffrn_orient_matrix_UB_13      0.0444543000
_diffrn_orient_matrix_UB_21      0.0044684000
_diffrn_orient_matrix_UB_22      -0.0658570000
_diffrn_orient_matrix_UB_23      -0.0423298000
_diffrn_orient_matrix_UB_31      0.0800060000
_diffrn_orient_matrix_UB_32      0.0742780000
_diffrn_orient_matrix_UB_33      -0.0306418000
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19714
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.981
_diffrn_reflns_theta_min         3.477
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.743
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       prism
_exptl_crystal_F_000             2466
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1783P)^2^+7.2680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2422
_refine_ls_wR_factor_ref         0.2440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2620
_reflns_number_total             2747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_original_cell_volume        6164.6(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7716547
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28CrH55N12O10
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.661
_reflns_odcompleteness_completeness 99.82
_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
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2), C5(H5), C6(H6)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1103 electrons were 
found in a volume of 3805\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
10[CH3OH] per Formula Unit 
which account for 1080 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15369
_shelx_hkl_checksum              36163
_shelx_fab_checksum              53553
_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 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.886