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_7716552
_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 H20 Cr N8, C F3 O3 S, 1.5(C H4 O)'
_chemical_formula_sum            'C32.5 H26 Cr F3 N8 O4.5 S'
_chemical_formula_weight         741.67
_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             2024-01-17
_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                107.378(3)
_cell_angle_beta                 98.544(3)
_cell_angle_gamma                96.353(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7735(4)
_cell_length_b                   11.8329(4)
_cell_length_c                   12.6821(4)
_cell_measurement_reflns_used    8352
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.6220
_cell_measurement_theta_min      3.8270
_cell_volume                     1644.79(10)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_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    -79.00 -53.00   1.00    1.00    --  -41.71 125.00 120.00   26
  2  \w    -64.00  26.00   1.00    1.00    --  -41.71  57.00  60.00   90
  3  \w    -62.00  30.00   1.00    1.00    --  -41.71  38.00-150.00   92
  4  \w   -113.00 -19.00   1.00    1.00    --  -41.71 -57.00 -90.00   94
  5  \w     28.00 126.00   1.00    4.00    --  100.00 -45.00 150.00   98
  6  \w     37.00  79.00   1.00    4.00    --  100.00-125.00-150.00   42
  7  \w     38.00  98.00   1.00    4.00    --  100.00 -77.00  30.00   60
  8  \w     75.00 107.00   1.00    4.00    --  100.00 -94.00 -30.00   32
  9  \w     59.00 129.00   1.00    4.00    --  100.00 -61.00-120.00   70
 10  \w     28.00  71.00   1.00    4.00    --  100.00 -45.00  60.00   43
 11  \w    110.00 162.00   1.00    4.00    --  100.00  77.00-180.00   52
 12  \w     49.00  75.00   1.00    4.00    --  100.00 -30.00 -60.00   26
 13  \w    100.00 127.00   1.00    4.00    --  100.00 -30.00 -60.00   27
 14  \w     23.00 106.00   1.00    4.00    --  100.00 -94.00 150.00   83
 15  \w     84.00 111.00   1.00    4.00    --  100.00-125.00  90.00   27
 16  \w     61.00 107.00   1.00    4.00    --  100.00 -94.00-120.00   46
 17  \w     75.00 126.00   1.00    4.00    --  100.00  45.00 -30.00   51
 18  \w     65.00 107.00   1.00    4.00    --  100.00 -94.00 120.00   42
 19  \w     16.00 167.00   1.00    4.00    --  100.00   0.00-180.00  151
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0642480000
_diffrn_orient_matrix_UB_12      -0.0121537000
_diffrn_orient_matrix_UB_13      0.0943806000
_diffrn_orient_matrix_UB_21      -0.0871983000
_diffrn_orient_matrix_UB_22      0.0774212000
_diffrn_orient_matrix_UB_23      -0.0326658000
_diffrn_orient_matrix_UB_31      -0.0791360000
_diffrn_orient_matrix_UB_32      -0.1139512000
_diffrn_orient_matrix_UB_33      -0.0827250000
_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  0.0311
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12239
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.623
_diffrn_reflns_theta_min         3.721
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.068
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.504
_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    1.498
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0563
_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^)+(0.1208P)^2^+1.2810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5675
_reflns_number_total             6162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_original_cell_volume        1644.79(9)
_cod_original_formula_sum        'C32.50 H26 Cr F3 N8 O4.50 S'
_cod_database_code               7716552
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32.5 H26 Cr F3 N8 O4.5 S'
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.395
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_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
2. Others
 Fixed Sof: O4S(0.5) H4S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C17(H17), C22(H22), C9(H9), C20(H20), C15(H15), C3(H3),
 C5(H5), C30(H30), C29(H29), C8(H8), C1(H1), C21(H21), C25(H25), C14(H14),
 C18(H18), C26(H26), C10(H10), C13(H13)
3.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C3S(H3SA,H3SB,H3SC)
3.c Idealised tetrahedral OH refined as rotating group:
 O2S(H2S), O4S(H4S)
;
_shelx_res_checksum              95281
_shelx_hkl_checksum              28646
_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 3.201
_oxdiff_exptl_absorpt_empirical_full_min 0.429