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_7716550
_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 H22 Cr N8, 3(C F3 O3 S), 0.25(H2 O)'
_chemical_formula_sum            'C33 H22.5 Cr F9 N8 O9.25 S3'
_chemical_formula_weight         998.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-30
_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                 93.9394(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8506(3)
_cell_length_b                   17.2070(3)
_cell_length_c                   12.78022(17)
_cell_measurement_reflns_used    14003
_cell_measurement_temperature    109.99(10)
_cell_measurement_theta_max      73.6040
_cell_measurement_theta_min      2.4860
_cell_volume                     3916.24(11)
_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      109.99(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 0.970
_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    -90.00 -56.00   0.50    8.00    --  -57.33   0.00-120.00   68
  2  \w    -97.00 -43.00   0.50    8.00    --  -57.33   0.00 -30.00  108
  3  \w    -68.00 -35.00   0.50    8.00    --  -57.33 125.00 -90.00   66
  4  \w    -87.00 -35.00   0.50    8.00    --  -57.33   0.00  90.00  104
  5  \w     28.00 100.00   0.50    8.00    --   60.24  15.00 150.00  144
  6  \w     31.00  65.00   0.50    8.00    --   60.24 -94.00-120.00   68
  7  \w     22.00  58.00   0.50    8.00    --   60.24 -94.00-180.00   72
  8  \w     35.00  69.00   0.50    8.00    --   60.24-125.00  60.00   68
  9  \w     37.00  66.00   0.50    8.00    --   74.64 -94.00 120.00   58
 10  \w     51.00  88.00   0.50    8.00    --   79.80-125.00-180.00   74
 11  \w     49.00 100.00   0.50    8.00    --   79.80-125.00-150.00  102
 12  \w     44.00  80.00   0.50    8.00    --   79.80 -94.00-150.00   72
 13  \w     46.00 127.00   0.50    8.00    --   79.80  15.00 -90.00  162
 14  \w     44.00  70.00   0.50    8.00    --   79.80 -94.00-120.00   52
 15  \w     42.00  85.00   0.50    8.00    --   79.80 -94.00 -60.00   86
 16  \w     36.00  90.00   0.50    8.00    --   79.80-125.00  90.00  108
 17  \w     64.00  91.00   0.50    8.00    --   79.80  15.00 -30.00   54
 18  \w     50.00 102.00   0.50    8.00    --   79.80-125.00  60.00  104
 19  \w     48.00  73.00   0.50    8.00    --   79.80 -94.00-180.00   50
 20  \w     46.00 127.00   0.50    8.00    --   79.80  15.00  60.00  162
 21  \w     59.00 106.00   0.50    8.00    --   79.80-125.00 150.00   94
 22  \w     40.00  66.00   0.50    8.00    --   79.80 -94.00  90.00   52
 23  \w     43.00  68.00   0.50    8.00    --   83.50 -63.00 -78.31   50
 24  \w     51.00 113.00   0.50    8.00    --   83.50  16.00 156.42  124
;
_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      0.0109494000
_diffrn_orient_matrix_UB_12      0.0622123000
_diffrn_orient_matrix_UB_13      -0.0844733000
_diffrn_orient_matrix_UB_21      -0.0850168000
_diffrn_orient_matrix_UB_22      -0.0008309000
_diffrn_orient_matrix_UB_23      -0.0303366000
_diffrn_orient_matrix_UB_31      -0.0115732000
_diffrn_orient_matrix_UB_32      0.0643498000
_diffrn_orient_matrix_UB_33      0.0809568000
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.422
_diffrn_reflns_theta_min         2.481
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.889
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.470
_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    1.693
_exptl_crystal_description       plate
_exptl_crystal_F_000             2014
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         7876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0720
_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^)+(0.1006P)^2^+9.0352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.1952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6745
_reflns_number_total             7876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_original_cell_volume        3916.23(10)
_cod_original_formula_sum        'C33 H22.50 Cr F9 N8 O9.25 S3'
_cod_database_code               7716550
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C33 H22.5 Cr F9 N8 O9.3 S3'
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.331
_reflns_odcompleteness_completeness 99.90
_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. Uiso/Uaniso restraints and constraints
Uiso(F11) = Uiso(F8)
Uiso(F12) = Uiso(F7)
Uiso(F5A) = Uiso(F5B)
Uiso(C32A) = Uiso(C32B)
Uiso(F6A) = Uiso(F6B)
Uiso(F4A) = Uiso(F4B)
Uiso(C33A) = Uiso(C33B)
3. Others
 Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(C32B)=1-FVAR(1)
 Sof(C32A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
 Fixed Sof: S3(0.75) S4(0.25) F7(0.75) F8(0.75) F9(0.25) F10(0.75) O9(0.75)
 O10(0.25) C33B(0.25) O11(0.25) H11A(0.25) H11B(0.25) F11(0.25) F12(0.25)
 C33A(0.75)
4.a Free rotating group:
 O11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 N7(H7), N8(H8), C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8A), 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              12300
_shelx_hkl_checksum              82123
_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 1.723
_oxdiff_exptl_absorpt_empirical_full_min 0.493