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_7716553
_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 H14 Cr N12, C24 H20 P'
_chemical_formula_sum            'C42 H34 Cr N12 P'
_chemical_formula_weight         789.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-09
_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                 99.692(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.11093(16)
_cell_length_b                   25.0497(6)
_cell_length_c                   19.6595(6)
_cell_measurement_reflns_used    11915
_cell_measurement_temperature    286(6)
_cell_measurement_theta_max      68.6280
_cell_measurement_theta_min      2.8690
_cell_volume                     3937.33(17)
_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      air
_diffrn_ambient_temperature      286(6)
_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 0.961
_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 -18.00   0.50    5.00    --  -57.32   0.00-150.00  132
  2  \w    -91.00 -25.00   0.50    5.00    --  -57.32   0.00 150.00  132
  3  \w    -86.00 -45.00   0.50    5.00    --  -57.32 125.00  60.00   82
  4  \w    -61.00 -35.00   0.50    5.00    --  -57.32 125.00 150.00   52
  5  \w     22.00  70.00   0.50    5.00    --   60.32 -94.00-180.00   96
  6  \w     30.00  70.00   0.50    5.00    --   60.32 -94.00   0.00   80
  7  \w     22.00  47.00   0.50    5.00    --   60.32 -91.00 -51.00   50
  8  \w     25.00  65.00   0.50    5.00    --   60.32 -94.00  60.00   80
  9  \w     37.00  70.00   0.50    5.00    --   60.32 -94.00-120.00   66
 10  \w     35.00  63.00   0.50    5.00    --   74.75 -94.00 -90.00   56
 11  \w     39.00  64.00   0.50    5.00    --   77.03   0.00  60.00   50
 12  \w     46.00  72.00   0.50    5.00    --   77.03 -94.00   0.00   52
 13  \w     50.00 107.00   0.50    5.00    --   77.03-125.00 150.00  114
 14  \w     68.00 109.00   0.50    5.00    --   77.03   0.00  60.00   82
 15  \w     66.00 121.00   0.50    5.00    --   77.03  15.00 120.00  110
 16  \w     37.00  76.00   0.50    5.00    --   77.03 -94.00  30.00   78
 17  \w     76.00 107.00   0.50    5.00    --   77.03  15.00 -30.00   62
 18  \w     72.00 119.00   0.50    5.00    --   77.03  15.00-180.00   94
 19  \w     60.00  87.00   0.50    5.00    --   77.03 -94.00 -90.00   54
 20  \w     65.00 106.00   0.50    5.00    --   77.03-125.00-180.00   82
 21  \w     49.00 123.00   0.50    5.00    --   77.03  15.00 -90.00  148
 22  \w     38.00  71.00   0.50    5.00    --   77.03 -94.00  90.00   66
 23  \w     47.00  72.00   0.50    5.00    --   77.03 -94.00-180.00   50
 24  \w     79.00 105.00   0.50    5.00    --   77.03-125.00 120.00   52
 25  \w     49.00  75.00   0.50    5.00    --   77.03-125.00 -90.00   52
 26  \w     83.00 108.00   0.50    5.00    --   77.03-125.00 -90.00   50
 27  \w     60.00 122.00   0.50    5.00    --   77.03  15.00  60.00  124
 28  \w     36.00  61.00   0.50    5.00    --   77.03-125.00-150.00   50
 29  \w     57.00  83.00   0.50    5.00    --   77.03-125.00-120.00   52
 30  \w     79.00 104.00   0.50    5.00    --   77.03-125.00 -60.00   50
 31  \w     79.00 106.00   0.50    5.00    --   81.25-119.00 -17.18   54
 32  \w     37.00  76.00   0.50    5.00    --   81.25-119.00 -17.18   78
;
_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      -0.0668850000
_diffrn_orient_matrix_UB_12      0.0563408000
_diffrn_orient_matrix_UB_13      0.0113033000
_diffrn_orient_matrix_UB_21      -0.0672072000
_diffrn_orient_matrix_UB_22      0.0046620000
_diffrn_orient_matrix_UB_23      -0.0778296000
_diffrn_orient_matrix_UB_31      -0.1677624000
_diffrn_orient_matrix_UB_32      -0.0243020000
_diffrn_orient_matrix_UB_33      0.0113175000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37800
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.609
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.155
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.773
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       prism
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0358P)^2^+3.8191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6680
_reflns_number_total             7738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_database_code               7716553
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H34 Cr N12 P'
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.703
_reflns_odcompleteness_completeness 99.35
_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), N6(H6), C1(H1), C2(H2), C5(H5), C6(H6A), C7(H7), C8(H8), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42)
;
_shelx_res_checksum              56462
_shelx_hkl_checksum              22012
_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 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.661