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_7716548
_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, C H4 O'
_chemical_formula_sum            'C43 H38 Cr N12 O P'
_chemical_formula_weight         821.82
_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   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                 99.0717(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.24157(6)
_cell_length_b                   24.44046(17)
_cell_length_c                   20.22184(13)
_cell_measurement_reflns_used    23772
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      72.6200
_cell_measurement_theta_min      2.8400
_cell_volume                     4022.29(5)
_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      100.00(13)
_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     77.00 116.00   0.50    0.50    --   77.03  15.00   0.00   78
  2  \w     61.00 110.00   0.50    0.50    --   77.03  15.00  60.00   98
  3  \w     64.00  97.00   0.50    0.50    --   77.03  15.00 120.00   66
  4  \w     53.00 117.00   0.50    0.50    --   77.03   0.00 -30.00  128
  5  \w     87.00 113.00   0.50    0.50    --   75.05  15.00 -90.00   52
  6  \w     96.00 121.00   0.50    0.50    --   77.03  15.00-120.00   50
  7  \w     47.00 126.00   0.50    0.50    --   81.25  11.00-145.13  158
  8  \w   -101.00 -75.00   0.50    0.50    --  -57.32 -15.00  30.00   52
  9  \w    -70.00 -45.00   0.50    0.50    --  -57.32 125.00 -30.00   50
 10  \w    -85.00 -37.00   0.50    0.50    --  -57.32 125.00  30.00   96
 11  \w    -63.00 -37.00   0.50    0.50    --  -57.32 -15.00  30.00   52
 12  \w    -86.00 -19.00   0.50    0.50    --  -57.32   0.00-120.00  134
 13  \w    -53.00 -25.00   0.50    0.50    --  -57.32 -15.00-180.00   56
 14  \w     40.00  80.00   0.50    0.50    --   60.51-125.00   0.00   80
 15  \w     35.00  98.00   0.50    0.50    --   77.03-125.00 150.00  126
 16  \w     51.00  76.00   0.50    0.50    --   77.03-125.00  30.00   50
 17  \w     43.00  84.00   0.50    0.50    --   77.03 -94.00   0.00   82
 18  \w     35.00  67.00   0.50    0.50    --   77.03-125.00 -30.00   64
 19  \w     46.00  86.00   0.50    0.50    --   77.03 -94.00  60.00   80
 20  \w     53.00 104.00   0.50    0.50    --   81.25-111.00 -32.51  102
 21  \w     21.00  47.00   0.50    0.50    --   60.51 -94.00  60.00   52
 22  \w     21.00  53.00   0.50    0.50    --   60.51 -94.00-120.00   64
 23  \w     58.00 108.00   0.50    0.50    --   77.03-125.00-180.00  100
 24  \w     38.00  81.00   0.50    0.50    --   77.03 -94.00-180.00   86
 25  \w     22.00  71.00   0.50    0.50    --   60.51 -94.00-180.00   98
 26  \w     54.00  86.00   0.50    0.50    --   77.03 -94.00-150.00   64
 27  \w     37.00  62.00   0.50    0.50    --   77.03 -94.00-120.00   50
 28  \w     35.00  61.00   0.50    0.50    --   75.05 -94.00 -30.00   52
 29  \w     50.00  80.00   0.50    0.50    --   77.03 -94.00  30.00   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      -0.0811290000
_diffrn_orient_matrix_UB_12      -0.0413822000
_diffrn_orient_matrix_UB_13      -0.0525237000
_diffrn_orient_matrix_UB_21      -0.1678193000
_diffrn_orient_matrix_UB_22      0.0109827000
_diffrn_orient_matrix_UB_23      0.0218254000
_diffrn_orient_matrix_UB_31      -0.0328236000
_diffrn_orient_matrix_UB_32      0.0462688000
_diffrn_orient_matrix_UB_33      -0.0521363000
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38665
_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         74.667
_diffrn_reflns_theta_min         2.858
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.128
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.643
_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    1.357
_exptl_crystal_description       prism
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0607P)^2^+3.7181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7637
_reflns_number_total             7991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_database_code               7716548
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43 H38 Cr N12 O P'
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.574
_reflns_odcompleteness_completeness 99.85
_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 C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(H1B)=Sof(C43B)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(1)
 Sof(H1A)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 N8(H8), N12(H12), C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8A), C11(H11),
 C12(H12A), 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)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1B), O1(H1A)
3.c Idealised Me refined as rotating group:
 C43B(H43A,H43B,H43C), C43A(H43D,H43E,H43F)
;
_shelx_res_checksum              89693
_shelx_hkl_checksum              81310
_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 1.161
_oxdiff_exptl_absorpt_empirical_full_min 0.829