Imidazo[1,5]carbachlorin as a hybrid ligand.
Szydełko, Kinga; Koniarz, Sebastian; Białek, Michał J; Chmielewski, Piotr J.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16461–16474; doi:10.1039/d4dt03034f

data_7719678
_publ_section_title
;
 Imidazo[1,5]carbachlorin as a hybrid ligand.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16461
_journal_page_last               16474
_journal_paper_doi               10.1039/d4dt03034f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C50 H36 Ag0.94 Au0.9 Cl0.84 N5, 0.5[C6H14], 1[CH2Cl2]'
_chemical_formula_sum            'C54 H45 Ag0.94 Au0.9 Cl2.84 N5'
_chemical_formula_weight         1143.29
_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
_audit_creation_date             2025-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-09 deposited with the CCDC.	2025-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7667(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4860(2)
_cell_length_b                   9.15880(12)
_cell_length_c                   30.2897(4)
_cell_measurement_reflns_used    31615
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.5400
_cell_measurement_theta_min      2.8940
_cell_volume                     4568.17(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.123a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.123a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(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 0.999
_diffrn_measured_fraction_theta_max 0.986
_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     69.00  94.00   0.50    0.05    --   80.75  23.00 122.26   50
  2  \w     88.00 117.00   0.50    0.05    --   80.75  31.00 121.12   58
  3  \w     86.00 122.00   0.50    0.05    --   80.75  24.00   9.95   72
  4  \w     60.00  99.00   0.50    0.05    --   80.75  20.00 -18.17   78
  5  \w     88.00 118.00   0.50    0.05    --   80.75  31.00 -29.20   60
  6  \w     81.00 124.00   0.50    0.05    --   80.75  20.00 -45.40   86
  7  \w     66.00  96.00   0.50    0.05    --   80.75  22.00 -88.46   60
  8  \w    101.00 126.00   0.50    0.05    --   80.75  22.00-148.33   50
  9  \w     47.00  74.00   0.50    0.05    --   80.75   8.00-136.03   54
 10  \w     83.00 115.00   0.50    0.05    --   80.75   8.00-136.03   64
 11  \w     78.00 116.00   0.50    0.05    --   80.75  19.00 -59.94   76
 12  \w     47.00  96.00   0.50    0.05    --   80.75   4.00 -39.99   98
 13  \w     45.00  77.00   0.50    0.05    --   80.75   4.00  52.38   64
 14  \w     60.00 116.00   0.50    0.05    --   80.75   4.00  87.01  112
 15  \w     62.00  95.00   0.50    0.05    --   80.75  19.00  95.63   66
 16  \w     71.00 126.00   0.50    0.05    --   80.75  14.00 124.01  110
 17  \w     82.00 111.00   0.50    0.05    --   80.75  -2.00 159.97   58
 18  \w     44.00  70.00   0.50    0.05    --   80.75 -60.00 107.65   52
 19  \w     40.00  65.00   0.50    0.05    --   80.75 -63.00  -7.06   50
 20  \w     39.00  68.00   0.50    0.05    --   80.75 -58.00-149.23   58
 21  \w     24.00  69.00   0.50    0.05    --   61.86 -95.00  30.00   90
 22  \w     55.00  94.00   0.50    0.05    --   80.75-105.00 -28.87   78
 23  \w     42.00  67.00   0.50    0.05    --   80.75-106.00 -31.45   50
 24  \w     25.00  57.00   0.50    0.05    --   61.86 -95.00-120.00   64
 25  \w     28.00  60.00   0.50    0.05    --   61.86 -95.00 -30.00   64
 26  \w     25.00  62.00   0.50    0.05    --   61.86 -95.00 -60.00   74
 27  \w     27.00  53.00   0.50    0.05    --   61.86 -95.00-150.00   52
 28  \w     59.00  85.00   0.50    0.05    --   80.75 -97.00  21.42   52
 29  \w     25.00  51.00   0.50    0.05    --   61.86 -95.00  60.00   52
 30  \w     36.00  63.00   0.50    0.05    --   75.43-126.00 120.00   54
 31  \w     43.00  68.00   0.50    0.05    --   80.75 -97.00 111.48   50
 32  \w     29.00  55.00   0.50    0.05    --   61.86 -95.00 150.00   52
 33  \w    -83.00 -58.00   0.50    0.05    --  -79.25  88.00 154.02   50
 34  \w   -118.00 -92.00   0.50    0.05    --  -79.25 146.00 170.86   52
 35  \w    -76.00 -50.00   0.50    0.05    --  -79.25  88.00  60.49   52
 36  \w    -92.00 -53.00   0.50    0.05    --  -79.25 117.00  19.42   78
 37  \w    -75.00 -50.00   0.50    0.05    --  -79.25 120.00-126.73   50
 38  \w    -62.00 -36.00   0.50    0.05    --  -79.25  56.00-125.53   52
 39  \w    -99.00 -72.00   0.50    0.05    --  -63.14   0.00 -30.00   54
 40  \w    -58.00 -26.00   0.50    0.05    --  -63.14   0.00 -30.00   64
 41  \w   -106.00 -37.00   0.50    0.05    --  -74.78   0.00  90.00  138
 42  \w   -120.00 -43.00   0.50    0.05    --  -74.78 -15.00  30.00  154
 43  \w   -114.00 -89.00   0.50    0.05    --  -79.25 -77.00 -26.21   50
 44  \w   -114.00 -89.00   0.50    0.05    --  -79.25 -62.00-113.66   50
 45  \w   -114.00 -89.00   0.50    0.05    --  -79.25 -77.00-100.60   50
 46  \w   -114.00 -89.00   0.50    0.05    --  -79.25 -77.00 -70.16   50
 47  \w   -115.00 -90.00   0.50    0.05    --  -79.25 -76.00 119.12   50
 48  \w   -117.00 -92.00   0.50    0.05    --  -79.25 -95.00  60.44   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0319598000
_diffrn_orient_matrix_UB_12      0.0082726000
_diffrn_orient_matrix_UB_13      0.0468732000
_diffrn_orient_matrix_UB_21      0.0703573000
_diffrn_orient_matrix_UB_22      0.1031545000
_diffrn_orient_matrix_UB_23      0.0141629000
_diffrn_orient_matrix_UB_31      -0.0527343000
_diffrn_orient_matrix_UB_32      0.1326553000
_diffrn_orient_matrix_UB_33      -0.0139331000
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            59029
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.751
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.471
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.152
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.123a (Rigaku Oxford Diffraction, 2024)
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            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       needle
_exptl_crystal_F_000             2270
_exptl_crystal_size_max          0.536
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.704
_refine_diff_density_min         -2.721
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0661P)^2^+28.8470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8491
_reflns_number_total             9385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03034f2.cif
_cod_data_source_block           agau(i)cl
_cod_depositor_comments
'Adding full bibliography for 7719677--7719681.cif.'
_cod_original_cell_volume        4568.18(10)
_cod_original_formula_sum        'C54 H45 Ag0.94 Au0.90 Cl2.84 N5'
_cod_database_code               7719678
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H N O S Ag '
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.071
_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
2. Shared sites
{Au10, Ag1}
{C2A, N2}
{C3A, N3}
3. Uiso/Uaniso restraints and constraints
Uanis(Au10) = Uanis(Ag1)
Uanis(C2A) = Uanis(N2)
Uanis(N2) = Uanis(C2A)
Uanis(C3A) = Uanis(N3)
4. Others
 Sof(Ag1)=1-FVAR(1)
 Sof(Au10)=FVAR(1)
 Fixed Sof: Au1(0.84) Cl1(0.84) N2(0.5) N3(0.5) C2A(0.5) C3A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C102(H102), C106(H106), C18(H18), C202(H202), C206(H206),
 C33(H33), C103(H103), C205(H205), C13(H13), C32(H32), C105(H105), C155(H155),
 C203(H203), C17(H17), C12(H12), C56(H56), C153(H153), C156(H156), C152(H152),
 C55(H55), C52(H52), C53(H53)
5.b Idealised Me refined as rotating group:
 C207(H20A,H20B,H20C), C157(H15A,H15B,H15C), C107(H10A,H10B,H10C), C57(H57A,
 H57B,H57C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52079
_shelx_fab_checksum              18115
_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 1.546
_oxdiff_exptl_absorpt_empirical_full_min 0.639