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_7719679
_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         'C44 H27 Au2 Cl3 N4, 1[CH2Cl2], 0.5[CH2Cl2]'
_chemical_formula_sum            'C45.5 H30 Au2 Cl6 N4'
_chemical_formula_weight         1239.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-29
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-03 deposited with the CCDC.	2025-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.673(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8854(4)
_cell_length_b                   27.5952(6)
_cell_length_c                   8.02367(19)
_cell_measurement_reflns_used    9135
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.7460
_cell_measurement_theta_min      2.7440
_cell_volume                     4373.09(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.123a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 41.104a 64-bit (release 16-03-2021))'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(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 0.997
_diffrn_measured_fraction_theta_max 0.981
_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     87.00 117.00   0.50    1.00    --   83.00  79.00-122.20   60
  2  \w     78.00 117.00   0.50    1.00    --   83.00  23.00 -88.09   78
  3  \w     49.00 101.00   0.50    1.00    --   83.00   7.00 -90.83  104
  4  \w     74.00 133.00   0.50    1.00    --   83.00  26.00  54.26  118
  5  \w     73.00 126.00   0.50    1.00    --   83.00  23.00 130.82  106
  6  \w     76.00 123.00   0.50    1.00    --   83.00   0.00 134.36   94
  7  \w     78.00 103.00   0.50    1.00    --   79.25 126.00  90.00   50
  8  \w     10.00  35.00   0.50    1.00    --   59.17 -30.00  90.00   50
  9  \w     10.00  35.00   0.50    1.00    --   59.17 -30.00-120.00   50
 10  \w     41.00  66.00   0.50    1.00    --   83.00 -57.00 -91.02   50
 11  \w     38.00  65.00   0.50    1.00    --   83.00 -56.00  79.82   54
 12  \w     52.00  77.00   0.50    1.00    --   83.00 -90.00 142.14   50
 13  \w     58.00  91.00   0.50    1.00    --   83.00-150.00 147.96   66
 14  \w     93.00 124.00   0.50    1.00    --   83.00-150.00 147.96   62
 15  \w     34.00  60.00   0.50    1.00    --   79.25-126.00 -30.00   52
 16  \w     69.00 110.00   0.50    1.00    --   79.25-126.00 -30.00   82
 17  \w     74.00 102.00   0.50    1.00    --   79.25-126.00 -60.00   56
 18  \w     44.00  71.00   0.50    1.00    --   83.00-155.00-126.45   54
 19  \w    100.00 125.00   0.50    1.00    --   83.00-155.00-126.45   50
 20  \w     61.00  88.00   0.50    1.00    --   79.25 -95.00-180.00   54
 21  \w     40.00  99.00   0.50    1.00    --   83.00-104.00-135.34  118
 22  \w     53.00  78.00   0.50    1.00    --   79.25 -95.00-120.00   50
 23  \w     41.00  79.00   0.50    1.00    --   73.61 -95.00 -60.00   76
 24  \w     60.00  88.00   0.50    1.00    --   79.25 -95.00   0.00   56
 25  \w     61.00  86.00   0.50    1.00    --   83.00-102.00  73.68   50
 26  \w     36.00  84.00   0.50    1.00    --   73.61 -95.00  90.00   96
 27  \w     50.00  79.00   0.50    1.00    --   73.61 -95.00  30.00   58
 28  \w     39.00  86.00   0.50    1.00    --   79.25 -95.00 -30.00   94
 29  \w     39.00  64.00   0.50    1.00    --   79.25 -95.00-150.00   50
 30  \w   -122.00 -81.00   0.50    1.00    --  -74.97 -15.00 -60.00   82
 31  \w   -103.00 -77.00   0.50    1.00    --  -60.81 -30.00-150.00   52
 32  \w    -99.00 -71.00   0.50    1.00    --  -60.81 -30.00-180.00   56
 33  \w    -80.00 -54.00   0.50    1.00    --  -74.97 -15.00 -60.00   52
 34  \w   -113.00 -85.00   0.50    1.00    --  -74.77-126.00 150.00   56
;
_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      -0.0245734000
_diffrn_orient_matrix_UB_12      -0.0515557000
_diffrn_orient_matrix_UB_13      -0.0490894000
_diffrn_orient_matrix_UB_21      0.0740401000
_diffrn_orient_matrix_UB_22      -0.0171147000
_diffrn_orient_matrix_UB_23      0.0068998000
_diffrn_orient_matrix_UB_31      0.0001460000
_diffrn_orient_matrix_UB_32      -0.0129223000
_diffrn_orient_matrix_UB_33      0.1867695000
_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  0.0544
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            19402
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.617
_diffrn_reflns_theta_min         2.751
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.102
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.152
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.123a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.882
_exptl_crystal_description       needle
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.024
_refine_diff_density_max         2.646
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       0.00018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4458
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+137.7519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3970
_reflns_number_total             4458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03034f2.cif
_cod_data_source_block           sk38
_cod_depositor_comments
'Adding full bibliography for 7719677--7719681.cif.'
_cod_original_cell_volume        4373.09(16)
_cod_original_formula_sum        'C45.50 H30 Au2 Cl6 N4'
_cod_database_code               7719679
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C42.5H27Au2Cl6N5
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{N2, C18}
{C21, N23}
3. Restrained distances
 C101-C102 = C102-C103 = C11-C12
 1.39 with sigma of 0.02
 C13-C13_$1
 2.41 with sigma of 0.02
 C11-C12 \\sim C12-C13 \\sim C13-C14
 with sigma of 0.0001
4. Uiso/Uaniso restraints and constraints
C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 2A
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.2
Uanis(C21) = Uanis(N23)
Uanis(N2) = Uanis(C18)
Uanis(Au1) = Uanis(Au3)
5. Others
 Fixed Sof: Au1(0.45909) C21(0.5) N2(0.5) Au2(0.5) Cl1(0.5) Cl2(0.5) Cl3(0.5)
 N23(0.5) C18(0.5) H18(0.5) H3A(0.5) H3B(0.5) Au3(0.04091)
6.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C3(H3A), C3(H3B), C7(H7), C8(H8), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C102(H102), C103(H103), C104(H104), C12(H12), C13(H13),
 C14(H14)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 248 electrons were 
found in a volume of 714\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[CH2Cl2], 0.5[CH2Cl2] per Formula Unit 
which account for 252 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99211
_shelx_fab_checksum              8376
_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 2.414
_oxdiff_exptl_absorpt_empirical_full_min 0.548