Thermally stable carbazole tagged Au(i)–mesoionic N-heterocyclic carbene complexes with diverse gold–hydrogen bonds
Kalaivanan, Subramaniyam; Moulali, Vaddamanu; Siddhant, Kumar; Velappan, Kavitha; Hisano, Kyohei; Tsutsumi, Osamu; Prabusankar, Ganesan; New Journal of Chemistry 47 (2023) 491–499; doi:10.1039/D2NJ03215E

data_7062147
_publ_section_title
;
 Thermally stable carbazole tagged Au(i)--mesoionic N-heterocyclic carbene
 complexes with diverse gold--hydrogen bonds
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              491
_journal_page_last               499
_journal_paper_doi               10.1039/D2NJ03215E
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C25 H24 Au Cl N4'
_chemical_formula_sum            'C25 H24 Au Cl N4'
_chemical_formula_weight         612.89
_chemical_name_systematic        'Abnormal Au complex 2'
_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     iterative
_audit_creation_date             2022-10-31
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-01 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.521(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6671(4)
_cell_length_b                   13.2879(3)
_cell_length_c                   21.1978(5)
_cell_measurement_reflns_used    15205
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      28.9900
_cell_measurement_theta_min      2.8760
_cell_volume                     4654.30(19)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.872
_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     11.00  89.00   0.50    5.00    --    7.10  38.00 120.00  156
  2  \w     61.00  91.00   0.50    5.00    --    7.10  77.00 -30.00   60
  3  \w     68.00  96.00   0.50    5.00    --    7.10  77.00  90.00   56
  4  \w     19.00  46.00   0.50    5.00    --    7.10 -82.00 -90.00   54
  5  \w    -94.00  12.00   0.50    5.00    --   -7.50 -57.00   0.00  212
  6  \w    -47.00  11.00   0.50    5.00    --   -7.50 -77.00 150.00  116
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0370395000
_diffrn_orient_matrix_UB_12      -0.0268942000
_diffrn_orient_matrix_UB_13      -0.0047285000
_diffrn_orient_matrix_UB_21      0.0209756000
_diffrn_orient_matrix_UB_22      -0.0451988000
_diffrn_orient_matrix_UB_23      0.0092180000
_diffrn_orient_matrix_UB_31      -0.0055128000
_diffrn_orient_matrix_UB_32      0.0090355000
_diffrn_orient_matrix_UB_33      0.0321399000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41742
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.965
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       cube
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.125
_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     567
_refine_ls_number_reflns         10748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+2.5867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9010
_reflns_number_total             10748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03215e2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
Adding full bibliography for 7062146--7062148.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C50 H48 Au2 Cl2 N8'
_cod_original_formula_weight         1225.79
_cod_original_formula_moiety         '2(C25 H24 Au Cl N4)'
_cod_original_formula_units_Z            4
_cod_database_code               7062147
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H24N4AuCl
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.425
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C29(H29A,H29B)
1.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C45(H45), C48(H48), C38(H38), C37(H37), C34(H34), C12(H12),
 C39(H39), C9(H9), C33(H33), C32(H32), C15(H15), C20(H20), C40(H40), C6(H6),
 C7(H7), C8(H8), C13(H13), C23(H23), C14(H14)
1.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C28(H28A,H28B,H28C), C3(H3A,H3B,H3C), C25(H25A,H25B,
 H25C), C19(H19A,H19B,H19C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C22(H22A,
 H22B,H22C)
;
_shelx_res_checksum              79126
_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 1.750
_oxdiff_exptl_absorpt_empirical_full_min 0.776