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_7062148
_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         'I, C26 H21 N4'
_chemical_formula_sum            'C26 H21 I N4'
_chemical_formula_weight         516.388
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-21 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.190(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.2137(3)
_cell_length_b                   27.0679(10)
_cell_length_c                   22.9078(7)
_cell_measurement_reflns_used    10864
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      28.6050
_cell_measurement_theta_min      2.9460
_cell_volume                     4472.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.9632
_diffrn_measured_fraction_theta_max 0.8280
_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    -41.00 -14.00   0.50   18.62    --    7.20 -60.00-142.00   54
  2  \w     27.00  52.00   0.50   18.62    --    7.20  68.00 140.00   50
  3  \w     50.00  75.00   0.50   18.62    --    7.20  77.00 -90.00   50
  4  \w     62.00  97.00   0.50   18.62    --    7.20  77.00-150.00   70
  5  \w    -79.00  22.00   0.50   18.62    --    7.20 -38.00  60.00  202
  6  \w    -67.00 -42.00   0.50   18.62    --    7.20 -57.00 150.00   50
  7  \w    -50.00 -24.00   0.50   18.62    --    7.20 -38.00 -30.00   52
  8  \w     52.00  96.00   0.50   18.62    --    7.20  77.00-180.00   88
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0218429000
_diffrn_orient_matrix_UB_12      0.0249013000
_diffrn_orient_matrix_UB_13      -0.0067988000
_diffrn_orient_matrix_UB_21      -0.0655195000
_diffrn_orient_matrix_UB_22      -0.0004542000
_diffrn_orient_matrix_UB_23      -0.0231467000
_diffrn_orient_matrix_UB_31      -0.0699369000
_diffrn_orient_matrix_UB_32      0.0081936000
_diffrn_orient_matrix_UB_33      0.0194104000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.9632
_diffrn_reflns_Laue_measured_fraction_max 0.8280
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38669
_diffrn_reflns_point_group_measured_fraction_full 0.9632
_diffrn_reflns_point_group_measured_fraction_max 0.8280
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07215
_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            'metallic whiteish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             2061.886
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.8744
_refine_diff_density_min         -0.7494
_refine_diff_density_rms         0.1095
_refine_ls_d_res_high            0.7297
_refine_ls_d_res_low             7.2137
_refine_ls_goodness_of_fit_ref   1.0221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    78
_refine_ls_number_parameters     561
_refine_ls_number_reflns         9968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0221
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+2.3677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                7479
_reflns_number_total             9968
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj03215e2.cif
_cod_data_source_block           L
_cod_depositor_comments
'Adding full bibliography for 7062146--7062148.cif.'
_cod_original_cell_volume        4473.0(3)
_cod_database_code               7062148
_chemical_oxdiff_formula         CHNI
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b), C4(H4a,H4b)
2.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C9(H9), C35(H35), C14(H14), C50(H50), C27(H27), C19(H19), C15(H15),
 C18(H18), C49(H49), C24(H24), C41(H41), C20(H20), C40(H40), C38(H38), C34(H34),
  C33(H33), C1(H1), C48(H48), C45(H45), C46(H46), C32(H32), C13(H13), C6(H6),
 C23(H23), C22(H22), C7(H7), C44(H44), C12(H12), C8(H8), C25(H25), C39(H39)
2.c Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C3(H3a,H3b,H3c)
;
_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 5.232
_oxdiff_exptl_absorpt_empirical_full_min 0.205