Indazolin-3-ylidenes (Indy*): easily accessible, sterically-hindered indazole-derived N-heterocyclic carbenes and their application in gold catalysis.
Zhang, Jin; Liu, Ting; Zhang, Gaopeng; Cai, Jianglong; Wang, Yue; Tong, Jianbo; Ma, Yangmin; Szostak, Roman; Szostak, Michal; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4260–4265; doi:10.1039/d4dt00287c

data_7715084
_publ_section_title
;
 Indazolin-3-ylidenes (Indy*): easily accessible, sterically-hindered
 indazole-derived N-heterocyclic carbenes and their application in gold
 catalysis.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4260
_journal_page_last               4265
_journal_paper_doi               10.1039/d4dt00287c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C41 H34 Au Cl N2 O'
_chemical_formula_sum            'C41 H34 Au Cl N2 O'
_chemical_formula_weight         803.11
_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
_audit_creation_date             2022-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-03-12 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.026(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.499(4)
_cell_length_b                   11.4792(15)
_cell_length_c                   22.902(3)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.300
_cell_measurement_theta_min      2.361
_cell_volume                     6880.2(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1747
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            179149
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.071
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.389
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1103 before and 0.0871 after correction.
The Ratio of minimum to maximum transmission is 0.8262.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         12126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+13.3639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7737
_reflns_number_total             12126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00287c2.cif
_cod_data_source_block           sust_3314_0ma
_cod_depositor_comments
;
Adding full bibliography for 7715084--7715085.cif.

2024-11-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C82 H68 Au2 Cl2 N4 O2'
_cod_original_formula_weight         1606.23
_cod_original_formula_moiety         '2(C41 H34 Au Cl N2 O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        6880.1(15)
_cod_database_code               7715084
_shelx_shelxl_version_number     2018/3
_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.a Ternary CH refined with riding coordinates:
 C6(H6), C34(H34), C4(H4), C58(H58)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C11(H11), C13(H13), C15(H15), C22(H22), C25(H25),
 C28(H28), C29(H29), C31(H31), C36(H36), C41(H41), C43(H43), C44(H44), C49(H49),
  C55(H55), C59(H59), C61(H61), C64(H64), C65(H65), C68(H68), C70(H70),
 C75(H75), C77(H77), C78(H78), C5(H5), C9(H9), C17(H17), C19(H19), C23(H23),
 C33(H33), C35(H35), C38(H38), C39(H39), C40(H40), C47(H47), C51(H51), C52(H52),
  C53(H53), C57(H57), C63(H63), C66(H66), C67(H67), C69(H69), C71(H71),
 C73(H73), C74(H74), C79(H79), C80(H80), C81(H81), C82(H82)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C45(H45A,H45B,
 H45C)
;
_shelx_res_checksum              731
_olex2_submission_special_instructions 'No special instructions were received'