Monocyclometalated Gold(III) Complexes Bearing π-Accepting Cyanide Ligands: Syntheses, Structural, Photophysical, and Electrochemical Investigations.
Szentkuti, Alexander; Garg, Jai Anand; Blacque, Olivier; Venkatesan, Koushik; Inorganic chemistry 54 (2015) 10748–10760; doi:10.1021/acs.inorgchem.5b01762

data_4344423
_publ_section_title
;
 Monocyclometalated Gold(III) Complexes Bearing \p-Accepting Cyanide
 Ligands: Syntheses, Structural, Photophysical, and Electrochemical
 Investigations.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10748
_journal_page_last               10760
_journal_paper_doi               10.1021/acs.inorgchem.5b01762
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '2(C23 H15 Au N4), C4 H10 O'
_chemical_formula_sum            'C50 H40 Au2 N8 O'
_chemical_formula_weight         1162.83
_chemical_name_systematic
;
Bis(cyano-\kC)[2-(3,5-diphenyl-1H-pyrrol-2-yl-\kN)pyridinato-\kN]gold(iii)
diethyl ether solvate (2:1)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-07
_audit_creation_method
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Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                75.611(4)
_cell_angle_beta                 84.488(4)
_cell_angle_gamma                84.492(3)
_cell_formula_units_Z            1
_cell_length_a                   4.8031(2)
_cell_length_b                   11.6531(5)
_cell_length_c                   19.9543(11)
_cell_measurement_reflns_used    4884
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      3.1
_cell_volume                     1073.81(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -91.00  -78.20   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.5264  -77.0000  -30.0000 16

  2 omega -104.00  -75.20   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.5264  179.0000  120.0000 36

  3 omega  -20.80   41.60   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1514  -38.0000 -150.0000 78

  4 omega   13.20   86.00   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1514   77.0000  120.0000 91

  5 omega  -15.40   88.60   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1514   77.0000    0.0000 130

  6 omega  -34.80   58.80   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.5264   38.0000   60.0000 117
;
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0273365000
_diffrn_orient_matrix_UB_12      0.0188336000
_diffrn_orient_matrix_UB_13      -0.0364818000
_diffrn_orient_matrix_UB_21      -0.0914895000
_diffrn_orient_matrix_UB_22      -0.0412626000
_diffrn_orient_matrix_UB_23      -0.0046131000
_diffrn_orient_matrix_UB_31      -0.1140954000
_diffrn_orient_matrix_UB_32      0.0437453000
_diffrn_orient_matrix_UB_33      -0.0014480000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8792
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.872
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
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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)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       plate
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.881
_refine_diff_density_min         -1.986
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4027
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0679P)^2^+8.3179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3173
_reflns_number_total             4027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01762_si_007.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4344422--4344427.cif.'
_cod_database_code               4344423
_shelxl_version_number           2014/6
_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. Restrained distances
 O1-C24 \\sim O1-C26
 with sigma of 0.005
 C24-C25 \\sim C26-C27
 with sigma of 0.005
3. Rigid bond restraints
 C24, C25, C26, C27, O1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C24 \\sim C25 \\sim C26 \\sim C27 \\sim O1: within 1.7A with sigma of 0.008 and
sigma for terminal atoms of 0.016
5. Others
 Fixed Sof: C24(0.5) H24A(0.5) H24B(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C26(0.5) H26A(0.5) H26B(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
 O1(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B)
6.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
;
_shelx_res_checksum              6165
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