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#$Date: 2023-05-05 06:06:37 +0300 (Fri, 05 May 2023) $
#$Revision: 283419 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/22/7062288.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7062288
loop_
_publ_author_name
'Leitner, Zdeněk'
'Císařová, Ivana'
'Štěpnička, Petr'
_publ_section_title
;
 Synthesis and characterisation of group 11 metal complexes with a
 guanidine-tagged triphenylphosphine and evaluation of the isolated Au(i)
 complexes in gold-mediated organic reactions
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5930
_journal_page_last               5938
_journal_paper_doi               10.1039/D3NJ00451A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C25 H31 Au Cl N3 P, Cl, H2 O, C H2 Cl2'
_chemical_formula_sum            'C26 H35 Au Cl4 N3 O P'
_chemical_formula_weight         775.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-01-23 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                85.7170(10)
_cell_angle_beta                 81.7560(10)
_cell_angle_gamma                84.9010(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5896(3)
_cell_length_b                   9.5972(3)
_cell_length_c                   19.1254(5)
_cell_measurement_reflns_used    9639
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.40
_cell_volume                     1551.09(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'PLATON (Spek, 2017)'
_computing_publication_material  'PLATON (Spek, 2017)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_source         'I\mS micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29187
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.135
_exptl_absorpt_coefficient_mu    5.162
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       prism
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.058
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0193
_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/[σ²(Fo²)+2.2412P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6974
_reflns_number_total             7106
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj00451a2.cif
_cod_data_source_block           zl168_sq
_cod_depositor_comments
'Adding full bibliography for 7062284--7062291.cif.'
_cod_database_code               7062288
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.626
_shelx_estimated_absorpt_t_max   0.747
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.73746(2) 0.66584(2) 0.31851(2) 0.02156(3) Uani 1 1 d . . . . .
Cl1 Cl 0.79202(10) 0.88775(7) 0.33656(4) 0.03603(16) Uani 1 1 d . . . . .
P1 P 0.69901(8) 0.44770(7) 0.29655(3) 0.01917(12) Uani 1 1 d . . . . .
N1 N 0.8331(2) 0.5485(2) 0.14745(11) 0.0196(4) Uani 1 1 d . . . . .
H1N H 0.916936 0.499412 0.127658 0.024 Uiso 1 1 d R U . . .
N2 N 0.6897(2) 0.7645(2) 0.14538(12) 0.0221(4) Uani 1 1 d . . . . .
H2N H 0.608366 0.720893 0.150034 0.027 Uiso 1 1 d R U . . .
N3 N 0.9630(2) 0.7526(2) 0.12922(12) 0.0210(4) Uani 1 1 d . . . . .
H3N H 0.954385 0.844807 0.120102 0.025 Uiso 1 1 d R U . . .
C1 C 0.8296(3) 0.6905(3) 0.13963(12) 0.0186(5) Uani 1 1 d . . . . .
C2 C 0.6895(3) 0.4795(2) 0.15057(13) 0.0193(5) Uani 1 1 d . . . . .
C3 C 0.6122(3) 0.4317(2) 0.21628(13) 0.0183(5) Uani 1 1 d . . . . .
C4 C 0.4704(3) 0.3700(3) 0.21799(15) 0.0240(5) Uani 1 1 d . . . . .
H4 H 0.415016 0.338449 0.262126 0.029 Uiso 1 1 calc R U . . .
C5 C 0.4092(3) 0.3541(3) 0.15558(15) 0.0267(6) Uani 1 1 d . . . . .
H5 H 0.311356 0.313963 0.157431 0.032 Uiso 1 1 calc R U . . .
C6 C 0.4905(3) 0.3967(3) 0.09129(15) 0.0282(6) Uani 1 1 d . . . . .
H6 H 0.450835 0.382359 0.048720 0.034 Uiso 1 1 calc R U . . .
C7 C 0.6306(3) 0.4606(3) 0.08853(14) 0.0254(5) Uani 1 1 d . . . . .
H7 H 0.685808 0.491123 0.044174 0.031 Uiso 1 1 calc R U . . .
C8 C 0.5730(3) 0.3573(3) 0.36657(13) 0.0223(5) Uani 1 1 d . . . . .
C9 C 0.5812(3) 0.2118(3) 0.37303(16) 0.0297(6) Uani 1 1 d . . . . .
H9 H 0.650623 0.159152 0.339725 0.036 Uiso 1 1 calc R U . . .
C10 C 0.4884(4) 0.1434(3) 0.42787(17) 0.0364(7) Uani 1 1 d . . . . .
H10 H 0.494358 0.043866 0.432056 0.044 Uiso 1 1 calc R U . . .
C11 C 0.3875(4) 0.2192(4) 0.47646(16) 0.0369(7) Uani 1 1 d . . . . .
H11 H 0.324776 0.171918 0.514306 0.044 Uiso 1 1 calc R U . . .
C12 C 0.3776(4) 0.3631(4) 0.47010(16) 0.0376(7) Uani 1 1 d . . . . .
H12 H 0.306945 0.414833 0.503356 0.045 Uiso 1 1 calc R U . . .
C13 C 0.4700(3) 0.4338(3) 0.41537(15) 0.0306(6) Uani 1 1 d . . . . .
H13 H 0.462951 0.533319 0.411324 0.037 Uiso 1 1 calc R U . . .
C14 C 0.8818(3) 0.3359(3) 0.28828(14) 0.0215(5) Uani 1 1 d . . . . .
C15 C 0.9191(3) 0.2364(3) 0.23848(15) 0.0257(5) Uani 1 1 d . . . . .
H15 H 0.852397 0.229650 0.203508 0.031 Uiso 1 1 calc R U . . .
C16 C 1.0553(4) 0.1459(3) 0.23999(17) 0.0329(6) Uani 1 1 d . . . . .
H16 H 1.081949 0.077968 0.205672 0.040 Uiso 1 1 calc R U . . .
C17 C 1.1512(3) 0.1548(3) 0.29103(18) 0.0371(7) Uani 1 1 d . . . . .
H17 H 1.242236 0.091379 0.292683 0.045 Uiso 1 1 calc R U . . .
C18 C 1.1154(4) 0.2554(4) 0.33962(19) 0.0443(8) Uani 1 1 d . . . . .
H18 H 1.182716 0.261976 0.374369 0.053 Uiso 1 1 calc R U . . .
C19 C 0.9819(4) 0.3472(4) 0.33823(17) 0.0365(7) Uani 1 1 d . . . . .
H19 H 0.958763 0.417702 0.371345 0.044 Uiso 1 1 calc R U . . .
C20 C 0.6587(3) 0.9178(3) 0.14388(15) 0.0248(5) Uani 1 1 d . . . . .
H20 H 0.752626 0.959391 0.156715 0.030 Uiso 1 1 calc R U . . .
C21 C 0.5172(4) 0.9538(3) 0.19842(18) 0.0357(7) Uani 1 1 d . . . . .
H21A H 0.495731 1.055865 0.198152 0.053 Uiso 1 1 calc R U . . .
H21B H 0.539479 0.917145 0.245465 0.053 Uiso 1 1 calc R U . . .
H21C H 0.424889 0.911767 0.186876 0.053 Uiso 1 1 calc R U . . .
C22 C 0.6319(4) 0.9742(4) 0.06952(18) 0.0416(8) Uani 1 1 d . . . . .
H22A H 0.717593 0.935971 0.035010 0.062 Uiso 1 1 calc R U . . .
H22B H 0.630121 1.076706 0.066420 0.062 Uiso 1 1 calc R U . . .
H22C H 0.530958 0.946184 0.059338 0.062 Uiso 1 1 calc R U . . .
C23 C 1.1209(3) 0.6838(3) 0.13612(15) 0.0251(5) Uani 1 1 d . . . . .
H23 H 1.120825 0.582339 0.127511 0.030 Uiso 1 1 calc R U . . .
C24 C 1.1576(4) 0.6953(4) 0.21047(18) 0.0397(7) Uani 1 1 d . . . . .
H24A H 1.260674 0.645922 0.215513 0.060 Uiso 1 1 calc R U . . .
H24B H 1.076119 0.653225 0.244638 0.060 Uiso 1 1 calc R U . . .
H24C H 1.159932 0.794323 0.219393 0.060 Uiso 1 1 calc R U . . .
C25 C 1.2400(3) 0.7497(4) 0.08002(18) 0.0384(7) Uani 1 1 d . . . . .
H25A H 1.209602 0.741361 0.033132 0.058 Uiso 1 1 calc R U . . .
H25B H 1.344740 0.701409 0.082356 0.058 Uiso 1 1 calc R U . . .
H25C H 1.242722 0.848964 0.088286 0.058 Uiso 1 1 calc R U . . .
Cl2A Cl 1.0782(4) 0.3737(3) 0.04643(16) 0.0251(5) Uani 0.502(5) 1 d . . P A 1
O1WA O 1.0030(14) 0.0476(10) 0.0759(6) 0.0330(6) Uani 0.502(5) 1 d . . P A 1
H11W H 1.030043 0.145872 0.067837 0.040 Uiso 0.502(5) 1 d R U P A 1
H12W H 0.999341 0.021772 0.036137 0.040 Uiso 0.502(5) 1 d R U P A 1
Cl2B Cl 1.0076(5) 0.0780(2) 0.0710(2) 0.0330(6) Uani 0.498(5) 1 d . . P A 2
O1WB O 1.0753(14) 0.3926(12) 0.0582(6) 0.0251(5) Uani 0.498(5) 1 d . . P A 2
H21W H 1.050247 0.454194 0.022674 0.030 Uiso 0.498(5) 1 d R U P A 2
H22W H 1.043248 0.295794 0.052574 0.030 Uiso 0.498(5) 1 d R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au1 Cl1 176.35(3) . . ?
C8 P1 C14 103.50(12) . . ?
C8 P1 C3 105.16(12) . . ?
C14 P1 C3 106.11(12) . . ?
C8 P1 Au1 114.19(9) . . ?
C14 P1 Au1 111.85(9) . . ?
C3 P1 Au1 115.03(8) . . ?
C1 N1 C2 120.1(2) . . ?
C1 N1 H1N 118.3 . . ?
C2 N1 H1N 113.2 . . ?
C1 N2 C20 127.7(2) . . ?
C1 N2 H2N 118.2 . . ?
C20 N2 H2N 114.1 . . ?
C1 N3 C23 125.7(2) . . ?
C1 N3 H3N 116.1 . . ?
C23 N3 H3N 118.0 . . ?
N3 C1 N2 121.4(2) . . ?
N3 C1 N1 119.9(2) . . ?
N2 C1 N1 118.6(2) . . ?
C7 C2 C3 120.9(2) . . ?
C7 C2 N1 119.6(2) . . ?
C3 C2 N1 119.5(2) . . ?
C4 C3 C2 118.3(2) . . ?
C4 C3 P1 121.70(19) . . ?
C2 C3 P1 119.98(18) . . ?
C5 C4 C3 120.7(2) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C6 C5 C4 120.0(2) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 119.9(2) . . ?
C2 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C9 C8 C13 119.5(2) . . ?
C9 C8 P1 120.4(2) . . ?
C13 C8 P1 120.1(2) . . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 119.5(3) . . ?
C12 C13 H13 120.3 . . ?
C8 C13 H13 120.3 . . ?
C15 C14 C19 119.9(3) . . ?
C15 C14 P1 123.3(2) . . ?
C19 C14 P1 116.7(2) . . ?
C14 C15 C16 119.6(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C14 119.8(3) . . ?
C18 C19 H19 120.1 . . ?
C14 C19 H19 120.1 . . ?
N2 C20 C21 108.7(2) . . ?
N2 C20 C22 109.6(2) . . ?
C21 C20 C22 111.9(2) . . ?
N2 C20 H20 108.8 . . ?
C21 C20 H20 108.8 . . ?
C22 C20 H20 108.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 C24 109.7(2) . . ?
N3 C23 C25 108.7(2) . . ?
C24 C23 C25 112.7(2) . . ?
N3 C23 H23 108.6 . . ?
C24 C23 H23 108.6 . . ?
C25 C23 H23 108.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
H11W O1WA H12W 104.8 . . ?
H21W O1WB H22W 111.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 P1 2.2276(6) . ?
Au1 Cl1 2.2822(7) . ?
P1 C8 1.815(3) . ?
P1 C14 1.816(3) . ?
P1 C3 1.822(3) . ?
N1 C1 1.358(3) . ?
N1 C2 1.443(3) . ?
N1 H1N 0.8786 . ?
N2 C1 1.335(3) . ?
N2 C20 1.471(3) . ?
N2 H2N 0.8364 . ?
N3 C1 1.321(3) . ?
N3 C23 1.474(3) . ?
N3 H3N 0.8879 . ?
C2 C7 1.385(4) . ?
C2 C3 1.400(3) . ?
C3 C4 1.396(4) . ?
C4 C5 1.395(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.377(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.389(4) . ?
C8 C13 1.393(4) . ?
C9 C10 1.385(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.373(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.384(4) . ?
C14 C19 1.390(4) . ?
C15 C16 1.396(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.374(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.517(4) . ?
C20 C22 1.525(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.514(4) . ?
C23 C25 1.515(4) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O1WA H11W 0.9872 . ?
O1WA H12W 0.8226 . ?
O1WB H21W 0.9046 . ?
O1WB H22W 1.0097 . ?
