Gold(I) Complexes Bearing a PNP-Type Pincer Ligand: Photophysi-cal Properties and Catalytic Investigations
Casciotti, Martina; Romo, Guillermo; Alvarez, Maria; Molina, Francisco; Muñoz-Molina, José M; Belderrain, Tomás R. R.; Rodriguez, Laura; Dalton Transactions  (2022) –; doi:10.1039/D2DT02429B

data_7711513
_publ_section_title
;
 Gold(I) Complexes Bearing a PNP-Type Pincer Ligand: Photophysi-cal
 Properties and Catalytic Investigations
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02429B
_journal_year                    2022
_chemical_formula_moiety         'C31 H27 Au2 Cl2 N P2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C31.5 H28 Au2 Cl3 N P2'
_chemical_formula_weight         982.77
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-04
_audit_creation_method
; 
Olex2 1.2 
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335) 
;
_audit_update_record
;
2022-04-25 deposited with the CCDC.	2022-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.049(2)
_cell_angle_beta                 95.592(2)
_cell_angle_gamma                107.456(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9762(4)
_cell_length_b                   12.4423(5)
_cell_length_c                   14.4881(7)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.20
_cell_measurement_theta_min      2.39
_cell_volume                     1535.46(12)
_computing_cell_refinement       'Bruker Apex3, 2016'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.35A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'D8_Quest_Mo Huelva'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            148921
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.932
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.1031 before and 0.0754 after correction. 
The Ratio of minimum to maximum transmission is 0.7031. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_description       prism
_exptl_crystal_F_000             926
_exptl_crystal_recrystallization_method
'From a mixture of DCM and diethyl ether by saturate solution at r.t.'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         8988
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0177
_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^)+(0.0090P)^2^+1.4440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7972
_reflns_number_total             8988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02429b2.cif
_cod_data_source_block           Complex_Fig1
_cod_original_formula_sum        'C31.50 H28 Au2 Cl3 N P2'
_cod_database_code               7711513
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.486
_shelx_estimated_absorpt_t_min   0.358
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
2. Restrained distances 
 Cl3-C32 = Cl4-C32 
 1.771 with sigma of 0.01 
 Cl3-Cl4 
 2.916 with sigma of 0.03 
3. Uiso/Uaniso restraints and constraints 
Cl3 \\sim Cl4 \\sim C32: within 2A with sigma of 0.04 and sigma for terminal 
atoms of 0.08 
4. Rigid body (RIGU) restrains 
 Cl3, Cl4, C32 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
5. Others 
 Fixed Sof: Cl3(0.5) Cl4(0.5) C32(0.5) H32A(0.5) H32B(0.5) 
6.a Secondary CH2 refined with riding coordinates: 
 C6(H6A,H6B), C19(H19A,H19B), C32(H32A,H32B) 
6.b Aromatic/amide H refined with riding coordinates: 
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), 
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), 
 C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), 
 C30(H30), C31(H31) 
;
_olex2_exptl_crystal_mounting_method
'Mounted on a 150 micro/m MITIGEN holder in perfluoroether '
_olex2_submission_special_instructions 'No special instructions were received'