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_7711511
_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         'C62 H54 Au4 Cl2 N2 P4, 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C66 H60 Au4 B2 Cl2 F8 N4 P4'
_chemical_formula_weight         2065.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-04-25 deposited with the CCDC.	2022-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.162(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1241(12)
_cell_length_b                   10.3724(8)
_cell_length_c                   20.8748(16)
_cell_measurement_reflns_used    9773
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.40
_cell_volume                     3212.8(4)
_computing_cell_refinement       'Bruker Apex3, 2020'
_computing_data_collection       'Bruker Apex3, 2020'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker CHi Fixed Quest'
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11200
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         0.994
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.356
_exptl_absorpt_correction_T_max  0.046758
_exptl_absorpt_correction_T_min  0.012757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 124823 reflections, Rint = 0.0696
 (67402 with I > 3sig(I), Rint = 0.0609)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_description       prism
_exptl_crystal_F_000             1952
_exptl_crystal_recrystallization_method
'Crystallized from a mixture of acetonitrile, hexane and dichloromethane by cooling'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.716
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5730
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0596
_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^)+127.7063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4951
_reflns_number_total             5730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02429b2.cif
_cod_data_source_block           Complex_Fig4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7711511
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9485(9)
 0.0515(9)
2. 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
3. Restrained distances
 C14-N1 \\sim N1-C18
 with sigma of 0.01
4. Rigid bond restraints
 N2, C32, C33
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
N2 \\sim C32 \\sim C33: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C25(H25), C24(H24), C23(H23), C22(H22),
  C21(H21), C31(H31), C30(H30), C29(H29), C28(H28), C27(H27)
6.c Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C7(C8,C9,C10,C11,C12), C20(C25,C24,C23,C22,C21), C26(C31,
 C30,C29,C28,C27)
6.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C)
;
_shelx_res_checksum              51325
_shelx_hkl_checksum              19543
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a 100 micro/m MITEGEN holder in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'