Oxidant speciation and anionic ligand effects in the gold-catalyzed oxidative coupling of arenes and alkynes
Hofer, Manuel; de Haro, Teresa; Gómez-Bengoa, Enrique; Genoux, Alexandre; Nevado, Cristina; Chemical Science  (2019) –; doi:10.1039/C9SC02372K

data_1552137
_publ_section_title
;
 Oxidant speciation and anionic ligand effects in the gold-catalyzed
 oxidative coupling of arenes and alkynes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02372K
_journal_year                    2019
_chemical_formula_moiety         'C22 H18 Au Cl2 O2 P, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C22.5 H19 Au Cl3 O2 P'
_chemical_formula_weight         655.69
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             9-Aug-2016
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-26 deposited with the CCDC.    2019-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.3351(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.59949(18)
_cell_length_b                   10.66900(13)
_cell_length_c                   17.9124(3)
_cell_measurement_reflns_used    14109
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      30.3908
_cell_measurement_theta_min      2.2491
_cell_volume                     2285.62(6)
_computing_cell_refinement
'CrysAlisPro, Version 1.171.35.4 (Agilent Technologies, 2010)'
_computing_data_collection
'CrysAlisPro, Version 1.171.35.4 (Agilent Technologies, 2010)'
_computing_data_reduction
'CrysAlisPro, Version 1.171.35.4 (Agilent Technologies, 2010)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-2014 and PLATON (Spek, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Atlas CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_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            23037
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.46
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro, Version 1.171.35.4 (Agilent Technologies, 2010)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.240
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00076(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         6250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0197P)^2^+2.9702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                5692
_reflns_number_total             6250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02372k2.cif
_cod_data_source_block           NV1102
_cod_original_cell_volume        2285.61(5)
_cod_original_formula_sum        'C22.50 H19 Au Cl3 O2 P'
_cod_database_code               1552137
_shelx_res_checksum              46397