Competitive gold/nickel transmetalation
Demchuk, Mitchell J.; Zurakowski, Joseph A.; Austen, Brady J. H.; Nelson, David J.; Drover, Marcus W.; Chemical Communications  (2021) –; doi:10.1039/D1CC06064C

data_7129348
_publ_section_title
;
 Competitive gold/nickel transmetalation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06064C
_journal_year                    2021
_chemical_formula_moiety         'C23 H19 Au N P'
_chemical_formula_sum            'C23 H19 Au N P'
_chemical_formula_weight         537.33
_chemical_name_systematic        '[Au(PPh3)(4-C5H4N)]'
_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
_audit_creation_date             2021-09-08
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-12 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                82.9700(10)
_cell_angle_beta                 86.1880(10)
_cell_angle_gamma                68.0260(10)
_cell_formula_units_Z            6
_cell_length_a                   11.6301(3)
_cell_length_b                   12.1425(3)
_cell_length_c                   24.6036(7)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      53.304
_cell_measurement_theta_min      3.621
_cell_volume                     3197.04(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            82892
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        53.425
_diffrn_reflns_theta_max         53.425
_diffrn_reflns_theta_min         3.621
_exptl_absorpt_coefficient_mu    13.706
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1188 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.6572.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       block
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         7490
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0307P)^2^+19.3809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6080
_reflns_number_total             7490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06064c3.cif
_cod_data_source_block           final
_cod_original_cell_volume        3197.05(15)
_cod_database_code               7129348
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.407
_shelx_estimated_absorpt_t_min   0.290
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53),
 C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62),
  C63(H63), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C25(H25),
 C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              40060
_shelx_fab_checksum              16472
_olex2_submission_special_instructions 'No special instructions were received'