Unlocking Structural Diversity in Gold(III) Hydrides: Unexpected Interplay of cis/ trans-Influence on Stability, Insertion Chemistry, and NMR Chemical Shifts.
Rocchigiani, Luca; Fernandez-Cestau, Julio; Chambrier, Isabelle; Hrobárik, Peter; Bochmann, Manfred; Journal of the American Chemical Society 140 (2018) 8287–8302; doi:10.1021/jacs.8b04478

data_4132512
_publ_section_title
;
 Unlocking Structural Diversity in Gold(III) Hydrides: Unexpected
 Interplay of cis/ trans-Influence on Stability, Insertion Chemistry, and
 NMR Chemical Shifts.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8287
_journal_page_last               8302
_journal_paper_doi               10.1021/jacs.8b04478
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_sum            'C29 H40 Au O4 P'
_chemical_formula_weight         680.54
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-02-02T12:23:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.30570(10)
_cell_length_b                   14.22560(10)
_cell_length_c                   19.7173(2)
_cell_measurement_reflns_used    31882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.791
_cell_measurement_theta_min      1.871
_cell_volume                     2890.65(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0028637
_diffrn_orient_matrix_UB_12      0.0493619
_diffrn_orient_matrix_UB_13      0.0048047
_diffrn_orient_matrix_UB_21      -0.0042586
_diffrn_orient_matrix_UB_22      -0.0065285
_diffrn_orient_matrix_UB_23      0.0356024
_diffrn_orient_matrix_UB_31      0.0686317
_diffrn_orient_matrix_UB_32      -0.0024542
_diffrn_orient_matrix_UB_33      0.0020087
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53827
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.175
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.65901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 2816 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.421(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+11.7727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     1
_reflns_number_gt                6546
_reflns_number_total             6628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04478_si_002.cif
_cod_data_source_block           complex12
_cod_database_code               4132512
_shelx_estimated_absorpt_t_min   0.424
_shelx_estimated_absorpt_t_max   0.904