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_4132511
_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_formula_sum            'C24 H35.5 Au O0.25 P'
_chemical_formula_weight         555.96
_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             2018-01-30T11:44:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.63
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.39390(10)
_cell_length_b                   25.81310(10)
_cell_length_c                   21.81150(10)
_cell_measurement_reflns_used    114103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.185
_cell_measurement_theta_min      3.044
_cell_volume                     9789.19(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0729902
_diffrn_orient_matrix_UB_12      0.0212499
_diffrn_orient_matrix_UB_13      0.0295624
_diffrn_orient_matrix_UB_21      0.0460648
_diffrn_orient_matrix_UB_22      0.0468324
_diffrn_orient_matrix_UB_23      0.0248812
_diffrn_orient_matrix_UB_31      -0.0200496
_diffrn_orient_matrix_UB_32      0.0302943
_diffrn_orient_matrix_UB_33      -0.0591449
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            178709
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.064
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.938
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.42148
_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            'clear colourless'
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plate
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.987
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         17859
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+48.9944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0
_reflns_number_gt                17653
_reflns_number_total             17859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04478_si_002.cif
_cod_data_source_block           complex9
_cod_depositor_comments
;

2020-08-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H142 Au4 O P4'
_cod_original_formula_weight         2223.86
_cod_original_formula_units_Z            4
_cod_original_cell_volume        9789.18(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132511
_shelx_estimated_absorpt_t_min   0.268
_shelx_estimated_absorpt_t_max   0.647