Bis(metallaethynyl) Ketones: Synthesis and Structure of {(Ph3P)AuC\τb C}2CO and Attempted Transmetalation: Formation and Structure of [1,3-{Ru(dppe)Cp}2{c-COC(OMe)CHCCH}]PF6
Armitt, David J.; Bruce, Michael I.; Morris, Jonathan C.; Nicholson, Brian K.; Parker, Christian R.; Skelton, Brian W.; Zaitseva, Natasha N.; Organometallics 30 (2011) 5452–; doi:10.1021/om200659t

data_4065261
_publ_section_title
;
 Bis(metallaethynyl) Ketones: Synthesis and Structure of {(Ph3P)AuC\\tb
 C}2CO and Attempted Transmetalation: Formation and Structure of
 [1,3-{Ru(dppe)Cp}2{c-COC(OMe)CHCCH}]PF6
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5452
_journal_paper_doi               10.1021/om200659t
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C82 H60 Au4 O2 P4, C6 H6'
_chemical_formula_sum            'C88 H66 Au4 O2 P4'
_chemical_formula_weight         2067.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-11-03T14:46:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.800(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6684(6)
_cell_length_b                   17.1866(6)
_cell_length_c                   25.4564(10)
_cell_measurement_reflns_used    17590
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.9747
_cell_measurement_theta_min      2.7515
_cell_volume                     7360.0(5)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0005122
_diffrn_orient_matrix_UB_12      -0.0164787
_diffrn_orient_matrix_UB_13      0.0254238
_diffrn_orient_matrix_UB_21      0.018559
_diffrn_orient_matrix_UB_22      0.0338894
_diffrn_orient_matrix_UB_23      0.0140489
_diffrn_orient_matrix_UB_31      -0.0378802
_diffrn_orient_matrix_UB_32      0.0168208
_diffrn_orient_matrix_UB_33      -0.0034483
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            93696
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    8.085
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
         CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.296
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         21444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                16025
_reflns_number_total             21444
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200659t_si_001.cif
_cod_data_source_block           br1518
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_database_code               4065261