Gold(I) Compounds without Significant Aurophilic Intermolecular Interactions: Synthesis, Structure, and Electronic Properties of Ph~3~PAuC(O)NHCH~3~ and Au~3~(PhCH~2~N=COCH~3~)~3~: Comparative Monomeric and Trimeric Analogues of the Solvoluminescent Trimer, Au~3~(CH~3~N=COCH~3~)~3~.
Alan L. Balch; Marilyn M. Olmstead; Jess C. Vickery; Inorganic Chemistry 38 (1999) 3494–3499; doi:10.1021/ic990080b

data_4322158
_publ_contact_author
; Dr. Alan L. Balch
  Department of Chemistry
  University of California
  Davis, CA 95616
  USA
;
_publ_contact_author_email       balch@indigo.ucdavis.edu
_publ_contact_author_fax         530-752-8995
_publ_contact_author_phone       530-752-0941
_publ_section_title
;
 Gold(I) Compounds without Significant Aurophilic Intermolecular
 Interactions: Synthesis, Structure, and Electronic Properties of
 Ph~3~PAuC(O)NHCH~3~ and Au~3~(PhCH~2~N=COCH~3~)~3~: Comparative Monomeric
 and Trimeric Analogues of the Solvoluminescent Trimer,
 Au~3~(CH~3~N=COCH~3~)~3~.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3494
_journal_page_last               3499
_journal_paper_doi               10.1021/ic990080b
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C27 H30 Au3 N3 O3'
_chemical_formula_weight         1035.44
_chemical_name_common            Au~3~(PhCH~2~N=COCH~3~)~3~
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.73(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   17.311(6)
_cell_length_b                   34.761(10)
_cell_length_c                   18.052(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      2.35
_cell_volume                     10826(6)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL V.5.03 (Sheldrick, 1995) XP'
_computing_publication_material  'SHELXTL V.5.03 (Sheldrick, 1995) XCIF'
_computing_structure_refinement  'SHELXTL V.5.03 (Sheldrick, 1995) XL'
_computing_structure_solution    'SHELXTL V.5.03 (Sheldrick, 1995) XS'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device_type  'Siemens R3m/v'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1572
_diffrn_reflns_av_sigmaI/netI    0.0880
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16250
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.17
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    16.255
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_correction_T_min  0.214
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2: an empirical absorption correction program. Parkin,S.;
Moezzi, B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56. 
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.541
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Needle
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.809
_refine_diff_density_min         -3.235
_refine_diff_density_rms         0.412
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.002
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     985
_refine_ls_number_reflns         14434
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.032
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_obs          0.0735
_refine_ls_shift/su_max          -0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2149
_refine_ls_wR_factor_obs         0.1775
_reflns_number_gt                9762
_reflns_number_total             14448
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990080b_1.cif
_cod_data_source_block           jv02q
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10825.8(61)
_cod_database_code               4322158