Gold(I) Heteroatom-Substituted Imido Complexes. Amino Nitrene Loss from [(LAu)3(μ-NNR2)]+
Bruce W. Flint; Yi Yang; Paul R. Sharp; Inorganic Chemistry 39 (2000) 602–608; doi:10.1021/ic990586u

data_4300052
_publ_contact_author
;
 Paul R. Sharp
 Department of Chemistry
 University of Missouri
 Columbia, MO  65211
;
_publ_contact_author_email       SharpP@missouri.edu
_publ_contact_author_fax         573-882-2754
_publ_contact_author_phone       573-882-7715
_publ_section_title
;
Gold(I) Heteroatom-Substituted Imido Complexes. Amino Nitrene Loss from
[(LAu)3(\m-NNR2)]+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              602
_journal_page_last               608
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     '[{(o-tol)3PAu}3(u-NOH)]BF4.3THF'
_chemical_formula_sum            'C75 H88 Au3 B F4 N O4 P3'
_chemical_formula_weight         1838.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.98(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.813(8)
_cell_length_b                   26.145(4)
_cell_length_c                   17.768(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      9.00
_cell_volume                     7291(5)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    'RES2INS (Len Barbour, 1996)'
_computing_publication_material  'ORTEP III'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       'Theta/2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7762
_diffrn_reflns_theta_full        20.91
_diffrn_reflns_theta_max         20.91
_diffrn_reflns_theta_min         1.39
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.526
_refine_diff_density_min         -2.194
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         7762
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.109
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1438
_reflns_number_gt                5836
_reflns_number_total             7762
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        7291.4
_cod_database_code               4300052
_journal_paper_doi 10.1021/ic990586u