#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:48:25 +0100 (mar 22 de mar de 2016) $
#$Revision: 178917 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/46/4114660.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4114660
loop_
_publ_author_name
'Rochelle L. White-Morris'
'Marilyn M. Olmstead'
'Feilong Jiang'
'Dino S. Tinti'
'Alan L. Balch'
_publ_section_title
;
 Remarkable Variations in the Luminescence of Frozen Solutions of
 [Au{C(NHMe)2}2](PF6).0.5(Acetone). Structural and Spectroscopic Studies
 of the Effects of Anions and Solvents on Gold(I) Carbene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2327
_journal_page_last               2336
_journal_paper_doi               10.1021/ja012397s
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C8 H20 Au F6 N4 P'
_chemical_formula_weight         514.22
_chemical_name_common            '[Au{C(NMe2)(NHMe)}2](PF6)'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.4280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2551(6)
_cell_length_b                   7.2162(4)
_cell_length_c                   8.5987(4)
_cell_measurement_reflns_used    4768
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      3.3
_cell_volume                     752.22(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2243
_diffrn_reflns_theta_full        31.38
_diffrn_reflns_theta_max         31.38
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    9.944
_exptl_absorpt_correction_T_max  0.5034
_exptl_absorpt_correction_T_min  0.3816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.270
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0143
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0246P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0350
_refine_ls_wR_factor_ref         0.0350
_reflns_number_gt                1267
_reflns_number_total             1267
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja012397s_3.cif
_cod_data_source_block           rw01
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4114660
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Au1 Au 0.0000 0.0000 0.5000 0.01336(5) Uani 1 4 d S
P1 P 0.5000 0.0000 1.0000 0.01605(18) Uani 1 4 d S
F1 F 0.43037(13) 0.1575(2) 0.89761(19) 0.0336(3) Uani 1 1 d .
F2 F 0.4128(2) 0.0000 1.1203(3) 0.0452(6) Uani 1 2 d S
N1 N 0.23791(19) 0.0000 0.4595(3) 0.0172(4) Uani 1 2 d S
N2 N 0.21210(19) 0.0000 0.7156(3) 0.0203(5) Uani 1 2 d S
H2 H 0.284(4) 0.0000 0.743(5) 0.020(10) Uiso 1 2 d S
C1 C 0.1678(2) 0.0000 0.5640(3) 0.0144(4) Uiso 1 2 d S
C2 C 0.2006(2) 0.0000 0.2900(3) 0.0206(5) Uani 1 2 d S
H2A H 0.230(2) 0.112(5) 0.244(3) 0.026(8) Uiso 1 1 d .
H2B H 0.124(4) 0.0000 0.275(5) 0.024(10) Uiso 1 2 d S
C3 C 0.3580(3) 0.0000 0.5058(4) 0.0201(5) Uiso 1 2 d S
H3A H 0.381(3) 0.100(5) 0.565(4) 0.031(8) Uiso 1 1 d .
H3B H 0.394(4) 0.0000 0.411(6) 0.034(13) Uiso 1 2 d S
C4 C 0.1481(3) 0.0000 0.8460(4) 0.0300(7) Uani 1 2 d S
H4A H 0.191(6) 0.0000 0.935(9) 0.08(2) Uiso 1 2 d S
H4B H 0.100(4) 0.096(7) 0.849(6) 0.075(15) Uiso 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.00891(7) 0.01656(8) 0.01418(7) 0.000 0.00027(4) 0.000
P1 0.0105(4) 0.0236(5) 0.0134(4) 0.000 -0.0003(3) 0.000
F1 0.0325(7) 0.0281(7) 0.0348(8) 0.0033(6) -0.0134(6) 0.0042(6)
F2 0.0400(13) 0.0585(17) 0.0429(14) 0.000 0.0262(11) 0.000
N1 0.0115(9) 0.0239(12) 0.0161(10) 0.000 0.0009(8) 0.000
N2 0.0115(10) 0.0317(14) 0.0171(11) 0.000 0.0001(8) 0.000
C2 0.0144(12) 0.0297(15) 0.0173(12) 0.000 0.0013(9) 0.000
C4 0.0185(13) 0.053(2) 0.0180(14) 0.000 0.0028(10) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Au1 C1 180.0 5_556 .
F2 P1 F2 180.000(1) . 5_657
F2 P1 F1 89.85(10) . 2_657
F2 P1 F1 90.15(10) 5_657 2_657
F2 P1 F1 90.15(10) . 6
F2 P1 F1 89.85(10) 5_657 6
F1 P1 F1 180.00(8) 2_657 6
F2 P1 F1 90.15(10) . .
F2 P1 F1 89.85(10) 5_657 .
F1 P1 F1 89.81(11) 2_657 .
F1 P1 F1 90.19(11) 6 .
F2 P1 F1 89.85(10) . 5_657
F2 P1 F1 90.15(10) 5_657 5_657
F1 P1 F1 90.19(11) 2_657 5_657
F1 P1 F1 89.81(11) 6 5_657
F1 P1 F1 180.000(1) . 5_657
C1 N1 C2 122.3(2) . .
C1 N1 C3 122.5(2) . .
C2 N1 C3 115.2(2) . .
C1 N2 C4 124.2(2) . .
N1 C1 N2 116.7(2) . .
N1 C1 Au1 122.68(19) . .
N2 C1 Au1 120.66(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 C1 2.050(3) 5_556
Au1 C1 2.050(3) .
P1 F2 1.593(2) .
P1 F2 1.593(2) 5_657
P1 F1 1.6045(15) 2_657
P1 F1 1.6045(15) 6
P1 F1 1.6045(15) .
P1 F1 1.6045(15) 5_657
N1 C1 1.331(3) .
N1 C2 1.462(4) .
N1 C3 1.467(4) .
N2 C1 1.336(4) .
N2 C4 1.460(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2 F1 0.87(4) 2.37(4) 3.110(3) 143(2)
