#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:49:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179395 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/92/4329209.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_4329209
loop_
_publ_author_name
'Atiya T. Overton'
'Ahmed A. Mohamed'
_publ_section_title
;
 Gold(III) Diazonium Complexes for Electrochemical Reductive Grafting
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5500
_journal_page_last               5502
_journal_paper_doi               10.1021/ic300307z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C7 H4 Au Cl4 N3'
_chemical_formula_weight         468.90
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.681(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.551(5)
_cell_length_b                   11.393(4)
_cell_length_c                   15.612(6)
_cell_measurement_temperature    110(2)
_cell_volume                     2376.0(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26964
_diffrn_reflns_theta_full        28.68
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    13.250
_exptl_absorpt_correction_T_max  0.266
_exptl_absorpt_correction_T_min  0.222
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.622
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0185P)²+1.9250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                4894
_reflns_number_total             6124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300307z_si_001_3.cif
_cod_data_source_block           diazonium
_cod_original_cell_volume        2375.8(15)
_cod_database_code               4329209
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Au2 Au 1.006191(13) 0.655631(15) 0.283909(11) 0.01527(5) Uani 1 1 d .
Au1 Au 0.717371(13) 0.215654(15) 0.956425(11) 0.01416(5) Uani 1 1 d .
Cl6 Cl 0.93003(10) 0.50655(10) 0.20138(8) 0.0268(3) Uani 1 1 d .
Cl5 Cl 0.88939(9) 0.64144(12) 0.37182(8) 0.0289(3) Uani 1 1 d .
Cl7 Cl 1.12566(9) 0.66625(10) 0.19681(8) 0.0219(2) Uani 1 1 d .
Cl8 Cl 1.07811(10) 0.80981(11) 0.36458(8) 0.0256(3) Uani 1 1 d .
Cl1 Cl 0.64061(9) 0.38692(10) 0.90496(8) 0.0208(2) Uani 1 1 d .
Cl2 Cl 0.83350(9) 0.31840(10) 1.04904(7) 0.0213(2) Uani 1 1 d .
Cl3 Cl 0.79127(9) 0.04428(10) 1.00500(8) 0.0231(3) Uani 1 1 d .
Cl4 Cl 0.60169(9) 0.11213(10) 0.86366(7) 0.0208(2) Uani 1 1 d .
N3 N 0.7129(3) 0.5365(4) 0.7351(3) 0.0236(9) Uani 1 1 d .
N2 N 0.7632(3) 0.5848(3) 0.7843(3) 0.0173(8) Uani 1 1 d .
C1 C 0.8251(3) 0.6475(4) 0.8508(3) 0.0166(10) Uani 1 1 d .
N4 N 0.8090(3) -0.1736(4) 0.1702(3) 0.0275(10) Uani 1 1 d .
N5 N 0.9001(3) 0.2966(4) 0.4271(3) 0.0227(9) Uani 1 1 d .
N6 N 0.9083(3) 0.3747(4) 0.4680(3) 0.0299(10) Uani 1 1 d .
C2 C 0.8441(4) 0.5977(4) 0.9315(3) 0.0234(11) Uani 1 1 d .
H2 H 0.8225 0.5221 0.9413 0.028 Uiso 1 1 calc R
C3 C 0.8967(4) 0.6640(4) 0.9978(3) 0.0230(11) Uani 1 1 d .
H3 H 0.9108 0.6342 1.0539 0.028 Uiso 1 1 calc R
C4 C 0.9287(3) 0.7767(4) 0.9797(3) 0.0175(10) Uani 1 1 d .
C6 C 0.8574(4) 0.7568(4) 0.8290(3) 0.0203(10) Uani 1 1 d .
H6 H 0.8440 0.7850 0.7723 0.024 Uiso 1 1 calc R
C5 C 0.9107(4) 0.8217(4) 0.8959(3) 0.0204(10) Uani 1 1 d .
H5 H 0.9345 0.8958 0.8848 0.024 Uiso 1 1 calc R
C14 C 0.8295(4) -0.0957(5) 0.2149(3) 0.0242(11) Uani 1 1 d .
C8 C 0.8528(3) 0.0052(4) 0.2713(3) 0.0179(10) Uani 1 1 d .
C9 C 0.8547(4) -0.0068(4) 0.3597(3) 0.0236(11) Uani 1 1 d .
H9 H 0.8450 -0.0801 0.3832 0.028 Uiso 1 1 calc R
C10 C 0.8709(4) 0.0896(4) 0.4126(3) 0.0240(11) Uani 1 1 d .
H10 H 0.8709 0.0845 0.4720 0.029 Uiso 1 1 calc R
C11 C 0.8871(4) 0.1942(4) 0.3735(3) 0.0217(11) Uani 1 1 d .
C13 C 0.8711(4) 0.1123(4) 0.2337(3) 0.0219(11) Uani 1 1 d .
H13 H 0.8716 0.1177 0.1743 0.026 Uiso 1 1 calc R
C12 C 0.8885(4) 0.2105(4) 0.2863(3) 0.0212(10) Uani 1 1 d .
H12 H 0.9005 0.2837 0.2638 0.025 Uiso 1 1 calc R
N1 N 1.0129(3) 0.9060(4) 1.1054(3) 0.0257(10) Uani 1 1 d .
C7 C 0.9776(3) 0.8484(4) 1.0494(3) 0.0197(10) Uani 1 1 d .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Cl5 Au2 Cl6 89.61(5)
Cl5 Au2 Cl8 89.86(5)
Cl6 Au2 Cl8 177.92(5)
Cl5 Au2 Cl7 178.70(5)
Cl6 Au2 Cl7 90.10(5)
Cl8 Au2 Cl7 90.46(5)
Cl3 Au1 Cl2 90.64(5)
Cl3 Au1 Cl4 89.13(5)
Cl2 Au1 Cl4 179.72(4)
Cl3 Au1 Cl1 178.80(4)
Cl2 Au1 Cl1 90.54(5)
Cl4 Au1 Cl1 89.70(5)
N3 N2 C1 177.2(5)
C2 C1 C6 125.7(4)
C2 C1 N2 117.6(4)
C6 C1 N2 116.6(4)
N6 N5 C11 178.8(5)
C1 C2 C3 117.2(5)
C1 C2 H2 121.4
C3 C2 H2 121.4
C2 C3 C4 119.4(4)
C2 C3 H3 120.3
C4 C3 H3 120.3
C5 C4 C3 121.2(4)
C5 C4 C7 119.4(4)
C3 C4 C7 119.3(4)
C5 C6 C1 116.3(4)
C5 C6 H6 121.8
C1 C6 H6 121.8
C6 C5 C4 120.1(4)
C6 C5 H5 120.0
C4 C5 H5 120.0
N4 C14 C8 178.3(6)
C9 C8 C13 122.1(4)
C9 C8 C14 119.5(4)
C13 C8 C14 118.3(4)
C10 C9 C8 119.7(4)
C10 C9 H9 120.1
C8 C9 H9 120.1
C9 C10 C11 116.8(5)
C9 C10 H10 121.6
C11 C10 H10 121.6
C10 C11 C12 125.9(5)
C10 C11 N5 117.5(4)
C12 C11 N5 116.6(4)
C12 C13 C8 118.9(4)
C12 C13 H13 120.6
C8 C13 H13 120.6
C11 C12 C13 116.6(4)
C11 C12 H12 121.7
C13 C12 H12 121.7
N1 C7 C4 177.4(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Au2 Cl5 2.2683(14)
Au2 Cl6 2.2721(13)
Au2 Cl8 2.2822(13)
Au2 Cl7 2.2858(13)
Au1 Cl3 2.2659(13)
Au1 Cl2 2.2742(12)
Au1 Cl4 2.2764(12)
Au1 Cl1 2.2921(13)
N3 N2 1.087(5)
N2 C1 1.414(6)
C1 C2 1.367(6)
C1 C6 1.381(6)
N4 C14 1.134(6)
N5 N6 1.089(5)
N5 C11 1.429(6)
C2 C3 1.379(7)
C2 H2 0.9300
C3 C4 1.398(6)
C3 H3 0.9300
C4 C5 1.388(6)
C4 C7 1.431(6)
C6 C5 1.381(6)
C6 H6 0.9300
C5 H5 0.9300
C14 C8 1.450(7)
C8 C9 1.383(6)
C8 C13 1.394(6)
C9 C10 1.370(7)
C9 H9 0.9300
C10 C11 1.372(7)
C10 H10 0.9300
C11 C12 1.378(7)
C13 C12 1.384(7)
C13 H13 0.9300
C12 H12 0.9300
N1 C7 1.133(6)
