#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:37:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179757 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/53/7005358.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_7005358
loop_
_publ_author_name
'Stol, Marianne'
'Snelders, Dennis J. M.'
'Kooijman, Huub'
'Spek, Anthony L.'
'van Klink, Gerard P. M.'
'van Koten, Gerard'
_publ_section_title
;
 A new, easily recyclable arylating agent based on a
 diphosphino-digold(I) complex.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2589
_journal_page_last               2593
_journal_paper_doi               10.1039/b701271c
_journal_year                    2007
_chemical_formula_moiety         'C60 H66 Au2 N4 P2, C7 H8'
_chemical_formula_sum            'C67 H74 Au2 N4 P2'
_chemical_formula_weight         1391.18
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.35(3)
_cell_angle_beta                 90.04(4)
_cell_angle_gamma                115.51(4)
_cell_formula_units_Z            1
_cell_length_a                   10.6883(10)
_cell_length_b                   11.8062(10)
_cell_length_c                   13.7445(10)
_cell_measurement_temperature    150(2)
_cell_volume                     1505.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)''
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43053
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    4.964
_exptl_absorpt_correction_T_max  0.4371
_exptl_absorpt_correction_T_min  0.3177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON/MULABS (Spek, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6878
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0253P)²+1.2048P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0527
_reflns_number_gt                6469
_reflns_number_total             6878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701271c.txt
_cod_data_source_block           shelxl
_cod_database_code               7005358
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.058984(9) 0.469721(8) 0.269726(7) 0.02215(4) Uani 1 1 d . . .
P1 P 0.19958(7) 0.68335(6) 0.27849(5) 0.01946(12) Uani 1 1 d . . .
N1 N -0.3442(3) 0.3635(3) 0.3528(2) 0.0371(6) Uani 1 1 d . . .
N2 N 0.1813(3) 0.1670(3) 0.2087(2) 0.0447(7) Uani 1 1 d . . .
C1 C -0.0709(3) 0.2784(2) 0.26656(19) 0.0230(5) Uani 1 1 d . . .
C2 C -0.0470(3) 0.1737(3) 0.2114(2) 0.0266(5) Uani 1 1 d . . .
C3 C -0.1420(3) 0.0455(3) 0.2055(2) 0.0325(6) Uani 1 1 d . . .
H3 H -0.1240 -0.0243 0.1687 0.039 Uiso 1 1 calc R . .
C4 C -0.2618(3) 0.0187(3) 0.2522(2) 0.0354(7) Uani 1 1 d . . .
H4 H -0.3266 -0.0691 0.2469 0.042 Uiso 1 1 calc R . .
C5 C -0.2869(3) 0.1209(3) 0.3069(2) 0.0333(6) Uani 1 1 d . . .
H5 H -0.3699 0.1028 0.3384 0.040 Uiso 1 1 calc R . .
C6 C -0.1915(3) 0.2499(3) 0.3161(2) 0.0266(5) Uani 1 1 d . . .
C7 C -0.2187(3) 0.3573(3) 0.3856(2) 0.0316(6) Uani 1 1 d . . .
H7A H -0.2256 0.3439 0.4540 0.038 Uiso 1 1 calc R . .
H7B H -0.1375 0.4424 0.3908 0.038 Uiso 1 1 calc R . .
C8 C -0.3277(4) 0.4053(4) 0.2599(3) 0.0525(10) Uani 1 1 d . . .
H8A H -0.3108 0.3429 0.2066 0.079 Uiso 1 1 calc R . .
H8B H -0.2483 0.4919 0.2726 0.079 Uiso 1 1 calc R . .
H8C H -0.4129 0.4092 0.2385 0.079 Uiso 1 1 calc R . .
C9 C -0.3702(4) 0.4557(3) 0.4323(3) 0.0439(8) Uani 1 1 d . . .
H9A H -0.4552 0.4597 0.4105 0.066 Uiso 1 1 calc R . .
H9B H -0.2908 0.5424 0.4456 0.066 Uiso 1 1 calc R . .
H9C H -0.3821 0.4270 0.4942 0.066 Uiso 1 1 calc R . .
C10 C 0.0816(3) 0.1939(3) 0.1571(2) 0.0353(7) Uani 1 1 d . . .
H10A H 0.0525 0.1358 0.0872 0.042 Uiso 1 1 calc R . .
H10B H 0.1279 0.2852 0.1529 0.042 Uiso 1 1 calc R . .
C11 C 0.2551(4) 0.2720(4) 0.2997(3) 0.0525(9) Uani 1 1 d . . .
H11A H 0.3204 0.2516 0.3336 0.079 Uiso 1 1 calc R . .
H11B H 0.1877 0.2814 0.3454 0.079 Uiso 1 1 calc R . .
H11C H 0.3070 0.3538 0.2816 0.079 Uiso 1 1 calc R . .
C12 C 0.2818(5) 0.1501(5) 0.1409(4) 0.0769(14) Uani 1 1 d . . .
H12A H 0.3480 0.1324 0.1765 0.115 Uiso 1 1 calc R . .
H12B H 0.3327 0.2300 0.1199 0.115 Uiso 1 1 calc R . .
H12C H 0.2318 0.0767 0.0811 0.115 Uiso 1 1 calc R . .
C13 C 0.1346(3) 0.7937(2) 0.35151(19) 0.0208(5) Uani 1 1 d . . .
C14 C 0.0840(3) 0.7742(3) 0.4422(2) 0.0292(6) Uani 1 1 d . . .
H14 H 0.0833 0.7037 0.4641 0.035 Uiso 1 1 calc R . .
C15 C 0.0346(3) 0.8561(3) 0.5011(2) 0.0285(6) Uani 1 1 d . . .
H15 H 0.0056 0.8440 0.5646 0.034 Uiso 1 1 calc R . .
C16 C 0.0269(2) 0.9560(2) 0.46867(18) 0.0195(5) Uani 1 1 d . . .
C17 C 0.0727(3) 0.9712(3) 0.3759(2) 0.0299(6) Uani 1 1 d . . .
H17 H 0.0666 1.0372 0.3512 0.036 Uiso 1 1 calc R . .
C18 C 0.1272(3) 0.8926(3) 0.3186(2) 0.0276(6) Uani 1 1 d . . .
H18 H 0.1597 0.9068 0.2563 0.033 Uiso 1 1 calc R . .
C19 C 0.2299(3) 0.7292(3) 0.16084(19) 0.0241(5) Uani 1 1 d . . .
C20 C 0.1226(3) 0.6673(3) 0.0810(2) 0.0358(7) Uani 1 1 d . . .
H20 H 0.0376 0.5968 0.0865 0.043 Uiso 1 1 calc R . .
C21 C 0.1391(4) 0.7081(3) -0.0065(2) 0.0478(9) Uani 1 1 d . . .
H21 H 0.0648 0.6667 -0.0604 0.057 Uiso 1 1 calc R . .
C22 C 0.2640(4) 0.8093(3) -0.0154(2) 0.0439(8) Uani 1 1 d . . .
H22 H 0.2760 0.8365 -0.0756 0.053 Uiso 1 1 calc R . .
C23 C 0.3709(4) 0.8702(3) 0.0635(3) 0.0430(8) Uani 1 1 d . . .
H23 H 0.4566 0.9393 0.0573 0.052 Uiso 1 1 calc R . .
C24 C 0.3543(3) 0.8314(3) 0.1517(2) 0.0343(6) Uani 1 1 d . . .
H24 H 0.4280 0.8745 0.2060 0.041 Uiso 1 1 calc R . .
C25 C 0.3732(3) 0.7321(2) 0.3388(2) 0.0229(5) Uani 1 1 d . . .
C26 C 0.4323(3) 0.8243(3) 0.4309(2) 0.0303(6) Uani 1 1 d . . .
H26 H 0.3839 0.8708 0.4647 0.036 Uiso 1 1 calc R . .
C27 C 0.5629(3) 0.8493(3) 0.4743(3) 0.0406(7) Uani 1 1 d . . .
H27 H 0.6024 0.9114 0.5383 0.049 Uiso 1 1 calc R . .
C28 C 0.6345(3) 0.7842(3) 0.4245(3) 0.0397(7) Uani 1 1 d . . .
H28 H 0.7236 0.8019 0.4541 0.048 Uiso 1 1 calc R . .
C29 C 0.5778(3) 0.6937(3) 0.3321(3) 0.0379(7) Uani 1 1 d . . .
H29 H 0.6286 0.6504 0.2976 0.045 Uiso 1 1 calc R . .
C30 C 0.4464(3) 0.6654(3) 0.2891(2) 0.0313(6) Uani 1 1 d . . .
H30 H 0.4064 0.6011 0.2261 0.038 Uiso 1 1 calc R . .
C41 C 0.7519(14) 0.6420(13) 0.0774(11) 0.101(4) Uiso 0.50 1 d P . .
H41A H 0.7677 0.7332 0.0970 0.151 Uiso 0.50 1 calc PR . .
H41B H 0.8129 0.6307 0.0265 0.151 Uiso 0.50 1 calc PR . .
H41C H 0.7729 0.6188 0.1370 0.151 Uiso 0.50 1 calc PR . .
C42 C 0.5962(9) 0.5516(8) 0.0320(7) 0.071(2) Uiso 0.50 1 d PD . .
C43 C 0.5063(10) 0.6061(9) 0.0217(9) 0.074(3) Uiso 0.50 1 d PD . .
H43 H 0.5385 0.6981 0.0421 0.089 Uiso 0.50 1 calc PR . .
C44 C 0.3680(10) 0.5227(10) -0.0194(9) 0.091(3) Uiso 0.50 1 d PD . .
H44 H 0.3044 0.5585 -0.0237 0.109 Uiso 0.50 1 calc PR . .
C45 C 0.3223(10) 0.3920(10) -0.0533(10) 0.088(3) Uiso 0.50 1 d PD . .
H45 H 0.2283 0.3372 -0.0829 0.106 Uiso 0.50 1 calc PR . .
C46 C 0.4133(10) 0.3384(8) -0.0447(8) 0.085(3) Uiso 0.50 1 d PD . .
H46 H 0.3828 0.2468 -0.0688 0.102 Uiso 0.50 1 calc PR . .
C47 C 0.5508(9) 0.4214(8) 0.0002(7) 0.062(2) Uiso 0.50 1 d PD . .
H47 H 0.6130 0.3854 0.0084 0.074 Uiso 0.50 1 calc PR . .
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'
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
_geom_angle_publ_flag
C1 Au1 P1 177.95(7) . . ?
C19 P1 C25 104.37(13) . . ?
C19 P1 C13 103.55(12) . . ?
C25 P1 C13 107.38(12) . . ?
C19 P1 Au1 118.08(10) . . ?
C25 P1 Au1 109.92(9) . . ?
C13 P1 Au1 112.72(9) . . ?
C7 N1 C9 109.3(3) . . ?
C7 N1 C8 110.1(3) . . ?
C9 N1 C8 109.7(3) . . ?
C11 N2 C10 110.7(3) . . ?
C11 N2 C12 109.8(3) . . ?
C10 N2 C12 110.4(3) . . ?
C2 C1 C6 118.2(2) . . ?
C2 C1 Au1 122.00(19) . . ?
C6 C1 Au1 119.72(19) . . ?
C3 C2 C1 120.3(3) . . ?
C3 C2 C10 117.3(2) . . ?
C1 C2 C10 122.4(2) . . ?
C4 C3 C2 120.9(3) . . ?
C3 C4 C5 119.4(3) . . ?
C4 C5 C6 120.6(3) . . ?
C5 C6 C1 120.5(3) . . ?
C5 C6 C7 117.8(2) . . ?
C1 C6 C7 121.7(2) . . ?
N1 C7 C6 114.6(2) . . ?
N2 C10 C2 112.1(2) . . ?
C18 C13 C14 118.3(2) . . ?
C18 C13 P1 122.92(19) . . ?
C14 C13 P1 118.70(19) . . ?
C15 C14 C13 121.0(2) . . ?
C14 C15 C16 121.0(2) . . ?
C17 C16 C15 117.4(2) . . ?
C17 C16 C16 121.3(3) . 2_576 ?
C15 C16 C16 121.3(3) . 2_576 ?
C18 C17 C16 121.8(2) . . ?
C13 C18 C17 120.4(2) . . ?
C20 C19 C24 119.4(3) . . ?
C20 C19 P1 119.2(2) . . ?
C24 C19 P1 121.3(2) . . ?
C21 C20 C19 120.3(3) . . ?
C22 C21 C20 120.0(3) . . ?
C23 C22 C21 119.8(3) . . ?
C22 C23 C24 120.5(3) . . ?
C23 C24 C19 120.1(3) . . ?
C26 C25 C30 119.4(2) . . ?
C26 C25 P1 124.2(2) . . ?
C30 C25 P1 116.3(2) . . ?
C25 C26 C27 120.1(3) . . ?
C28 C27 C26 120.1(3) . . ?
C29 C28 C27 120.4(3) . . ?
C28 C29 C30 120.3(3) . . ?
C29 C30 C25 119.8(3) . . ?
C47 C42 C43 120.4(6) . . ?
C47 C42 C41 119.7(9) . . ?
C43 C42 C41 119.9(9) . . ?
C41 C42 C42 175.2(10) . 2_665 ?
C42 C43 C44 118.5(6) . . ?
C44 C43 C45 142.6(6) . 2_665 ?
C45 C44 C43 121.5(6) . . ?
C44 C45 C46 119.8(7) . . ?
C44 C45 C43 95.9(6) . 2_665 ?
C45 C46 C47 118.9(6) . . ?
C42 C47 C46 121.0(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 2.069(3) . ?
Au1 P1 2.2844(12) . ?
P1 C19 1.816(3) . ?
P1 C25 1.818(3) . ?
P1 C13 1.822(3) . ?
N1 C7 1.451(4) . ?
N1 C9 1.459(4) . ?
N1 C8 1.464(4) . ?
N2 C11 1.453(5) . ?
N2 C10 1.463(4) . ?
N2 C12 1.468(5) . ?
C1 C2 1.406(4) . ?
C1 C6 1.407(4) . ?
C2 C3 1.393(4) . ?
C2 C10 1.520(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.386(4) . ?
C5 C6 1.393(4) . ?
C6 C7 1.524(4) . ?
C13 C18 1.384(4) . ?
C13 C14 1.391(4) . ?
C14 C15 1.387(4) . ?
C15 C16 1.393(3) . ?
C16 C17 1.391(4) . ?
C16 C16 1.491(5) 2_576 ?
C17 C18 1.388(4) . ?
C19 C20 1.390(4) . ?
C19 C24 1.390(4) . ?
C20 C21 1.387(4) . ?
C21 C22 1.387(5) . ?
C22 C23 1.380(5) . ?
C23 C24 1.384(4) . ?
C25 C26 1.383(4) . ?
C25 C30 1.401(4) . ?
C26 C27 1.396(4) . ?
C27 C28 1.375(5) . ?
C28 C29 1.375(5) . ?
C29 C30 1.390(4) . ?
C41 C42 1.561(15) . ?
C42 C47 1.347(8) . ?
C42 C43 1.391(8) . ?
C43 C44 1.394(9) . ?
C44 C45 1.353(9) . ?
C45 C46 1.390(9) . ?
C46 C47 1.399(9) . ?
