Electronic Supplementary Material for CrystEngComm
This Journal is (c) The Royal Society of Chemistry 2007
data_global
_journal_name_full CrystEngComm
_journal_coden_Cambridge 1350
_publ_contact_author_name 'Andrea Deak'
_publ_contact_author_address
; Institute of Structural Chemistry,
Chemical Research Center of the Hungarian Academy of Sciences,
H-1525 Budapest,
P.O.Box 17,
Hungary
;
_publ_contact_author_email deak@chemres.hu
_publ_contact_author_phone 00-36-1-438-1161/327
_publ_contact_author_fax 00-36-1-438-4141/201
loop_
_publ_author_name
_publ_author_address
'Andrea Deak'
; Institute of Structural Chemistry,
Chemical Research Center of the Hungarian Academy of Sciences,
H-1525 Budapest,
P.O. Box 17,
Hungary
;
'Tunde Tunyogi'
; Institute of Structural Chemistry,
Chemical Research Center of the Hungarian Academy of Sciences,
H-1525 Budapest,
P.O. Box 17,
Hungary
;
'Gabor Tarkanyi'
; Institute of Structural Chemistry,
Chemical Research Center of the Hungarian Academy of Sciences,
H-1525 Budapest,
P.O. Box 17,
Hungary
;
'Peter Kiraly'
; Institute of Structural Chemistry,
Chemical Research Center of the Hungarian Academy of Sciences,
H-1525 Budapest,
P.O. Box 17,
Hungary
;
'Gabor Palinkas'
; Institute of Structural Chemistry,
Chemical Research Center of the Hungarian Academy of Sciences,
H-1525 Budapest,
P.O. Box 17,
Hungary
;
_publ_section_title
;
;
# Attachment 'complex11.cif'
data_complex1
_database_code_depnum_ccdc_archive 'CCDC 641198'
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C34 H24 Au2 F6 O4 P2, 2(C H2 Cl2)'
_chemical_formula_sum 'C36 H28 Au2 Cl4 F6 O4 P2'
_chemical_formula_weight 1236.26
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.143(4)
_cell_length_b 12.325(4)
_cell_length_c 13.869(4)
_cell_angle_alpha 99.008(12)
_cell_angle_beta 96.572(12)
_cell_angle_gamma 95.481(13)
_cell_volume 2022.9(11)
_cell_formula_units_Z 2
_cell_measurement_temperature 153(2)
_cell_measurement_reflns_used 49715
_cell_measurement_theta_min 3.00
_cell_measurement_theta_max 28.46
_exptl_crystal_description prism
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.26
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.030
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1172
_exptl_absorpt_coefficient_mu 7.652
_exptl_absorpt_correction_type empirical
_exptl_absorpt_correction_T_min 0.102
_exptl_absorpt_correction_T_max 0.135
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 153(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'R Axis Rapid'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 59040
_diffrn_reflns_av_R_equivalents 0.1159
_diffrn_reflns_av_sigmaI/netI 0.0741
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 3.00
_diffrn_reflns_theta_max 25.03
_reflns_number_total 7151
_reflns_number_gt 6223
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'WinGX (Farrugia, 1999), PLATON (Spek, 2003)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+26.7093P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7151
_refine_ls_number_parameters 447
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0629
_refine_ls_R_factor_gt 0.0558
_refine_ls_wR_factor_ref 0.1424
_refine_ls_wR_factor_gt 0.1372
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_restrained_S_all 1.060
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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 0.13374(3) 0.08444(3) 0.16735(3) 0.03013(13) Uani 1 1 d . . .
Au2 Au 0.27471(3) 0.11971(3) 0.35620(3) 0.03102(13) Uani 1 1 d . . .
P1 P 0.00479(19) -0.0468(2) 0.18995(18) 0.0274(5) Uani 1 1 d . . .
P2 P 0.2426(2) -0.0603(2) 0.35613(18) 0.0274(5) Uani 1 1 d . . .
O1 O 0.2318(6) 0.2163(6) 0.1318(5) 0.0393(17) Uani 1 1 d . . .
O2 O 0.3955(7) 0.1469(7) 0.1565(6) 0.050(2) Uani 1 1 d . . .
O3 O 0.3120(8) 0.2876(6) 0.3647(7) 0.056(2) Uani 1 1 d . . .
O4 O 0.1341(15) 0.3173(12) 0.3628(16) 0.163(9) Uani 1 1 d . . .
C7 C 0.3375(9) 0.2156(9) 0.1366(7) 0.038(2) Uani 1 1 d . . .
C8 C 0.3970(7) 0.3236(7) 0.1063(8) 0.062(4) Uani 1 1 d . . .
F8A F 0.4369(13) 0.2967(7) 0.0223(9) 0.113(4) Uani 0.50 1 calc PR . .
F8B F 0.4796(10) 0.3687(10) 0.1756(9) 0.113(4) Uani 0.50 1 calc PR . .
F8C F 0.3239(7) 0.3950(8) 0.0960(13) 0.113(4) Uani 0.50 1 calc PR . .
F8D F 0.3900(13) 0.4103(7) 0.1736(10) 0.113(4) Uani 0.50 1 calc PR . .
F8E F 0.3474(10) 0.3382(10) 0.0203(9) 0.113(4) Uani 0.50 1 calc PR . .
F8F F 0.5030(7) 0.3119(8) 0.0999(13) 0.113(4) Uani 0.50 1 calc PR . .
C9 C 0.2371(19) 0.3471(10) 0.3681(15) 0.099(7) Uani 1 1 d D . .
C10 C 0.2758(13) 0.4731(7) 0.3715(12) 0.206(19) Uani 1 1 d D . .
F10A F 0.250(3) 0.5309(7) 0.4527(16) 0.186(9) Uani 0.50 1 calc PR . .
F10B F 0.225(2) 0.5065(9) 0.2940(17) 0.186(9) Uani 0.50 1 calc PR . .
F10C F 0.3848(14) 0.4877(7) 0.371(3) 0.186(9) Uani 0.50 1 calc PR . .
F10D F 0.323(3) 0.4858(7) 0.2923(17) 0.186(9) Uani 0.50 1 calc PR . .
F10E F 0.348(2) 0.5102(9) 0.4510(17) 0.186(9) Uani 0.50 1 calc PR . .
F10F F 0.1885(14) 0.5291(7) 0.374(3) 0.186(9) Uani 0.50 1 calc PR . .
C1 C 0.0031(8) -0.0905(8) 0.3117(7) 0.0275(19) Uani 1 1 d . . .
C2 C 0.0988(8) -0.0997(8) 0.3765(7) 0.029(2) Uani 1 1 d . . .
C3 C 0.0830(9) -0.1392(9) 0.4640(7) 0.037(2) Uani 1 1 d . . .
H3 H 0.1464 -0.1458 0.5086 0.044 Uiso 1 1 calc R . .
C4 C -0.0213(9) -0.1685(10) 0.4868(8) 0.044(3) Uani 1 1 d . . .
H4 H -0.0295 -0.1952 0.5466 0.053 Uiso 1 1 calc R . .
C5 C -0.1145(9) -0.1592(10) 0.4227(7) 0.039(2) Uani 1 1 d . . .
H5 H -0.1872 -0.1802 0.4374 0.047 Uiso 1 1 calc R . .
C6 C -0.1004(8) -0.1191(9) 0.3369(8) 0.036(2) Uani 1 1 d . . .
H6 H -0.1646 -0.1109 0.2939 0.043 Uiso 1 1 calc R . .
C1A C -0.0040(8) -0.1739(8) 0.1014(7) 0.028(2) Uani 1 1 d . . .
C2A C 0.0498(8) -0.1741(9) 0.0193(8) 0.037(2) Uani 1 1 d . . .
H2A H 0.0945 -0.1094 0.0113 0.044 Uiso 1 1 calc R . .
C3A C 0.0390(10) -0.2684(10) -0.0520(8) 0.049(3) Uani 1 1 d . . .
H3A H 0.0774 -0.2687 -0.1080 0.059 Uiso 1 1 calc R . .
C4A C -0.0273(11) -0.3614(10) -0.0413(9) 0.050(3) Uani 1 1 d . . .
H4A H -0.0372 -0.4248 -0.0915 0.060 Uiso 1 1 calc R . .
C5A C -0.0794(10) -0.3637(9) 0.0413(9) 0.047(3) Uani 1 1 d . . .
H5A H -0.1230 -0.4292 0.0492 0.057 Uiso 1 1 calc R . .
C6A C -0.0682(9) -0.2700(9) 0.1133(8) 0.042(3) Uani 1 1 d . . .
H6A H -0.1041 -0.2713 0.1705 0.050 Uiso 1 1 calc R . .
C1B C -0.1296(8) 0.0044(9) 0.1694(7) 0.033(2) Uani 1 1 d . . .
C2B C -0.2153(8) -0.0500(9) 0.1003(8) 0.036(2) Uani 1 1 d . . .
H2B H -0.2058 -0.1182 0.0613 0.044 Uiso 1 1 calc R . .
C3B C -0.3167(10) -0.0050(11) 0.0873(9) 0.052(3) Uani 1 1 d . . .
H3B H -0.3754 -0.0430 0.0392 0.062 Uiso 1 1 calc R . .
C4B C -0.3320(10) 0.0916(12) 0.1423(10) 0.057(3) Uani 1 1 d . . .
H4B H -0.4009 0.1215 0.1325 0.069 Uiso 1 1 calc R . .
C5B C -0.2466(10) 0.1471(11) 0.2131(9) 0.052(3) Uani 1 1 d . . .
H5B H -0.2582 0.2137 0.2535 0.062 Uiso 1 1 calc R . .
C6B C -0.1438(9) 0.1054(9) 0.2252(8) 0.039(2) Uani 1 1 d . . .
H6B H -0.0840 0.1455 0.2710 0.047 Uiso 1 1 calc R . .
C1C C 0.2653(8) -0.1509(8) 0.2467(7) 0.028(2) Uani 1 1 d . . .
C2C C 0.3363(8) -0.1134(9) 0.1838(8) 0.037(2) Uani 1 1 d . . .
H2C H 0.3685 -0.0384 0.1963 0.044 Uiso 1 1 calc R . .
C3C C 0.3602(11) -0.1841(11) 0.1034(9) 0.053(3) Uani 1 1 d . . .
H3C H 0.4084 -0.1580 0.0606 0.064 Uiso 1 1 calc R . .
C4C C 0.3135(12) -0.2934(11) 0.0857(10) 0.058(3) Uani 1 1 d . . .
H4C H 0.3311 -0.3429 0.0314 0.070 Uiso 1 1 calc R . .
C5C C 0.2426(10) -0.3305(10) 0.1454(9) 0.050(3) Uani 1 1 d . . .
H5C H 0.2099 -0.4053 0.1314 0.060 Uiso 1 1 calc R . .
C6C C 0.2174(9) -0.2616(9) 0.2256(8) 0.038(2) Uani 1 1 d . . .
H6C H 0.1676 -0.2888 0.2667 0.046 Uiso 1 1 calc R . .
C1D C 0.3289(8) -0.0973(9) 0.4585(7) 0.035(2) Uani 1 1 d . . .
C2D C 0.3579(11) -0.2018(11) 0.4589(9) 0.053(3) Uani 1 1 d . . .
H2D H 0.3355 -0.2572 0.4024 0.063 Uiso 1 1 calc R . .
C3D C 0.4205(11) -0.2282(12) 0.5419(11) 0.065(4) Uani 1 1 d . . .
H3D H 0.4422 -0.3003 0.5407 0.078 Uiso 1 1 calc R . .
C4D C 0.4501(10) -0.1495(13) 0.6244(9) 0.057(4) Uani 1 1 d . . .
H4D H 0.4897 -0.1675 0.6817 0.069 Uiso 1 1 calc R . .
C5D C 0.4221(10) -0.0448(13) 0.6238(8) 0.053(3) Uani 1 1 d . . .
H5D H 0.4436 0.0103 0.6807 0.063 Uiso 1 1 calc R . .
C6D C 0.3635(9) -0.0185(10) 0.5419(8) 0.041(3) Uani 1 1 d . . .
H6D H 0.3463 0.0551 0.5423 0.049 Uiso 1 1 calc R . .
C11 C 0.054(2) 0.496(4) 0.638(3) 0.28(3) Uani 1 1 d D . .
H11A H -0.0220 0.5180 0.6388 0.338 Uiso 1 1 calc R . .
H11B H 0.0519 0.4278 0.5895 0.338 Uiso 1 1 calc R . .
Cl1 Cl 0.104(3) 0.482(2) 0.7368(18) 0.71(4) Uani 1 1 d . . .
Cl2 Cl 0.1499(15) 0.6074(13) 0.6100(12) 0.305(8) Uani 1 1 d D . .
C12 C 0.407(4) 0.385(3) 0.7524(17) 0.44(5) Uani 1 1 d D . .
H12A H 0.4824 0.4215 0.7826 0.523 Uiso 1 1 calc R . .
H12B H 0.3491 0.4325 0.7702 0.523 Uiso 1 1 calc R . .
Cl3 Cl 0.3813(8) 0.2546(11) 0.7741(11) 0.266(7) Uani 1 1 d . . .
Cl4 Cl 0.3983(10) 0.3357(14) 0.6201(10) 0.310(9) Uani 1 1 d 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 0.0242(2) 0.0357(2) 0.0314(2) 0.01255(16) 0.00044(15) 0.00077(15)
Au2 0.0306(2) 0.0293(2) 0.0320(2) 0.00703(15) -0.00028(16) -0.00056(15)
P1 0.0229(12) 0.0321(13) 0.0275(12) 0.0101(10) -0.0008(9) 0.0020(9)
P2 0.0238(12) 0.0302(13) 0.0272(12) 0.0080(10) -0.0032(9) 0.0005(9)
O1 0.029(4) 0.041(4) 0.050(4) 0.021(3) -0.002(3) 0.002(3)
O2 0.042(4) 0.049(5) 0.063(5) 0.023(4) 0.000(4) 0.010(4)
O3 0.073(6) 0.023(4) 0.066(6) 0.004(4) 0.000(5) -0.007(4)
O4 0.164(15) 0.101(11) 0.29(2) 0.119(13) 0.163(17) 0.075(10)
C7 0.037(6) 0.048(7) 0.030(5) 0.009(5) 0.005(4) 0.004(5)
C8 0.036(7) 0.069(9) 0.076(9) 0.009(7) 0.008(6) -0.019(6)
F8A 0.076(6) 0.093(7) 0.189(12) 0.067(7) 0.044(6) 0.002(5)
F8B 0.076(6) 0.093(7) 0.189(12) 0.067(7) 0.044(6) 0.002(5)
F8C 0.076(6) 0.093(7) 0.189(12) 0.067(7) 0.044(6) 0.002(5)
F8D 0.076(6) 0.093(7) 0.189(12) 0.067(7) 0.044(6) 0.002(5)
F8E 0.076(6) 0.093(7) 0.189(12) 0.067(7) 0.044(6) 0.002(5)
F8F 0.076(6) 0.093(7) 0.189(12) 0.067(7) 0.044(6) 0.002(5)
C9 0.155(19) 0.040(8) 0.132(16) 0.031(9) 0.111(15) 0.025(10)
C10 0.39(5) 0.12(2) 0.17(3) 0.049(19) 0.15(3) 0.17(3)
F10A 0.233(18) 0.067(6) 0.30(2) 0.053(10) 0.147(17) 0.029(8)
F10B 0.233(18) 0.067(6) 0.30(2) 0.053(10) 0.147(17) 0.029(8)
F10C 0.233(18) 0.067(6) 0.30(2) 0.053(10) 0.147(17) 0.029(8)
F10D 0.233(18) 0.067(6) 0.30(2) 0.053(10) 0.147(17) 0.029(8)
F10E 0.233(18) 0.067(6) 0.30(2) 0.053(10) 0.147(17) 0.029(8)
F10F 0.233(18) 0.067(6) 0.30(2) 0.053(10) 0.147(17) 0.029(8)
C1 0.028(5) 0.028(5) 0.028(5) 0.010(4) 0.005(4) 0.004(4)
C2 0.030(5) 0.029(5) 0.026(5) 0.008(4) 0.000(4) -0.001(4)
C3 0.034(5) 0.041(6) 0.034(5) 0.014(4) -0.001(4) -0.006(4)
C4 0.047(7) 0.053(7) 0.033(6) 0.019(5) 0.007(5) -0.006(5)
C5 0.032(5) 0.055(7) 0.032(5) 0.013(5) 0.010(4) -0.002(5)
C6 0.028(5) 0.046(6) 0.036(6) 0.016(5) -0.001(4) 0.003(4)
C1A 0.026(5) 0.031(5) 0.029(5) 0.010(4) 0.003(4) 0.006(4)
C2A 0.035(5) 0.040(6) 0.037(6) 0.015(5) 0.004(4) 0.007(4)
C3A 0.053(7) 0.059(8) 0.035(6) 0.008(5) 0.005(5) 0.007(6)
C4A 0.063(8) 0.036(6) 0.047(7) -0.002(5) 0.005(6) 0.006(5)
C5A 0.048(7) 0.036(6) 0.055(7) 0.007(5) 0.002(5) -0.004(5)
C6A 0.045(6) 0.043(6) 0.040(6) 0.012(5) 0.012(5) 0.002(5)
C1B 0.031(5) 0.045(6) 0.025(5) 0.017(4) 0.004(4) 0.008(4)
C2B 0.026(5) 0.046(6) 0.037(6) 0.012(5) -0.003(4) 0.006(4)
C3B 0.033(6) 0.069(9) 0.055(7) 0.018(6) -0.004(5) 0.009(6)
C4B 0.040(7) 0.079(10) 0.064(8) 0.029(7) 0.008(6) 0.025(6)
C5B 0.051(7) 0.063(8) 0.052(7) 0.018(6) 0.020(6) 0.028(6)
C6B 0.037(6) 0.037(6) 0.043(6) 0.009(5) 0.001(5) 0.008(4)
C1C 0.029(5) 0.025(5) 0.031(5) 0.005(4) -0.004(4) 0.008(4)
C2C 0.034(5) 0.037(6) 0.042(6) 0.012(5) 0.005(4) 0.010(4)
C3C 0.057(8) 0.068(9) 0.040(6) 0.015(6) 0.015(6) 0.014(6)
C4C 0.069(9) 0.052(8) 0.052(8) -0.004(6) 0.008(6) 0.024(7)
C5C 0.054(7) 0.035(6) 0.058(8) -0.001(5) 0.005(6) 0.003(5)
C6C 0.036(6) 0.035(6) 0.043(6) 0.008(5) -0.001(5) 0.001(4)
C1D 0.024(5) 0.049(6) 0.033(5) 0.013(5) -0.006(4) 0.007(4)
C2D 0.055(7) 0.054(8) 0.046(7) 0.010(6) -0.014(6) 0.010(6)
C3D 0.057(8) 0.060(9) 0.081(10) 0.037(8) -0.015(7) 0.013(7)
C4D 0.034(6) 0.097(11) 0.044(7) 0.040(7) -0.010(5) -0.004(6)
C5D 0.038(6) 0.092(10) 0.028(6) 0.018(6) 0.001(5) 0.001(6)
C6D 0.041(6) 0.047(7) 0.037(6) 0.017(5) -0.001(5) 0.006(5)
C11 0.072(19) 0.50(9) 0.29(5) 0.18(6) 0.01(2) -0.03(3)
Cl1 1.44(9) 0.58(4) 0.46(3) 0.42(3) 0.64(5) 0.74(5)
Cl2 0.311(18) 0.254(15) 0.300(17) -0.042(13) 0.000(14) -0.027(13)
C12 0.59(10) 0.23(5) 0.35(6) 0.12(4) -0.30(7) -0.32(6)
Cl3 0.141(7) 0.269(13) 0.355(17) 0.104(12) -0.115(9) -0.046(8)
Cl4 0.199(10) 0.42(2) 0.245(13) -0.095(13) 0.103(10) -0.152(12)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O1 2.078(7) . ?
Au1 P1 2.226(2) . ?
Au1 Au2 2.9077(9) . ?
Au2 O3 2.057(8) . ?
Au2 P2 2.215(3) . ?
P1 C1B 1.814(10) . ?
P1 C1A 1.819(10) . ?
P1 C1 1.852(9) . ?
P2 C1C 1.802(10) . ?
P2 C1D 1.809(9) . ?
P2 C2 1.833(10) . ?
O1 C7 1.279(12) . ?
O2 C7 1.195(13) . ?
O3 C9 1.22(2) . ?
O4 C9 1.26(3) . ?
C7 C8 1.591(12) . ?
C9 C10 1.571(13) . ?
C1 C6 1.371(13) . ?
C1 C2 1.411(13) . ?
C2 C3 1.402(13) . ?
C3 C4 1.369(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(14) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1A C2A 1.376(14) . ?
C1A C6A 1.397(14) . ?
C2A C3A 1.388(16) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.374(17) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.374(17) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.387(16) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C1B C2B 1.374(14) . ?
C1B C6B 1.396(15) . ?
C2B C3B 1.402(15) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.351(19) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.389(19) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.398(15) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
C1C C2C 1.393(14) . ?
C1C C6C 1.404(14) . ?
C2C C3C 1.381(16) . ?
C2C H2C 0.9500 . ?
C3C C4C 1.384(19) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.356(18) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.372(16) . ?
C5C H5C 0.9500 . ?
C6C H6C 0.9500 . ?
C1D C2D 1.368(16) . ?
C1D C6D 1.384(15) . ?
C2D C3D 1.404(17) . ?
C2D H2D 0.9500 . ?
C3D C4D 1.37(2) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.37(2) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.369(15) . ?
C5D H5D 0.9500 . ?
C6D H6D 0.9500 . ?
C11 Cl1 1.48(4) . ?
C11 Cl2 1.825(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 Cl3 1.69(4) . ?
C12 Cl4 1.827(19) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
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
O1 Au1 P1 170.1(2) . . ?
O1 Au1 Au2 87.7(2) . . ?
P1 Au1 Au2 100.53(6) . . ?
O3 Au2 P2 176.1(3) . . ?
O3 Au2 Au1 95.9(2) . . ?
P2 Au2 Au1 87.97(6) . . ?
C1B P1 C1A 105.5(5) . . ?
C1B P1 C1 102.8(4) . . ?
C1A P1 C1 105.7(4) . . ?
C1B P1 Au1 107.2(3) . . ?
C1A P1 Au1 113.5(3) . . ?
C1 P1 Au1 120.7(3) . . ?
C1C P2 C1D 107.0(5) . . ?
C1C P2 C2 106.1(4) . . ?
C1D P2 C2 105.0(4) . . ?
C1C P2 Au2 116.7(3) . . ?
C1D P2 Au2 109.9(4) . . ?
C2 P2 Au2 111.4(3) . . ?
C7 O1 Au1 119.9(7) . . ?
C9 O3 Au2 119.5(9) . . ?
O2 C7 O1 130.7(10) . . ?
O2 C7 C8 117.2(9) . . ?
O1 C7 C8 112.1(9) . . ?
O3 C9 O4 127.2(13) . . ?
O3 C9 C10 114.7(15) . . ?
O4 C9 C10 118.0(16) . . ?
C6 C1 C2 119.1(9) . . ?
C6 C1 P1 115.9(7) . . ?
C2 C1 P1 125.0(7) . . ?
C3 C2 C1 117.8(9) . . ?
C3 C2 P2 117.5(7) . . ?
C1 C2 P2 124.7(7) . . ?
C4 C3 C2 121.9(10) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119.8(10) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 119.0(9) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C1 C6 C5 122.3(9) . . ?
C1 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C2A C1A C6A 119.4(9) . . ?
C2A C1A P1 119.4(8) . . ?
C6A C1A P1 121.1(7) . . ?
C1A C2A C3A 120.3(10) . . ?
C1A C2A H2A 119.8 . . ?
C3A C2A H2A 119.8 . . ?
C4A C3A C2A 119.8(11) . . ?
C4A C3A H3A 120.1 . . ?
C2A C3A H3A 120.1 . . ?
C5A C4A C3A 120.7(11) . . ?
C5A C4A H4A 119.7 . . ?
C3A C4A H4A 119.7 . . ?
C4A C5A C6A 119.8(11) . . ?
C4A C5A H5A 120.1 . . ?
C6A C5A H5A 120.1 . . ?
C5A C6A C1A 119.9(10) . . ?
C5A C6A H6A 120.0 . . ?
C1A C6A H6A 120.0 . . ?
C2B C1B C6B 119.5(9) . . ?
C2B C1B P1 123.0(8) . . ?
C6B C1B P1 117.5(8) . . ?
C1B C2B C3B 120.1(11) . . ?
C1B C2B H2B 120.0 . . ?
C3B C2B H2B 120.0 . . ?
C4B C3B C2B 120.9(11) . . ?
C4B C3B H3B 119.5 . . ?
C2B C3B H3B 119.5 . . ?
C3B C4B C5B 119.7(11) . . ?
C3B C4B H4B 120.1 . . ?
C5B C4B H4B 120.1 . . ?
C4B C5B C6B 120.2(12) . . ?
C4B C5B H5B 119.9 . . ?
C6B C5B H5B 119.9 . . ?
C1B C6B C5B 119.4(10) . . ?
C1B C6B H6B 120.3 . . ?
C5B C6B H6B 120.3 . . ?
C2C C1C C6C 118.5(9) . . ?
C2C C1C P2 120.1(7) . . ?
C6C C1C P2 121.3(8) . . ?
C3C C2C C1C 120.6(11) . . ?
C3C C2C H2C 119.7 . . ?
C1C C2C H2C 119.7 . . ?
C2C C3C C4C 119.5(12) . . ?
C2C C3C H3C 120.3 . . ?
C4C C3C H3C 120.3 . . ?
C5C C4C C3C 120.5(12) . . ?
C5C C4C H4C 119.8 . . ?
C3C C4C H4C 119.8 . . ?
C4C C5C C6C 121.1(11) . . ?
C4C C5C H5C 119.5 . . ?
C6C C5C H5C 119.5 . . ?
C5C C6C C1C 119.8(11) . . ?
C5C C6C H6C 120.1 . . ?
C1C C6C H6C 120.1 . . ?
C2D C1D C6D 118.1(10) . . ?
C2D C1D P2 122.7(8) . . ?
C6D C1D P2 119.1(8) . . ?
C1D C2D C3D 120.7(12) . . ?
C1D C2D H2D 119.6 . . ?
C3D C2D H2D 119.6 . . ?
C4D C3D C2D 119.7(13) . . ?
C4D C3D H3D 120.1 . . ?
C2D C3D H3D 120.1 . . ?
C5D C4D C3D 119.6(11) . . ?
C5D C4D H4D 120.2 . . ?
C3D C4D H4D 120.2 . . ?
C4D C5D C6D 120.6(12) . . ?
C4D C5D H5D 119.7 . . ?
C6D C5D H5D 119.7 . . ?
C5D C6D C1D 121.2(12) . . ?
C5D C6D H6D 119.4 . . ?
C1D C6D H6D 119.4 . . ?
Cl1 C11 Cl2 103(2) . . ?
Cl1 C11 H11A 111.2 . . ?
Cl2 C11 H11A 111.2 . . ?
Cl1 C11 H11B 111.2 . . ?
Cl2 C11 H11B 111.2 . . ?
H11A C11 H11B 109.1 . . ?
Cl3 C12 Cl4 91.3(16) . . ?
Cl3 C12 H12A 113.4 . . ?
Cl4 C12 H12A 113.4 . . ?
Cl3 C12 H12B 113.4 . . ?
Cl4 C12 H12B 113.4 . . ?
H12A C12 H12B 110.7 . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 3.082
_refine_diff_density_min -2.138
_refine_diff_density_rms 0.218
data_complex2
_database_code_depnum_ccdc_archive 'CCDC 641199'
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C20 H16 Au N P), 2(C2 F3 O2), C H2 Cl2'
_chemical_formula_sum 'C45 H34 Au2 Cl2 F6 N2 O4 P2'
_chemical_formula_weight 1307.52
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'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_H-M 'I -4 2 d'
_symmetry_space_group_name_Hall 'I -4 2bw'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'-y+1/2, -x, z+3/4'
'x+1/2, -y, -z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'x+1, -y+1/2, -z+5/4'
'y+1, x+1/2, z+5/4'
_cell_length_a 19.827(2)
_cell_length_b 19.827(2)
_cell_length_c 22.206(3)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 8729.4(17)
_cell_formula_units_Z 8
_cell_measurement_temperature 103(2)
_cell_measurement_reflns_used 122284
_cell_measurement_theta_min 3.21
_cell_measurement_theta_max 27.63
_exptl_crystal_description platelet
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.39
_exptl_crystal_size_mid 0.37
_exptl_crystal_size_min 0.36
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.990
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5008
_exptl_absorpt_coefficient_mu 6.983
_exptl_absorpt_correction_type empirical
_exptl_absorpt_correction_T_min 0.075
_exptl_absorpt_correction_T_max 0.082
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 103(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'R Axis Rapid'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 131109
_diffrn_reflns_av_R_equivalents 0.1282
_diffrn_reflns_av_sigmaI/netI 0.0314
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 3.22
_diffrn_reflns_theta_max 25.02
_reflns_number_total 3866
_reflns_number_gt 3730
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'WinGX (Farrugia, 1999), PLATON (Spek, 2003)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+325.6981P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.04(2)
_refine_ls_number_reflns 3866
_refine_ls_number_parameters 285
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0655
_refine_ls_R_factor_gt 0.0634
_refine_ls_wR_factor_ref 0.1371
_refine_ls_wR_factor_gt 0.1360
_refine_ls_goodness_of_fit_ref 1.207
_refine_ls_restrained_S_all 1.206
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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 0.20202(3) 0.19647(3) 0.06362(3) 0.0520(2) Uani 1 1 d . . .
P1 P 0.28410(19) 0.2713(2) 0.04807(16) 0.0415(9) Uani 1 1 d . . .
N1 N 0.1290(8) 0.1248(8) 0.0694(7) 0.059(4) Uani 1 1 d . . .
C1 C 0.3592(7) 0.2588(8) 0.0937(6) 0.038(3) Uani 1 1 d . . .
C2 C 0.4226(7) 0.2688(9) 0.0658(7) 0.049(4) Uani 1 1 d . . .
H2 H 0.4239 0.2831 0.0260 0.059 Uiso 1 1 calc R . .
C3 C 0.4824(9) 0.2583(12) 0.0956(7) 0.071(6) Uani 1 1 d . . .
H3 H 0.5230 0.2626 0.0750 0.085 Uiso 1 1 calc R . .
C4 C 0.1383(10) 0.0612(11) 0.0586(8) 0.064(6) Uani 1 1 d . . .
H4 H 0.1818 0.0491 0.0472 0.076 Uiso 1 1 calc R . .
C5 C 0.0928(11) 0.0097(10) 0.0618(9) 0.071(6) Uani 1 1 d . . .
H5 H 0.1047 -0.0343 0.0520 0.085 Uiso 1 1 calc R . .
C6 C 0.0276(11) 0.0262(11) 0.0804(7) 0.063(5) Uani 1 1 d . . .
C7 C 0.0133(11) 0.0931(11) 0.0928(8) 0.069(6) Uani 1 1 d . . .
H7 H -0.0300 0.1067 0.1035 0.083 Uiso 1 1 calc R . .
C8 C 0.0658(11) 0.1392(11) 0.0888(7) 0.067(6) Uani 1 1 d . . .
H8 H 0.0569 0.1834 0.1004 0.080 Uiso 1 1 calc R . .
C9 C -0.0040(16) 0.3075(17) 0.0149(17) 0.128(13) Uani 1 1 d . . .
O1 O 0.0527(9) 0.3001(12) 0.0225(9) 0.123(7) Uani 1 1 d . . .
O2 O -0.0518(13) 0.2711(16) 0.029(3) 0.32(3) Uani 1 1 d . . .
C10 C -0.0287(16) 0.3756(18) -0.0098(15) 0.108(9) Uani 1 1 d . . .
F1 F 0.0222(12) 0.3989(14) -0.0448(12) 0.192(11) Uani 1 1 d . . .
F2 F -0.0450(14) 0.4197(11) 0.0311(9) 0.194(12) Uani 1 1 d . . .
F3 F -0.0826(12) 0.3759(18) -0.0446(11) 0.226(15) Uani 1 1 d . . .
C1A C 0.3118(8) 0.2675(9) -0.0293(7) 0.047(4) Uani 1 1 d . . .
C2A C 0.3301(8) 0.3294(12) -0.0601(8) 0.064(5) Uani 1 1 d . . .
H2A H 0.3272 0.3715 -0.0419 0.077 Uiso 1 1 calc R . .
C3A C 0.3529(10) 0.3207(12) -0.1207(8) 0.065(6) Uani 1 1 d . . .
H3A H 0.3679 0.3587 -0.1412 0.078 Uiso 1 1 calc R . .
C4A C 0.3542(11) 0.2644(17) -0.1488(11) 0.093(9) Uani 1 1 d . . .
H4A H 0.3673 0.2633 -0.1890 0.111 Uiso 1 1 calc R . .
C5A C 0.3360(9) 0.2034(12) -0.1192(9) 0.073(6) Uani 1 1 d . . .
H5A H 0.3384 0.1623 -0.1393 0.087 Uiso 1 1 calc R . .
C6A C 0.3139(10) 0.2064(14) -0.0584(11) 0.093(7) Uani 1 1 d . . .
H6A H 0.3010 0.1672 -0.0384 0.112 Uiso 1 1 calc R . .
C1B C 0.2585(8) 0.3562(7) 0.0585(7) 0.038(3) Uani 1 1 d . . .
C2B C 0.1918(8) 0.3744(7) 0.0387(5) 0.037(3) Uani 1 1 d . . .
H2B H 0.1624 0.3418 0.0239 0.045 Uiso 1 1 calc R . .
C3B C 0.1722(10) 0.4414(8) 0.0421(7) 0.052(4) Uani 1 1 d . . .
H3B H 0.1291 0.4537 0.0295 0.063 Uiso 1 1 calc R . .
C4B C 0.2149(12) 0.4896(8) 0.0635(8) 0.065(5) Uani 1 1 d . . .
H4B H 0.2011 0.5344 0.0646 0.078 Uiso 1 1 calc R . .
C5B C 0.2770(14) 0.4728(11) 0.0831(10) 0.083(7) Uani 1 1 d . . .
H5B H 0.3054 0.5063 0.0977 0.099 Uiso 1 1 calc R . .
C6B C 0.2990(10) 0.4070(9) 0.0821(7) 0.055(4) Uani 1 1 d . . .
H6B H 0.3414 0.3964 0.0973 0.066 Uiso 1 1 calc R . .
Cl1 Cl 0.4315(11) 0.489(3) 0.967(2) 0.67(4) Uani 1 1 d D . .
C11 C 0.5000 0.5000 0.919(3) 0.28(5) Uani 1 2 d SD . .
H11A H 0.5064 0.4607 0.8934 0.337 Uiso 0.50 1 calc PR . .
H11B H 0.4936 0.5393 0.8934 0.337 Uiso 0.50 1 calc PR . .
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 0.0520(4) 0.0528(4) 0.0511(3) 0.0047(3) -0.0134(3) -0.0205(3)
P1 0.037(2) 0.050(2) 0.038(2) -0.0015(16) -0.0064(16) -0.0023(16)
N1 0.055(9) 0.061(10) 0.061(9) 0.004(8) -0.040(8) -0.032(7)
C1 0.032(7) 0.055(9) 0.025(7) -0.007(6) 0.000(6) -0.007(6)
C2 0.038(8) 0.082(12) 0.026(7) -0.011(8) 0.006(7) -0.013(8)
C3 0.050(11) 0.131(19) 0.031(8) 0.011(10) 0.008(8) 0.014(11)
C4 0.064(11) 0.098(16) 0.028(8) 0.021(9) -0.013(8) -0.042(10)
C5 0.094(15) 0.060(11) 0.059(11) -0.014(10) 0.003(12) -0.030(11)
C6 0.078(14) 0.074(13) 0.037(9) -0.005(9) 0.000(9) -0.037(11)
C7 0.067(13) 0.086(15) 0.054(11) -0.028(11) 0.013(9) -0.020(11)
C8 0.097(16) 0.076(13) 0.027(8) -0.022(8) 0.005(9) -0.033(12)
C9 0.080(18) 0.11(2) 0.19(3) -0.09(2) -0.03(2) 0.005(19)
O1 0.080(12) 0.155(18) 0.132(16) -0.053(15) 0.019(11) -0.039(13)
O2 0.086(17) 0.16(3) 0.73(9) -0.06(4) -0.04(3) -0.045(17)
C10 0.09(2) 0.12(3) 0.11(2) -0.02(2) 0.017(18) -0.016(19)
F1 0.142(18) 0.23(3) 0.21(3) -0.06(2) 0.046(18) -0.065(18)
F2 0.32(3) 0.147(17) 0.117(15) -0.059(13) -0.075(17) 0.10(2)
F3 0.136(18) 0.40(5) 0.142(19) -0.04(2) -0.041(16) -0.05(2)
C1A 0.036(8) 0.070(10) 0.035(8) -0.005(7) -0.012(7) -0.001(8)
C2A 0.045(9) 0.110(16) 0.038(8) 0.008(10) 0.005(8) -0.008(9)
C3A 0.060(11) 0.095(16) 0.040(10) 0.023(10) 0.002(9) 0.029(11)
C4A 0.050(12) 0.16(3) 0.071(15) 0.026(17) -0.019(11) 0.011(15)
C5A 0.058(10) 0.091(15) 0.069(12) -0.037(13) -0.014(9) 0.016(12)
C6A 0.060(11) 0.115(18) 0.104(16) -0.033(16) -0.034(12) 0.049(13)
C1B 0.052(9) 0.041(8) 0.022(6) 0.007(6) 0.001(7) -0.004(6)
C2B 0.053(9) 0.036(7) 0.022(6) -0.013(5) 0.011(6) 0.012(7)
C3B 0.069(11) 0.049(10) 0.038(9) 0.017(7) 0.006(8) 0.016(8)
C4B 0.110(17) 0.033(8) 0.053(10) 0.008(8) 0.028(12) -0.004(10)
C5B 0.12(2) 0.056(12) 0.072(14) -0.013(10) 0.022(14) -0.004(13)
C6B 0.054(10) 0.069(11) 0.041(9) 0.009(8) -0.002(8) 0.000(9)
Cl1 0.18(2) 0.46(4) 1.36(14) 0.16(7) -0.12(5) -0.03(3)
C11 0.13(5) 0.20(8) 0.52(15) 0.000 0.000 0.06(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N1 2.033(12) . ?
Au1 P1 2.229(4) . ?
P1 C1B 1.774(15) . ?
P1 C1A 1.805(15) . ?
P1 C1 1.818(14) . ?
N1 C4 1.30(2) . ?
N1 C8 1.35(3) . ?
C1 C2 1.416(19) . ?
C1 C1 1.43(3) 15_454 ?
C2 C3 1.37(2) . ?
C2 H2 0.9300 . ?
C3 C3 1.35(3) 15_454 ?
C3 H3 0.9300 . ?
C4 C5 1.36(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.40(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.38(3) . ?
C6 C6 1.51(3) 3 ?
C7 C8 1.39(3) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 O1 1.15(3) . ?
C9 O2 1.23(4) . ?
C9 C10 1.54(4) . ?
C10 F2 1.30(3) . ?
C10 F3 1.32(4) . ?
C10 F1 1.35(3) . ?
C1A C6A 1.37(3) . ?
C1A C2A 1.45(2) . ?
C2A C3A 1.43(2) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.28(3) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.42(3) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.42(3) . ?
C5A H5A 0.9300 . ?
C6A H6A 0.9300 . ?
C1B C6B 1.39(2) . ?
C1B C2B 1.44(2) . ?
C2B C3B 1.387(19) . ?
C2B H2B 0.9300 . ?
C3B C4B 1.36(3) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.35(3) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.37(3) . ?
C5B H5B 0.9300 . ?
C6B H6B 0.9300 . ?
Cl1 C11 1.75(2) . ?
Cl1 Cl1 2.43(6) 2_567 ?
Cl1 Cl1 2.43(6) 4_657 ?
C11 Cl1 1.75(2) 3_665 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
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
N1 Au1 P1 174.3(5) . . ?
C1B P1 C1A 104.5(7) . . ?
C1B P1 C1 106.9(7) . . ?
C1A P1 C1 106.0(7) . . ?
C1B P1 Au1 113.7(5) . . ?
C1A P1 Au1 110.0(5) . . ?
C1 P1 Au1 114.9(5) . . ?
C4 N1 C8 113.3(15) . . ?
C4 N1 Au1 124.5(14) . . ?
C8 N1 Au1 122.1(14) . . ?
C2 C1 C1 117.3(9) . 15_454 ?
C2 C1 P1 117.7(11) . . ?
C1 C1 P1 125.0(4) 15_454 . ?
C3 C2 C1 122.3(15) . . ?
C3 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
C3 C3 C2 120.3(9) 15_454 . ?
C3 C3 H3 119.9 15_454 . ?
C2 C3 H3 119.9 . . ?
N1 C4 C5 129(2) . . ?
N1 C4 H4 115.7 . . ?
C5 C4 H4 115.7 . . ?
C4 C5 C6 117(2) . . ?
C4 C5 H5 121.5 . . ?
C6 C5 H5 121.5 . . ?
C7 C6 C5 118.2(16) . . ?
C7 C6 C6 121(3) . 3 ?
C5 C6 C6 121(2) . 3 ?
C6 C7 C8 118(2) . . ?
C6 C7 H7 121.2 . . ?
C8 C7 H7 121.2 . . ?
N1 C8 C7 125.2(19) . . ?
N1 C8 H8 117.4 . . ?
C7 C8 H8 117.4 . . ?
O1 C9 O2 130(4) . . ?
O1 C9 C10 119(4) . . ?
O2 C9 C10 111(3) . . ?
F2 C10 F3 102(3) . . ?
F2 C10 F1 111(3) . . ?
F3 C10 F1 105(3) . . ?
F2 C10 C9 115(3) . . ?
F3 C10 C9 118(3) . . ?
F1 C10 C9 105(3) . . ?
C6A C1A C2A 121.0(18) . . ?
C6A C1A P1 119.6(16) . . ?
C2A C1A P1 119.4(13) . . ?
C3A C2A C1A 115(2) . . ?
C3A C2A H2A 122.5 . . ?
C1A C2A H2A 122.5 . . ?
C4A C3A C2A 125(2) . . ?
C4A C3A H3A 117.6 . . ?
C2A C3A H3A 117.6 . . ?
C3A C4A C5A 121(2) . . ?
C3A C4A H4A 119.6 . . ?
C5A C4A H4A 119.6 . . ?
C6A C5A C4A 119(2) . . ?
C6A C5A H5A 120.6 . . ?
C4A C5A H5A 120.6 . . ?
C1A C6A C5A 120(2) . . ?
C1A C6A H6A 120.2 . . ?
C5A C6A H6A 120.2 . . ?
C6B C1B C2B 117.7(14) . . ?
C6B C1B P1 124.8(13) . . ?
C2B C1B P1 117.4(11) . . ?
C3B C2B C1B 118.7(15) . . ?
C3B C2B H2B 120.6 . . ?
C1B C2B H2B 120.6 . . ?
C4B C3B C2B 121.1(18) . . ?
C4B C3B H3B 119.4 . . ?
C2B C3B H3B 119.4 . . ?
C5B C4B C3B 120.5(17) . . ?
C5B C4B H4B 119.8 . . ?
C3B C4B H4B 119.8 . . ?
C4B C5B C6B 121(2) . . ?
C4B C5B H5B 119.4 . . ?
C6B C5B H5B 119.4 . . ?
C5B C6B C1B 120.6(19) . . ?
C5B C6B H6B 119.7 . . ?
C1B C6B H6B 119.7 . . ?
C11 Cl1 Cl1 86(2) . 2_567 ?
C11 Cl1 Cl1 86(2) . 4_657 ?
Cl1 Cl1 Cl1 69(2) 2_567 4_657 ?
Cl1 C11 Cl1 104(3) 3_665 . ?
Cl1 C11 H11A 111.0 3_665 . ?
Cl1 C11 H11A 111.0 . . ?
Cl1 C11 H11B 111.0 3_665 . ?
Cl1 C11 H11B 111.0 . . ?
H11A C11 H11B 109.0 . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 25.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 1.181
_refine_diff_density_min -1.516
_refine_diff_density_rms 0.162
# Attachment 'complex3.cif'
data_complex3
_database_code_depnum_ccdc_archive 'CCDC 641200'
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C84 H68 Au4 N4 P4, 4(C2 F3 O2), 2(C H2 Cl2), 4(H2 O)'
_chemical_formula_sum 'C94 H80 Au4 Cl4 F12 N4 O12 P4'
_chemical_formula_weight 2739.17
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 10.0634(14)
_cell_length_b 21.126(3)
_cell_length_c 22.728(4)
_cell_angle_alpha 90.00
_cell_angle_beta 100.424(6)
_cell_angle_gamma 90.00
_cell_volume 4752.2(13)
_cell_formula_units_Z 2
_cell_measurement_temperature 123(2)
_cell_measurement_reflns_used 100341
_cell_measurement_theta_min 3.03
_cell_measurement_theta_max 27.66
_exptl_crystal_description platelet
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.914
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2640
_exptl_absorpt_coefficient_mu 6.421
_exptl_absorpt_correction_type empirical
_exptl_absorpt_correction_T_min 0.286
_exptl_absorpt_correction_T_max 0.384
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 123(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'R Axis Rapid'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 114260
_diffrn_reflns_av_R_equivalents 0.0787
_diffrn_reflns_av_sigmaI/netI 0.0370
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 3.03
_diffrn_reflns_theta_max 25.03
_reflns_number_total 8324
_reflns_number_gt 7158
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'WinGX (Farrugia, 1999), PLATON (Spek, 2003)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+38.7606P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8324
_refine_ls_number_parameters 620
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0486
_refine_ls_R_factor_gt 0.0386
_refine_ls_wR_factor_ref 0.0841
_refine_ls_wR_factor_gt 0.0801
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_restrained_S_all 1.037
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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 0.08830(3) 0.223458(12) 0.307005(11) 0.02201(8) Uani 1 1 d . . .
Au2 Au -0.00761(2) 0.318710(12) 0.386674(11) 0.02077(8) Uani 1 1 d . . .
P1 P 0.03381(17) 0.29852(8) 0.23767(7) 0.0197(4) Uani 1 1 d . . .
P2 P 0.03294(16) 0.41324(8) 0.34867(7) 0.0202(4) Uani 1 1 d . . .
N1 N 0.1069(5) 0.1367(3) 0.3530(2) 0.0218(12) Uani 1 1 d . . .
N2 N 0.0220(5) -0.2387(3) 0.5620(2) 0.0224(12) Uani 1 1 d . . .
C1 C 0.1309(6) 0.3725(3) 0.2426(3) 0.0192(14) Uani 1 1 d . . .
C2 C 0.1373(6) 0.4160(3) 0.2901(3) 0.0188(14) Uani 1 1 d . . .
C3 C 0.2183(7) 0.4701(3) 0.2909(3) 0.0247(15) Uani 1 1 d . . .
H3 H 0.2271 0.4984 0.3239 0.030 Uiso 1 1 calc R . .
C4 C 0.2862(6) 0.4830(3) 0.2437(3) 0.0262(16) Uani 1 1 d . . .
H4 H 0.3382 0.5206 0.2440 0.031 Uiso 1 1 calc R . .
C5 C 0.2771(6) 0.4410(3) 0.1970(3) 0.0252(15) Uani 1 1 d . . .
H5 H 0.3226 0.4497 0.1647 0.030 Uiso 1 1 calc R . .
C6 C 0.2020(6) 0.3859(3) 0.1966(3) 0.0231(15) Uani 1 1 d . . .
H6 H 0.1989 0.3567 0.1646 0.028 Uiso 1 1 calc R . .
C1A C 0.0572(7) 0.2585(3) 0.1690(3) 0.0248(15) Uani 1 1 d . . .
C2A C 0.1781(8) 0.2262(4) 0.1691(3) 0.0358(18) Uani 1 1 d . . .
H2A H 0.2511 0.2310 0.2017 0.043 Uiso 1 1 calc R . .
C3A C 0.1917(9) 0.1873(4) 0.1220(4) 0.0388(19) Uani 1 1 d . . .
H3A H 0.2751 0.1664 0.1218 0.047 Uiso 1 1 calc R . .
C4A C 0.0863(10) 0.1787(4) 0.0756(4) 0.046(2) Uani 1 1 d . . .
H4A H 0.0961 0.1512 0.0436 0.055 Uiso 1 1 calc R . .
C5A C -0.0350(9) 0.2099(4) 0.0753(3) 0.0377(19) Uani 1 1 d . . .
H5A H -0.1089 0.2031 0.0435 0.045 Uiso 1 1 calc R . .
C6A C -0.0485(8) 0.2509(3) 0.1213(3) 0.0308(17) Uani 1 1 d . . .
H6A H -0.1302 0.2738 0.1201 0.037 Uiso 1 1 calc R . .
C1B C -0.1407(6) 0.3236(3) 0.2259(3) 0.0217(14) Uani 1 1 d . . .
C2B C -0.2348(7) 0.2883(3) 0.2499(3) 0.0260(15) Uani 1 1 d . . .
H2B H -0.2065 0.2525 0.2743 0.031 Uiso 1 1 calc R . .
C3B C -0.3708(7) 0.3055(4) 0.2379(4) 0.0359(18) Uani 1 1 d . . .
H3B H -0.4357 0.2812 0.2536 0.043 Uiso 1 1 calc R . .
C4B C -0.4109(8) 0.3580(4) 0.2030(4) 0.042(2) Uani 1 1 d . . .
H4B H -0.5036 0.3696 0.1948 0.050 Uiso 1 1 calc R . .
C5B C -0.3176(7) 0.3937(4) 0.1802(3) 0.0360(18) Uani 1 1 d . . .
H5B H -0.3462 0.4300 0.1566 0.043 Uiso 1 1 calc R . .
C6B C -0.1823(7) 0.3770(3) 0.1915(3) 0.0278(16) Uani 1 1 d . . .
H6B H -0.1181 0.4019 0.1758 0.033 Uiso 1 1 calc R . .
C1C C -0.1137(6) 0.4618(3) 0.3193(3) 0.0210(14) Uani 1 1 d . . .
C2C C -0.2383(7) 0.4459(3) 0.3326(3) 0.0265(15) Uani 1 1 d . . .
H2C H -0.2470 0.4089 0.3553 0.032 Uiso 1 1 calc R . .
C3C C -0.3500(7) 0.4834(4) 0.3133(3) 0.0347(18) Uani 1 1 d . . .
H3C H -0.4355 0.4717 0.3221 0.042 Uiso 1 1 calc R . .
C4C C -0.3376(7) 0.5374(4) 0.2815(3) 0.0332(17) Uani 1 1 d . . .
H4C H -0.4144 0.5634 0.2686 0.040 Uiso 1 1 calc R . .
C5C C -0.2131(7) 0.5542(3) 0.2680(3) 0.0285(16) Uani 1 1 d . . .
H5C H -0.2047 0.5917 0.2458 0.034 Uiso 1 1 calc R . .
C6C C -0.1024(7) 0.5167(3) 0.2869(3) 0.0299(17) Uani 1 1 d . . .
H6C H -0.0173 0.5283 0.2777 0.036 Uiso 1 1 calc R . .
C1D C 0.1304(7) 0.4570(3) 0.4114(3) 0.0246(15) Uani 1 1 d . . .
C2D C 0.0903(8) 0.5150(4) 0.4304(3) 0.0330(17) Uani 1 1 d . . .
H2D H 0.0108 0.5350 0.4098 0.040 Uiso 1 1 calc R . .
C3D C 0.1690(8) 0.5439(4) 0.4807(3) 0.041(2) Uani 1 1 d . . .
H3D H 0.1413 0.5832 0.4946 0.049 Uiso 1 1 calc R . .
C4D C 0.2862(8) 0.5156(4) 0.5100(4) 0.047(2) Uani 1 1 d . . .
H4D H 0.3407 0.5363 0.5429 0.057 Uiso 1 1 calc R . .
C5D C 0.3236(8) 0.4575(4) 0.4914(4) 0.042(2) Uani 1 1 d . . .
H5D H 0.4032 0.4377 0.5121 0.050 Uiso 1 1 calc R . .
C6D C 0.2454(7) 0.4274(4) 0.4423(3) 0.0332(17) Uani 1 1 d . . .
H6D H 0.2708 0.3868 0.4301 0.040 Uiso 1 1 calc R . .
C7 C 0.2248(7) 0.1115(3) 0.3798(3) 0.0265(15) Uani 1 1 d . . .
H7 H 0.3060 0.1341 0.3789 0.032 Uiso 1 1 calc R . .
C8 C 0.2318(7) 0.0537(3) 0.4087(3) 0.0230(14) Uani 1 1 d . . .
H8 H 0.3168 0.0369 0.4269 0.028 Uiso 1 1 calc R . .
C9 C 0.1149(7) 0.0206(3) 0.4111(3) 0.0228(15) Uani 1 1 d . . .
C10 C -0.0065(7) 0.0463(3) 0.3826(3) 0.0269(16) Uani 1 1 d . . .
H10 H -0.0886 0.0240 0.3824 0.032 Uiso 1 1 calc R . .
C11 C -0.0083(7) 0.1046(3) 0.3543(3) 0.0267(16) Uani 1 1 d . . .
H11 H -0.0922 0.1222 0.3355 0.032 Uiso 1 1 calc R . .
C12 C 0.1228(7) -0.0397(3) 0.4445(3) 0.0263(15) Uani 1 1 d . . .
H12 H 0.2100 -0.0560 0.4600 0.032 Uiso 1 1 calc R . .
C13 C 0.0165(7) -0.0727(3) 0.4543(3) 0.0225(14) Uani 1 1 d . . .
H13 H -0.0704 -0.0576 0.4366 0.027 Uiso 1 1 calc R . .
C14 C 0.0226(6) -0.1308(3) 0.4902(3) 0.0214(14) Uani 1 1 d . . .
C15 C 0.1427(7) -0.1565(3) 0.5227(3) 0.0272(16) Uani 1 1 d . . .
H15 H 0.2269 -0.1374 0.5200 0.033 Uiso 1 1 calc R . .
C16 C 0.1394(7) -0.2086(3) 0.5580(3) 0.0261(15) Uani 1 1 d . . .
H16 H 0.2216 -0.2242 0.5805 0.031 Uiso 1 1 calc R . .
C17 C -0.0944(6) -0.2157(3) 0.5293(3) 0.0229(15) Uani 1 1 d . . .
H17 H -0.1768 -0.2371 0.5307 0.028 Uiso 1 1 calc R . .
C18 C -0.0969(7) -0.1624(3) 0.4942(3) 0.0232(15) Uani 1 1 d . . .
H18 H -0.1805 -0.1472 0.4725 0.028 Uiso 1 1 calc R . .
C19 C 0.5063(7) 0.3177(4) 0.3875(4) 0.0378(19) Uani 1 1 d . . .
O1 O 0.4189(6) 0.2267(3) 0.3323(3) 0.0507(15) Uani 1 1 d . . .
O2 O 0.2923(5) 0.2758(2) 0.3897(2) 0.0344(12) Uani 1 1 d . . .
C20 C 0.3954(8) 0.2676(4) 0.3679(4) 0.0333(18) Uani 1 1 d . . .
F1 F 0.6276(4) 0.3011(2) 0.3767(3) 0.0595(15) Uani 1 1 d . . .
F2 F 0.4748(5) 0.3716(2) 0.3577(3) 0.0730(19) Uani 1 1 d . . .
F3 F 0.5207(6) 0.3326(3) 0.4455(3) 0.0702(16) Uani 1 1 d . . .
C21 C 0.4977(8) 0.3151(4) 0.0379(4) 0.052(2) Uani 1 1 d . . .
O3 O 0.5601(5) 0.4193(3) 0.0245(3) 0.0484(15) Uani 1 1 d . . .
O4 O 0.3888(5) 0.4034(3) 0.0719(2) 0.0383(13) Uani 1 1 d . . .
C22 C 0.4799(7) 0.3867(4) 0.0456(3) 0.0312(17) Uani 1 1 d . . .
F4 F 0.4861(12) 0.3023(4) -0.0202(4) 0.169(5) Uani 1 1 d . . .
F5 F 0.4105(7) 0.2805(3) 0.0550(6) 0.168(6) Uani 1 1 d . . .
F6 F 0.6172(5) 0.2935(3) 0.0618(3) 0.0607(15) Uani 1 1 d . . .
C23 C -0.3491(9) 0.1533(4) 0.1760(5) 0.058(3) Uani 1 1 d . . .
H23A H -0.3915 0.1523 0.2120 0.069 Uiso 1 1 calc R . .
H23B H -0.3593 0.1966 0.1592 0.069 Uiso 1 1 calc R . .
Cl1 Cl -0.1750(2) 0.13506(10) 0.19651(10) 0.0465(5) Uani 1 1 d . . .
Cl2 Cl -0.4318(3) 0.09951(13) 0.12315(11) 0.0640(7) Uani 1 1 d . . .
O5 O 0.3870(7) 0.5375(3) 0.0859(3) 0.0539(16) Uani 1 1 d D . .
O6 O -0.3814(7) 0.1303(3) 0.3208(3) 0.0549(16) Uani 1 1 d D . .
H61 H -0.425(8) 0.162(2) 0.331(3) 0.06(3) Uiso 1 1 d D . .
H52 H 0.405(10) 0.553(3) 0.054(2) 0.07(3) Uiso 1 1 d D . .
H51 H 0.388(8) 0.4975(6) 0.082(3) 0.03(2) Uiso 1 1 d D . .
H62 H -0.386(9) 0.101(2) 0.346(3) 0.05(3) Uiso 1 1 d 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 0.02705(15) 0.01962(14) 0.01966(14) 0.00470(10) 0.00505(10) 0.00156(11)
Au2 0.02365(14) 0.02051(14) 0.01923(14) 0.00470(10) 0.00676(10) 0.00004(10)
P1 0.0225(9) 0.0191(9) 0.0182(9) 0.0033(7) 0.0052(7) -0.0005(7)
P2 0.0205(9) 0.0220(9) 0.0187(9) 0.0043(7) 0.0053(7) 0.0007(7)
N1 0.026(3) 0.024(3) 0.015(3) 0.004(2) 0.002(2) -0.003(2)
N2 0.022(3) 0.023(3) 0.021(3) 0.008(2) 0.002(2) 0.001(2)
C1 0.018(3) 0.018(3) 0.023(4) 0.006(3) 0.007(3) 0.005(3)
C2 0.015(3) 0.026(4) 0.017(3) 0.005(3) 0.009(2) 0.004(3)
C3 0.026(4) 0.027(4) 0.022(4) 0.004(3) 0.006(3) 0.000(3)
C4 0.019(3) 0.023(4) 0.037(4) 0.010(3) 0.008(3) -0.001(3)
C5 0.020(3) 0.028(4) 0.030(4) 0.007(3) 0.011(3) 0.004(3)
C6 0.025(4) 0.026(4) 0.019(4) 0.004(3) 0.005(3) 0.001(3)
C1A 0.033(4) 0.021(4) 0.022(4) 0.000(3) 0.009(3) -0.003(3)
C2A 0.047(5) 0.033(4) 0.029(4) 0.005(3) 0.012(3) 0.004(4)
C3A 0.050(5) 0.030(4) 0.043(5) 0.001(4) 0.027(4) 0.009(4)
C4A 0.094(7) 0.020(4) 0.029(5) -0.004(3) 0.024(5) -0.001(4)
C5A 0.055(5) 0.033(5) 0.025(4) -0.006(3) 0.009(4) -0.010(4)
C6A 0.041(4) 0.029(4) 0.024(4) 0.004(3) 0.010(3) -0.001(3)
C1B 0.024(3) 0.022(4) 0.020(4) -0.001(3) 0.004(3) 0.004(3)
C2B 0.030(4) 0.028(4) 0.021(4) -0.003(3) 0.006(3) -0.007(3)
C3B 0.021(4) 0.048(5) 0.042(5) -0.005(4) 0.011(3) -0.001(3)
C4B 0.025(4) 0.050(5) 0.049(5) -0.009(4) 0.003(4) 0.007(4)
C5B 0.035(4) 0.036(5) 0.033(4) 0.000(3) -0.002(3) 0.012(4)
C6B 0.030(4) 0.029(4) 0.025(4) -0.003(3) 0.005(3) -0.001(3)
C1C 0.022(3) 0.021(4) 0.020(4) -0.001(3) 0.004(3) -0.002(3)
C2C 0.027(4) 0.022(4) 0.031(4) 0.009(3) 0.007(3) 0.001(3)
C3C 0.027(4) 0.035(5) 0.043(5) 0.004(3) 0.011(3) 0.003(3)
C4C 0.026(4) 0.030(4) 0.044(5) 0.007(3) 0.008(3) 0.003(3)
C5C 0.030(4) 0.028(4) 0.027(4) 0.011(3) 0.004(3) -0.002(3)
C6C 0.021(4) 0.033(4) 0.039(5) 0.007(3) 0.014(3) -0.004(3)
C1D 0.024(4) 0.033(4) 0.018(4) 0.003(3) 0.008(3) -0.001(3)
C2D 0.040(4) 0.032(4) 0.027(4) -0.002(3) 0.006(3) 0.003(3)
C3D 0.054(5) 0.038(5) 0.030(4) -0.008(3) 0.004(4) -0.003(4)
C4D 0.044(5) 0.060(6) 0.033(5) -0.005(4) -0.007(4) -0.009(4)
C5D 0.041(5) 0.046(5) 0.034(5) 0.004(4) -0.005(4) 0.000(4)
C6D 0.037(4) 0.042(5) 0.018(4) 0.000(3) -0.002(3) 0.003(3)
C7 0.031(4) 0.031(4) 0.018(4) 0.003(3) 0.006(3) 0.000(3)
C8 0.028(4) 0.023(4) 0.018(3) 0.004(3) 0.004(3) 0.002(3)
C9 0.032(4) 0.017(4) 0.020(4) 0.003(3) 0.008(3) 0.003(3)
C10 0.026(4) 0.024(4) 0.029(4) 0.005(3) 0.000(3) -0.003(3)
C11 0.027(4) 0.028(4) 0.024(4) 0.002(3) 0.001(3) -0.007(3)
C12 0.028(4) 0.027(4) 0.024(4) 0.002(3) 0.004(3) 0.006(3)
C13 0.027(4) 0.019(4) 0.021(4) 0.001(3) 0.001(3) 0.002(3)
C14 0.027(4) 0.021(4) 0.018(3) 0.002(3) 0.009(3) -0.001(3)
C15 0.027(4) 0.029(4) 0.029(4) 0.000(3) 0.015(3) -0.003(3)
C16 0.028(4) 0.023(4) 0.025(4) -0.002(3) 0.000(3) 0.000(3)
C17 0.019(3) 0.029(4) 0.023(4) -0.003(3) 0.011(3) 0.001(3)
C18 0.028(4) 0.027(4) 0.016(3) 0.004(3) 0.007(3) 0.001(3)
C19 0.023(4) 0.034(5) 0.057(6) 0.013(4) 0.008(4) 0.000(3)
O1 0.061(4) 0.039(4) 0.057(4) -0.001(3) 0.026(3) -0.001(3)
O2 0.026(3) 0.046(3) 0.031(3) 0.006(2) 0.006(2) -0.004(2)
C20 0.033(4) 0.028(4) 0.040(5) 0.013(3) 0.010(3) -0.001(3)
F1 0.025(3) 0.052(3) 0.105(5) 0.023(3) 0.023(3) 0.006(2)
F2 0.041(3) 0.034(3) 0.148(6) 0.037(3) 0.027(3) 0.003(2)
F3 0.061(4) 0.071(4) 0.074(4) -0.016(3) -0.002(3) -0.025(3)
C21 0.032(5) 0.052(6) 0.067(7) -0.018(5) -0.004(4) -0.005(4)
O3 0.036(3) 0.069(4) 0.042(4) 0.014(3) 0.011(3) -0.010(3)
O4 0.029(3) 0.052(4) 0.034(3) -0.003(3) 0.009(2) -0.004(2)
C22 0.022(4) 0.046(5) 0.023(4) 0.001(3) -0.005(3) -0.006(3)
F4 0.255(12) 0.107(7) 0.101(7) -0.073(6) -0.081(7) 0.049(7)
F5 0.055(4) 0.036(4) 0.429(18) 0.042(6) 0.085(7) 0.002(3)
F6 0.034(3) 0.059(3) 0.083(4) -0.014(3) -0.003(3) 0.007(2)
C23 0.056(6) 0.043(6) 0.069(7) -0.007(5) -0.005(5) 0.004(5)
Cl1 0.0492(12) 0.0344(11) 0.0540(13) 0.0037(9) 0.0038(10) -0.0089(9)
Cl2 0.0640(15) 0.0635(16) 0.0575(16) -0.0135(12) -0.0074(12) -0.0077(12)
O5 0.084(5) 0.046(4) 0.039(4) 0.004(3) 0.028(3) 0.006(4)
O6 0.067(4) 0.054(4) 0.048(4) 0.001(3) 0.024(3) 0.015(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N1 2.101(5) . ?
Au1 P1 2.2330(17) . ?
Au1 Au2 2.9820(5) . ?
Au2 N2 2.073(5) 3_556 ?
Au2 P2 2.2424(17) . ?
P1 C1B 1.807(7) . ?
P1 C1A 1.827(7) . ?
P1 C1 1.836(7) . ?
P2 C1C 1.823(7) . ?
P2 C1D 1.828(7) . ?
P2 C2 1.839(6) . ?
N1 C7 1.342(8) . ?
N1 C11 1.347(8) . ?
N2 C17 1.359(8) . ?
N2 C16 1.359(9) . ?
N2 Au2 2.073(5) 3_556 ?
C1 C6 1.398(9) . ?
C1 C2 1.410(9) . ?
C2 C3 1.403(9) . ?
C3 C4 1.399(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1A C6A 1.385(10) . ?
C1A C2A 1.395(10) . ?
C2A C3A 1.375(10) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.366(12) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.386(12) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.383(10) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C1B C2B 1.393(9) . ?
C1B C6B 1.393(9) . ?
C2B C3B 1.395(10) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.380(11) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.377(11) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.385(10) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
C1C C2C 1.384(9) . ?
C1C C6C 1.389(9) . ?
C2C C3C 1.380(10) . ?
C2C H2C 0.9500 . ?
C3C C4C 1.368(10) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.389(10) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.371(10) . ?
C5C H5C 0.9500 . ?
C6C H6C 0.9500 . ?
C1D C2D 1.383(10) . ?
C1D C6D 1.390(10) . ?
C2D C3D 1.407(10) . ?
C2D H2D 0.9500 . ?
C3D C4D 1.380(11) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.372(12) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.397(10) . ?
C5D H5D 0.9500 . ?
C6D H6D 0.9500 . ?
C7 C8 1.383(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.378(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(9) . ?
C9 C12 1.477(9) . ?
C10 C11 1.388(9) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.330(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.469(9) . ?
C13 H13 0.9500 . ?
C14 C18 1.392(9) . ?
C14 C15 1.406(9) . ?
C15 C16 1.368(10) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.378(9) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 F2 1.333(9) . ?
C19 F1 1.336(9) . ?
C19 F3 1.336(10) . ?
C19 C20 1.545(11) . ?
O1 C20 1.234(9) . ?
O2 C20 1.240(9) . ?
C21 F5 1.257(11) . ?
C21 F6 1.309(10) . ?
C21 F4 1.333(12) . ?
C21 C22 1.536(12) . ?
O3 C22 1.224(9) . ?
O4 C22 1.233(9) . ?
C23 Cl2 1.751(9) . ?
C23 Cl1 1.772(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
O5 H52 0.851(10) . ?
O5 H51 0.851(10) . ?
O6 H61 0.850(10) . ?
O6 H62 0.851(10) . ?
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
N1 Au1 P1 163.52(15) . . ?
N1 Au1 Au2 107.19(15) . . ?
P1 Au1 Au2 83.35(5) . . ?
N2 Au2 P2 168.19(16) 3_556 . ?
N2 Au2 Au1 81.63(16) 3_556 . ?
P2 Au2 Au1 105.40(5) . . ?
C1B P1 C1A 106.3(3) . . ?
C1B P1 C1 104.5(3) . . ?
C1A P1 C1 107.3(3) . . ?
C1B P1 Au1 114.9(2) . . ?
C1A P1 Au1 102.8(2) . . ?
C1 P1 Au1 120.1(2) . . ?
C1C P2 C1D 106.6(3) . . ?
C1C P2 C2 104.3(3) . . ?
C1D P2 C2 104.6(3) . . ?
C1C P2 Au2 116.8(2) . . ?
C1D P2 Au2 105.0(2) . . ?
C2 P2 Au2 118.3(2) . . ?
C7 N1 C11 119.0(6) . . ?
C7 N1 Au1 124.3(4) . . ?
C11 N1 Au1 116.7(4) . . ?
C17 N2 C16 118.0(6) . . ?
C17 N2 Au2 117.3(4) . 3_556 ?
C16 N2 Au2 124.7(4) . 3_556 ?
C6 C1 C2 118.8(6) . . ?
C6 C1 P1 117.7(5) . . ?
C2 C1 P1 123.5(5) . . ?
C3 C2 C1 119.2(6) . . ?
C3 C2 P2 115.0(5) . . ?
C1 C2 P2 125.5(5) . . ?
C4 C3 C2 120.8(6) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 119.6(6) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.4(6) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 121.2(6) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
C6A C1A C2A 119.4(7) . . ?
C6A C1A P1 121.6(5) . . ?
C2A C1A P1 118.2(5) . . ?
C3A C2A C1A 120.0(8) . . ?
C3A C2A H2A 120.0 . . ?
C1A C2A H2A 120.0 . . ?
C4A C3A C2A 120.5(8) . . ?
C4A C3A H3A 119.7 . . ?
C2A C3A H3A 119.7 . . ?
C3A C4A C5A 120.0(7) . . ?
C3A C4A H4A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C6A C5A C4A 120.0(8) . . ?
C6A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C6A C1A 119.9(7) . . ?
C5A C6A H6A 120.1 . . ?
C1A C6A H6A 120.1 . . ?
C2B C1B C6B 119.8(6) . . ?
C2B C1B P1 119.7(5) . . ?
C6B C1B P1 120.4(5) . . ?
C1B C2B C3B 119.8(7) . . ?
C1B C2B H2B 120.1 . . ?
C3B C2B H2B 120.1 . . ?
C4B C3B C2B 119.7(7) . . ?
C4B C3B H3B 120.1 . . ?
C2B C3B H3B 120.1 . . ?
C5B C4B C3B 120.5(7) . . ?
C5B C4B H4B 119.7 . . ?
C3B C4B H4B 119.7 . . ?
C4B C5B C6B 120.4(7) . . ?
C4B C5B H5B 119.8 . . ?
C6B C5B H5B 119.8 . . ?
C5B C6B C1B 119.7(7) . . ?
C5B C6B H6B 120.2 . . ?
C1B C6B H6B 120.2 . . ?
C2C C1C C6C 118.9(6) . . ?
C2C C1C P2 119.2(5) . . ?
C6C C1C P2 121.7(5) . . ?
C3C C2C C1C 120.6(6) . . ?
C3C C2C H2C 119.7 . . ?
C1C C2C H2C 119.7 . . ?
C4C C3C C2C 120.0(7) . . ?
C4C C3C H3C 120.0 . . ?
C2C C3C H3C 120.0 . . ?
C3C C4C C5C 120.1(7) . . ?
C3C C4C H4C 119.9 . . ?
C5C C4C H4C 119.9 . . ?
C6C C5C C4C 119.8(6) . . ?
C6C C5C H5C 120.1 . . ?
C4C C5C H5C 120.1 . . ?
C5C C6C C1C 120.6(6) . . ?
C5C C6C H6C 119.7 . . ?
C1C C6C H6C 119.7 . . ?
C2D C1D C6D 120.3(7) . . ?
C2D C1D P2 123.1(5) . . ?
C6D C1D P2 116.5(5) . . ?
C1D C2D C3D 118.9(7) . . ?
C1D C2D H2D 120.5 . . ?
C3D C2D H2D 120.5 . . ?
C4D C3D C2D 120.8(8) . . ?
C4D C3D H3D 119.6 . . ?
C2D C3D H3D 119.6 . . ?
C5D C4D C3D 119.7(8) . . ?
C5D C4D H4D 120.1 . . ?
C3D C4D H4D 120.1 . . ?
C4D C5D C6D 120.4(8) . . ?
C4D C5D H5D 119.8 . . ?
C6D C5D H5D 119.8 . . ?
C1D C6D C5D 119.7(7) . . ?
C1D C6D H6D 120.1 . . ?
C5D C6D H6D 120.1 . . ?
N1 C7 C8 122.0(6) . . ?
N1 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 119.8(6) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 118.0(6) . . ?
C8 C9 C12 119.4(6) . . ?
C10 C9 C12 122.6(6) . . ?
C9 C10 C11 120.1(6) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
N1 C11 C10 121.1(6) . . ?
N1 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C13 C12 C9 124.7(6) . . ?
C13 C12 H12 117.6 . . ?
C9 C12 H12 117.6 . . ?
C12 C13 C14 125.4(6) . . ?
C12 C13 H13 117.3 . . ?
C14 C13 H13 117.3 . . ?
C18 C14 C15 116.9(6) . . ?
C18 C14 C13 119.1(6) . . ?
C15 C14 C13 124.0(6) . . ?
C16 C15 C14 120.5(6) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
N2 C16 C15 122.0(6) . . ?
N2 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
N2 C17 C18 122.2(6) . . ?
N2 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C17 C18 C14 120.2(6) . . ?
C17 C18 H18 119.9 . . ?
C14 C18 H18 119.9 . . ?
F2 C19 F1 105.8(6) . . ?
F2 C19 F3 105.9(7) . . ?
F1 C19 F3 107.8(7) . . ?
F2 C19 C20 110.2(6) . . ?
F1 C19 C20 113.7(7) . . ?
F3 C19 C20 113.0(6) . . ?
O1 C20 O2 129.2(8) . . ?
O1 C20 C19 117.1(7) . . ?
O2 C20 C19 113.7(7) . . ?
F5 C21 F6 108.0(9) . . ?
F5 C21 F4 104.4(10) . . ?
F6 C21 F4 104.5(8) . . ?
F5 C21 C22 115.8(8) . . ?
F6 C21 C22 114.4(7) . . ?
F4 C21 C22 108.8(8) . . ?
O3 C22 O4 129.0(8) . . ?
O3 C22 C21 114.3(7) . . ?
O4 C22 C21 116.7(7) . . ?
Cl2 C23 Cl1 111.3(5) . . ?
Cl2 C23 H23A 109.4 . . ?
Cl1 C23 H23A 109.4 . . ?
Cl2 C23 H23B 109.4 . . ?
Cl1 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
H52 O5 H51 106(3) . . ?
H61 O6 H62 107(3) . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 25.03
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 2.188
_refine_diff_density_min -1.179
_refine_diff_density_rms 0.158