# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
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data_ah302a_2
_database_code_depnum_ccdc_archive 'CCDC 1457705'
_audit_update_record
;
2016-03-03 deposited with the CCDC.
2016-04-07 downloaded from the CCDC.
;
_vrf_CHEMW03_ah302a_2
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: PLATON/SQUEEZE was used to treat the heavily disordered
benzene molecules in the unit cell. These were removed from the
model, but included in the empirical formula. Additional PLATON/SQUEEZE
details appear in _refine_special_details.
;
_audit_creation_method SHELXL-2013
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C48 H50 N2 P -, C14 H24 N4 P +, 5.41 (C6 H6)'
_chemical_formula_sum 'C94.45 H106.45 N6 P2'
_chemical_formula_weight 1387.64
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.2213(6)
_cell_length_b 16.2437(9)
_cell_length_c 22.0973(12)
_cell_angle_alpha 97.700(3)
_cell_angle_beta 93.029(3)
_cell_angle_gamma 106.714(2)
_cell_volume 4144.2(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 123(2)
_cell_measurement_reflns_used 9818
_cell_measurement_theta_min 2.45
_cell_measurement_theta_max 24.33
_exptl_crystal_description rod
_exptl_crystal_colour yellow
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.112
_exptl_crystal_F_000 1490
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.600
_exptl_crystal_size_mid 0.140
_exptl_crystal_size_min 0.110
_exptl_absorpt_coefficient_mu 0.101
_shelx_estimated_absorpt_T_min 0.942
_shelx_estimated_absorpt_T_max 0.989
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6548
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 123(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa-II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 133897
_diffrn_reflns_av_unetI/netI 0.0633
_diffrn_reflns_av_R_equivalents 0.0610
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 1.869
_diffrn_reflns_theta_max 27.498
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total 18856
_reflns_number_gt 12108
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-2013
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
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^ > 2\s(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.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.027 0.500 0.550 1644 431 ' '
_platon_squeeze_details
;
The unit cell contains in average 10.82 benzene molecules which have been
treated as a diffuse contribution to the overall scattering without
specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0808P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 18856
_refine_ls_number_parameters 657
_refine_ls_number_restraints 64
_refine_ls_R_factor_all 0.0817
_refine_ls_R_factor_gt 0.0526
_refine_ls_wR_factor_ref 0.1424
_refine_ls_wR_factor_gt 0.1330
_refine_ls_goodness_of_fit_ref 0.958
_refine_ls_restrained_S_all 0.959
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.76677(3) 0.85186(2) 0.23098(2) 0.02563(10) Uani 1 1 d . . . . .
P2 P 0.56223(4) 0.20706(3) 0.22823(2) 0.03866(12) Uani 1 1 d . . . . .
N1 N 0.76295(10) 0.92712(8) 0.19272(5) 0.0268(3) Uani 1 1 d . . . . .
N2 N 0.64694(10) 0.82482(8) 0.25952(5) 0.0279(3) Uani 1 1 d . . . . .
N3 N 0.34785(11) 0.23673(8) 0.25137(6) 0.0327(3) Uani 1 1 d . . . . .
N4 N 0.46282(12) 0.33879(8) 0.21178(6) 0.0385(3) Uani 1 1 d . . . . .
N5 N 0.38530(10) 0.07555(8) 0.14900(5) 0.0263(3) Uani 1 1 d . . . . .
N6 N 0.48225(10) 0.02554(8) 0.21168(6) 0.0290(3) Uani 1 1 d . . . . .
C1 C 0.85322(12) 0.96870(9) 0.16167(6) 0.0245(3) Uani 1 1 d . . . . .
C2 C 0.96212(12) 1.01981(9) 0.19037(6) 0.0259(3) Uani 1 1 d . . . . .
C3 C 1.04506(13) 1.06338(10) 0.15524(7) 0.0283(3) Uani 1 1 d . . . . .
H3 H 1.1184 1.0969 0.1749 0.034 Uiso 1 1 calc R U . . .
C4 C 1.02358(13) 1.05912(10) 0.09267(7) 0.0306(3) Uani 1 1 d . . . . .
H4 H 1.0810 1.0895 0.0696 0.037 Uiso 1 1 calc R U . . .
C5 C 0.91703(13) 1.00986(10) 0.06426(7) 0.0298(3) Uani 1 1 d . . . . .
H5 H 0.9013 1.0069 0.0213 0.036 Uiso 1 1 calc R U . . .
C6 C 0.83264(12) 0.96464(9) 0.09733(6) 0.0255(3) Uani 1 1 d . . . . .
C7 C 0.99395(12) 1.03146(10) 0.25809(6) 0.0269(3) Uani 1 1 d . . . . .
C8 C 1.06427(13) 0.98669(10) 0.28147(7) 0.0307(3) Uani 1 1 d . . . . .
C9 C 1.10274(14) 1.00525(11) 0.34366(7) 0.0400(4) Uani 1 1 d . . . . .
H9 H 1.1512 0.9749 0.3592 0.048 Uiso 1 1 calc R U . . .
C10 C 1.07239(16) 1.06658(12) 0.38344(7) 0.0457(5) Uani 1 1 d . . . . .
C11 C 1.00059(16) 1.10931(11) 0.35982(7) 0.0426(4) Uani 1 1 d . . . . .
H11 H 0.9784 1.1512 0.3867 0.051 Uiso 1 1 calc R U . . .
C12 C 0.95998(14) 1.09277(10) 0.29795(7) 0.0327(4) Uani 1 1 d . . . . .
C13 C 1.09879(15) 0.91804(11) 0.24124(8) 0.0388(4) Uani 1 1 d . . . . .
H13A H 1.0300 0.8742 0.2199 0.058 Uiso 0.67(4) 1 calc R U P A 1
H13B H 1.1414 0.8902 0.2665 0.058 Uiso 0.67(4) 1 calc R U P A 1
H13C H 1.1476 0.9449 0.2111 0.058 Uiso 0.67(4) 1 calc R U P A 1
H13D H 1.1790 0.9226 0.2531 0.058 Uiso 0.33(4) 1 calc R U P A 2
H13E H 1.0905 0.9264 0.1983 0.058 Uiso 0.33(4) 1 calc R U P A 2
H13F H 1.0495 0.8604 0.2460 0.058 Uiso 0.33(4) 1 calc R U P A 2
C14 C 1.1140(2) 1.08440(16) 0.45076(8) 0.0684(7) Uani 1 1 d . . . . .
H14A H 1.1981 1.1052 0.4557 0.103 Uiso 0.68(4) 1 calc R U P B 1
H14B H 1.0875 1.0307 0.4685 0.103 Uiso 0.68(4) 1 calc R U P B 1
H14C H 1.0835 1.1288 0.4719 0.103 Uiso 0.68(4) 1 calc R U P B 1
H14D H 1.1513 1.1469 0.4632 0.103 Uiso 0.32(4) 1 calc R U P B 2
H14E H 1.1692 1.0525 0.4581 0.103 Uiso 0.32(4) 1 calc R U P B 2
H14F H 1.0487 1.0654 0.4747 0.103 Uiso 0.32(4) 1 calc R U P B 2
C15 C 0.88143(15) 1.14027(11) 0.27441(8) 0.0405(4) Uani 1 1 d . . . . .
H15A H 0.9242 1.1845 0.2513 0.061 Uiso 1 1 calc R U . . .
H15B H 0.8517 1.1684 0.3091 0.061 Uiso 1 1 calc R U . . .
H15C H 0.8173 1.0988 0.2475 0.061 Uiso 1 1 calc R U . . .
C16 C 0.71812(12) 0.91063(10) 0.06640(6) 0.0265(3) Uani 1 1 d . . . . .
C17 C 0.62858(12) 0.94810(10) 0.06193(6) 0.0271(3) Uani 1 1 d . . . . .
C18 C 0.52180(13) 0.89673(11) 0.03387(7) 0.0312(4) Uani 1 1 d . . . . .
H18 H 0.4615 0.9224 0.0303 0.037 Uiso 1 1 calc R U . . .
C19 C 0.50056(13) 0.80934(11) 0.01096(7) 0.0324(4) Uani 1 1 d . . . . .
C20 C 0.58996(14) 0.77335(10) 0.01641(7) 0.0331(4) Uani 1 1 d . . . . .
H20 H 0.5767 0.7134 0.0012 0.040 Uiso 1 1 calc R U . . .
C21 C 0.69861(13) 0.82243(10) 0.04352(6) 0.0290(3) Uani 1 1 d . . . . .
C22 C 0.64748(14) 1.04153(10) 0.08887(7) 0.0328(4) Uani 1 1 d . . . . .
H22A H 0.7056 1.0791 0.0676 0.049 Uiso 1 1 calc R U . . .
H22B H 0.6739 1.0505 0.1326 0.049 Uiso 1 1 calc R U . . .
H22C H 0.5753 1.0560 0.0840 0.049 Uiso 1 1 calc R U . . .
C23 C 0.38428(15) 0.75502(12) -0.01977(9) 0.0457(4) Uani 1 1 d . . . . .
H23A H 0.3736 0.7701 -0.0607 0.069 Uiso 0.67(3) 1 calc R U P C 1
H23B H 0.3244 0.7664 0.0049 0.069 Uiso 0.67(3) 1 calc R U P C 1
H23C H 0.3793 0.6932 -0.0234 0.069 Uiso 0.67(3) 1 calc R U P C 1
H23D H 0.3498 0.7100 0.0048 0.069 Uiso 0.33(3) 1 calc R U P C 2
H23E H 0.3929 0.7275 -0.0608 0.069 Uiso 0.33(3) 1 calc R U P C 2
H23F H 0.3346 0.7923 -0.0233 0.069 Uiso 0.33(3) 1 calc R U P C 2
C24 C 0.79311(15) 0.78064(11) 0.04992(8) 0.0392(4) Uani 1 1 d . . . . .
H24A H 0.7725 0.7248 0.0224 0.059 Uiso 0.85(6) 1 calc R U P D 1
H24B H 0.8035 0.7710 0.0924 0.059 Uiso 0.85(6) 1 calc R U P D 1
H24C H 0.8647 0.8190 0.0391 0.059 Uiso 0.85(6) 1 calc R U P D 1
H24D H 0.8392 0.8054 0.0893 0.059 Uiso 0.15(6) 1 calc R U P D 2
H24E H 0.8421 0.7916 0.0164 0.059 Uiso 0.15(6) 1 calc R U P D 2
H24F H 0.7594 0.7178 0.0482 0.059 Uiso 0.15(6) 1 calc R U P D 2
C25A C 0.6230(8) 0.7547(3) 0.2985(2) 0.0296(5) Uani 0.488(5) 1 d DG . P E 1
C26A C 0.6380(7) 0.6738(3) 0.2799(2) 0.0304(5) Uani 0.488(5) 1 d DG . P E 1
C27A C 0.6196(4) 0.6123(3) 0.3193(2) 0.0307(6) Uani 0.488(5) 1 d DG . P E 1
H27A H 0.6299 0.5570 0.3065 0.037 Uiso 0.488(5) 1 calc R U P E 1
C28A C 0.5862(3) 0.6317(2) 0.37730(17) 0.0296(5) Uani 0.488(5) 1 d DG . P E 1
H28A H 0.5736 0.5896 0.4042 0.036 Uiso 0.488(5) 1 calc R U P E 1
C29A C 0.5712(3) 0.7126(2) 0.39594(16) 0.0304(5) Uani 0.488(5) 1 d DG . P E 1
H29A H 0.5483 0.7258 0.4356 0.037 Uiso 0.488(5) 1 calc R U P E 1
C30A C 0.5896(6) 0.7741(2) 0.3565(2) 0.0307(6) Uani 0.488(5) 1 d DG . P E 1
C31A C 0.6565(10) 0.6418(10) 0.2145(3) 0.0289(4) Uani 0.488(5) 1 d D . P E 1
C32A C 0.5734(8) 0.6303(7) 0.1650(3) 0.0304(5) Uani 0.488(5) 1 d D . P E 1
C33A C 0.5890(5) 0.5906(4) 0.1076(3) 0.0297(5) Uani 0.488(5) 1 d D . P E 1
H33A H 0.5315 0.5813 0.0746 0.036 Uiso 0.488(5) 1 calc R U P E 1
C34A C 0.6855(4) 0.5643(4) 0.09666(19) 0.0289(4) Uani 0.488(5) 1 d D . P E 1
C35A C 0.7654(6) 0.5747(4) 0.1461(2) 0.0304(5) Uani 0.488(5) 1 d D . P E 1
H35A H 0.8311 0.5556 0.1398 0.036 Uiso 0.488(5) 1 calc R U P E 1
C36A C 0.7526(8) 0.6121(5) 0.2046(3) 0.0297(5) Uani 0.488(5) 1 d D . P E 1
C37A C 0.4698(12) 0.6608(13) 0.1712(6) 0.0405(10) Uani 0.488(5) 1 d D . P E 1
H37A H 0.4893 0.7223 0.1664 0.061 Uiso 0.488(5) 1 calc R U P E 1
H37B H 0.4431 0.6537 0.2118 0.061 Uiso 0.488(5) 1 calc R U P E 1
H37C H 0.4088 0.6263 0.1394 0.061 Uiso 0.488(5) 1 calc R U P E 1
C38A C 0.7072(12) 0.5220(14) 0.0353(4) 0.0512(17) Uani 0.488(5) 1 d D . P E 1
H38A H 0.6350 0.4995 0.0086 0.077 Uiso 0.488(5) 1 calc R U P E 1
H38B H 0.7381 0.4739 0.0410 0.077 Uiso 0.488(5) 1 calc R U P E 1
H38C H 0.7626 0.5650 0.0162 0.077 Uiso 0.488(5) 1 calc R U P E 1
C39A C 0.8466(15) 0.6294(18) 0.2556(6) 0.0434(9) Uani 0.488(5) 1 d D . P E 1
H39A H 0.9051 0.6027 0.2416 0.065 Uiso 0.488(5) 1 calc R U P E 1
H39B H 0.8144 0.6044 0.2911 0.065 Uiso 0.488(5) 1 calc R U P E 1
H39C H 0.8815 0.6923 0.2673 0.065 Uiso 0.488(5) 1 calc R U P E 1
C40A C 0.5624(5) 0.8576(4) 0.3756(5) 0.0354(8) Uani 0.488(5) 1 d D . P E 1
C41A C 0.4478(5) 0.8599(3) 0.3784(2) 0.0349(7) Uani 0.488(5) 1 d D . P E 1
C42A C 0.4261(4) 0.9365(2) 0.4028(2) 0.0334(7) Uani 0.488(5) 1 d D . P E 1
H42A H 0.3491 0.9371 0.4058 0.040 Uiso 0.488(5) 1 calc R U P E 1
C43A C 0.5162(4) 1.0128(3) 0.4230(3) 0.0354(8) Uani 0.488(5) 1 d D . P E 1
C44A C 0.6283(4) 1.0090(3) 0.4211(4) 0.0349(7) Uani 0.488(5) 1 d D . P E 1
H44A H 0.6902 1.0601 0.4354 0.042 Uiso 0.488(5) 1 calc R U P E 1
C45A C 0.6520(5) 0.9327(4) 0.3990(5) 0.0334(7) Uani 0.488(5) 1 d D . P E 1
C46A C 0.3495(7) 0.7791(4) 0.3531(3) 0.0447(13) Uani 0.488(5) 1 d D . P E 1
H46A H 0.2772 0.7938 0.3520 0.067 Uiso 0.488(5) 1 calc R U P E 1
H46B H 0.3457 0.7346 0.3794 0.067 Uiso 0.488(5) 1 calc R U P E 1
H46C H 0.3623 0.7567 0.3114 0.067 Uiso 0.488(5) 1 calc R U P E 1
C47A C 0.4885(10) 1.0947(6) 0.4478(6) 0.0557(18) Uani 0.488(5) 1 d D . P E 1
H47A H 0.5188 1.1396 0.4224 0.084 Uiso 0.488(5) 1 calc R U P E 1
H47B H 0.5237 1.1153 0.4901 0.084 Uiso 0.488(5) 1 calc R U P E 1
H47C H 0.4051 1.0826 0.4471 0.084 Uiso 0.488(5) 1 calc R U P E 1
C48A C 0.7744(7) 0.9314(9) 0.4033(8) 0.0363(14) Uani 0.488(5) 1 d D . P E 1
H48A H 0.7971 0.9190 0.3620 0.054 Uiso 0.488(5) 1 calc R U P E 1
H48B H 0.7821 0.8863 0.4270 0.054 Uiso 0.488(5) 1 calc R U P E 1
H48C H 0.8241 0.9882 0.4237 0.054 Uiso 0.488(5) 1 calc R U P E 1
C25B C 0.6180(8) 0.7590(3) 0.2937(2) 0.0296(5) Uani 0.512(5) 1 d DG . P E 2
C26B C 0.6282(7) 0.6762(3) 0.2766(2) 0.0304(5) Uani 0.512(5) 1 d DG . P E 2
C27B C 0.5957(4) 0.6137(2) 0.3148(2) 0.0307(6) Uani 0.512(5) 1 d DG . P E 2
H27B H 0.6027 0.5572 0.3031 0.037 Uiso 0.512(5) 1 calc R U P E 2
C28B C 0.5529(3) 0.6340(2) 0.37003(15) 0.0296(5) Uani 0.512(5) 1 d DG . P E 2
H28B H 0.5306 0.5913 0.3961 0.036 Uiso 0.512(5) 1 calc R U P E 2
C29B C 0.5426(3) 0.7168(2) 0.38714(14) 0.0304(5) Uani 0.512(5) 1 d DG . P E 2
H29B H 0.5133 0.7306 0.4249 0.037 Uiso 0.512(5) 1 calc R U P E 2
C30B C 0.5751(6) 0.7793(2) 0.3490(2) 0.0307(6) Uani 0.512(5) 1 d DG . P E 2
C31B C 0.6640(10) 0.6433(10) 0.2154(3) 0.0289(4) Uani 0.512(5) 1 d D . P E 2
C32B C 0.5896(7) 0.6311(6) 0.1618(3) 0.0304(5) Uani 0.512(5) 1 d D . P E 2
C33B C 0.6165(5) 0.5926(4) 0.1063(3) 0.0297(5) Uani 0.512(5) 1 d D . P E 2
H33B H 0.5661 0.5845 0.0703 0.036 Uiso 0.512(5) 1 calc R U P E 2
C34B C 0.7146(4) 0.5654(4) 0.10192(19) 0.0289(4) Uani 0.512(5) 1 d D . P E 2
C35B C 0.7887(5) 0.5826(4) 0.1542(2) 0.0304(5) Uani 0.512(5) 1 d D . P E 2
H35B H 0.8578 0.5671 0.1518 0.036 Uiso 0.512(5) 1 calc R U P E 2
C36B C 0.7670(7) 0.6217(5) 0.2106(2) 0.0297(5) Uani 0.512(5) 1 d D . P E 2
C37B C 0.4835(11) 0.6595(13) 0.1646(6) 0.0405(10) Uani 0.512(5) 1 d D . P E 2
H37D H 0.4448 0.6503 0.1232 0.061 Uiso 0.512(5) 1 calc R U P E 2
H37E H 0.5044 0.7214 0.1819 0.061 Uiso 0.512(5) 1 calc R U P E 2
H37F H 0.4317 0.6254 0.1906 0.061 Uiso 0.512(5) 1 calc R U P E 2
C38B C 0.7367(12) 0.5232(13) 0.0406(4) 0.0512(17) Uani 0.512(5) 1 d D . P E 2
H38D H 0.7076 0.4598 0.0376 0.077 Uiso 0.512(5) 1 calc R U P E 2
H38E H 0.8195 0.5404 0.0367 0.077 Uiso 0.512(5) 1 calc R U P E 2
H38F H 0.6975 0.5421 0.0077 0.077 Uiso 0.512(5) 1 calc R U P E 2
C39B C 0.8534(15) 0.6369(16) 0.2649(5) 0.0434(9) Uani 0.512(5) 1 d D . P E 2
H39D H 0.9253 0.6297 0.2508 0.065 Uiso 0.512(5) 1 calc R U P E 2
H39E H 0.8238 0.5948 0.2924 0.065 Uiso 0.512(5) 1 calc R U P E 2
H39F H 0.8676 0.6961 0.2869 0.065 Uiso 0.512(5) 1 calc R U P E 2
C40B C 0.5486(5) 0.8622(3) 0.3694(5) 0.0354(8) Uani 0.512(5) 1 d D . P E 2
C41B C 0.4335(5) 0.8628(3) 0.36074(19) 0.0349(7) Uani 0.512(5) 1 d D . P E 2
C42B C 0.4068(4) 0.9388(2) 0.38097(19) 0.0334(7) Uani 0.512(5) 1 d D . P E 2
H42B H 0.3297 0.9391 0.3737 0.040 Uiso 0.512(5) 1 calc R U P E 2
C43B C 0.4856(4) 1.0131(3) 0.4108(3) 0.0354(8) Uani 0.512(5) 1 d D . P E 2
C44B C 0.5994(4) 1.0123(3) 0.4171(3) 0.0349(7) Uani 0.512(5) 1 d D . P E 2
H44B H 0.6563 1.0635 0.4368 0.042 Uiso 0.512(5) 1 calc R U P E 2
C45B C 0.6335(4) 0.9389(3) 0.3955(5) 0.0334(7) Uani 0.512(5) 1 d D . P E 2
C46B C 0.3375(6) 0.7832(4) 0.3311(3) 0.0447(13) Uani 0.512(5) 1 d D . P E 2
H46D H 0.2716 0.8010 0.3172 0.067 Uiso 0.512(5) 1 calc R U P E 2
H46E H 0.3146 0.7436 0.3611 0.067 Uiso 0.512(5) 1 calc R U P E 2
H46F H 0.3642 0.7534 0.2960 0.067 Uiso 0.512(5) 1 calc R U P E 2
C47B C 0.4530(9) 1.0933(6) 0.4344(6) 0.0557(18) Uani 0.512(5) 1 d D . P E 2
H47D H 0.5002 1.1431 0.4175 0.084 Uiso 0.512(5) 1 calc R U P E 2
H47E H 0.4659 1.1049 0.4793 0.084 Uiso 0.512(5) 1 calc R U P E 2
H47F H 0.3718 1.0842 0.4217 0.084 Uiso 0.512(5) 1 calc R U P E 2
C48B C 0.7579(6) 0.9430(8) 0.3989(8) 0.0363(14) Uani 0.512(5) 1 d D . P E 2
H48D H 0.7864 0.9501 0.3587 0.054 Uiso 0.512(5) 1 calc R U P E 2
H48E H 0.7666 0.8890 0.4107 0.054 Uiso 0.512(5) 1 calc R U P E 2
H48F H 0.8020 0.9924 0.4295 0.054 Uiso 0.512(5) 1 calc R U P E 2
C49 C 0.45349(14) 0.26103(10) 0.23019(7) 0.0337(4) Uani 1 1 d . . . . .
C50 C 0.29102(14) 0.29825(11) 0.24415(8) 0.0375(4) Uani 1 1 d . . . . .
C51 C 0.36290(15) 0.36225(11) 0.21995(8) 0.0411(4) Uani 1 1 d . . . . .
C52 C 0.30676(14) 0.16134(11) 0.28223(8) 0.0382(4) Uani 1 1 d . . . . .
H52A H 0.2712 0.1096 0.2516 0.057 Uiso 1 1 calc R U . . .
H52B H 0.2500 0.1711 0.3099 0.057 Uiso 1 1 calc R U . . .
H52C H 0.3715 0.1527 0.3060 0.057 Uiso 1 1 calc R U . . .
C53 C 0.17269(16) 0.28882(13) 0.26227(9) 0.0510(5) Uani 1 1 d . . . . .
H53A H 0.1481 0.3382 0.2524 0.076 Uiso 1 1 calc R U . . .
H53B H 0.1723 0.2875 0.3065 0.076 Uiso 1 1 calc R U . . .
H53C H 0.1199 0.2346 0.2399 0.076 Uiso 1 1 calc R U . . .
C54 C 0.34940(19) 0.44521(12) 0.20428(11) 0.0598(6) Uani 1 1 d . . . . .
H54A H 0.3586 0.4472 0.1607 0.090 Uiso 1 1 calc R U . . .
H54B H 0.4078 0.4944 0.2291 0.090 Uiso 1 1 calc R U . . .
H54C H 0.2729 0.4488 0.2128 0.090 Uiso 1 1 calc R U . . .
C55 C 0.56249(18) 0.38858(12) 0.18503(11) 0.0589(6) Uani 1 1 d . . . . .
H55A H 0.5940 0.3486 0.1594 0.088 Uiso 0.72(2) 1 calc R U P F 1
H55B H 0.6210 0.4234 0.2179 0.088 Uiso 0.72(2) 1 calc R U P F 1
H55C H 0.5395 0.4272 0.1599 0.088 Uiso 0.72(2) 1 calc R U P F 1
H55D H 0.5760 0.4509 0.1990 0.088 Uiso 0.28(2) 1 calc R U P F 2
H55E H 0.5484 0.3765 0.1402 0.088 Uiso 0.28(2) 1 calc R U P F 2
H55F H 0.6300 0.3719 0.1979 0.088 Uiso 0.28(2) 1 calc R U P F 2
C56 C 0.47018(12) 0.10024(10) 0.19616(7) 0.0290(3) Uani 1 1 d . . . . .
C57 C 0.34464(12) -0.01433(9) 0.13568(7) 0.0273(3) Uani 1 1 d . . . . .
C58 C 0.40629(12) -0.04583(9) 0.17421(7) 0.0287(3) Uani 1 1 d . . . . .
C59 C 0.35278(14) 0.13495(10) 0.11257(7) 0.0343(4) Uani 1 1 d . . . . .
H59A H 0.4202 0.1844 0.1104 0.052 Uiso 1 1 calc R U . . .
H59B H 0.2934 0.1560 0.1318 0.052 Uiso 1 1 calc R U . . .
H59C H 0.3229 0.1043 0.0711 0.052 Uiso 1 1 calc R U . . .
C60 C 0.25028(13) -0.06138(10) 0.08678(7) 0.0344(4) Uani 1 1 d . . . . .
H60A H 0.2735 -0.0461 0.0470 0.052 Uiso 1 1 calc R U . . .
H60B H 0.1811 -0.0447 0.0955 0.052 Uiso 1 1 calc R U . . .
H60C H 0.2343 -0.1243 0.0857 0.052 Uiso 1 1 calc R U . . .
C61 C 0.40631(15) -0.13592(11) 0.17969(9) 0.0433(4) Uani 1 1 d . . . . .
H61A H 0.3586 -0.1763 0.1448 0.065 Uiso 1 1 calc R U . . .
H61B H 0.3753 -0.1515 0.2180 0.065 Uiso 1 1 calc R U . . .
H61C H 0.4850 -0.1394 0.1798 0.065 Uiso 1 1 calc R U . . .
C62 C 0.56373(14) 0.01833(11) 0.26011(8) 0.0397(4) Uani 1 1 d . . . . .
H62A H 0.6230 -0.0037 0.2416 0.060 Uiso 1 1 calc R U . . .
H62B H 0.5231 -0.0219 0.2865 0.060 Uiso 1 1 calc R U . . .
H62C H 0.5997 0.0757 0.2846 0.060 Uiso 1 1 calc R U . . .
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
P1 0.0253(2) 0.0265(2) 0.0280(2) 0.00593(16) 0.00379(15) 0.01127(16)
P2 0.0284(2) 0.0264(2) 0.0589(3) 0.0018(2) 0.00922(19) 0.00594(17)
N1 0.0263(7) 0.0314(7) 0.0250(6) 0.0049(5) 0.0019(5) 0.0121(5)
N2 0.0272(7) 0.0269(7) 0.0309(7) 0.0037(5) 0.0038(5) 0.0101(5)
N3 0.0328(7) 0.0254(7) 0.0425(8) 0.0078(6) 0.0147(6) 0.0097(6)
N4 0.0411(8) 0.0231(7) 0.0519(9) 0.0074(6) 0.0190(7) 0.0072(6)
N5 0.0268(7) 0.0243(7) 0.0323(7) 0.0086(5) 0.0094(5) 0.0117(5)
N6 0.0228(7) 0.0269(7) 0.0398(7) 0.0065(6) 0.0051(5) 0.0103(5)
C1 0.0290(8) 0.0252(8) 0.0250(7) 0.0052(6) 0.0044(6) 0.0163(6)
C2 0.0289(8) 0.0270(8) 0.0260(7) 0.0043(6) 0.0036(6) 0.0149(6)
C3 0.0263(8) 0.0302(8) 0.0302(8) 0.0029(6) 0.0024(6) 0.0118(6)
C4 0.0290(8) 0.0386(9) 0.0291(8) 0.0080(7) 0.0094(6) 0.0154(7)
C5 0.0318(9) 0.0400(9) 0.0232(7) 0.0043(7) 0.0044(6) 0.0196(7)
C6 0.0277(8) 0.0296(8) 0.0245(7) 0.0033(6) 0.0021(6) 0.0173(6)
C7 0.0270(8) 0.0274(8) 0.0242(7) 0.0036(6) 0.0018(6) 0.0050(6)
C8 0.0301(9) 0.0280(8) 0.0325(8) 0.0082(7) -0.0002(6) 0.0054(6)
C9 0.0404(10) 0.0397(10) 0.0357(9) 0.0130(8) -0.0067(7) 0.0039(8)
C10 0.0500(11) 0.0474(11) 0.0281(9) 0.0079(8) -0.0027(8) -0.0034(9)
C11 0.0516(11) 0.0380(10) 0.0305(9) -0.0013(7) 0.0094(8) 0.0033(8)
C12 0.0371(9) 0.0281(8) 0.0295(8) 0.0031(7) 0.0044(7) 0.0048(7)
C13 0.0394(10) 0.0360(9) 0.0454(10) 0.0087(8) 0.0001(7) 0.0179(7)
C14 0.0836(17) 0.0755(16) 0.0319(10) 0.0070(10) -0.0066(10) 0.0042(12)
C15 0.0424(10) 0.0376(10) 0.0440(10) 0.0004(8) 0.0129(8) 0.0170(8)
C16 0.0299(8) 0.0342(9) 0.0205(7) 0.0069(6) 0.0037(6) 0.0161(7)
C17 0.0276(8) 0.0353(9) 0.0226(7) 0.0052(6) 0.0047(6) 0.0152(7)
C18 0.0268(8) 0.0428(10) 0.0292(8) 0.0088(7) 0.0068(6) 0.0166(7)
C19 0.0292(9) 0.0395(10) 0.0288(8) 0.0113(7) 0.0049(6) 0.0077(7)
C20 0.0406(10) 0.0287(9) 0.0322(8) 0.0107(7) 0.0066(7) 0.0107(7)
C21 0.0345(9) 0.0333(9) 0.0244(7) 0.0080(6) 0.0051(6) 0.0164(7)
C22 0.0325(9) 0.0401(9) 0.0312(8) 0.0022(7) 0.0016(6) 0.0210(7)
C23 0.0338(10) 0.0435(11) 0.0558(11) 0.0091(9) 0.0035(8) 0.0048(8)
C24 0.0434(10) 0.0346(9) 0.0451(10) 0.0054(8) 0.0006(8) 0.0210(8)
C25A 0.0203(9) 0.0322(7) 0.0391(8) 0.0114(6) 0.0049(8) 0.0093(6)
C26A 0.0224(12) 0.0338(7) 0.0380(8) 0.0094(6) 0.0068(8) 0.0107(6)
C27A 0.0240(14) 0.0313(7) 0.0396(9) 0.0089(6) 0.0060(10) 0.0108(7)
C28A 0.0203(9) 0.0322(7) 0.0391(8) 0.0114(6) 0.0049(8) 0.0093(6)
C29A 0.0224(12) 0.0338(7) 0.0380(8) 0.0094(6) 0.0068(8) 0.0107(6)
C30A 0.0240(14) 0.0313(7) 0.0396(9) 0.0089(6) 0.0060(10) 0.0108(7)
C31A 0.0290(13) 0.0210(6) 0.0389(7) 0.0062(5) 0.0064(7) 0.0094(9)
C32A 0.0255(19) 0.0220(7) 0.0451(9) 0.0062(6) 0.0055(7) 0.0087(11)
C33A 0.0261(18) 0.0223(9) 0.0403(8) 0.0055(6) 0.0026(9) 0.0064(12)
C34A 0.0290(13) 0.0210(6) 0.0389(7) 0.0062(5) 0.0064(7) 0.0094(9)
C35A 0.0255(19) 0.0220(7) 0.0451(9) 0.0062(6) 0.0055(7) 0.0087(11)
C36A 0.0261(18) 0.0223(9) 0.0403(8) 0.0055(6) 0.0026(9) 0.0064(12)
C37A 0.032(2) 0.0296(11) 0.061(2) 0.003(2) -0.0043(19) 0.0146(17)
C38A 0.069(5) 0.0359(14) 0.0498(17) 0.0024(15) 0.016(2) 0.017(5)
C39A 0.0392(17) 0.053(4) 0.046(3) 0.013(3) 0.0024(18) 0.024(2)
C40A 0.0316(13) 0.0367(7) 0.0382(18) 0.0010(8) 0.0097(13) 0.0118(8)
C41A 0.0300(13) 0.0373(7) 0.0351(11) 0.0015(8) 0.0077(15) 0.0076(8)
C42A 0.0334(12) 0.0402(8) 0.0281(11) 0.0044(9) 0.0080(13) 0.0126(8)
C43A 0.0316(13) 0.0367(7) 0.0382(18) 0.0010(8) 0.0097(13) 0.0118(8)
C44A 0.0300(13) 0.0373(7) 0.0351(11) 0.0015(8) 0.0077(15) 0.0076(8)
C45A 0.0334(12) 0.0402(8) 0.0281(11) 0.0044(9) 0.0080(13) 0.0126(8)
C46A 0.0290(18) 0.0519(14) 0.049(4) 0.003(2) 0.001(2) 0.0087(11)
C47A 0.062(6) 0.0459(13) 0.066(5) 0.0059(19) 0.022(3) 0.026(3)
C48A 0.0305(19) 0.043(3) 0.035(2) 0.0079(19) -0.005(2) 0.0100(15)
C25B 0.0203(9) 0.0322(7) 0.0391(8) 0.0114(6) 0.0049(8) 0.0093(6)
C26B 0.0224(12) 0.0338(7) 0.0380(8) 0.0094(6) 0.0068(8) 0.0107(6)
C27B 0.0240(14) 0.0313(7) 0.0396(9) 0.0089(6) 0.0060(10) 0.0108(7)
C28B 0.0203(9) 0.0322(7) 0.0391(8) 0.0114(6) 0.0049(8) 0.0093(6)
C29B 0.0224(12) 0.0338(7) 0.0380(8) 0.0094(6) 0.0068(8) 0.0107(6)
C30B 0.0240(14) 0.0313(7) 0.0396(9) 0.0089(6) 0.0060(10) 0.0108(7)
C31B 0.0290(13) 0.0210(6) 0.0389(7) 0.0062(5) 0.0064(7) 0.0094(9)
C32B 0.0255(19) 0.0220(7) 0.0451(9) 0.0062(6) 0.0055(7) 0.0087(11)
C33B 0.0261(18) 0.0223(9) 0.0403(8) 0.0055(6) 0.0026(9) 0.0064(12)
C34B 0.0290(13) 0.0210(6) 0.0389(7) 0.0062(5) 0.0064(7) 0.0094(9)
C35B 0.0255(19) 0.0220(7) 0.0451(9) 0.0062(6) 0.0055(7) 0.0087(11)
C36B 0.0261(18) 0.0223(9) 0.0403(8) 0.0055(6) 0.0026(9) 0.0064(12)
C37B 0.032(2) 0.0296(11) 0.061(2) 0.003(2) -0.0043(19) 0.0146(17)
C38B 0.069(5) 0.0359(14) 0.0498(17) 0.0024(15) 0.016(2) 0.017(5)
C39B 0.0392(17) 0.053(4) 0.046(3) 0.013(3) 0.0024(18) 0.024(2)
C40B 0.0316(13) 0.0367(7) 0.0382(18) 0.0010(8) 0.0097(13) 0.0118(8)
C41B 0.0300(13) 0.0373(7) 0.0351(11) 0.0015(8) 0.0077(15) 0.0076(8)
C42B 0.0334(12) 0.0402(8) 0.0281(11) 0.0044(9) 0.0080(13) 0.0126(8)
C43B 0.0316(13) 0.0367(7) 0.0382(18) 0.0010(8) 0.0097(13) 0.0118(8)
C44B 0.0300(13) 0.0373(7) 0.0351(11) 0.0015(8) 0.0077(15) 0.0076(8)
C45B 0.0334(12) 0.0402(8) 0.0281(11) 0.0044(9) 0.0080(13) 0.0126(8)
C46B 0.0290(18) 0.0519(14) 0.049(4) 0.003(2) 0.001(2) 0.0087(11)
C47B 0.062(6) 0.0459(13) 0.066(5) 0.0059(19) 0.022(3) 0.026(3)
C48B 0.0305(19) 0.043(3) 0.035(2) 0.0079(19) -0.005(2) 0.0100(15)
C49 0.0351(9) 0.0252(8) 0.0394(9) 0.0032(7) 0.0120(7) 0.0064(7)
C50 0.0404(10) 0.0296(9) 0.0465(10) 0.0049(7) 0.0142(8) 0.0153(7)
C51 0.0482(11) 0.0281(9) 0.0528(11) 0.0082(8) 0.0158(8) 0.0180(8)
C52 0.0380(9) 0.0339(9) 0.0458(10) 0.0132(8) 0.0175(7) 0.0099(7)
C53 0.0435(11) 0.0481(11) 0.0676(13) 0.0072(10) 0.0214(9) 0.0218(9)
C54 0.0645(14) 0.0346(11) 0.0880(16) 0.0180(10) 0.0165(11) 0.0217(10)
C55 0.0582(13) 0.0335(10) 0.0885(15) 0.0205(10) 0.0399(11) 0.0083(9)
C56 0.0251(8) 0.0261(8) 0.0388(9) 0.0074(7) 0.0122(7) 0.0098(6)
C57 0.0262(8) 0.0265(8) 0.0319(8) 0.0055(6) 0.0104(6) 0.0102(6)
C58 0.0265(8) 0.0237(8) 0.0374(8) 0.0056(7) 0.0070(6) 0.0090(6)
C59 0.0435(10) 0.0312(9) 0.0369(9) 0.0149(7) 0.0140(7) 0.0185(7)
C60 0.0315(9) 0.0338(9) 0.0385(9) 0.0014(7) 0.0029(7) 0.0130(7)
C61 0.0436(11) 0.0299(9) 0.0593(11) 0.0119(8) -0.0006(8) 0.0141(8)
C62 0.0295(9) 0.0387(10) 0.0529(11) 0.0061(8) -0.0051(7) 0.0153(7)
#==============================================================================
# MOLECULAR GEOMETRY
_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
P1 N1 1.5864(12) . ?
P1 N2 1.5929(13) . ?
P2 C49 1.7897(17) . ?
P2 C56 1.8006(16) . ?
N1 C1 1.3856(18) . ?
N2 C25B 1.366(4) . ?
N2 C25A 1.490(4) . ?
N3 C49 1.3645(19) . ?
N3 C50 1.392(2) . ?
N3 C52 1.4571(19) . ?
N4 C49 1.354(2) . ?
N4 C51 1.393(2) . ?
N4 C55 1.458(2) . ?
N5 C56 1.3629(19) . ?
N5 C57 1.3846(19) . ?
N5 C59 1.4600(19) . ?
N6 C56 1.3494(19) . ?
N6 C58 1.3907(19) . ?
N6 C62 1.462(2) . ?
C1 C2 1.413(2) . ?
C1 C6 1.4201(19) . ?
C2 C3 1.396(2) . ?
C2 C7 1.499(2) . ?
C3 C4 1.382(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(2) . ?
C5 H5 0.9500 . ?
C6 C16 1.493(2) . ?
C7 C8 1.396(2) . ?
C7 C12 1.408(2) . ?
C8 C9 1.393(2) . ?
C8 C13 1.502(2) . ?
C9 C10 1.384(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(3) . ?
C10 C14 1.509(2) . ?
C11 C12 1.393(2) . ?
C11 H11 0.9500 . ?
C12 C15 1.506(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 H13D 0.9800 . ?
C13 H13E 0.9800 . ?
C13 H13F 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 H14D 0.9800 . ?
C14 H14E 0.9800 . ?
C14 H14F 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.401(2) . ?
C16 C17 1.402(2) . ?
C17 C18 1.390(2) . ?
C17 C22 1.501(2) . ?
C18 C19 1.386(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.387(2) . ?
C19 C23 1.508(2) . ?
C20 C21 1.392(2) . ?
C20 H20 0.9500 . ?
C21 C24 1.508(2) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 H23D 0.9800 . ?
C23 H23E 0.9800 . ?
C23 H23F 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9800 . ?
C25A C26A 1.3900 . ?
C25A C30A 1.3900 . ?
C26A C27A 1.3900 . ?
C26A C31A 1.519(4) . ?
C27A C28A 1.3900 . ?
C27A H27A 0.9500 . ?
C28A C29A 1.3900 . ?
C28A H28A 0.9500 . ?
C29A C30A 1.3900 . ?
C29A H29A 0.9500 . ?
C30A C40A 1.499(4) . ?
C31A C32A 1.408(5) . ?
C31A C36A 1.409(5) . ?
C32A C33A 1.393(5) . ?
C32A C37A 1.493(5) . ?
C33A C34A 1.387(4) . ?
C33A H33A 0.9500 . ?
C34A C35A 1.385(5) . ?
C34A C38A 1.509(5) . ?
C35A C36A 1.390(5) . ?
C35A H35A 0.9500 . ?
C36A C39A 1.504(5) . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
C38A H38A 0.9800 . ?
C38A H38B 0.9800 . ?
C38A H38C 0.9800 . ?
C39A H39A 0.9800 . ?
C39A H39B 0.9800 . ?
C39A H39C 0.9800 . ?
C40A C45A 1.399(5) . ?
C40A C41A 1.416(5) . ?
C41A C42A 1.391(5) . ?
C41A C46A 1.518(5) . ?
C42A C43A 1.401(5) . ?
C42A H42A 0.9500 . ?
C43A C44A 1.391(5) . ?
C43A C47A 1.507(5) . ?
C44A C45A 1.386(5) . ?
C44A H44A 0.9500 . ?
C45A C48A 1.500(5) . ?
C46A H46A 0.9800 . ?
C46A H46B 0.9800 . ?
C46A H46C 0.9800 . ?
C47A H47A 0.9800 . ?
C47A H47B 0.9800 . ?
C47A H47C 0.9800 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C25B C26B 1.3900 . ?
C25B C30B 1.3900 . ?
C26B C27B 1.3900 . ?
C26B C31B 1.519(4) . ?
C27B C28B 1.3900 . ?
C27B H27B 0.9500 . ?
C28B C29B 1.3900 . ?
C28B H28B 0.9500 . ?
C29B C30B 1.3900 . ?
C29B H29B 0.9500 . ?
C30B C40B 1.493(4) . ?
C31B C36B 1.407(5) . ?
C31B C32B 1.412(5) . ?
C32B C33B 1.399(5) . ?
C32B C37B 1.497(5) . ?
C33B C34B 1.395(4) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.375(4) . ?
C34B C38B 1.509(5) . ?
C35B C36B 1.395(5) . ?
C35B H35B 0.9500 . ?
C36B C39B 1.501(5) . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
C39B H39D 0.9800 . ?
C39B H39E 0.9800 . ?
C39B H39F 0.9800 . ?
C40B C45B 1.401(5) . ?
C40B C41B 1.412(5) . ?
C41B C42B 1.389(5) . ?
C41B C46B 1.515(5) . ?
C42B C43B 1.367(4) . ?
C42B H42B 0.9500 . ?
C43B C44B 1.395(4) . ?
C43B C47B 1.505(5) . ?
C44B C45B 1.406(5) . ?
C44B H44B 0.9500 . ?
C45B C48B 1.500(5) . ?
C46B H46D 0.9800 . ?
C46B H46E 0.9800 . ?
C46B H46F 0.9800 . ?
C47B H47D 0.9800 . ?
C47B H47E 0.9800 . ?
C47B H47F 0.9800 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C50 C51 1.346(2) . ?
C50 C53 1.492(2) . ?
C51 C54 1.487(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C55 H55D 0.9800 . ?
C55 H55E 0.9800 . ?
C55 H55F 0.9800 . ?
C57 C58 1.351(2) . ?
C57 C60 1.490(2) . ?
C58 C61 1.484(2) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
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 P1 N2 106.31(7) . . ?
C49 P2 C56 96.96(7) . . ?
C1 N1 P1 123.46(10) . . ?
C25B N2 P1 122.7(4) . . ?
C25A N2 P1 119.8(4) . . ?
C49 N3 C50 110.18(13) . . ?
C49 N3 C52 123.97(13) . . ?
C50 N3 C52 125.61(13) . . ?
C49 N4 C51 110.56(13) . . ?
C49 N4 C55 124.07(14) . . ?
C51 N4 C55 125.33(14) . . ?
C56 N5 C57 110.20(12) . . ?
C56 N5 C59 124.66(12) . . ?
C57 N5 C59 124.67(13) . . ?
C56 N6 C58 110.36(12) . . ?
C56 N6 C62 126.06(13) . . ?
C58 N6 C62 123.58(13) . . ?
N1 C1 C2 124.25(12) . . ?
N1 C1 C6 117.87(13) . . ?
C2 C1 C6 117.73(13) . . ?
C3 C2 C1 119.73(13) . . ?
C3 C2 C7 117.12(13) . . ?
C1 C2 C7 123.14(12) . . ?
C4 C3 C2 121.87(14) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C5 C4 C3 118.82(14) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 121.17(13) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 120.67(13) . . ?
C5 C6 C16 121.05(12) . . ?
C1 C6 C16 118.28(12) . . ?
C8 C7 C12 119.62(13) . . ?
C8 C7 C2 120.40(13) . . ?
C12 C7 C2 119.81(13) . . ?
C9 C8 C7 119.48(15) . . ?
C9 C8 C13 118.95(15) . . ?
C7 C8 C13 121.57(14) . . ?
C10 C9 C8 121.86(16) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C9 C10 C11 118.04(15) . . ?
C9 C10 C14 120.68(19) . . ?
C11 C10 C14 121.26(19) . . ?
C10 C11 C12 122.04(17) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C11 C12 C7 118.92(15) . . ?
C11 C12 C15 120.21(15) . . ?
C7 C12 C15 120.87(14) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C8 C13 H13D 109.5 . . ?
C8 C13 H13E 109.5 . . ?
H13D C13 H13E 109.5 . . ?
C8 C13 H13F 109.5 . . ?
H13D C13 H13F 109.5 . . ?
H13E C13 H13F 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C14 H14D 109.5 . . ?
C10 C14 H14E 109.5 . . ?
H14D C14 H14E 109.5 . . ?
C10 C14 H14F 109.5 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 119.89(14) . . ?
C21 C16 C6 120.56(13) . . ?
C17 C16 C6 119.53(13) . . ?
C18 C17 C16 118.97(14) . . ?
C18 C17 C22 120.86(13) . . ?
C16 C17 C22 120.14(13) . . ?
C19 C18 C17 122.11(14) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C18 C19 C20 118.00(14) . . ?
C18 C19 C23 121.20(15) . . ?
C20 C19 C23 120.80(15) . . ?
C19 C20 C21 121.93(15) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C16 119.09(14) . . ?
C20 C21 C24 120.48(14) . . ?
C16 C21 C24 120.40(14) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C23 H23D 109.5 . . ?
C19 C23 H23E 109.5 . . ?
H23D C23 H23E 109.5 . . ?
C19 C23 H23F 109.5 . . ?
H23D C23 H23F 109.5 . . ?
H23E C23 H23F 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C24 H24D 109.5 . . ?
C21 C24 H24E 109.5 . . ?
H24D C24 H24E 109.5 . . ?
C21 C24 H24F 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
C26A C25A C30A 120.0 . . ?
C26A C25A N2 122.4(3) . . ?
C30A C25A N2 117.5(3) . . ?
C27A C26A C25A 120.0 . . ?
C27A C26A C31A 115.8(5) . . ?
C25A C26A C31A 123.6(5) . . ?
C26A C27A C28A 120.0 . . ?
C26A C27A H27A 120.0 . . ?
C28A C27A H27A 120.0 . . ?
C27A C28A C29A 120.0 . . ?
C27A C28A H28A 120.0 . . ?
C29A C28A H28A 120.0 . . ?
C30A C29A C28A 120.0 . . ?
C30A C29A H29A 120.0 . . ?
C28A C29A H29A 120.0 . . ?
C29A C30A C25A 120.0 . . ?
C29A C30A C40A 118.8(5) . . ?
C25A C30A C40A 120.9(5) . . ?
C32A C31A C36A 119.0(4) . . ?
C32A C31A C26A 121.9(6) . . ?
C36A C31A C26A 118.6(5) . . ?
C33A C32A C31A 119.1(4) . . ?
C33A C32A C37A 118.3(6) . . ?
C31A C32A C37A 122.6(6) . . ?
C34A C33A C32A 122.5(4) . . ?
C34A C33A H33A 118.8 . . ?
C32A C33A H33A 118.8 . . ?
C35A C34A C33A 117.6(4) . . ?
C35A C34A C38A 117.7(5) . . ?
C33A C34A C38A 124.6(5) . . ?
C34A C35A C36A 122.1(4) . . ?
C34A C35A H35A 119.0 . . ?
C36A C35A H35A 119.0 . . ?
C35A C36A C31A 119.7(4) . . ?
C35A C36A C39A 120.1(6) . . ?
C31A C36A C39A 119.9(6) . . ?
C32A C37A H37A 109.5 . . ?
C32A C37A H37B 109.5 . . ?
H37A C37A H37B 109.5 . . ?
C32A C37A H37C 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
C34A C38A H38A 109.5 . . ?
C34A C38A H38B 109.5 . . ?
H38A C38A H38B 109.5 . . ?
C34A C38A H38C 109.5 . . ?
H38A C38A H38C 109.5 . . ?
H38B C38A H38C 109.5 . . ?
C36A C39A H39A 109.5 . . ?
C36A C39A H39B 109.5 . . ?
H39A C39A H39B 109.5 . . ?
C36A C39A H39C 109.5 . . ?
H39A C39A H39C 109.5 . . ?
H39B C39A H39C 109.5 . . ?
C45A C40A C41A 118.8(4) . . ?
C45A C40A C30A 119.1(4) . . ?
C41A C40A C30A 121.5(5) . . ?
C42A C41A C40A 119.9(4) . . ?
C42A C41A C46A 120.5(5) . . ?
C40A C41A C46A 119.5(5) . . ?
C41A C42A C43A 121.0(4) . . ?
C41A C42A H42A 119.5 . . ?
C43A C42A H42A 119.5 . . ?
C44A C43A C42A 118.3(4) . . ?
C44A C43A C47A 122.5(5) . . ?
C42A C43A C47A 119.1(5) . . ?
C45A C44A C43A 121.7(4) . . ?
C45A C44A H44A 119.2 . . ?
C43A C44A H44A 119.2 . . ?
C44A C45A C40A 120.1(4) . . ?
C44A C45A C48A 118.7(6) . . ?
C40A C45A C48A 121.1(6) . . ?
C41A C46A H46A 109.5 . . ?
C41A C46A H46B 109.5 . . ?
H46A C46A H46B 109.5 . . ?
C41A C46A H46C 109.5 . . ?
H46A C46A H46C 109.5 . . ?
H46B C46A H46C 109.5 . . ?
C43A C47A H47A 109.5 . . ?
C43A C47A H47B 109.5 . . ?
H47A C47A H47B 109.5 . . ?
C43A C47A H47C 109.5 . . ?
H47A C47A H47C 109.5 . . ?
H47B C47A H47C 109.5 . . ?
C45A C48A H48A 109.5 . . ?
C45A C48A H48B 109.5 . . ?
H48A C48A H48B 109.5 . . ?
C45A C48A H48C 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
N2 C25B C26B 124.6(3) . . ?
N2 C25B C30B 115.4(3) . . ?
C26B C25B C30B 120.0 . . ?
C25B C26B C27B 120.0 . . ?
C25B C26B C31B 125.3(5) . . ?
C27B C26B C31B 114.5(5) . . ?
C28B C27B C26B 120.0 . . ?
C28B C27B H27B 120.0 . . ?
C26B C27B H27B 120.0 . . ?
C27B C28B C29B 120.0 . . ?
C27B C28B H28B 120.0 . . ?
C29B C28B H28B 120.0 . . ?
C28B C29B C30B 120.0 . . ?
C28B C29B H29B 120.0 . . ?
C30B C29B H29B 120.0 . . ?
C29B C30B C25B 120.0 . . ?
C29B C30B C40B 114.7(4) . . ?
C25B C30B C40B 125.0(4) . . ?
C36B C31B C32B 118.7(4) . . ?
C36B C31B C26B 122.3(5) . . ?
C32B C31B C26B 119.0(5) . . ?
C33B C32B C31B 119.2(4) . . ?
C33B C32B C37B 120.8(6) . . ?
C31B C32B C37B 120.0(5) . . ?
C34B C33B C32B 122.4(4) . . ?
C34B C33B H33B 118.8 . . ?
C32B C33B H33B 118.8 . . ?
C35B C34B C33B 117.1(4) . . ?
C35B C34B C38B 123.6(5) . . ?
C33B C34B C38B 119.2(5) . . ?
C34B C35B C36B 122.9(4) . . ?
C34B C35B H35B 118.5 . . ?
C36B C35B H35B 118.5 . . ?
C35B C36B C31B 119.4(4) . . ?
C35B C36B C39B 118.5(6) . . ?
C31B C36B C39B 122.0(6) . . ?
C32B C37B H37D 109.5 . . ?
C32B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
C32B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C34B C38B H38D 109.5 . . ?
C34B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C34B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C36B C39B H39D 109.5 . . ?
C36B C39B H39E 109.5 . . ?
H39D C39B H39E 109.5 . . ?
C36B C39B H39F 109.5 . . ?
H39D C39B H39F 109.5 . . ?
H39E C39B H39F 109.5 . . ?
C45B C40B C41B 119.5(4) . . ?
C45B C40B C30B 122.4(4) . . ?
C41B C40B C30B 118.1(4) . . ?
C42B C41B C40B 118.8(4) . . ?
C42B C41B C46B 118.6(5) . . ?
C40B C41B C46B 122.5(4) . . ?
C43B C42B C41B 123.5(4) . . ?
C43B C42B H42B 118.2 . . ?
C41B C42B H42B 118.2 . . ?
C42B C43B C44B 116.8(4) . . ?
C42B C43B C47B 122.3(4) . . ?
C44B C43B C47B 121.0(4) . . ?
C43B C44B C45B 122.8(4) . . ?
C43B C44B H44B 118.6 . . ?
C45B C44B H44B 118.6 . . ?
C40B C45B C44B 118.3(4) . . ?
C40B C45B C48B 120.7(6) . . ?
C44B C45B C48B 121.0(6) . . ?
C41B C46B H46D 109.5 . . ?
C41B C46B H46E 109.5 . . ?
H46D C46B H46E 109.5 . . ?
C41B C46B H46F 109.5 . . ?
H46D C46B H46F 109.5 . . ?
H46E C46B H46F 109.5 . . ?
C43B C47B H47D 109.5 . . ?
C43B C47B H47E 109.5 . . ?
H47D C47B H47E 109.5 . . ?
C43B C47B H47F 109.5 . . ?
H47D C47B H47F 109.5 . . ?
H47E C47B H47F 109.5 . . ?
C45B C48B H48D 109.5 . . ?
C45B C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C45B C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
N4 C49 N3 105.24(13) . . ?
N4 C49 P2 125.40(11) . . ?
N3 C49 P2 129.33(12) . . ?
C51 C50 N3 107.10(14) . . ?
C51 C50 C53 130.31(16) . . ?
N3 C50 C53 122.59(15) . . ?
C50 C51 N4 106.90(14) . . ?
C50 C51 C54 130.75(17) . . ?
N4 C51 C54 122.34(15) . . ?
N3 C52 H52A 109.5 . . ?
N3 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N3 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N4 C55 H55A 109.5 . . ?
N4 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
N4 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N4 C55 H55D 109.5 . . ?
N4 C55 H55E 109.5 . . ?
H55D C55 H55E 109.5 . . ?
N4 C55 H55F 109.5 . . ?
H55D C55 H55F 109.5 . . ?
H55E C55 H55F 109.5 . . ?
N6 C56 N5 105.55(12) . . ?
N6 C56 P2 124.26(11) . . ?
N5 C56 P2 129.86(11) . . ?
C58 C57 N5 106.96(13) . . ?
C58 C57 C60 129.98(14) . . ?
N5 C57 C60 123.05(13) . . ?
C57 C58 N6 106.91(13) . . ?
C57 C58 C61 131.91(14) . . ?
N6 C58 C61 121.15(14) . . ?
N5 C59 H59A 109.5 . . ?
N5 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
N5 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C58 C61 H61A 109.5 . . ?
C58 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C58 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N6 C62 H62A 109.5 . . ?
N6 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
N6 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P1 N1 C1 178.95(11) . . . . ?
N1 P1 N2 C25B 177.5(3) . . . . ?
N1 P1 N2 C25A 180.0(3) . . . . ?
P1 N1 C1 C2 -63.71(18) . . . . ?
P1 N1 C1 C6 120.79(13) . . . . ?
N1 C1 C2 C3 -176.05(13) . . . . ?
C6 C1 C2 C3 -0.5(2) . . . . ?
N1 C1 C2 C7 2.9(2) . . . . ?
C6 C1 C2 C7 178.39(13) . . . . ?
C1 C2 C3 C4 0.9(2) . . . . ?
C7 C2 C3 C4 -178.13(14) . . . . ?
C2 C3 C4 C5 -0.4(2) . . . . ?
C3 C4 C5 C6 -0.5(2) . . . . ?
C4 C5 C6 C1 0.8(2) . . . . ?
C4 C5 C6 C16 -179.26(14) . . . . ?
N1 C1 C6 C5 175.54(13) . . . . ?
C2 C1 C6 C5 -0.3(2) . . . . ?
N1 C1 C6 C16 -4.43(19) . . . . ?
C2 C1 C6 C16 179.78(13) . . . . ?
C3 C2 C7 C8 -77.46(18) . . . . ?
C1 C2 C7 C8 103.58(17) . . . . ?
C3 C2 C7 C12 97.73(17) . . . . ?
C1 C2 C7 C12 -81.23(18) . . . . ?
C12 C7 C8 C9 -2.0(2) . . . . ?
C2 C7 C8 C9 173.25(13) . . . . ?
C12 C7 C8 C13 177.43(14) . . . . ?
C2 C7 C8 C13 -7.4(2) . . . . ?
C7 C8 C9 C10 0.6(2) . . . . ?
C13 C8 C9 C10 -178.80(15) . . . . ?
C8 C9 C10 C11 0.7(2) . . . . ?
C8 C9 C10 C14 179.13(16) . . . . ?
C9 C10 C11 C12 -0.6(3) . . . . ?
C14 C10 C11 C12 -179.06(16) . . . . ?
C10 C11 C12 C7 -0.7(2) . . . . ?
C10 C11 C12 C15 179.54(15) . . . . ?
C8 C7 C12 C11 2.0(2) . . . . ?
C2 C7 C12 C11 -173.22(14) . . . . ?
C8 C7 C12 C15 -178.25(14) . . . . ?
C2 C7 C12 C15 6.5(2) . . . . ?
C5 C6 C16 C21 90.64(17) . . . . ?
C1 C6 C16 C21 -89.39(17) . . . . ?
C5 C6 C16 C17 -91.26(17) . . . . ?
C1 C6 C16 C17 88.70(17) . . . . ?
C21 C16 C17 C18 -0.9(2) . . . . ?
C6 C16 C17 C18 -179.00(12) . . . . ?
C21 C16 C17 C22 177.25(13) . . . . ?
C6 C16 C17 C22 -0.9(2) . . . . ?
C16 C17 C18 C19 1.0(2) . . . . ?
C22 C17 C18 C19 -177.17(13) . . . . ?
C17 C18 C19 C20 -0.3(2) . . . . ?
C17 C18 C19 C23 -179.51(14) . . . . ?
C18 C19 C20 C21 -0.4(2) . . . . ?
C23 C19 C20 C21 178.78(14) . . . . ?
C19 C20 C21 C16 0.5(2) . . . . ?
C19 C20 C21 C24 178.64(14) . . . . ?
C17 C16 C21 C20 0.2(2) . . . . ?
C6 C16 C21 C20 178.29(13) . . . . ?
C17 C16 C21 C24 -177.97(13) . . . . ?
C6 C16 C21 C24 0.1(2) . . . . ?
C25B N2 C25A C26A 94(6) . . . . ?
P1 N2 C25A C26A -50.9(4) . . . . ?
C25B N2 C25A C30A -89(6) . . . . ?
P1 N2 C25A C30A 126.1(3) . . . . ?
C30A C25A C26A C27A 0.0 . . . . ?
N2 C25A C26A C27A 176.9(7) . . . . ?
C30A C25A C26A C31A 170.3(7) . . . . ?
N2 C25A C26A C31A -12.7(6) . . . . ?
C25A C26A C27A C28A 0.0 . . . . ?
C31A C26A C27A C28A -171.1(6) . . . . ?
C26A C27A C28A C29A 0.0 . . . . ?
C27A C28A C29A C30A 0.0 . . . . ?
C28A C29A C30A C25A 0.0 . . . . ?
C28A C29A C30A C40A 174.5(5) . . . . ?
C26A C25A C30A C29A 0.0 . . . . ?
N2 C25A C30A C29A -177.1(6) . . . . ?
C26A C25A C30A C40A -174.4(5) . . . . ?
N2 C25A C30A C40A 8.5(5) . . . . ?
C27A C26A C31A C32A 108.8(11) . . . . ?
C25A C26A C31A C32A -61.9(15) . . . . ?
C27A C26A C31A C36A -62.7(14) . . . . ?
C25A C26A C31A C36A 126.6(10) . . . . ?
C36A C31A C32A C33A -0.6(18) . . . . ?
C26A C31A C32A C33A -172.1(9) . . . . ?
C36A C31A C32A C37A -179.2(14) . . . . ?
C26A C31A C32A C37A 9(2) . . . . ?
C31A C32A C33A C34A -2.0(13) . . . . ?
C37A C32A C33A C34A 176.6(12) . . . . ?
C32A C33A C34A C35A 3.1(9) . . . . ?
C32A C33A C34A C38A -179.3(13) . . . . ?
C33A C34A C35A C36A -1.6(9) . . . . ?
C38A C34A C35A C36A -179.4(12) . . . . ?
C34A C35A C36A C31A -0.9(12) . . . . ?
C34A C35A C36A C39A -174.5(14) . . . . ?
C32A C31A C36A C35A 2.0(18) . . . . ?
C26A C31A C36A C35A 173.8(9) . . . . ?
C32A C31A C36A C39A 175.7(16) . . . . ?
C26A C31A C36A C39A -13(2) . . . . ?
C29A C30A C40A C45A 100.9(10) . . . . ?
C25A C30A C40A C45A -84.6(10) . . . . ?
C29A C30A C40A C41A -70.3(10) . . . . ?
C25A C30A C40A C41A 104.2(9) . . . . ?
C45A C40A C41A C42A 1.5(13) . . . . ?
C30A C40A C41A C42A 172.7(6) . . . . ?
C45A C40A C41A C46A 179.9(8) . . . . ?
C30A C40A C41A C46A -8.9(12) . . . . ?
C40A C41A C42A C43A 2.0(6) . . . . ?
C46A C41A C42A C43A -176.3(5) . . . . ?
C41A C42A C43A C44A -3.3(8) . . . . ?
C41A C42A C43A C47A 178.6(8) . . . . ?
C42A C43A C44A C45A 1.0(11) . . . . ?
C47A C43A C44A C45A 179.0(10) . . . . ?
C43A C44A C45A C40A 2.5(13) . . . . ?
C43A C44A C45A C48A -174.8(11) . . . . ?
C41A C40A C45A C44A -3.7(16) . . . . ?
C30A C40A C45A C44A -175.1(8) . . . . ?
C41A C40A C45A C48A 173.5(11) . . . . ?
C30A C40A C45A C48A 2.0(17) . . . . ?
C25A N2 C25B C26B -86(6) . . . . ?
P1 N2 C25B C26B -49.1(5) . . . . ?
C25A N2 C25B C30B 95(6) . . . . ?
P1 N2 C25B C30B 131.2(2) . . . . ?
N2 C25B C26B C27B -179.7(7) . . . . ?
C30B C25B C26B C27B 0.0 . . . . ?
N2 C25B C26B C31B -5.2(6) . . . . ?
C30B C25B C26B C31B 174.5(7) . . . . ?
C25B C26B C27B C28B 0.0 . . . . ?
C31B C26B C27B C28B -175.1(6) . . . . ?
C26B C27B C28B C29B 0.0 . . . . ?
C27B C28B C29B C30B 0.0 . . . . ?
C28B C29B C30B C25B 0.0 . . . . ?
C28B C29B C30B C40B 173.9(4) . . . . ?
N2 C25B C30B C29B 179.7(6) . . . . ?
C26B C25B C30B C29B 0.0 . . . . ?
N2 C25B C30B C40B 6.4(5) . . . . ?
C26B C25B C30B C40B -173.3(5) . . . . ?
C25B C26B C31B C36B 114.3(10) . . . . ?
C27B C26B C31B C36B -70.9(14) . . . . ?
C25B C26B C31B C32B -67.9(13) . . . . ?
C27B C26B C31B C32B 106.9(11) . . . . ?
C36B C31B C32B C33B 4.3(17) . . . . ?
C26B C31B C32B C33B -173.5(8) . . . . ?
C36B C31B C32B C37B -175.6(13) . . . . ?
C26B C31B C32B C37B 6.6(19) . . . . ?
C31B C32B C33B C34B 0.0(12) . . . . ?
C37B C32B C33B C34B 179.9(11) . . . . ?
C32B C33B C34B C35B -3.6(9) . . . . ?
C32B C33B C34B C38B 179.2(11) . . . . ?
C33B C34B C35B C36B 2.9(9) . . . . ?
C38B C34B C35B C36B 180.0(12) . . . . ?
C34B C35B C36B C31B 1.4(12) . . . . ?
C34B C35B C36B C39B 179.5(13) . . . . ?
C32B C31B C36B C35B -5.1(17) . . . . ?
C26B C31B C36B C35B 172.7(9) . . . . ?
C32B C31B C36B C39B 176.9(15) . . . . ?
C26B C31B C36B C39B -5(2) . . . . ?
C29B C30B C40B C45B 105.8(10) . . . . ?
C25B C30B C40B C45B -80.6(11) . . . . ?
C29B C30B C40B C41B -75.4(9) . . . . ?
C25B C30B C40B C41B 98.2(8) . . . . ?
C45B C40B C41B C42B -2.9(13) . . . . ?
C30B C40B C41B C42B 178.3(5) . . . . ?
C45B C40B C41B C46B 178.2(8) . . . . ?
C30B C40B C41B C46B -0.7(11) . . . . ?
C40B C41B C42B C43B -2.2(6) . . . . ?
C46B C41B C42B C43B 176.9(5) . . . . ?
C41B C42B C43B C44B 4.3(8) . . . . ?
C41B C42B C43B C47B -177.5(8) . . . . ?
C42B C43B C44B C45B -1.5(10) . . . . ?
C47B C43B C44B C45B -179.7(10) . . . . ?
C41B C40B C45B C44B 5.4(15) . . . . ?
C30B C40B C45B C44B -175.8(8) . . . . ?
C41B C40B C45B C48B -173.2(11) . . . . ?
C30B C40B C45B C48B 5.6(17) . . . . ?
C43B C44B C45B C40B -3.3(12) . . . . ?
C43B C44B C45B C48B 175.3(11) . . . . ?
C51 N4 C49 N3 -1.39(18) . . . . ?
C55 N4 C49 N3 -179.22(16) . . . . ?
C51 N4 C49 P2 -179.51(12) . . . . ?
C55 N4 C49 P2 2.7(2) . . . . ?
C50 N3 C49 N4 1.88(18) . . . . ?
C52 N3 C49 N4 -172.76(14) . . . . ?
C50 N3 C49 P2 179.89(13) . . . . ?
C52 N3 C49 P2 5.3(2) . . . . ?
C56 P2 C49 N4 -134.78(14) . . . . ?
C56 P2 C49 N3 47.57(16) . . . . ?
C49 N3 C50 C51 -1.68(19) . . . . ?
C52 N3 C50 C51 172.85(15) . . . . ?
C49 N3 C50 C53 179.02(16) . . . . ?
C52 N3 C50 C53 -6.4(3) . . . . ?
N3 C50 C51 N4 0.77(19) . . . . ?
C53 C50 C51 N4 179.99(18) . . . . ?
N3 C50 C51 C54 -178.00(19) . . . . ?
C53 C50 C51 C54 1.2(3) . . . . ?
C49 N4 C51 C50 0.4(2) . . . . ?
C55 N4 C51 C50 178.19(17) . . . . ?
C49 N4 C51 C54 179.29(17) . . . . ?
C55 N4 C51 C54 -2.9(3) . . . . ?
C58 N6 C56 N5 0.56(15) . . . . ?
C62 N6 C56 N5 179.75(13) . . . . ?
C58 N6 C56 P2 -173.43(10) . . . . ?
C62 N6 C56 P2 5.8(2) . . . . ?
C57 N5 C56 N6 0.32(15) . . . . ?
C59 N5 C56 N6 -172.13(12) . . . . ?
C57 N5 C56 P2 173.84(11) . . . . ?
C59 N5 C56 P2 1.4(2) . . . . ?
C49 P2 C56 N6 -143.41(13) . . . . ?
C49 P2 C56 N5 44.14(14) . . . . ?
C56 N5 C57 C58 -1.08(16) . . . . ?
C59 N5 C57 C58 171.35(13) . . . . ?
C56 N5 C57 C60 179.15(13) . . . . ?
C59 N5 C57 C60 -8.4(2) . . . . ?
N5 C57 C58 N6 1.38(16) . . . . ?
C60 C57 C58 N6 -178.88(14) . . . . ?
N5 C57 C58 C61 -176.40(16) . . . . ?
C60 C57 C58 C61 3.3(3) . . . . ?
C56 N6 C58 C57 -1.24(16) . . . . ?
C62 N6 C58 C57 179.54(14) . . . . ?
C56 N6 C58 C61 176.83(14) . . . . ?
C62 N6 C58 C61 -2.4(2) . . . . ?
_refine_diff_density_max 0.568
_refine_diff_density_min -0.444
_refine_diff_density_rms 0.045
_shelxl_version_number 2013-4
_shelx_res_file
;
TITL ah301a_2 in P-1
CELL 0.71073 12.2213 16.2437 22.0973 97.700 93.029 106.714
ZERR 2.00 0.0006 0.0009 0.0012 0.003 0.003 0.002
LATT 1
SFAC C H N P
UNIT 188.9 212.9 12 4
LIST 4
TEMP -149.960
SIZE 0.11 0.14 0.60
OMIT -3 55
OMIT 0 -1 1
OMIT -1 1 0
OMIT 0 0 1
OMIT 0 1 0
OMIT -1 0 1
OMIT -6 2 2
OMIT -3 -3 3
OMIT -6 -5 2
OMIT 0 -1 2
OMIT -1 1 1
OMIT 1 0 1
OMIT -2 -1 1
OMIT -1 2 0
OMIT -1 -1 4
OMIT -1 -1 1
OMIT 0 1 7
OMIT 2 0 5
OMIT 1 2 1
OMIT -1 2 3
OMIT -2 1 0
OMIT 2 -4 1
OMIT 2 2 2
OMIT 2 4 0
OMIT 3 -2 7
OMIT -3 1 0
OMIT -1 0 3
OMIT -1 2 1
OMIT 1 1 1
L.S. 8
ACTA
CONF
BOND $H
FMAP 2
PLAN 40
EADP C25A C25B C28A C28B
EADP C26A C26B C29A C29B
EADP C27A C27B C30A C30B
EADP C31A C31B C34A C34B
EADP C32A C32B C35A C35B
EADP C33A C33B C36A C36B
EADP C37A C37B
EADP C38A C38B
EADP C39A C39B
EADP C40A C40B C43A C43B
EADP C41A C41B C44A C44B
EADP C42A C42B C45A C45B
EADP C46A C46B
EADP C47A C47B
EADP C48A C48B
WGHT 0.080800
FVAR 1.27717 0.66512 0.67239 0.72435 0.67752 0.84879 0.48847
MOLE 1
P1 4 0.766769 0.851863 0.230978 11.00000 0.02528 0.02651 =
0.02801 0.00593 0.00379 0.01127
P2 4 0.562233 0.207058 0.228234 11.00000 0.02838 0.02643 =
0.05890 0.00176 0.00922 0.00594
N1 3 0.762950 0.927118 0.192725 11.00000 0.02629 0.03140 =
0.02495 0.00489 0.00189 0.01205
N2 3 0.646937 0.824817 0.259522 11.00000 0.02724 0.02687 =
0.03089 0.00369 0.00383 0.01008
N3 3 0.347851 0.236735 0.251371 11.00000 0.03283 0.02543 =
0.04253 0.00784 0.01468 0.00967
N4 3 0.462817 0.338789 0.211777 11.00000 0.04112 0.02309 =
0.05193 0.00738 0.01904 0.00716
N5 3 0.385295 0.075547 0.148997 11.00000 0.02680 0.02428 =
0.03227 0.00856 0.00938 0.01173
N6 3 0.482250 0.025537 0.211682 11.00000 0.02279 0.02691 =
0.03976 0.00647 0.00509 0.01033
C1 1 0.853219 0.968697 0.161668 11.00000 0.02898 0.02520 =
0.02503 0.00521 0.00444 0.01631
C2 1 0.962119 1.019806 0.190369 11.00000 0.02894 0.02704 =
0.02603 0.00431 0.00359 0.01489
C3 1 1.045064 1.063382 0.155244 11.00000 0.02625 0.03021 =
0.03020 0.00295 0.00244 0.01182
AFIX 43
H3 2 1.118358 1.096914 0.174897 11.00000 -1.20000
AFIX 0
C4 1 1.023576 1.059124 0.092669 11.00000 0.02902 0.03861 =
0.02910 0.00804 0.00938 0.01539
AFIX 43
H4 2 1.081038 1.089527 0.069608 11.00000 -1.20000
AFIX 0
C5 1 0.917031 1.009860 0.064260 11.00000 0.03183 0.03997 =
0.02323 0.00426 0.00438 0.01958
AFIX 43
H5 2 0.901291 1.006903 0.021328 11.00000 -1.20000
AFIX 0
C6 1 0.832644 0.964642 0.097327 11.00000 0.02768 0.02957 =
0.02449 0.00326 0.00215 0.01727
C7 1 0.993952 1.031462 0.258093 11.00000 0.02697 0.02740 =
0.02423 0.00359 0.00176 0.00497
C8 1 1.064269 0.986692 0.281472 11.00000 0.03010 0.02804 =
0.03249 0.00824 -0.00016 0.00537
C9 1 1.102736 1.005246 0.343661 11.00000 0.04039 0.03971 =
0.03573 0.01303 -0.00672 0.00395
AFIX 43
H9 2 1.151179 0.974939 0.359216 11.00000 -1.20000
AFIX 0
C10 1 1.072393 1.066578 0.383437 11.00000 0.05004 0.04742 =
0.02812 0.00791 -0.00265 -0.00341
C11 1 1.000587 1.109315 0.359818 11.00000 0.05164 0.03802 =
0.03051 -0.00130 0.00938 0.00331
AFIX 43
H11 2 0.978407 1.151169 0.386662 11.00000 -1.20000
AFIX 0
C12 1 0.959978 1.092769 0.297949 11.00000 0.03711 0.02810 =
0.02946 0.00309 0.00444 0.00483
C13 1 1.098793 0.918036 0.241240 11.00000 0.03940 0.03598 =
0.04541 0.00874 0.00011 0.01785
PART 1
AFIX 137
H13A 2 1.029975 0.874241 0.219862 31.00000 -1.50000
H13B 2 1.141358 0.890170 0.266533 31.00000 -1.50000
H13C 2 1.147568 0.944909 0.211077 31.00000 -1.50000
AFIX 137
PART 2
H13D 2 1.178956 0.922581 0.253141 -31.00000 -1.50000
H13E 2 1.090457 0.926378 0.198320 -31.00000 -1.50000
H13F 2 1.049487 0.860361 0.246012 -31.00000 -1.50000
AFIX 0
PART 0
C14 1 1.114034 1.084397 0.450761 11.00000 0.08362 0.07554 =
0.03195 0.00700 -0.00658 0.00424
PART 1
AFIX 137
H14A 2 1.198108 1.105215 0.455701 51.00000 -1.50000
H14B 2 1.087532 1.030722 0.468461 51.00000 -1.50000
H14C 2 1.083514 1.128829 0.471856 51.00000 -1.50000
AFIX 137
PART 2
H14D 2 1.151322 1.146914 0.463229 -51.00000 -1.50000
H14E 2 1.169163 1.052493 0.458075 -51.00000 -1.50000
H14F 2 1.048669 1.065359 0.474714 -51.00000 -1.50000
AFIX 0
PART 0
C15 1 0.881428 1.140273 0.274414 11.00000 0.04236 0.03755 =
0.04402 0.00038 0.01287 0.01699
AFIX 137
H15A 2 0.924177 1.184491 0.251300 11.00000 -1.50000
H15B 2 0.851660 1.168428 0.309106 11.00000 -1.50000
H15C 2 0.817335 1.098809 0.247523 11.00000 -1.50000
AFIX 0
C16 1 0.718116 0.910626 0.066398 11.00000 0.02988 0.03424 =
0.02055 0.00691 0.00369 0.01615
C17 1 0.628581 0.948095 0.061931 11.00000 0.02763 0.03531 =
0.02261 0.00515 0.00470 0.01524
C18 1 0.521804 0.896731 0.033870 11.00000 0.02684 0.04284 =
0.02916 0.00882 0.00680 0.01659
AFIX 43
H18 2 0.461477 0.922367 0.030286 11.00000 -1.20000
AFIX 0
C19 1 0.500559 0.809343 0.010963 11.00000 0.02917 0.03950 =
0.02875 0.01129 0.00491 0.00767
C20 1 0.589959 0.773349 0.016407 11.00000 0.04064 0.02865 =
0.03217 0.01070 0.00664 0.01068
AFIX 43
H20 2 0.576653 0.713426 0.001182 11.00000 -1.20000
AFIX 0
C21 1 0.698608 0.822425 0.043518 11.00000 0.03449 0.03327 =
0.02445 0.00800 0.00513 0.01639
C22 1 0.647478 1.041529 0.088874 11.00000 0.03249 0.04006 =
0.03119 0.00218 0.00159 0.02102
AFIX 137
H22A 2 0.705582 1.079103 0.067609 11.00000 -1.50000
H22B 2 0.673882 1.050506 0.132580 11.00000 -1.50000
H22C 2 0.575308 1.055982 0.084024 11.00000 -1.50000
AFIX 0
C23 1 0.384285 0.755021 -0.019765 11.00000 0.03377 0.04352 =
0.05577 0.00914 0.00346 0.00481
PART 1
AFIX 137
H23A 2 0.373643 0.770099 -0.060701 21.00000 -1.50000
H23B 2 0.324377 0.766448 0.004884 21.00000 -1.50000
H23C 2 0.379291 0.693222 -0.023443 21.00000 -1.50000
AFIX 137
PART 2
H23D 2 0.349830 0.709989 0.004799 -21.00000 -1.50000
H23E 2 0.392859 0.727472 -0.060765 -21.00000 -1.50000
H23F 2 0.334621 0.792307 -0.023293 -21.00000 -1.50000
AFIX 0
PART 0
C24 1 0.793114 0.780641 0.049919 11.00000 0.04338 0.03457 =
0.04509 0.00537 0.00057 0.02105
PART 1
AFIX 137
H24A 2 0.772513 0.724767 0.022448 61.00000 -1.50000
H24B 2 0.803512 0.771012 0.092410 61.00000 -1.50000
H24C 2 0.864734 0.818990 0.039060 61.00000 -1.50000
AFIX 137
PART 2
H24D 2 0.839243 0.805356 0.089294 -61.00000 -1.50000
H24E 2 0.842093 0.791648 0.016380 -61.00000 -1.50000
H24F 2 0.759422 0.717766 0.048244 -61.00000 -1.50000
AFIX 66
PART 1
SAME 0.01 C25B > C48B
C25A 1 0.623002 0.754727 0.298500 71.00000 0.02031 0.03224 =
0.03911 0.01139 0.00488 0.00928
C26A 1 0.638048 0.673832 0.279863 71.00000 0.02242 0.03384 =
0.03805 0.00944 0.00682 0.01066
C27A 1 0.619646 0.612303 0.319264 71.00000 0.02401 0.03133 =
0.03962 0.00890 0.00603 0.01077
AFIX 43
H27A 2 0.629930 0.557015 0.306526 71.00000 -1.20000
AFIX 65
C28A 1 0.586197 0.631669 0.377301 71.00000 0.02031 0.03224 =
0.03911 0.01139 0.00488 0.00928
AFIX 43
H28A 2 0.573620 0.589617 0.404230 71.00000 -1.20000
AFIX 65
C29A 1 0.571150 0.712564 0.395939 71.00000 0.02242 0.03384 =
0.03805 0.00944 0.00682 0.01066
AFIX 43
H29A 2 0.548289 0.725800 0.435606 71.00000 -1.20000
AFIX 65
C30A 1 0.589552 0.774093 0.356540 71.00000 0.02401 0.03133 =
0.03962 0.00890 0.00603 0.01077
AFIX 0
C31A 1 0.656521 0.641819 0.214510 71.00000 0.02901 0.02096 =
0.03890 0.00622 0.00641 0.00937
C32A 1 0.573376 0.630293 0.165004 71.00000 0.02552 0.02198 =
0.04512 0.00620 0.00546 0.00872
C33A 1 0.589047 0.590638 0.107583 71.00000 0.02606 0.02226 =
0.04027 0.00551 0.00259 0.00641
AFIX 43
H33A 2 0.531495 0.581294 0.074642 71.00000 -1.20000
AFIX 0
C34A 1 0.685469 0.564269 0.096660 71.00000 0.02901 0.02096 =
0.03890 0.00622 0.00641 0.00937
C35A 1 0.765428 0.574679 0.146083 71.00000 0.02552 0.02198 =
0.04512 0.00620 0.00546 0.00872
AFIX 43
H35A 2 0.831100 0.555623 0.139787 71.00000 -1.20000
AFIX 0
C36A 1 0.752597 0.612121 0.204585 71.00000 0.02606 0.02226 =
0.04027 0.00551 0.00259 0.00641
C37A 1 0.469767 0.660771 0.171179 71.00000 0.03214 0.02962 =
0.06095 0.00263 -0.00432 0.01459
AFIX 137
H37A 2 0.489316 0.722287 0.166395 71.00000 -1.50000
H37B 2 0.443143 0.653743 0.211772 71.00000 -1.50000
H37C 2 0.408814 0.626294 0.139425 71.00000 -1.50000
AFIX 0
C38A 1 0.707186 0.521969 0.035256 71.00000 0.06878 0.03586 =
0.04979 0.00245 0.01603 0.01713
AFIX 137
H38A 2 0.634990 0.499525 0.008622 71.00000 -1.50000
H38B 2 0.738111 0.473895 0.041038 71.00000 -1.50000
H38C 2 0.762560 0.565015 0.016227 71.00000 -1.50000
AFIX 0
C39A 1 0.846609 0.629378 0.255586 71.00000 0.03917 0.05331 =
0.04577 0.01275 0.00240 0.02425
AFIX 137
H39A 2 0.905127 0.602689 0.241626 71.00000 -1.50000
H39B 2 0.814413 0.604389 0.291069 71.00000 -1.50000
H39C 2 0.881544 0.692302 0.267294 71.00000 -1.50000
AFIX 0
C40A 1 0.562421 0.857602 0.375563 71.00000 0.03163 0.03672 =
0.03823 0.00100 0.00967 0.01180
C41A 1 0.447809 0.859901 0.378365 71.00000 0.02998 0.03731 =
0.03508 0.00150 0.00773 0.00763
C42A 1 0.426122 0.936507 0.402779 71.00000 0.03339 0.04017 =
0.02813 0.00441 0.00795 0.01263
AFIX 43
H42A 2 0.349085 0.937110 0.405759 71.00000 -1.20000
AFIX 0
C43A 1 0.516226 1.012797 0.423043 71.00000 0.03163 0.03672 =
0.03823 0.00100 0.00967 0.01180
C44A 1 0.628303 1.009030 0.421136 71.00000 0.02998 0.03731 =
0.03508 0.00150 0.00773 0.00763
AFIX 43
H44A 2 0.690153 1.060079 0.435390 71.00000 -1.20000
AFIX 0
C45A 1 0.652005 0.932663 0.398961 71.00000 0.03339 0.04017 =
0.02813 0.00441 0.00795 0.01263
C46A 1 0.349549 0.779097 0.353051 71.00000 0.02902 0.05189 =
0.04935 0.00290 0.00141 0.00871
AFIX 137
H46A 2 0.277214 0.793835 0.351972 71.00000 -1.50000
H46B 2 0.345727 0.734586 0.379407 71.00000 -1.50000
H46C 2 0.362256 0.756694 0.311428 71.00000 -1.50000
AFIX 0
C47A 1 0.488522 1.094742 0.447848 71.00000 0.06212 0.04594 =
0.06634 0.00591 0.02209 0.02607
AFIX 137
H47A 2 0.518787 1.139610 0.422419 71.00000 -1.50000
H47B 2 0.523658 1.115286 0.490132 71.00000 -1.50000
H47C 2 0.405103 1.082630 0.447127 71.00000 -1.50000
AFIX 0
C48A 1 0.774438 0.931447 0.403295 71.00000 0.03048 0.04276 =
0.03457 0.00786 -0.00471 0.00997
AFIX 137
H48A 2 0.797094 0.919042 0.361977 71.00000 -1.50000
H48B 2 0.782099 0.886259 0.427040 71.00000 -1.50000
H48C 2 0.824095 0.988247 0.423701 71.00000 -1.50000
AFIX 66
PART 2
C25B 1 0.617953 0.758999 0.293738 -71.00000 0.02031 0.03224 =
0.03911 0.01139 0.00488 0.00928
C26B 1 0.628243 0.676238 0.276631 -71.00000 0.02242 0.03384 =
0.03805 0.00944 0.00682 0.01066
C27B 1 0.595698 0.613734 0.314778 -71.00000 0.02401 0.03133 =
0.03962 0.00890 0.00603 0.01077
AFIX 43
H27B 2 0.602731 0.557170 0.303086 -71.00000 -1.20000
AFIX 65
C28B 1 0.552861 0.633991 0.370032 -71.00000 0.02031 0.03224 =
0.03911 0.01139 0.00488 0.00928
AFIX 43
H28B 2 0.530618 0.591272 0.396104 -71.00000 -1.20000
AFIX 65
C29B 1 0.542570 0.716752 0.387140 -71.00000 0.02242 0.03384 =
0.03805 0.00944 0.00682 0.01066
AFIX 43
H29B 2 0.513293 0.730596 0.424903 -71.00000 -1.20000
AFIX 65
C30B 1 0.575115 0.779257 0.348993 -71.00000 0.02401 0.03133 =
0.03962 0.00890 0.00603 0.01077
AFIX 0
C31B 1 0.663992 0.643348 0.215445 -71.00000 0.02901 0.02096 =
0.03890 0.00622 0.00641 0.00937
C32B 1 0.589567 0.631133 0.161761 -71.00000 0.02552 0.02198 =
0.04512 0.00620 0.00546 0.00872
C33B 1 0.616454 0.592552 0.106318 -71.00000 0.02606 0.02226 =
0.04027 0.00551 0.00259 0.00641
AFIX 43
H33B 2 0.566051 0.584523 0.070347 -71.00000 -1.20000
AFIX 0
C34B 1 0.714572 0.565440 0.101919 -71.00000 0.02901 0.02096 =
0.03890 0.00622 0.00641 0.00937
C35B 1 0.788738 0.582618 0.154207 -71.00000 0.02552 0.02198 =
0.04512 0.00620 0.00546 0.00872
AFIX 43
H35B 2 0.857846 0.567147 0.151819 -71.00000 -1.20000
AFIX 0
C36B 1 0.767027 0.621745 0.210599 -71.00000 0.02606 0.02226 =
0.04027 0.00551 0.00259 0.00641
C37B 1 0.483475 0.659503 0.164622 -71.00000 0.03214 0.02962 =
0.06095 0.00263 -0.00432 0.01459
AFIX 137
H37D 2 0.444836 0.650311 0.123195 -71.00000 -1.50000
H37E 2 0.504445 0.721384 0.181894 -71.00000 -1.50000
H37F 2 0.431708 0.625383 0.190649 -71.00000 -1.50000
AFIX 0
C38B 1 0.736738 0.523219 0.040611 -71.00000 0.06878 0.03586 =
0.04979 0.00245 0.01603 0.01713
AFIX 137
H38D 2 0.707634 0.459804 0.037599 -71.00000 -1.50000
H38E 2 0.819454 0.540362 0.036738 -71.00000 -1.50000
H38F 2 0.697526 0.542062 0.007670 -71.00000 -1.50000
AFIX 0
C39B 1 0.853434 0.636899 0.264872 -71.00000 0.03917 0.05331 =
0.04577 0.01275 0.00240 0.02425
AFIX 137
H39D 2 0.925332 0.629724 0.250802 -71.00000 -1.50000
H39E 2 0.823788 0.594801 0.292376 -71.00000 -1.50000
H39F 2 0.867615 0.696068 0.286884 -71.00000 -1.50000
AFIX 0
C40B 1 0.548551 0.862227 0.369403 -71.00000 0.03163 0.03672 =
0.03823 0.00100 0.00967 0.01180
C41B 1 0.433519 0.862783 0.360742 -71.00000 0.02998 0.03731 =
0.03508 0.00150 0.00773 0.00763
C42B 1 0.406812 0.938778 0.380974 -71.00000 0.03339 0.04017 =
0.02813 0.00441 0.00795 0.01263
AFIX 43
H42B 2 0.329663 0.939148 0.373673 -71.00000 -1.20000
AFIX 0
C43B 1 0.485571 1.013084 0.410832 -71.00000 0.03163 0.03672 =
0.03823 0.00100 0.00967 0.01180
C44B 1 0.599407 1.012279 0.417102 -71.00000 0.02998 0.03731 =
0.03508 0.00150 0.00773 0.00763
AFIX 43
H44B 2 0.656289 1.063465 0.436791 -71.00000 -1.20000
AFIX 0
C45B 1 0.633506 0.938878 0.395502 -71.00000 0.03339 0.04017 =
0.02813 0.00441 0.00795 0.01263
C46B 1 0.337524 0.783172 0.331120 -71.00000 0.02902 0.05189 =
0.04935 0.00290 0.00141 0.00871
AFIX 137
H46D 2 0.271619 0.801038 0.317151 -71.00000 -1.50000
H46E 2 0.314643 0.743581 0.361083 -71.00000 -1.50000
H46F 2 0.364230 0.753415 0.295970 -71.00000 -1.50000
AFIX 0
C47B 1 0.453031 1.093306 0.434386 -71.00000 0.06212 0.04594 =
0.06634 0.00591 0.02209 0.02607
AFIX 137
H47D 2 0.500223 1.143083 0.417527 -71.00000 -1.50000
H47E 2 0.465852 1.104866 0.479274 -71.00000 -1.50000
H47F 2 0.371830 1.084202 0.421695 -71.00000 -1.50000
AFIX 0
C48B 1 0.757916 0.942953 0.398887 -71.00000 0.03048 0.04276 =
0.03457 0.00786 -0.00471 0.00997
AFIX 137
H48D 2 0.786425 0.950134 0.358707 -71.00000 -1.50000
H48E 2 0.766632 0.888954 0.410663 -71.00000 -1.50000
H48F 2 0.801963 0.992432 0.429504 -71.00000 -1.50000
AFIX 0
PART 0
MOLE 2
C49 1 0.453486 0.261034 0.230186 11.00000 0.03511 0.02525 =
0.03945 0.00321 0.01200 0.00643
C50 1 0.291019 0.298250 0.244152 11.00000 0.04036 0.02964 =
0.04653 0.00488 0.01423 0.01530
C51 1 0.362903 0.362250 0.219953 11.00000 0.04823 0.02810 =
0.05284 0.00817 0.01580 0.01798
C52 1 0.306764 0.161344 0.282231 11.00000 0.03796 0.03391 =
0.04576 0.01320 0.01747 0.00989
AFIX 137
H52A 2 0.271165 0.109564 0.251613 11.00000 -1.50000
H52B 2 0.250038 0.171098 0.309858 11.00000 -1.50000
H52C 2 0.371457 0.152665 0.305978 11.00000 -1.50000
AFIX 0
C53 1 0.172693 0.288820 0.262270 11.00000 0.04354 0.04813 =
0.06765 0.00718 0.02136 0.02176
AFIX 137
H53A 2 0.148079 0.338204 0.252393 11.00000 -1.50000
H53B 2 0.172344 0.287496 0.306469 11.00000 -1.50000
H53C 2 0.119920 0.234563 0.239851 11.00000 -1.50000
AFIX 0
C54 1 0.349399 0.445214 0.204281 11.00000 0.06450 0.03461 =
0.08801 0.01797 0.01646 0.02171
AFIX 137
H54A 2 0.358624 0.447199 0.160665 11.00000 -1.50000
H54B 2 0.407810 0.494359 0.229057 11.00000 -1.50000
H54C 2 0.272863 0.448772 0.212791 11.00000 -1.50000
AFIX 0
C55 1 0.562488 0.388584 0.185029 11.00000 0.05816 0.03348 =
0.08851 0.02048 0.03990 0.00826
PART 1
AFIX 137
H55A 2 0.594049 0.348615 0.159366 41.00000 -1.50000
H55B 2 0.620953 0.423421 0.217886 41.00000 -1.50000
H55C 2 0.539473 0.427195 0.159854 41.00000 -1.50000
AFIX 137
PART 2
H55D 2 0.576000 0.450852 0.198988 -41.00000 -1.50000
H55E 2 0.548430 0.376452 0.140188 -41.00000 -1.50000
H55F 2 0.630043 0.371926 0.197929 -41.00000 -1.50000
AFIX 0
PART 0
C56 1 0.470184 0.100236 0.196157 11.00000 0.02511 0.02607 =
0.03882 0.00739 0.01225 0.00981
C57 1 0.344641 -0.014329 0.135676 11.00000 0.02615 0.02648 =
0.03194 0.00545 0.01041 0.01025
C58 1 0.406287 -0.045833 0.174212 11.00000 0.02649 0.02373 =
0.03740 0.00560 0.00699 0.00896
C59 1 0.352780 0.134950 0.112571 11.00000 0.04350 0.03123 =
0.03692 0.01493 0.01401 0.01851
AFIX 137
H59A 2 0.420181 0.184421 0.110394 11.00000 -1.50000
H59B 2 0.293433 0.156029 0.131806 11.00000 -1.50000
H59C 2 0.322903 0.104271 0.071063 11.00000 -1.50000
AFIX 0
C60 1 0.250284 -0.061376 0.086776 11.00000 0.03153 0.03383 =
0.03854 0.00143 0.00289 0.01299
AFIX 137
H60A 2 0.273467 -0.046053 0.046970 11.00000 -1.50000
H60B 2 0.181065 -0.044747 0.095493 11.00000 -1.50000
H60C 2 0.234279 -0.124261 0.085715 11.00000 -1.50000
AFIX 0
C61 1 0.406313 -0.135917 0.179686 11.00000 0.04363 0.02985 =
0.05933 0.01193 -0.00063 0.01406
AFIX 137
H61A 2 0.358642 -0.176307 0.144830 11.00000 -1.50000
H61B 2 0.375276 -0.151475 0.217993 11.00000 -1.50000
H61C 2 0.485041 -0.139442 0.179848 11.00000 -1.50000
AFIX 0
C62 1 0.563730 0.018327 0.260106 11.00000 0.02946 0.03873 =
0.05291 0.00611 -0.00513 0.01526
AFIX 137
H62A 2 0.622967 -0.003703 0.241605 11.00000 -1.50000
H62B 2 0.523123 -0.021890 0.286532 11.00000 -1.50000
H62C 2 0.599706 0.075743 0.284634 11.00000 -1.50000
AFIX 0
HKLF 4
REM ah301a_2 in P-1
REM R1 = 0.0526 for 12108 Fo > 4sig(Fo) and 0.0817 for all 18856 data
REM 657 parameters refined using 64 restraints
END
WGHT 0.0808 0.0000
REM Highest difference peak 0.568, deepest hole -0.444, 1-sigma level 0.045
Q1 1 0.6406 0.7758 0.2898 11.00000 0.05 0.57
Q2 1 0.5893 0.6165 0.3366 11.00000 0.05 0.28
Q3 1 0.8974 1.1010 0.3173 11.00000 0.05 0.27
Q4 1 0.6257 0.6609 0.2633 11.00000 0.05 0.26
Q5 1 0.5683 1.1642 0.4560 11.00000 0.05 0.24
Q6 1 0.5230 0.8631 0.3631 11.00000 0.05 0.24
Q7 1 0.5834 0.6712 0.3915 11.00000 0.05 0.22
Q8 1 0.4215 -0.0392 0.1387 11.00000 0.05 0.21
Q9 1 0.5884 0.6347 0.3934 11.00000 0.05 0.20
Q10 1 1.0161 1.1528 0.5549 11.00000 0.05 0.19
Q11 1 0.7615 1.0667 0.3403 11.00000 0.05 0.19
Q12 1 1.0282 0.8714 0.4152 11.00000 0.05 0.19
Q13 1 0.6145 0.3528 0.1700 11.00000 0.05 0.19
Q14 1 0.9714 0.8679 0.3712 11.00000 0.05 0.18
Q15 1 0.9166 1.1988 0.2878 11.00000 0.05 0.18
Q16 1 0.5257 0.1448 0.2301 11.00000 0.05 0.18
Q17 1 0.9783 0.8274 0.4061 11.00000 0.05 0.18
Q18 1 0.3429 0.6692 -0.0567 11.00000 0.05 0.17
Q19 1 0.7878 0.4781 0.0477 11.00000 0.05 0.17
Q20 1 0.5370 0.5938 0.0461 11.00000 0.05 0.17
Q21 1 0.4887 0.6948 0.4420 11.00000 0.05 0.17
Q22 1 0.5807 0.8924 0.2429 11.00000 0.05 0.17
Q23 1 0.9421 0.8655 0.4135 11.00000 0.05 0.17
Q24 1 0.3942 0.6459 -0.0674 11.00000 0.05 0.16
Q25 1 0.4932 0.7228 0.1993 11.00000 0.05 0.16
Q26 1 0.5554 1.1931 0.4013 11.00000 0.05 0.16
Q27 1 0.9015 0.8219 0.0269 11.00000 0.05 0.16
Q28 1 1.1007 1.1335 0.0599 11.00000 0.05 0.16
Q29 1 0.8973 0.8183 0.0695 11.00000 0.05 0.15
Q30 1 0.5984 0.2602 0.2865 11.00000 0.05 0.15
Q31 1 0.5842 1.1661 0.5154 11.00000 0.05 0.15
Q32 1 0.3616 0.2202 0.0775 11.00000 0.05 0.15
Q33 1 0.4589 0.8077 0.4410 11.00000 0.05 0.15
Q34 1 0.4588 0.9728 0.3924 11.00000 0.05 0.15
Q35 1 0.5955 0.5084 0.3118 11.00000 0.05 0.15
Q36 1 0.3630 0.7151 0.3478 11.00000 0.05 0.15
Q37 1 0.6960 0.8639 0.0702 11.00000 0.05 0.15
Q38 1 0.6518 0.9631 0.4705 11.00000 0.05 0.15
Q39 1 1.0655 1.2038 0.5617 11.00000 0.05 0.15
Q40 1 0.9766 1.0236 0.2245 11.00000 0.05 0.15
;
_shelx_res_checksum 65376
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_ah172e_2
_database_code_depnum_ccdc_archive 'CCDC 1457706'
_audit_update_record
;
2016-03-03 deposited with the CCDC.
2016-04-07 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2013
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'0.01 (C48 H50 N2 P2 Au2 Cl2), 0.99 (C48 H50 N2 P2 Au Cl), 1.49 (C6 H6)'
_chemical_formula_sum 'C56.95 H58.95 Au Cl N2 P2'
_chemical_formula_weight 1065.76
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'
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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.9400(9)
_cell_length_b 11.9932(14)
_cell_length_c 21.421(3)
_cell_angle_alpha 87.907(2)
_cell_angle_beta 76.158(2)
_cell_angle_gamma 65.570(2)
_cell_volume 2478.4(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 123(2)
_cell_measurement_reflns_used 9926
_cell_measurement_theta_min 2.17
_cell_measurement_theta_max 28.34
_exptl_crystal_description plate
_exptl_crystal_colour orange
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.428
_exptl_crystal_F_000 1081
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.260
_exptl_crystal_size_mid 0.080
_exptl_crystal_size_min 0.040
_exptl_absorpt_coefficient_mu 3.125
_shelx_estimated_absorpt_T_min 0.497
_shelx_estimated_absorpt_T_max 0.885
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5975
_exptl_absorpt_correction_T_max 0.7464
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 123(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa-II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 108962
_diffrn_reflns_av_unetI/netI 0.0583
_diffrn_reflns_av_R_equivalents 0.0536
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_theta_min 2.049
_diffrn_reflns_theta_max 32.500
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total 17555
_reflns_number_gt 14029
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-2013
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
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^ > 2\s(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
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.8180P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 17555
_refine_ls_number_parameters 587
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0563
_refine_ls_R_factor_gt 0.0356
_refine_ls_wR_factor_ref 0.0715
_refine_ls_wR_factor_gt 0.0656
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_restrained_S_all 1.023
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.28342(2) -0.26315(2) 0.29802(2) 0.0183(1) Uani 0.9939(2) 1 d D . P A 1
Cl1 Cl 0.17855(6) -0.3908(1) 0.3410(1) 0.02554(13) Uani 0.9939(2) 1 d D . P A 1
P1 P 0.38183(6) -0.14238(5) 0.24891(3) 0.01700(12) Uani 1 1 d D . . . .
P2 P 0.30079(6) 0.06859(5) 0.31173(3) 0.01805(12) Uani 1 1 d . . . . .
Cl2 Cl 0.788(2) -0.393(4) 0.113(2) 0.02554(13) Uani 0.0061(2) 1 d D . P A 2
Au2 Au 0.5767(7) -0.2714(9) 0.1811(5) 0.01831(3) Uani 0.0061(2) 1 d D . P A 2
N1 N 0.42559(19) -0.07116(16) 0.30665(9) 0.0153(4) Uani 1 1 d . . . . .
N2 N 0.24335(19) 0.00811(16) 0.26281(9) 0.0152(4) Uani 1 1 d . . . . .
C1 C 0.5588(2) -0.1065(2) 0.31928(11) 0.0167(4) Uani 1 1 d . . . . .
C2 C 0.6362(2) -0.0385(2) 0.29568(12) 0.0185(5) Uani 1 1 d . . . . .
C3 C 0.7709(3) -0.0810(2) 0.30389(13) 0.0259(6) Uani 1 1 d . . . . .
H3 H 0.8249 -0.0364 0.2881 0.031 Uiso 1 1 calc R U . . .
C4 C 0.8264(3) -0.1868(2) 0.33465(14) 0.0296(6) Uani 1 1 d . . . . .
H4 H 0.9192 -0.2162 0.3386 0.035 Uiso 1 1 calc R U . . .
C5 C 0.7465(3) -0.2500(2) 0.35984(13) 0.0242(5) Uani 1 1 d . . . . .
H5 H 0.7850 -0.3221 0.3815 0.029 Uiso 1 1 calc R U . . .
C6 C 0.6103(2) -0.2098(2) 0.35409(11) 0.0179(4) Uani 1 1 d . . . . .
C7 C 0.5785(2) 0.0788(2) 0.26410(12) 0.0184(5) Uani 1 1 d . . . . .
C8 C 0.5142(3) 0.1911(2) 0.30153(12) 0.0213(5) Uani 1 1 d . . . . .
C9 C 0.4618(3) 0.2997(2) 0.27139(13) 0.0234(5) Uani 1 1 d . . . . .
H9 H 0.4170 0.3757 0.2967 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4734(3) 0.3000(2) 0.20574(13) 0.0244(5) Uani 1 1 d . . . . .
C11 C 0.5387(3) 0.1883(2) 0.16952(13) 0.0231(5) Uani 1 1 d . . . . .
H11 H 0.5471 0.1877 0.1243 0.028 Uiso 1 1 calc R U . . .
C12 C 0.5923(2) 0.0771(2) 0.19727(12) 0.0192(5) Uani 1 1 d . . . . .
C13 C 0.4994(3) 0.1957(3) 0.37318(13) 0.0310(6) Uani 1 1 d . . . . .
H13A H 0.5908 0.1705 0.3818 0.047 Uiso 1 1 calc R U . . .
H13B H 0.4583 0.1400 0.3926 0.047 Uiso 1 1 calc R U . . .
H13C H 0.4393 0.2796 0.3918 0.047 Uiso 1 1 calc R U . . .
C14 C 0.4155(3) 0.4197(2) 0.17462(15) 0.0367(7) Uani 1 1 d . . . . .
H14A H 0.4881 0.4247 0.1390 0.055 Uiso 1 1 calc R U . . .
H14B H 0.3831 0.4885 0.2067 0.055 Uiso 1 1 calc R U . . .
H14C H 0.3379 0.4236 0.1580 0.055 Uiso 1 1 calc R U . . .
C15 C 0.6658(3) -0.0418(2) 0.15627(13) 0.0280(6) Uani 1 1 d . . . . .
H15A H 0.6606 -0.0258 0.1116 0.042 Uiso 1 1 calc R U . . .
H15B H 0.6217 -0.0971 0.1723 0.042 Uiso 1 1 calc R U . . .
H15C H 0.7631 -0.0801 0.1582 0.042 Uiso 1 1 calc R U . . .
C16 C 0.5243(2) -0.2727(2) 0.38840(11) 0.0176(4) Uani 1 1 d . . . . .
C17 C 0.4246(3) -0.2161(2) 0.44599(12) 0.0213(5) Uani 1 1 d . . . . .
C18 C 0.3526(3) -0.2795(2) 0.48099(12) 0.0246(5) Uani 1 1 d . . . . .
H18 H 0.2864 -0.2417 0.5203 0.029 Uiso 1 1 calc R U . . .
C19 C 0.3743(3) -0.3964(2) 0.46044(13) 0.0249(5) Uani 1 1 d . . . . .
C20 C 0.4725(3) -0.4499(2) 0.40326(13) 0.0256(5) Uani 1 1 d . . . . .
H20 H 0.4892 -0.5300 0.3886 0.031 Uiso 1 1 calc R U . . .
C21 C 0.5472(3) -0.3902(2) 0.36668(12) 0.0213(5) Uani 1 1 d . . . . .
C22 C 0.3970(3) -0.0894(2) 0.47123(13) 0.0304(6) Uani 1 1 d . . . . .
H22A H 0.4851 -0.0861 0.4711 0.046 Uiso 1 1 calc R U . . .
H22B H 0.3385 -0.0722 0.5153 0.046 Uiso 1 1 calc R U . . .
H22C H 0.3496 -0.0280 0.4436 0.046 Uiso 1 1 calc R U . . .
C23 C 0.2936(3) -0.4627(3) 0.49801(15) 0.0356(7) Uani 1 1 d . . . . .
H23A H 0.2247 -0.4620 0.4758 0.053 Uiso 1 1 calc R U . . .
H23B H 0.2465 -0.4217 0.5412 0.053 Uiso 1 1 calc R U . . .
H23C H 0.3568 -0.5478 0.5015 0.053 Uiso 1 1 calc R U . . .
C24 C 0.6519(3) -0.4525(2) 0.30486(14) 0.0343(6) Uani 1 1 d . . . . .
H24A H 0.6263 -0.5116 0.2871 0.051 Uiso 1 1 calc R U . . .
H24B H 0.7437 -0.4956 0.3134 0.051 Uiso 1 1 calc R U . . .
H24C H 0.6540 -0.3909 0.2738 0.051 Uiso 1 1 calc R U . . .
C25 C 0.1172(2) 0.0571(2) 0.24309(11) 0.0158(4) Uani 1 1 d . . . . .
C26 C 0.1074(2) 0.0084(2) 0.18679(11) 0.0167(4) Uani 1 1 d . . . . .
C27 C -0.0198(2) 0.0571(2) 0.17042(12) 0.0197(5) Uani 1 1 d . . . . .
H27 H -0.0283 0.0243 0.1328 0.024 Uiso 1 1 calc R U . . .
C28 C -0.1340(2) 0.1521(2) 0.20803(12) 0.0213(5) Uani 1 1 d . . . . .
H28 H -0.2200 0.1837 0.1964 0.026 Uiso 1 1 calc R U . . .
C29 C -0.1223(2) 0.2010(2) 0.26260(12) 0.0204(5) Uani 1 1 d . . . . .
H29 H -0.2005 0.2669 0.2880 0.024 Uiso 1 1 calc R U . . .
C30 C 0.0024(2) 0.1553(2) 0.28086(11) 0.0168(4) Uani 1 1 d . . . . .
C31 C 0.2295(2) -0.0897(2) 0.14252(11) 0.0181(5) Uani 1 1 d . . . . .
C32 C 0.3361(3) -0.0614(2) 0.10540(12) 0.0228(5) Uani 1 1 d . . . . .
C33 C 0.4475(3) -0.1527(3) 0.06329(12) 0.0291(6) Uani 1 1 d . . . . .
H33 H 0.5204 -0.1341 0.0386 0.035 Uiso 1 1 calc R U . . .
C34 C 0.4550(3) -0.2701(3) 0.05640(13) 0.0337(6) Uani 1 1 d . . . . .
C35 C 0.3468(3) -0.2951(2) 0.09238(13) 0.0295(6) Uani 1 1 d . . . . .
H35 H 0.3508 -0.3751 0.0877 0.035 Uiso 1 1 calc R U . . .
C36 C 0.2327(3) -0.2075(2) 0.13506(12) 0.0219(5) Uani 1 1 d . . . . .
C37 C 0.3303(3) 0.0661(2) 0.10954(13) 0.0280(6) Uani 1 1 d . . . . .
H37A H 0.4054 0.0717 0.0758 0.042 Uiso 1 1 calc R U . . .
H37B H 0.3408 0.0831 0.1519 0.042 Uiso 1 1 calc R U . . .
H37C H 0.2410 0.1262 0.1037 0.042 Uiso 1 1 calc R U . . .
C38 C 0.5776(4) -0.3672(3) 0.01064(17) 0.0550(10) Uani 1 1 d . . . . .
H38A H 0.5466 -0.4201 -0.0090 0.082 Uiso 1 1 calc R U . . .
H38B H 0.6457 -0.4168 0.0344 0.082 Uiso 1 1 calc R U . . .
H38C H 0.6201 -0.3277 -0.0232 0.082 Uiso 1 1 calc R U . . .
C39 C 0.1174(3) -0.2395(2) 0.17107(13) 0.0269(6) Uani 1 1 d . . . . .
H39A H 0.0398 -0.2055 0.1505 0.040 Uiso 1 1 calc R U . . .
H39B H 0.0865 -0.2050 0.2158 0.040 Uiso 1 1 calc R U . . .
H39C H 0.1504 -0.3290 0.1705 0.040 Uiso 1 1 calc R U . . .
C40 C 0.0170(2) 0.2081(2) 0.33880(11) 0.0171(4) Uani 1 1 d . . . . .
C41 C 0.0099(2) 0.1475(2) 0.39647(12) 0.0204(5) Uani 1 1 d . . . . .
C42 C 0.0393(3) 0.1890(2) 0.44824(12) 0.0237(5) Uani 1 1 d . . . . .
H42 H 0.0346 0.1486 0.4871 0.028 Uiso 1 1 calc R U . . .
C43 C 0.0753(3) 0.2877(2) 0.44510(12) 0.0226(5) Uani 1 1 d . . . . .
C44 C 0.0773(2) 0.3491(2) 0.38851(12) 0.0214(5) Uani 1 1 d . . . . .
H44 H 0.0988 0.4184 0.3862 0.026 Uiso 1 1 calc R U . . .
C45 C 0.0483(2) 0.3110(2) 0.33536(12) 0.0185(5) Uani 1 1 d . . . . .
C46 C -0.0218(3) 0.0363(2) 0.40072(13) 0.0276(6) Uani 1 1 d . . . . .
H46A H -0.1006 0.0522 0.3821 0.041 Uiso 1 1 calc R U . . .
H46B H -0.0448 0.0188 0.4460 0.041 Uiso 1 1 calc R U . . .
H46C H 0.0593 -0.0343 0.3768 0.041 Uiso 1 1 calc R U . . .
C47 C 0.1126(3) 0.3250(3) 0.50149(14) 0.0332(6) Uani 1 1 d . . . . .
H47A H 0.2015 0.2620 0.5061 0.050 Uiso 1 1 calc R U . . .
H47B H 0.0406 0.3340 0.5408 0.050 Uiso 1 1 calc R U . . .
H47C H 0.1199 0.4035 0.4944 0.050 Uiso 1 1 calc R U . . .
C48 C 0.0636(3) 0.3737(2) 0.27321(12) 0.0256(5) Uani 1 1 d . . . . .
H48A H 0.1482 0.3199 0.2420 0.038 Uiso 1 1 calc R U . . .
H48B H 0.0692 0.4509 0.2817 0.038 Uiso 1 1 calc R U . . .
H48C H -0.0167 0.3907 0.2556 0.038 Uiso 1 1 calc R U . . .
C49 C 0.8209(5) -0.5298(4) 0.13483(19) 0.0797(16) Uani 0.9939(2) 1 d . . P A 1
H49 H 0.7503 -0.5527 0.1581 0.096 Uiso 0.9939(2) 1 calc R U P A 1
C50 C 0.7866(5) -0.4072(5) 0.1288(2) 0.0741(15) Uani 0.9939(2) 1 d . . P A 1
H50 H 0.6943 -0.3464 0.1423 0.089 Uiso 0.9939(2) 1 calc R U P A 1
C51 C 0.8988(5) -0.3789(4) 0.1013(2) 0.0692(12) Uani 0.9939(2) 1 d . . P A 1
H51 H 0.8841 -0.2953 0.0988 0.083 Uiso 0.9939(2) 1 calc R U P A 1
C52 C 1.0257(5) -0.4661(4) 0.0784(3) 0.0929(18) Uani 0.9939(2) 1 d . . P A 1
H52 H 1.0993 -0.4445 0.0580 0.112 Uiso 0.9939(2) 1 calc R U P A 1
C53 C 1.0493(6) -0.5855(4) 0.0843(3) 0.0887(16) Uani 0.9939(2) 1 d . . P A 1
H53 H 1.1410 -0.6469 0.0695 0.106 Uiso 0.9939(2) 1 calc R U P A 1
C54 C 0.9457(5) -0.6197(3) 0.11065(18) 0.0574(10) Uani 0.9939(2) 1 d . . P A 1
H54 H 0.9611 -0.7037 0.1119 0.069 Uiso 0.9939(2) 1 calc R U P A 1
C55 C 0.8602(3) 0.0600(4) 0.00554(15) 0.0459(8) Uani 1 1 d . . . . .
H55 H 0.7632 0.1016 0.0096 0.055 Uiso 1 1 calc R U . . .
C56 C 0.9215(4) -0.0656(4) 0.00370(15) 0.0510(9) Uani 1 1 d . . . . .
H56 H 0.8674 -0.1111 0.0060 0.061 Uiso 1 1 calc R U . . .
C57 C 1.0621(4) -0.1259(3) -0.00155(15) 0.0480(9) Uani 1 1 d . . . . .
H57 H 1.1049 -0.2130 -0.0024 0.058 Uiso 1 1 calc R U . . .
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 0.01838(5) 0.01217(4) 0.02568(5) 0.00243(3) -0.00873(3) -0.00593(3)
Cl1 0.0223(3) 0.0181(3) 0.0396(4) 0.0088(3) -0.0103(3) -0.0108(2)
P1 0.0144(3) 0.0139(3) 0.0207(3) 0.0005(2) -0.0051(2) -0.0035(2)
P2 0.0149(3) 0.0132(3) 0.0261(3) -0.0001(2) -0.0085(2) -0.0040(2)
Cl2 0.0223(3) 0.0181(3) 0.0396(4) 0.0088(3) -0.0103(3) -0.0108(2)
Au2 0.01838(5) 0.01217(4) 0.02568(5) 0.00243(3) -0.00873(3) -0.00593(3)
N1 0.0132(9) 0.0131(9) 0.0203(10) 0.0026(7) -0.0059(7) -0.0055(7)
N2 0.0146(9) 0.0112(8) 0.0187(10) 0.0011(7) -0.0065(7) -0.0032(7)
C1 0.0134(10) 0.0146(10) 0.0208(12) 0.0027(9) -0.0061(8) -0.0036(8)
C2 0.0159(11) 0.0169(11) 0.0226(13) 0.0043(9) -0.0056(9) -0.0065(9)
C3 0.0189(12) 0.0240(13) 0.0386(16) 0.0130(11) -0.0121(11) -0.0108(10)
C4 0.0180(12) 0.0313(14) 0.0429(17) 0.0148(12) -0.0150(11) -0.0106(11)
C5 0.0196(12) 0.0214(12) 0.0324(15) 0.0105(11) -0.0124(10) -0.0067(10)
C6 0.0174(11) 0.0157(11) 0.0201(12) 0.0027(9) -0.0066(9) -0.0054(9)
C7 0.0148(11) 0.0179(11) 0.0252(13) 0.0079(9) -0.0088(9) -0.0079(9)
C8 0.0211(12) 0.0185(12) 0.0269(14) 0.0041(10) -0.0089(10) -0.0093(9)
C9 0.0237(13) 0.0151(11) 0.0316(15) 0.0020(10) -0.0080(10) -0.0075(9)
C10 0.0254(13) 0.0195(12) 0.0305(15) 0.0084(10) -0.0120(11) -0.0094(10)
C11 0.0228(12) 0.0239(13) 0.0256(13) 0.0068(10) -0.0104(10) -0.0106(10)
C12 0.0154(11) 0.0171(11) 0.0249(13) 0.0030(9) -0.0046(9) -0.0068(9)
C13 0.0420(17) 0.0266(14) 0.0282(15) 0.0031(11) -0.0121(12) -0.0160(12)
C14 0.0470(18) 0.0207(13) 0.0402(18) 0.0115(12) -0.0193(14) -0.0082(13)
C15 0.0284(14) 0.0236(13) 0.0276(14) 0.0008(11) -0.0008(11) -0.0099(11)
C16 0.0182(11) 0.0141(10) 0.0219(12) 0.0057(9) -0.0094(9) -0.0059(9)
C17 0.0230(12) 0.0208(12) 0.0229(13) 0.0053(10) -0.0107(10) -0.0094(10)
C18 0.0230(13) 0.0282(13) 0.0230(13) 0.0079(11) -0.0070(10) -0.0109(11)
C19 0.0223(12) 0.0238(13) 0.0342(15) 0.0135(11) -0.0150(11) -0.0117(10)
C20 0.0252(13) 0.0157(11) 0.0390(16) 0.0082(11) -0.0139(11) -0.0088(10)
C21 0.0213(12) 0.0161(11) 0.0262(13) 0.0056(10) -0.0106(10) -0.0051(9)
C22 0.0375(16) 0.0287(14) 0.0253(14) -0.0018(11) -0.0030(11) -0.0163(12)
C23 0.0293(15) 0.0352(16) 0.0514(19) 0.0208(14) -0.0168(13) -0.0201(13)
C24 0.0341(16) 0.0208(13) 0.0414(18) -0.0033(12) -0.0015(12) -0.0088(11)
C25 0.0150(10) 0.0136(10) 0.0198(12) 0.0041(9) -0.0059(8) -0.0064(8)
C26 0.0174(11) 0.0139(10) 0.0211(12) 0.0046(9) -0.0070(9) -0.0078(8)
C27 0.0219(12) 0.0184(11) 0.0232(13) 0.0059(9) -0.0105(9) -0.0103(9)
C28 0.0150(11) 0.0209(12) 0.0307(14) 0.0087(10) -0.0102(9) -0.0081(9)
C29 0.0143(11) 0.0142(11) 0.0301(14) 0.0054(10) -0.0050(9) -0.0041(9)
C30 0.0164(11) 0.0128(10) 0.0212(12) 0.0024(9) -0.0037(9) -0.0066(8)
C31 0.0192(11) 0.0186(11) 0.0157(11) 0.0017(9) -0.0083(9) -0.0051(9)
C32 0.0222(12) 0.0286(13) 0.0182(12) 0.0044(10) -0.0069(9) -0.0104(10)
C33 0.0235(13) 0.0417(16) 0.0179(13) 0.0014(11) -0.0028(10) -0.0108(12)
C34 0.0308(15) 0.0335(15) 0.0241(15) -0.0077(12) -0.0069(11) -0.0005(12)
C35 0.0357(15) 0.0180(12) 0.0297(15) -0.0012(11) -0.0129(12) -0.0035(11)
C36 0.0254(13) 0.0208(12) 0.0200(13) 0.0031(10) -0.0102(10) -0.0076(10)
C37 0.0296(14) 0.0325(15) 0.0264(14) 0.0060(11) -0.0044(11) -0.0189(12)
C38 0.045(2) 0.053(2) 0.041(2) -0.0193(17) 0.0010(15) 0.0008(17)
C39 0.0322(14) 0.0196(12) 0.0346(15) 0.0038(11) -0.0153(12) -0.0128(11)
C40 0.0114(10) 0.0133(10) 0.0236(12) -0.0003(9) -0.0020(8) -0.0036(8)
C41 0.0194(11) 0.0162(11) 0.0235(13) 0.0023(9) -0.0014(9) -0.0074(9)
C42 0.0258(13) 0.0239(13) 0.0195(13) 0.0028(10) -0.0015(10) -0.0107(10)
C43 0.0214(12) 0.0219(12) 0.0224(13) -0.0039(10) -0.0018(10) -0.0085(10)
C44 0.0195(12) 0.0160(11) 0.0277(14) -0.0020(10) -0.0025(10) -0.0081(9)
C45 0.0150(11) 0.0126(10) 0.0250(13) 0.0000(9) -0.0027(9) -0.0039(8)
C46 0.0359(15) 0.0246(13) 0.0264(14) 0.0044(11) -0.0048(11) -0.0183(12)
C47 0.0396(17) 0.0351(16) 0.0304(16) -0.0044(12) -0.0080(12) -0.0208(13)
C48 0.0294(14) 0.0204(12) 0.0280(14) 0.0052(10) -0.0058(11) -0.0125(10)
C49 0.068(3) 0.073(3) 0.042(2) 0.028(2) 0.0215(19) 0.004(2)
C50 0.067(3) 0.073(3) 0.050(3) -0.007(2) -0.009(2) 0.000(2)
C51 0.082(3) 0.040(2) 0.077(3) -0.006(2) -0.014(3) -0.019(2)
C52 0.069(3) 0.049(3) 0.150(5) -0.003(3) 0.001(3) -0.028(2)
C53 0.079(4) 0.050(3) 0.113(4) 0.017(3) -0.001(3) -0.016(2)
C54 0.077(3) 0.039(2) 0.051(2) 0.0051(17) -0.003(2) -0.027(2)
C55 0.0316(16) 0.068(2) 0.0273(17) 0.0009(16) -0.0098(13) -0.0085(16)
C56 0.061(2) 0.076(3) 0.0292(18) 0.0059(17) -0.0094(16) -0.042(2)
C57 0.058(2) 0.050(2) 0.0273(17) 0.0072(15) -0.0107(15) -0.0148(18)
#==============================================================================
# MOLECULAR GEOMETRY
_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 P1 2.2361(6) . ?
Au1 Cl1 2.3140(6) . ?
P1 N1 1.7853(19) . ?
P1 N2 1.7896(19) . ?
P1 Au2 2.2360(12) . ?
P1 P2 2.6117(9) . ?
P2 N1 1.6536(19) . ?
P2 N2 1.6633(19) . ?
Cl2 Au2 2.3148(11) . ?
N1 C1 1.431(3) . ?
N2 C25 1.421(3) . ?
C1 C6 1.401(3) . ?
C1 C2 1.405(3) . ?
C2 C3 1.400(3) . ?
C2 C7 1.495(3) . ?
C3 C4 1.381(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(3) . ?
C5 H5 0.9500 . ?
C6 C16 1.487(3) . ?
C7 C12 1.403(3) . ?
C7 C8 1.406(3) . ?
C8 C9 1.393(3) . ?
C8 C13 1.505(4) . ?
C9 C10 1.381(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(4) . ?
C10 C14 1.512(4) . ?
C11 C12 1.392(3) . ?
C11 H11 0.9500 . ?
C12 C15 1.503(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.402(3) . ?
C16 C17 1.406(3) . ?
C17 C18 1.389(3) . ?
C17 C22 1.515(3) . ?
C18 C19 1.392(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.387(4) . ?
C19 C23 1.501(4) . ?
C20 C21 1.391(3) . ?
C20 H20 0.9500 . ?
C21 C24 1.504(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.404(3) . ?
C25 C30 1.406(3) . ?
C26 C27 1.396(3) . ?
C26 C31 1.498(3) . ?
C27 C28 1.384(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.382(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(3) . ?
C29 H29 0.9500 . ?
C30 C40 1.484(3) . ?
C31 C32 1.404(3) . ?
C31 C36 1.412(3) . ?
C32 C33 1.393(4) . ?
C32 C37 1.509(3) . ?
C33 C34 1.387(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(4) . ?
C34 C38 1.509(4) . ?
C35 C36 1.392(4) . ?
C35 H35 0.9500 . ?
C36 C39 1.500(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C45 1.406(3) . ?
C40 C41 1.413(3) . ?
C41 C42 1.387(4) . ?
C41 C46 1.505(3) . ?
C42 C43 1.388(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.396(4) . ?
C43 C47 1.500(4) . ?
C44 C45 1.392(3) . ?
C44 H44 0.9500 . ?
C45 C48 1.513(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C54 1.334(5) . ?
C49 C50 1.368(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.397(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.331(6) . ?
C51 H51 0.9500 . ?
C52 C53 1.353(6) . ?
C52 H52 0.9500 . ?
C53 C54 1.355(6) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C57 1.367(5) 2_755 ?
C55 C56 1.371(5) . ?
C55 H55 0.9500 . ?
C56 C57 1.380(5) . ?
C56 H56 0.9500 . ?
C57 C55 1.367(5) 2_755 ?
C57 H57 0.9500 . ?
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
P1 Au1 Cl1 175.41(2) . . ?
N1 P1 N2 77.65(9) . . ?
N1 P1 Au2 109.0(3) . . ?
N2 P1 Au2 146.3(4) . . ?
N1 P1 Au1 109.75(7) . . ?
N2 P1 Au1 104.03(7) . . ?
N1 P1 P2 38.74(6) . . ?
N2 P1 P2 39.07(6) . . ?
Au2 P1 P2 135.7(3) . . ?
Au1 P1 P2 114.63(3) . . ?
N1 P2 N2 85.02(9) . . ?
N1 P2 P1 42.50(7) . . ?
N2 P2 P1 42.70(6) . . ?
P1 Au2 Cl2 174.5(8) . . ?
C1 N1 P2 128.03(15) . . ?
C1 N1 P1 127.44(15) . . ?
P2 N1 P1 98.76(10) . . ?
C25 N2 P2 130.76(15) . . ?
C25 N2 P1 130.78(15) . . ?
P2 N2 P1 98.23(10) . . ?
C6 C1 C2 121.4(2) . . ?
C6 C1 N1 119.12(19) . . ?
C2 C1 N1 119.44(19) . . ?
C3 C2 C1 118.3(2) . . ?
C3 C2 C7 119.1(2) . . ?
C1 C2 C7 122.5(2) . . ?
C4 C3 C2 121.0(2) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 119.8(2) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 121.4(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 117.9(2) . . ?
C5 C6 C16 119.0(2) . . ?
C1 C6 C16 123.0(2) . . ?
C12 C7 C8 120.2(2) . . ?
C12 C7 C2 120.2(2) . . ?
C8 C7 C2 119.5(2) . . ?
C9 C8 C7 118.9(2) . . ?
C9 C8 C13 119.7(2) . . ?
C7 C8 C13 121.4(2) . . ?
C10 C9 C8 121.8(2) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C9 C10 C11 118.4(2) . . ?
C9 C10 C14 120.4(2) . . ?
C11 C10 C14 121.2(2) . . ?
C10 C11 C12 122.1(2) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C11 C12 C7 118.6(2) . . ?
C11 C12 C15 120.6(2) . . ?
C7 C12 C15 120.8(2) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 119.7(2) . . ?
C21 C16 C6 121.2(2) . . ?
C17 C16 C6 119.0(2) . . ?
C18 C17 C16 119.0(2) . . ?
C18 C17 C22 119.6(2) . . ?
C16 C17 C22 121.4(2) . . ?
C17 C18 C19 122.2(2) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C20 C19 C18 117.7(2) . . ?
C20 C19 C23 120.6(2) . . ?
C18 C19 C23 121.7(3) . . ?
C19 C20 C21 122.1(2) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C16 119.3(2) . . ?
C20 C21 C24 119.8(2) . . ?
C16 C21 C24 121.0(2) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 120.6(2) . . ?
C26 C25 N2 120.5(2) . . ?
C30 C25 N2 118.9(2) . . ?
C27 C26 C25 118.4(2) . . ?
C27 C26 C31 119.0(2) . . ?
C25 C26 C31 122.5(2) . . ?
C28 C27 C26 121.2(2) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C29 C28 C27 119.7(2) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 121.0(2) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C29 C30 C25 118.9(2) . . ?
C29 C30 C40 121.6(2) . . ?
C25 C30 C40 119.5(2) . . ?
C32 C31 C36 120.3(2) . . ?
C32 C31 C26 119.5(2) . . ?
C36 C31 C26 120.1(2) . . ?
C33 C32 C31 118.9(2) . . ?
C33 C32 C37 119.9(2) . . ?
C31 C32 C37 121.2(2) . . ?
C34 C33 C32 121.9(3) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C35 118.2(2) . . ?
C33 C34 C38 120.5(3) . . ?
C35 C34 C38 121.3(3) . . ?
C34 C35 C36 122.5(3) . . ?
C34 C35 H35 118.8 . . ?
C36 C35 H35 118.8 . . ?
C35 C36 C31 118.2(2) . . ?
C35 C36 C39 119.8(2) . . ?
C31 C36 C39 122.1(2) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C45 C40 C41 120.1(2) . . ?
C45 C40 C30 120.8(2) . . ?
C41 C40 C30 118.9(2) . . ?
C42 C41 C40 118.6(2) . . ?
C42 C41 C46 120.6(2) . . ?
C40 C41 C46 120.8(2) . . ?
C41 C42 C43 122.2(2) . . ?
C41 C42 H42 118.9 . . ?
C43 C42 H42 118.9 . . ?
C42 C43 C44 118.5(2) . . ?
C42 C43 C47 120.0(2) . . ?
C44 C43 C47 121.6(2) . . ?
C45 C44 C43 121.4(2) . . ?
C45 C44 H44 119.3 . . ?
C43 C44 H44 119.3 . . ?
C44 C45 C40 119.2(2) . . ?
C44 C45 C48 119.4(2) . . ?
C40 C45 C48 121.2(2) . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C54 C49 C50 125.2(4) . . ?
C54 C49 H49 117.4 . . ?
C50 C49 H49 117.4 . . ?
C49 C50 C51 114.4(4) . . ?
C49 C50 H50 122.8 . . ?
C51 C50 H50 122.8 . . ?
C52 C51 C50 121.8(4) . . ?
C52 C51 H51 119.1 . . ?
C50 C51 H51 119.1 . . ?
C51 C52 C53 119.7(5) . . ?
C51 C52 H52 120.2 . . ?
C53 C52 H52 120.2 . . ?
C52 C53 C54 121.7(5) . . ?
C52 C53 H53 119.1 . . ?
C54 C53 H53 119.1 . . ?
C49 C54 C53 116.7(4) . . ?
C49 C54 H54 121.6 . . ?
C53 C54 H54 121.6 . . ?
C57 C55 C56 120.3(3) 2_755 . ?
C57 C55 H55 119.8 2_755 . ?
C56 C55 H55 119.8 . . ?
C55 C56 C57 119.9(3) . . ?
C55 C56 H56 120.1 . . ?
C57 C56 H56 120.1 . . ?
C55 C57 C56 119.8(3) 2_755 . ?
C55 C57 H57 120.1 2_755 . ?
C56 C57 H57 120.1 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P2 N1 C1 159.0(2) . . . . ?
P1 P2 N1 C1 154.3(2) . . . . ?
N2 P2 N1 P1 4.64(10) . . . . ?
N2 P1 N1 C1 -159.0(2) . . . . ?
Au2 P1 N1 C1 -13.4(4) . . . . ?
Au1 P1 N1 C1 100.37(18) . . . . ?
P2 P1 N1 C1 -154.6(2) . . . . ?
N2 P1 N1 P2 -4.40(9) . . . . ?
Au2 P1 N1 P2 141.2(4) . . . . ?
Au1 P1 N1 P2 -105.07(8) . . . . ?
N1 P2 N2 C25 170.2(2) . . . . ?
P1 P2 N2 C25 174.8(3) . . . . ?
N1 P2 N2 P1 -4.63(10) . . . . ?
N1 P1 N2 C25 -170.4(2) . . . . ?
Au2 P1 N2 C25 83.8(6) . . . . ?
Au1 P1 N2 C25 -62.9(2) . . . . ?
P2 P1 N2 C25 -174.8(3) . . . . ?
N1 P1 N2 P2 4.37(9) . . . . ?
Au2 P1 N2 P2 -101.4(6) . . . . ?
Au1 P1 N2 P2 111.94(8) . . . . ?
P2 N1 C1 C6 137.0(2) . . . . ?
P1 N1 C1 C6 -75.6(3) . . . . ?
P2 N1 C1 C2 -44.0(3) . . . . ?
P1 N1 C1 C2 103.4(2) . . . . ?
C6 C1 C2 C3 4.3(4) . . . . ?
N1 C1 C2 C3 -174.6(2) . . . . ?
C6 C1 C2 C7 -173.8(2) . . . . ?
N1 C1 C2 C7 7.2(3) . . . . ?
C1 C2 C3 C4 -0.3(4) . . . . ?
C7 C2 C3 C4 177.9(2) . . . . ?
C2 C3 C4 C5 -2.2(4) . . . . ?
C3 C4 C5 C6 0.9(4) . . . . ?
C4 C5 C6 C1 3.0(4) . . . . ?
C4 C5 C6 C16 -173.1(2) . . . . ?
C2 C1 C6 C5 -5.6(4) . . . . ?
N1 C1 C6 C5 173.3(2) . . . . ?
C2 C1 C6 C16 170.3(2) . . . . ?
N1 C1 C6 C16 -10.8(3) . . . . ?
C3 C2 C7 C12 92.1(3) . . . . ?
C1 C2 C7 C12 -89.8(3) . . . . ?
C3 C2 C7 C8 -86.0(3) . . . . ?
C1 C2 C7 C8 92.2(3) . . . . ?
C12 C7 C8 C9 1.5(3) . . . . ?
C2 C7 C8 C9 179.5(2) . . . . ?
C12 C7 C8 C13 -179.3(2) . . . . ?
C2 C7 C8 C13 -1.3(3) . . . . ?
C7 C8 C9 C10 -1.0(4) . . . . ?
C13 C8 C9 C10 179.8(2) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C8 C9 C10 C14 -179.9(2) . . . . ?
C9 C10 C11 C12 0.0(4) . . . . ?
C14 C10 C11 C12 -179.8(2) . . . . ?
C10 C11 C12 C7 0.5(4) . . . . ?
C10 C11 C12 C15 -178.3(2) . . . . ?
C8 C7 C12 C11 -1.2(3) . . . . ?
C2 C7 C12 C11 -179.3(2) . . . . ?
C8 C7 C12 C15 177.6(2) . . . . ?
C2 C7 C12 C15 -0.4(3) . . . . ?
C5 C6 C16 C21 -73.7(3) . . . . ?
C1 C6 C16 C21 110.5(3) . . . . ?
C5 C6 C16 C17 102.1(3) . . . . ?
C1 C6 C16 C17 -73.8(3) . . . . ?
C21 C16 C17 C18 1.4(3) . . . . ?
C6 C16 C17 C18 -174.5(2) . . . . ?
C21 C16 C17 C22 179.8(2) . . . . ?
C6 C16 C17 C22 4.0(3) . . . . ?
C16 C17 C18 C19 -1.1(4) . . . . ?
C22 C17 C18 C19 -179.5(2) . . . . ?
C17 C18 C19 C20 0.6(4) . . . . ?
C17 C18 C19 C23 -178.6(2) . . . . ?
C18 C19 C20 C21 -0.5(4) . . . . ?
C23 C19 C20 C21 178.8(2) . . . . ?
C19 C20 C21 C16 0.8(4) . . . . ?
C19 C20 C21 C24 -179.7(2) . . . . ?
C17 C16 C21 C20 -1.2(3) . . . . ?
C6 C16 C21 C20 174.5(2) . . . . ?
C17 C16 C21 C24 179.2(2) . . . . ?
C6 C16 C21 C24 -5.0(4) . . . . ?
P2 N2 C25 C26 159.38(17) . . . . ?
P1 N2 C25 C26 -27.4(3) . . . . ?
P2 N2 C25 C30 -20.5(3) . . . . ?
P1 N2 C25 C30 152.67(17) . . . . ?
C30 C25 C26 C27 -2.0(3) . . . . ?
N2 C25 C26 C27 178.06(19) . . . . ?
C30 C25 C26 C31 175.4(2) . . . . ?
N2 C25 C26 C31 -4.5(3) . . . . ?
C25 C26 C27 C28 0.8(3) . . . . ?
C31 C26 C27 C28 -176.7(2) . . . . ?
C26 C27 C28 C29 0.6(3) . . . . ?
C27 C28 C29 C30 -0.7(3) . . . . ?
C28 C29 C30 C25 -0.5(3) . . . . ?
C28 C29 C30 C40 179.1(2) . . . . ?
C26 C25 C30 C29 1.9(3) . . . . ?
N2 C25 C30 C29 -178.19(19) . . . . ?
C26 C25 C30 C40 -177.7(2) . . . . ?
N2 C25 C30 C40 2.2(3) . . . . ?
C27 C26 C31 C32 107.4(3) . . . . ?
C25 C26 C31 C32 -70.0(3) . . . . ?
C27 C26 C31 C36 -68.4(3) . . . . ?
C25 C26 C31 C36 114.2(3) . . . . ?
C36 C31 C32 C33 -2.7(4) . . . . ?
C26 C31 C32 C33 -178.5(2) . . . . ?
C36 C31 C32 C37 176.1(2) . . . . ?
C26 C31 C32 C37 0.3(3) . . . . ?
C31 C32 C33 C34 0.9(4) . . . . ?
C37 C32 C33 C34 -177.9(2) . . . . ?
C32 C33 C34 C35 0.7(4) . . . . ?
C32 C33 C34 C38 -179.6(3) . . . . ?
C33 C34 C35 C36 -0.5(4) . . . . ?
C38 C34 C35 C36 179.8(3) . . . . ?
C34 C35 C36 C31 -1.3(4) . . . . ?
C34 C35 C36 C39 178.2(2) . . . . ?
C32 C31 C36 C35 2.9(4) . . . . ?
C26 C31 C36 C35 178.6(2) . . . . ?
C32 C31 C36 C39 -176.6(2) . . . . ?
C26 C31 C36 C39 -0.9(3) . . . . ?
C29 C30 C40 C45 -85.2(3) . . . . ?
C25 C30 C40 C45 94.4(3) . . . . ?
C29 C30 C40 C41 99.7(3) . . . . ?
C25 C30 C40 C41 -80.7(3) . . . . ?
C45 C40 C41 C42 -2.3(3) . . . . ?
C30 C40 C41 C42 172.8(2) . . . . ?
C45 C40 C41 C46 -179.3(2) . . . . ?
C30 C40 C41 C46 -4.2(3) . . . . ?
C40 C41 C42 C43 0.0(4) . . . . ?
C46 C41 C42 C43 176.9(2) . . . . ?
C41 C42 C43 C44 2.2(4) . . . . ?
C41 C42 C43 C47 -177.1(2) . . . . ?
C42 C43 C44 C45 -2.0(4) . . . . ?
C47 C43 C44 C45 177.3(2) . . . . ?
C43 C44 C45 C40 -0.3(4) . . . . ?
C43 C44 C45 C48 -174.8(2) . . . . ?
C41 C40 C45 C44 2.5(3) . . . . ?
C30 C40 C45 C44 -172.5(2) . . . . ?
C41 C40 C45 C48 176.9(2) . . . . ?
C30 C40 C45 C48 1.9(3) . . . . ?
C54 C49 C50 C51 -7.6(7) . . . . ?
C49 C50 C51 C52 5.1(7) . . . . ?
C50 C51 C52 C53 -3.1(9) . . . . ?
C51 C52 C53 C54 2.8(9) . . . . ?
C50 C49 C54 C53 7.5(8) . . . . ?
C52 C53 C54 C49 -4.8(8) . . . . ?
C57 C55 C56 C57 0.7(5) 2_755 . . . ?
C55 C56 C57 C55 -0.6(5) . . . 2_755 ?
_refine_diff_density_max 1.744
_refine_diff_density_min -1.662
_refine_diff_density_rms 0.126
_shelxl_version_number 2013-4
_shelx_res_file
;
TITL ah172e_2 in P-1
CELL 0.71073 10.9400 11.9932 21.4209 87.907 76.158 65.570
ZERR 2.00 0.0009 0.0014 0.0028 0.002 0.002 0.002
LATT 1
SFAC C N P CL AU H
UNIT 113.9 4 4 2 2 117.9
LIST 4
TEMP -149.960
SIZE 0.040 0.080 0.260
ACTA
OMIT -3 65
OMIT 1 0 0
OMIT 0 0 1
OMIT 0 0 2
OMIT 1 1 1
OMIT 0 1 0
OMIT 1 0 1
OMIT 0 1 1
OMIT 1 1 0
OMIT 2 2 0
OMIT 1 6 0
OMIT 4 -1 3
OMIT 2 0 4
OMIT 1 -4 5
OMIT 0 1 8
OMIT -1 -2 3
OMIT -5 -5 1
OMIT -1 0 2
L.S. 8
ACTA
CONF
BOND $H
FMAP 2
PLAN 20
HTAB
BOND $H
CONF
EADP AU1 Au2
EADP Cl1 Cl2
SADI 0.001 P1 Au1 P1 Au2
SADI 0.001 P1 Cl1 P1 Cl2
SADI 0.001 Au1 Cl1 Au2 Cl2
WGHT 0.031200 0.818000
FVAR 0.09878 0.99386
PART 1
AU1 5 0.283418 -0.263145 0.298022 21.00000 0.01838 0.01217 =
0.02568 0.00243 -0.00873 -0.00593
CL1 4 0.178546 -0.390840 0.341010 21.00000 0.02231 0.01810 =
0.03963 0.00875 -0.01026 -0.01084
PART 0
P1 3 0.381826 -0.142378 0.248906 11.00000 0.01437 0.01395 =
0.02066 0.00054 -0.00511 -0.00346
P2 3 0.300787 0.068586 0.311730 11.00000 0.01494 0.01319 =
0.02612 -0.00011 -0.00853 -0.00398
PART 2
CL2 4 0.788110 -0.393050 0.113015 -21.00000 0.02231 0.01810 =
0.03963 0.00875 -0.01026 -0.01084
AU2 5 0.576664 -0.271390 0.181148 -21.00000 0.01838 0.01217 =
0.02568 0.00243 -0.00873 -0.00593
PART 0
N1 2 0.425594 -0.071159 0.306645 11.00000 0.01322 0.01314 =
0.02026 0.00262 -0.00593 -0.00545
N2 2 0.243351 0.008107 0.262814 11.00000 0.01462 0.01124 =
0.01873 0.00114 -0.00654 -0.00318
C1 1 0.558838 -0.106544 0.319279 11.00000 0.01343 0.01460 =
0.02077 0.00272 -0.00614 -0.00357
C2 1 0.636178 -0.038455 0.295676 11.00000 0.01588 0.01687 =
0.02261 0.00432 -0.00559 -0.00650
C3 1 0.770897 -0.080958 0.303887 11.00000 0.01892 0.02400 =
0.03856 0.01298 -0.01205 -0.01080
AFIX 43
H3 6 0.824906 -0.036355 0.288066 11.00000 -1.20000
AFIX 0
C4 1 0.826448 -0.186780 0.334651 11.00000 0.01797 0.03126 =
0.04292 0.01479 -0.01501 -0.01055
AFIX 43
H4 6 0.919155 -0.216209 0.338551 11.00000 -1.20000
AFIX 0
C5 1 0.746451 -0.249980 0.359842 11.00000 0.01962 0.02143 =
0.03237 0.01054 -0.01238 -0.00668
AFIX 43
H5 6 0.784971 -0.322091 0.381454 11.00000 -1.20000
AFIX 0
C6 1 0.610311 -0.209779 0.354092 11.00000 0.01741 0.01570 =
0.02007 0.00271 -0.00660 -0.00543
C7 1 0.578528 0.078818 0.264095 11.00000 0.01478 0.01790 =
0.02524 0.00795 -0.00877 -0.00792
C8 1 0.514173 0.191064 0.301528 11.00000 0.02106 0.01851 =
0.02692 0.00414 -0.00892 -0.00934
C9 1 0.461835 0.299721 0.271386 11.00000 0.02369 0.01509 =
0.03155 0.00197 -0.00797 -0.00749
AFIX 43
H9 6 0.417001 0.375651 0.296663 11.00000 -1.20000
AFIX 0
C10 1 0.473365 0.300041 0.205740 11.00000 0.02543 0.01947 =
0.03050 0.00836 -0.01200 -0.00936
C11 1 0.538716 0.188316 0.169524 11.00000 0.02279 0.02391 =
0.02557 0.00676 -0.01043 -0.01057
AFIX 43
H11 6 0.547117 0.187712 0.124345 11.00000 -1.20000
AFIX 0
C12 1 0.592334 0.077142 0.197271 11.00000 0.01536 0.01707 =
0.02488 0.00304 -0.00462 -0.00677
C13 1 0.499372 0.195709 0.373176 11.00000 0.04201 0.02656 =
0.02820 0.00314 -0.01215 -0.01603
AFIX 137
H13A 6 0.590805 0.170547 0.381800 11.00000 -1.50000
H13B 6 0.458337 0.139967 0.392622 11.00000 -1.50000
H13C 6 0.439336 0.279638 0.391763 11.00000 -1.50000
AFIX 0
C14 1 0.415527 0.419733 0.174622 11.00000 0.04696 0.02072 =
0.04025 0.01151 -0.01934 -0.00821
AFIX 137
H14A 6 0.488068 0.424658 0.139036 11.00000 -1.50000
H14B 6 0.383093 0.488548 0.206650 11.00000 -1.50000
H14C 6 0.337930 0.423574 0.158010 11.00000 -1.50000
AFIX 0
C15 1 0.665835 -0.041805 0.156271 11.00000 0.02842 0.02357 =
0.02761 0.00083 -0.00075 -0.00993
AFIX 137
H15A 6 0.660642 -0.025843 0.111570 11.00000 -1.50000
H15B 6 0.621673 -0.097099 0.172338 11.00000 -1.50000
H15C 6 0.763127 -0.080053 0.158164 11.00000 -1.50000
AFIX 0
C16 1 0.524314 -0.272667 0.388400 11.00000 0.01817 0.01405 =
0.02185 0.00566 -0.00936 -0.00591
C17 1 0.424591 -0.216098 0.445986 11.00000 0.02298 0.02080 =
0.02295 0.00525 -0.01068 -0.00943
C18 1 0.352645 -0.279479 0.480986 11.00000 0.02300 0.02818 =
0.02301 0.00794 -0.00705 -0.01092
AFIX 43
H18 6 0.286441 -0.241724 0.520265 11.00000 -1.20000
AFIX 0
C19 1 0.374297 -0.396428 0.460442 11.00000 0.02231 0.02377 =
0.03419 0.01351 -0.01503 -0.01169
C20 1 0.472465 -0.449939 0.403264 11.00000 0.02516 0.01571 =
0.03904 0.00824 -0.01394 -0.00885
AFIX 43
H20 6 0.489175 -0.529971 0.388622 11.00000 -1.20000
AFIX 0
C21 1 0.547216 -0.390179 0.366679 11.00000 0.02129 0.01608 =
0.02617 0.00564 -0.01062 -0.00513
C22 1 0.397015 -0.089439 0.471228 11.00000 0.03747 0.02873 =
0.02525 -0.00182 -0.00301 -0.01634
AFIX 137
H22A 6 0.485068 -0.086077 0.471097 11.00000 -1.50000
H22B 6 0.338487 -0.072240 0.515326 11.00000 -1.50000
H22C 6 0.349647 -0.028043 0.443596 11.00000 -1.50000
AFIX 0
C23 1 0.293563 -0.462742 0.498012 11.00000 0.02933 0.03522 =
0.05137 0.02076 -0.01677 -0.02009
AFIX 137
H23A 6 0.224665 -0.462034 0.475807 11.00000 -1.50000
H23B 6 0.246502 -0.421680 0.541237 11.00000 -1.50000
H23C 6 0.356829 -0.547792 0.501512 11.00000 -1.50000
AFIX 0
C24 1 0.651926 -0.452465 0.304859 11.00000 0.03406 0.02083 =
0.04139 -0.00331 -0.00150 -0.00877
AFIX 137
H24A 6 0.626294 -0.511575 0.287134 11.00000 -1.50000
H24B 6 0.743716 -0.495550 0.313385 11.00000 -1.50000
H24C 6 0.653988 -0.390850 0.273782 11.00000 -1.50000
AFIX 0
C25 1 0.117151 0.057143 0.243093 11.00000 0.01496 0.01356 =
0.01980 0.00406 -0.00587 -0.00636
C26 1 0.107433 0.008427 0.186789 11.00000 0.01739 0.01390 =
0.02107 0.00461 -0.00704 -0.00781
C27 1 -0.019846 0.057080 0.170420 11.00000 0.02190 0.01837 =
0.02322 0.00593 -0.01054 -0.01028
AFIX 43
H27 6 -0.028297 0.024328 0.132760 11.00000 -1.20000
AFIX 0
C28 1 -0.133972 0.152148 0.208032 11.00000 0.01499 0.02091 =
0.03067 0.00871 -0.01017 -0.00812
AFIX 43
H28 6 -0.220022 0.183667 0.196384 11.00000 -1.20000
AFIX 0
C29 1 -0.122252 0.201042 0.262602 11.00000 0.01434 0.01422 =
0.03009 0.00544 -0.00499 -0.00414
AFIX 43
H29 6 -0.200535 0.266898 0.288019 11.00000 -1.20000
AFIX 0
C30 1 0.002365 0.155311 0.280863 11.00000 0.01636 0.01280 =
0.02120 0.00241 -0.00373 -0.00662
C31 1 0.229546 -0.089741 0.142519 11.00000 0.01918 0.01858 =
0.01569 0.00170 -0.00828 -0.00505
C32 1 0.336125 -0.061370 0.105396 11.00000 0.02218 0.02865 =
0.01817 0.00439 -0.00689 -0.01040
C33 1 0.447477 -0.152736 0.063294 11.00000 0.02349 0.04167 =
0.01792 0.00145 -0.00279 -0.01079
AFIX 43
H33 6 0.520371 -0.134117 0.038595 11.00000 -1.20000
AFIX 0
C34 1 0.454992 -0.270076 0.056396 11.00000 0.03085 0.03353 =
0.02409 -0.00766 -0.00691 -0.00045
C35 1 0.346818 -0.295094 0.092384 11.00000 0.03567 0.01803 =
0.02967 -0.00124 -0.01293 -0.00349
AFIX 43
H35 6 0.350762 -0.375066 0.087716 11.00000 -1.20000
AFIX 0
C36 1 0.232746 -0.207460 0.135064 11.00000 0.02537 0.02080 =
0.02003 0.00312 -0.01015 -0.00764
C37 1 0.330322 0.066090 0.109544 11.00000 0.02956 0.03254 =
0.02639 0.00599 -0.00443 -0.01892
AFIX 137
H37A 6 0.405375 0.071741 0.075770 11.00000 -1.50000
H37B 6 0.340848 0.083113 0.151883 11.00000 -1.50000
H37C 6 0.240974 0.126218 0.103676 11.00000 -1.50000
AFIX 0
C38 1 0.577601 -0.367164 0.010636 11.00000 0.04482 0.05269 =
0.04102 -0.01935 0.00104 0.00082
AFIX 137
H38A 6 0.546618 -0.420070 -0.009016 11.00000 -1.50000
H38B 6 0.645712 -0.416780 0.034378 11.00000 -1.50000
H38C 6 0.620081 -0.327680 -0.023163 11.00000 -1.50000
AFIX 0
C39 1 0.117395 -0.239506 0.171068 11.00000 0.03219 0.01962 =
0.03459 0.00380 -0.01526 -0.01281
AFIX 137
H39A 6 0.039844 -0.205487 0.150477 11.00000 -1.50000
H39B 6 0.086527 -0.204990 0.215757 11.00000 -1.50000
H39C 6 0.150433 -0.328984 0.170499 11.00000 -1.50000
AFIX 0
C40 1 0.017014 0.208073 0.338795 11.00000 0.01143 0.01334 =
0.02362 -0.00030 -0.00197 -0.00356
C41 1 0.009899 0.147477 0.396472 11.00000 0.01935 0.01620 =
0.02347 0.00231 -0.00139 -0.00744
C42 1 0.039285 0.189034 0.448236 11.00000 0.02576 0.02388 =
0.01954 0.00282 -0.00152 -0.01072
AFIX 43
H42 6 0.034595 0.148618 0.487135 11.00000 -1.20000
AFIX 0
C43 1 0.075311 0.287683 0.445100 11.00000 0.02144 0.02187 =
0.02239 -0.00393 -0.00177 -0.00851
C44 1 0.077266 0.349132 0.388508 11.00000 0.01955 0.01600 =
0.02770 -0.00197 -0.00252 -0.00808
AFIX 43
H44 6 0.098821 0.418435 0.386230 11.00000 -1.20000
AFIX 0
C45 1 0.048301 0.310993 0.335359 11.00000 0.01499 0.01258 =
0.02495 0.00002 -0.00266 -0.00392
C46 1 -0.021815 0.036323 0.400716 11.00000 0.03589 0.02457 =
0.02638 0.00444 -0.00478 -0.01829
AFIX 137
H46A 6 -0.100582 0.052169 0.382128 11.00000 -1.50000
H46B 6 -0.044823 0.018751 0.445989 11.00000 -1.50000
H46C 6 0.059307 -0.034341 0.376796 11.00000 -1.50000
AFIX 0
C47 1 0.112553 0.325025 0.501488 11.00000 0.03959 0.03512 =
0.03037 -0.00437 -0.00795 -0.02081
AFIX 137
H47A 6 0.201527 0.262036 0.506113 11.00000 -1.50000
H47B 6 0.040585 0.333973 0.540815 11.00000 -1.50000
H47C 6 0.119871 0.403453 0.494366 11.00000 -1.50000
AFIX 0
C48 1 0.063600 0.373654 0.273213 11.00000 0.02945 0.02036 =
0.02802 0.00516 -0.00581 -0.01247
AFIX 137
H48A 6 0.148222 0.319927 0.242037 11.00000 -1.50000
H48B 6 0.069202 0.450912 0.281745 11.00000 -1.50000
H48C 6 -0.016715 0.390709 0.255605 11.00000 -1.50000
AFIX 0
MOLE 2
PART 1
C49 1 0.820925 -0.529790 0.134833 21.00000 0.06821 0.07289 =
0.04172 0.02787 0.02152 0.00425
AFIX 43
H49 6 0.750251 -0.552681 0.158079 21.00000 -1.20000
AFIX 0
C50 1 0.786627 -0.407202 0.128837 21.00000 0.06715 0.07314 =
0.04952 -0.00747 -0.00896 0.00020
AFIX 43
H50 6 0.694265 -0.346381 0.142294 21.00000 -1.20000
AFIX 0
C51 1 0.898793 -0.378938 0.101269 21.00000 0.08214 0.03989 =
0.07726 -0.00580 -0.01427 -0.01950
AFIX 43
H51 6 0.884082 -0.295256 0.098808 21.00000 -1.20000
AFIX 0
C52 1 1.025702 -0.466063 0.078359 21.00000 0.06874 0.04872 =
0.14964 -0.00348 0.00135 -0.02766
AFIX 43
H52 6 1.099332 -0.444483 0.057963 21.00000 -1.20000
AFIX 0
C53 1 1.049350 -0.585481 0.084254 21.00000 0.07871 0.05013 =
0.11255 0.01657 -0.00113 -0.01600
AFIX 43
H53 6 1.141010 -0.646919 0.069512 21.00000 -1.20000
AFIX 0
C54 1 0.945671 -0.619741 0.110645 21.00000 0.07716 0.03939 =
0.05108 0.00509 -0.00349 -0.02686
AFIX 43
H54 6 0.961076 -0.703685 0.111860 21.00000 -1.20000
AFIX 0
PART 0
MOLE 3
C55 1 0.860188 0.060031 0.005540 11.00000 0.03155 0.06777 =
0.02726 0.00094 -0.00978 -0.00849
AFIX 43
H55 6 0.763243 0.101551 0.009604 11.00000 -1.20000
AFIX 0
C56 1 0.921531 -0.065632 0.003697 11.00000 0.06066 0.07608 =
0.02921 0.00588 -0.00944 -0.04207
AFIX 43
H56 6 0.867386 -0.111138 0.006029 11.00000 -1.20000
AFIX 0
C57 1 1.062148 -0.125926 -0.001554 11.00000 0.05832 0.05011 =
0.02727 0.00723 -0.01070 -0.01483
AFIX 43
H57 6 1.104859 -0.212979 -0.002397 11.00000 -1.20000
REM #####
AFIX 0
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM ah172e_2 in P-1
REM R1 = 0.0356 for 14029 Fo > 4sig(Fo) and 0.0563 for all 17555 data
REM 587 parameters refined using 3 restraints
END
WGHT 0.0312 0.8180
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 1.744, deepest hole -1.662, 1-sigma level 0.126
Q1 1 0.8545 -0.5104 0.1474 11.00000 0.05 1.74
Q2 1 0.2915 0.0155 0.5494 11.00000 0.05 0.96
Q3 1 0.7918 -0.4932 0.1182 11.00000 0.05 0.95
Q4 1 0.2407 -0.1935 0.2601 11.00000 0.05 0.86
Q5 1 0.7217 -0.4605 0.1312 11.00000 0.05 0.86
Q6 1 0.5393 -0.2731 0.1913 11.00000 0.05 0.85
Q7 1 0.3162 -0.3224 0.3423 11.00000 0.05 0.82
Q8 1 0.2567 -0.2196 0.2515 11.00000 0.05 0.79
Q9 1 0.7626 -0.5064 0.1514 11.00000 0.05 0.77
Q10 1 0.8552 -0.5691 0.1179 11.00000 0.05 0.74
Q11 1 0.1710 -0.2676 0.3297 11.00000 0.05 0.71
Q12 1 0.2233 -0.1566 0.2925 11.00000 0.05 0.66
Q13 1 0.2564 -0.2618 0.2892 11.00000 0.05 0.65
Q14 1 0.2927 -0.2635 0.2402 11.00000 0.05 0.64
Q15 1 0.2508 -0.2525 0.3322 11.00000 0.05 0.64
Q16 1 0.3412 -0.2057 0.3062 11.00000 0.05 0.63
Q17 1 0.8623 -0.1721 0.1712 11.00000 0.05 0.62
Q18 1 0.3353 -0.2048 0.2485 11.00000 0.05 0.61
Q19 1 0.3178 -0.3368 0.2568 11.00000 0.05 0.61
Q20 1 0.0460 0.0291 0.1826 11.00000 0.05 0.59
;
_shelx_res_checksum 66949
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_ah172e
_database_code_depnum_ccdc_archive 'CCDC 1457707'
_audit_update_record
;
2016-03-03 deposited with the CCDC.
2016-04-07 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2013
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'0.33 (C48 H50 N2 P2 Au2 Cl2), 0.66 (C48 H50 N2 P2 Au Cl), 0.5 (C6 H6)'
_chemical_formula_sum 'C51 H53 Au1.33 Cl1.33 N2 P2'
_chemical_formula_weight 1065.59
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'
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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.168(5)
_cell_length_b 12.029(5)
_cell_length_c 18.686(5)
_cell_angle_alpha 94.538(5)
_cell_angle_beta 94.411(5)
_cell_angle_gamma 114.833(5)
_cell_volume 2254.1(15)
_cell_formula_units_Z 2
_cell_measurement_temperature 123(2)
_cell_measurement_reflns_used 9478
_cell_measurement_theta_min 2.42
_cell_measurement_theta_max 32.66
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.570
_exptl_crystal_F_000 1062
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.220
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.070
_exptl_absorpt_coefficient_mu 4.527
_shelx_estimated_absorpt_T_min 0.436
_shelx_estimated_absorpt_T_max 0.742
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5998
_exptl_absorpt_correction_T_max 0.7464
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 123(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa-II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 87601
_diffrn_reflns_av_unetI/netI 0.0389
_diffrn_reflns_av_R_equivalents 0.0483
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 1.101
_diffrn_reflns_theta_max 32.500
_diffrn_reflns_theta_full 25.240
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total 16144
_reflns_number_gt 14357
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-2013
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
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^ > 2\s(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
'w=1/[\s^2^(Fo^2^)+9.4339P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 16144
_refine_ls_number_parameters 549
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0522
_refine_ls_R_factor_gt 0.0434
_refine_ls_wR_factor_ref 0.1034
_refine_ls_wR_factor_gt 0.1011
_refine_ls_goodness_of_fit_ref 1.327
_refine_ls_restrained_S_all 1.327
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.21056(10) 0.35415(9) 0.22322(6) 0.0226(2) Uani 1 1 d . . . . .
P2 P 0.26071(10) 0.57032(10) 0.28856(7) 0.0257(2) Uani 1 1 d . . . . .
Au1 Au 0.29552(2) 0.24452(2) 0.28195(2) 0.02166(4) Uani 1 1 d . . . . .
Cl1 Cl 0.38958(11) 0.12862(11) 0.33507(7) 0.0340(3) Uani 1 1 d . . . . .
Au2 Au 0.05650(5) 0.26132(4) 0.13636(3) 0.0217(1) Uani 0.3320(8) 1 d . . P A 3
Cl2 Cl -0.1195(4) 0.1647(4) 0.0477(2) 0.0413(9) Uani 0.3320(8) 1 d . . P A 3
N1 N 0.3367(3) 0.5079(3) 0.2371(2) 0.0215(7) Uani 1 1 d . . . . .
N2 N 0.1424(3) 0.4291(3) 0.28269(19) 0.0190(6) Uani 1 1 d . . . . .
C1 C 0.4702(4) 0.5581(4) 0.2207(2) 0.0226(8) Uani 1 1 d . . . . .
C2 C 0.5033(4) 0.5093(4) 0.1585(3) 0.0266(9) Uani 1 1 d . . . . .
C3 C 0.6364(5) 0.5606(5) 0.1455(3) 0.0355(11) Uani 1 1 d . . . . .
H3 H 0.6601 0.5291 0.1047 0.043 Uiso 1 1 calc R U . . .
C4 C 0.7330(5) 0.6563(5) 0.1915(3) 0.0402(13) Uani 1 1 d . . . . .
H4 H 0.8209 0.6885 0.1819 0.048 Uiso 1 1 calc R U . . .
C5 C 0.6992(4) 0.7051(4) 0.2528(3) 0.0351(11) Uani 1 1 d . . . . .
H5 H 0.7651 0.7700 0.2837 0.042 Uiso 1 1 calc R U . . .
C6 C 0.5682(4) 0.6583(4) 0.2684(3) 0.0261(9) Uani 1 1 d . . . . .
C7 C 0.4030(5) 0.4097(4) 0.1052(3) 0.0282(9) Uani 1 1 d . . . . .
C8 C 0.3132(5) 0.4347(5) 0.0588(3) 0.0344(11) Uani 1 1 d . . . . .
C9 C 0.2225(6) 0.3421(6) 0.0091(3) 0.0442(13) Uani 1 1 d . . . . .
H9 H 0.1624 0.3586 -0.0203 0.053 Uiso 1 1 calc R U . . .
C10 C 0.2170(6) 0.2234(6) 0.0013(3) 0.0458(13) Uani 1 1 d . . . . .
C11 C 0.3074(6) 0.2009(5) 0.0458(3) 0.0408(12) Uani 1 1 d . . . . .
H11 H 0.3059 0.1228 0.0406 0.049 Uiso 1 1 calc R U . . .
C12 C 0.4003(5) 0.2910(4) 0.0979(3) 0.0300(9) Uani 1 1 d . . . . .
C13 C 0.3205(6) 0.5631(5) 0.0630(3) 0.0438(13) Uani 1 1 d . . . . .
H13A H 0.2659 0.5683 0.0223 0.066 Uiso 1 1 calc R U . . .
H13B H 0.4109 0.6217 0.0623 0.066 Uiso 1 1 calc R U . . .
H13C H 0.2893 0.5810 0.1069 0.066 Uiso 1 1 calc R U . . .
C14 C 0.1187(9) 0.1247(7) -0.0564(4) 0.074(2) Uani 1 1 d . . . . .
H14A H 0.1469 0.0601 -0.0653 0.111 Uiso 1 1 calc R U . . .
H14B H 0.1147 0.1603 -0.1002 0.111 Uiso 1 1 calc R U . . .
H14C H 0.0324 0.0911 -0.0402 0.111 Uiso 1 1 calc R U . . .
C15 C 0.4989(5) 0.2618(5) 0.1429(3) 0.0343(10) Uani 1 1 d . . . . .
H15A H 0.4647 0.1741 0.1432 0.051 Uiso 1 1 calc R U . . .
H15B H 0.5131 0.3012 0.1915 0.051 Uiso 1 1 calc R U . . .
H15C H 0.5815 0.2914 0.1226 0.051 Uiso 1 1 calc R U . . .
C16 C 0.5295(4) 0.7100(4) 0.3317(3) 0.0259(9) Uani 1 1 d . . . . .
C17 C 0.4997(4) 0.8125(4) 0.3283(3) 0.0266(9) Uani 1 1 d . . . . .
C18 C 0.4491(4) 0.8505(4) 0.3864(3) 0.0327(10) Uani 1 1 d . . . . .
H18 H 0.4285 0.9175 0.3839 0.039 Uiso 1 1 calc R U . . .
C19 C 0.4288(5) 0.7910(4) 0.4477(3) 0.0335(10) Uani 1 1 d . . . . .
C20 C 0.4641(5) 0.6936(4) 0.4520(3) 0.0344(10) Uani 1 1 d . . . . .
H20 H 0.4545 0.6557 0.4940 0.041 Uiso 1 1 calc R U . . .
C21 C 0.5134(4) 0.6513(4) 0.3952(3) 0.0290(9) Uani 1 1 d . . . . .
C22 C 0.5098(5) 0.8737(4) 0.2601(3) 0.0373(11) Uani 1 1 d . . . . .
H22A H 0.5141 0.9547 0.2713 0.056 Uiso 1 1 calc R U . . .
H22B H 0.4332 0.8251 0.2258 0.056 Uiso 1 1 calc R U . . .
H22C H 0.5886 0.8802 0.2399 0.056 Uiso 1 1 calc R U . . .
C23 C 0.3683(6) 0.8298(6) 0.5090(3) 0.0435(13) Uani 1 1 d . . . . .
H23A H 0.4272 0.8498 0.5531 0.065 Uiso 1 1 calc R U . . .
H23B H 0.2846 0.7633 0.5143 0.065 Uiso 1 1 calc R U . . .
H23C H 0.3547 0.9008 0.4986 0.065 Uiso 1 1 calc R U . . .
C24 C 0.5442(6) 0.5413(4) 0.4002(3) 0.0365(11) Uani 1 1 d . . . . .
H24A H 0.5628 0.5337 0.4502 0.055 Uiso 1 1 calc R U . . .
H24B H 0.6202 0.5524 0.3758 0.055 Uiso 1 1 calc R U . . .
H24C H 0.4691 0.4679 0.3780 0.055 Uiso 1 1 calc R U . . .
C25 C 0.0058(4) 0.3915(4) 0.2936(2) 0.0219(8) Uani 1 1 d . . . . .
C26 C -0.0615(4) 0.4597(4) 0.2692(3) 0.0261(9) Uani 1 1 d . . . . .
C27 C -0.1971(4) 0.4156(5) 0.2762(3) 0.0387(12) Uani 1 1 d . . . . .
H27 H -0.2436 0.4594 0.2604 0.046 Uiso 1 1 calc R U . . .
C28 C -0.2632(5) 0.3082(5) 0.3062(3) 0.0433(14) Uani 1 1 d . . . . .
H28 H -0.3542 0.2778 0.3083 0.052 Uiso 1 1 calc R U . . .
C29 C -0.1928(4) 0.2458(5) 0.3332(3) 0.0336(11) Uani 1 1 d . . . . .
H29 H -0.2374 0.1744 0.3542 0.040 Uiso 1 1 calc R U . . .
C30 C -0.0569(4) 0.2878(4) 0.3294(3) 0.0253(8) Uani 1 1 d . . . . .
C31 C 0.0074(4) 0.5782(4) 0.2388(2) 0.0241(8) Uani 1 1 d . . . . .
C32 C 0.0178(4) 0.5814(4) 0.1639(2) 0.0255(8) Uani 1 1 d . . . . .
C33 C 0.0829(5) 0.6951(5) 0.1393(3) 0.0319(10) Uani 1 1 d . . . . .
H33 H 0.0897 0.6973 0.0901 0.038 Uiso 1 1 calc R U . . .
C34 C 0.1383(4) 0.8054(4) 0.1848(3) 0.0290(9) Uani 1 1 d . . . . .
C35 C 0.1262(4) 0.8012(4) 0.2578(3) 0.0296(9) Uani 1 1 d . . . . .
H35 H 0.1627 0.8744 0.2891 0.036 Uiso 1 1 calc R U . . .
C36 C 0.0605(4) 0.6895(4) 0.2856(3) 0.0270(9) Uani 1 1 d . . . . .
C37 C -0.0431(7) 0.4657(6) 0.1130(3) 0.0524(16) Uani 1 1 d . . . . .
H37A H -0.0168 0.4829 0.0659 0.079 Uiso 1 1 calc R U . . .
H37B H -0.1382 0.4326 0.1103 0.079 Uiso 1 1 calc R U . . .
H37C H -0.0139 0.4068 0.1298 0.079 Uiso 1 1 calc R U . . .
C38 C 0.2109(5) 0.9267(5) 0.1567(3) 0.0413(12) Uani 1 1 d . . . . .
H38A H 0.1741 0.9826 0.1720 0.062 Uiso 1 1 calc R U . . .
H38B H 0.2015 0.9140 0.1048 0.062 Uiso 1 1 calc R U . . .
H38C H 0.3034 0.9610 0.1752 0.062 Uiso 1 1 calc R U . . .
C39 C 0.0489(6) 0.6899(5) 0.3648(3) 0.0409(12) Uani 1 1 d . . . . .
H39A H 0.1050 0.7707 0.3896 0.061 Uiso 1 1 calc R U . . .
H39B H 0.0761 0.6307 0.3832 0.061 Uiso 1 1 calc R U . . .
H39C H -0.0417 0.6688 0.3726 0.061 Uiso 1 1 calc R U . . .
C40 C 0.0152(4) 0.2254(4) 0.3676(2) 0.0219(8) Uani 1 1 d . . . . .
C41 C -0.0013(4) 0.1073(4) 0.3411(3) 0.0271(9) Uani 1 1 d . . . . .
C42 C 0.0566(4) 0.0473(4) 0.3825(3) 0.0288(9) Uani 1 1 d . . . . .
H42 H 0.0447 -0.0317 0.3652 0.035 Uiso 1 1 calc R U . . .
C43 C 0.1323(4) 0.1029(4) 0.4495(3) 0.0275(9) Uani 1 1 d . . . . .
C44 C 0.1482(4) 0.2200(4) 0.4736(3) 0.0299(9) Uani 1 1 d . . . . .
H44 H 0.1990 0.2585 0.5178 0.036 Uiso 1 1 calc R U . . .
C45 C 0.0913(4) 0.2834(4) 0.4345(2) 0.0250(8) Uani 1 1 d . . . . .
C46 C -0.0772(6) 0.0449(5) 0.2682(3) 0.0455(14) Uani 1 1 d . . . . .
H46A H -0.0710 -0.0318 0.2575 0.068 Uiso 1 1 calc R U . . .
H46B H -0.0402 0.0974 0.2319 0.068 Uiso 1 1 calc R U . . .
H46C H -0.1688 0.0292 0.2686 0.068 Uiso 1 1 calc R U . . .
C47 C 0.1967(5) 0.0367(5) 0.4918(3) 0.0373(11) Uani 1 1 d . . . . .
H47A H 0.2251 0.0768 0.5405 0.056 Uiso 1 1 calc R U . . .
H47B H 0.2722 0.0385 0.4696 0.056 Uiso 1 1 calc R U . . .
H47C H 0.1338 -0.0474 0.4921 0.056 Uiso 1 1 calc R U . . .
C48 C 0.1106(6) 0.4106(5) 0.4644(3) 0.0363(11) Uani 1 1 d . . . . .
H48A H 0.1456 0.4268 0.5146 0.054 Uiso 1 1 calc R U . . .
H48B H 0.0268 0.4155 0.4594 0.054 Uiso 1 1 calc R U . . .
H48C H 0.1718 0.4708 0.4382 0.054 Uiso 1 1 calc R U . . .
C49A C -0.443(3) -0.0439(19) 0.0760(13) 0.063(5) Uani 0.247(10) 1 d G . P B 1
H49A H -0.4577 -0.0983 0.1106 0.076 Uiso 0.247(10) 1 calc R U P B 1
C50A C -0.540(2) -0.0692(17) 0.0180(16) 0.064(5) Uani 0.247(10) 1 d G . P B 1
H50A H -0.6196 -0.1405 0.0137 0.076 Uiso 0.247(10) 1 calc R U P B 1
C51A C -0.519(2) 0.012(2) -0.0336(13) 0.066(5) Uani 0.247(10) 1 d G . P B 1
H51A H -0.5841 -0.0048 -0.0724 0.080 Uiso 0.247(10) 1 calc R U P B 1
C52A C -0.401(3) 0.119(2) -0.0272(14) 0.063(5) Uani 0.247(10) 1 d G . P B 1
H52A H -0.3866 0.1731 -0.0617 0.076 Uiso 0.247(10) 1 calc R U P B 1
C53A C -0.304(2) 0.1440(19) 0.0308(17) 0.064(5) Uani 0.247(10) 1 d G . P B 1
H53A H -0.2247 0.2153 0.0351 0.076 Uiso 0.247(10) 1 calc R U P B 1
C54A C -0.325(2) 0.063(2) 0.0824(13) 0.066(5) Uani 0.247(10) 1 d G . P B 1
H54A H -0.2603 0.0796 0.1213 0.080 Uiso 0.247(10) 1 calc R U P B 1
C49B C -0.367(3) 0.008(2) 0.1004(11) 0.063(5) Uani 0.253(10) 1 d G . P B 2
H49B H -0.3427 -0.0198 0.1418 0.076 Uiso 0.253(10) 1 calc R U P B 2
C50B C -0.491(2) -0.0606(17) 0.0607(14) 0.064(5) Uani 0.253(10) 1 d G . P B 2
H50B H -0.5496 -0.1338 0.0756 0.076 Uiso 0.253(10) 1 calc R U P B 2
C51B C -0.527(2) -0.019(2) -0.0012(14) 0.066(5) Uani 0.253(10) 1 d G . P B 2
H51B H -0.6100 -0.0651 -0.0277 0.080 Uiso 0.253(10) 1 calc R U P B 2
C52B C -0.439(3) 0.090(3) -0.0234(15) 0.063(5) Uani 0.253(10) 1 d G . P B 2
H52B H -0.4634 0.1176 -0.0648 0.076 Uiso 0.253(10) 1 calc R U P B 2
C53B C -0.315(2) 0.158(2) 0.0163(16) 0.064(5) Uani 0.253(10) 1 d G . P B 2
H53B H -0.2564 0.2316 0.0014 0.076 Uiso 0.253(10) 1 calc R U P B 2
C54B C -0.279(2) 0.117(2) 0.0782(13) 0.066(5) Uani 0.253(10) 1 d G . P B 2
H54B H -0.1961 0.1629 0.1047 0.080 Uiso 0.253(10) 1 calc R U P B 2
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
P1 0.0171(4) 0.0169(4) 0.0337(6) 0.0029(4) 0.0029(4) 0.0072(4)
P2 0.0152(4) 0.0188(5) 0.0401(7) -0.0025(4) 0.0082(4) 0.0045(4)
Au1 0.01692(7) 0.01716(7) 0.03373(9) 0.00862(5) 0.00772(5) 0.00834(5)
Cl1 0.0244(5) 0.0321(5) 0.0543(7) 0.0224(5) 0.0114(5) 0.0165(4)
Au2 0.0231(2) 0.0190(2) 0.0208(2) -0.00047(16) 0.00017(16) 0.00778(17)
Cl2 0.044(2) 0.0353(18) 0.0350(19) -0.0108(15) -0.0129(16) 0.0130(16)
N1 0.0174(14) 0.0157(14) 0.0330(19) 0.0064(13) 0.0099(13) 0.0068(12)
N2 0.0138(13) 0.0183(14) 0.0243(17) 0.0058(12) 0.0052(12) 0.0052(11)
C1 0.0168(16) 0.0197(17) 0.036(2) 0.0148(16) 0.0118(15) 0.0095(14)
C2 0.0258(19) 0.0244(19) 0.039(2) 0.0178(18) 0.0176(18) 0.0148(16)
C3 0.032(2) 0.040(3) 0.051(3) 0.026(2) 0.026(2) 0.024(2)
C4 0.022(2) 0.039(3) 0.072(4) 0.032(3) 0.024(2) 0.018(2)
C5 0.0176(18) 0.024(2) 0.065(3) 0.018(2) 0.007(2) 0.0074(16)
C6 0.0187(17) 0.0211(18) 0.043(3) 0.0161(17) 0.0091(17) 0.0101(15)
C7 0.033(2) 0.032(2) 0.030(2) 0.0140(18) 0.0169(18) 0.0205(19)
C8 0.037(2) 0.041(3) 0.037(3) 0.023(2) 0.017(2) 0.022(2)
C9 0.042(3) 0.054(3) 0.038(3) 0.025(3) 0.008(2) 0.018(3)
C10 0.055(3) 0.043(3) 0.035(3) 0.017(2) 0.009(2) 0.014(3)
C11 0.053(3) 0.035(3) 0.033(3) 0.012(2) 0.015(2) 0.015(2)
C12 0.038(2) 0.032(2) 0.031(2) 0.0162(19) 0.0196(19) 0.021(2)
C13 0.052(3) 0.044(3) 0.050(3) 0.022(3) 0.011(3) 0.032(3)
C14 0.087(6) 0.049(4) 0.062(5) 0.014(3) -0.013(4) 0.009(4)
C15 0.045(3) 0.033(2) 0.040(3) 0.016(2) 0.020(2) 0.028(2)
C16 0.0158(16) 0.0155(16) 0.043(3) 0.0047(16) -0.0013(16) 0.0045(14)
C17 0.0166(17) 0.0148(16) 0.045(3) 0.0038(16) -0.0036(16) 0.0044(14)
C18 0.027(2) 0.0187(18) 0.050(3) -0.0023(18) -0.009(2) 0.0117(16)
C19 0.031(2) 0.029(2) 0.038(3) -0.0055(19) -0.0113(19) 0.0153(19)
C20 0.040(3) 0.029(2) 0.035(3) 0.0002(19) -0.006(2) 0.018(2)
C21 0.029(2) 0.0182(18) 0.038(3) 0.0002(17) -0.0046(18) 0.0102(16)
C22 0.029(2) 0.025(2) 0.062(4) 0.017(2) 0.009(2) 0.0135(18)
C23 0.055(3) 0.050(3) 0.034(3) -0.002(2) -0.007(2) 0.035(3)
C24 0.050(3) 0.027(2) 0.037(3) 0.0029(19) -0.007(2) 0.023(2)
C25 0.0136(15) 0.0238(18) 0.029(2) 0.0097(16) 0.0051(14) 0.0068(14)
C26 0.0165(17) 0.030(2) 0.034(2) 0.0163(18) 0.0060(16) 0.0089(15)
C27 0.0180(19) 0.042(3) 0.062(3) 0.030(3) 0.010(2) 0.0142(19)
C28 0.0173(19) 0.049(3) 0.069(4) 0.035(3) 0.015(2) 0.013(2)
C29 0.0197(19) 0.035(2) 0.048(3) 0.023(2) 0.0134(19) 0.0087(17)
C30 0.0193(17) 0.0251(19) 0.033(2) 0.0119(17) 0.0090(16) 0.0090(15)
C31 0.0140(15) 0.0272(19) 0.032(2) 0.0145(17) 0.0040(15) 0.0079(15)
C32 0.0222(18) 0.028(2) 0.022(2) 0.0101(16) -0.0036(15) 0.0061(16)
C33 0.029(2) 0.040(3) 0.030(2) 0.019(2) 0.0079(18) 0.0141(19)
C34 0.0225(19) 0.029(2) 0.039(3) 0.0177(19) 0.0090(17) 0.0114(17)
C35 0.028(2) 0.029(2) 0.038(3) 0.0106(19) 0.0089(18) 0.0165(18)
C36 0.027(2) 0.032(2) 0.031(2) 0.0127(18) 0.0108(17) 0.0189(18)
C37 0.059(4) 0.044(3) 0.028(3) 0.005(2) -0.009(3) -0.001(3)
C38 0.037(3) 0.034(3) 0.051(3) 0.021(2) 0.007(2) 0.010(2)
C39 0.060(3) 0.037(3) 0.038(3) 0.012(2) 0.019(2) 0.029(3)
C40 0.0184(16) 0.0228(18) 0.027(2) 0.0122(15) 0.0091(15) 0.0087(14)
C41 0.0204(18) 0.0202(18) 0.037(2) 0.0089(17) 0.0072(17) 0.0031(15)
C42 0.0236(19) 0.0193(18) 0.044(3) 0.0099(18) 0.0132(18) 0.0070(15)
C43 0.0214(18) 0.030(2) 0.037(2) 0.0169(18) 0.0126(17) 0.0128(16)
C44 0.027(2) 0.032(2) 0.032(2) 0.0089(19) 0.0069(18) 0.0132(18)
C45 0.028(2) 0.0230(19) 0.027(2) 0.0069(16) 0.0099(16) 0.0127(16)
C46 0.050(3) 0.020(2) 0.052(3) 0.004(2) -0.012(3) 0.004(2)
C47 0.029(2) 0.038(3) 0.053(3) 0.022(2) 0.009(2) 0.018(2)
C48 0.054(3) 0.032(2) 0.028(2) 0.0030(19) 0.006(2) 0.024(2)
C49A 0.084(16) 0.052(12) 0.067(11) 0.024(8) 0.040(10) 0.033(11)
C50A 0.106(12) 0.056(8) 0.060(11) 0.026(8) 0.046(10) 0.056(9)
C51A 0.088(14) 0.058(12) 0.070(12) 0.007(11) 0.036(11) 0.043(11)
C52A 0.084(16) 0.052(12) 0.067(11) 0.024(8) 0.040(10) 0.033(11)
C53A 0.106(12) 0.056(8) 0.060(11) 0.026(8) 0.046(10) 0.056(9)
C54A 0.088(14) 0.058(12) 0.070(12) 0.007(11) 0.036(11) 0.043(11)
C49B 0.084(16) 0.052(12) 0.067(11) 0.024(8) 0.040(10) 0.033(11)
C50B 0.106(12) 0.056(8) 0.060(11) 0.026(8) 0.046(10) 0.056(9)
C51B 0.088(14) 0.058(12) 0.070(12) 0.007(11) 0.036(11) 0.043(11)
C52B 0.084(16) 0.052(12) 0.067(11) 0.024(8) 0.040(10) 0.033(11)
C53B 0.106(12) 0.056(8) 0.060(11) 0.026(8) 0.046(10) 0.056(9)
C54B 0.088(14) 0.058(12) 0.070(12) 0.007(11) 0.036(11) 0.043(11)
#==============================================================================
# MOLECULAR GEOMETRY
_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
P1 N1 1.776(3) . ?
P1 N2 1.781(3) . ?
P1 Au2 2.1240(13) . ?
P1 Au1 2.2278(12) . ?
P1 P2 2.5953(18) . ?
P2 N2 1.645(3) . ?
P2 N1 1.660(3) . ?
Au1 Cl1 2.3068(12) . ?
Au2 Cl2 2.288(4) . ?
N1 C1 1.424(5) . ?
N2 C25 1.434(5) . ?
C1 C2 1.404(6) . ?
C1 C6 1.421(6) . ?
C2 C3 1.399(6) . ?
C2 C7 1.481(7) . ?
C3 C4 1.373(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.394(6) . ?
C5 H5 0.9300 . ?
C6 C16 1.470(7) . ?
C7 C12 1.410(6) . ?
C7 C8 1.418(6) . ?
C8 C9 1.368(8) . ?
C8 C13 1.508(7) . ?
C9 C10 1.399(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(8) . ?
C10 C14 1.516(9) . ?
C11 C12 1.390(8) . ?
C11 H11 0.9300 . ?
C12 C15 1.507(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.410(5) . ?
C16 C21 1.413(7) . ?
C17 C18 1.393(7) . ?
C17 C22 1.508(7) . ?
C18 C19 1.382(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.390(6) . ?
C19 C23 1.512(8) . ?
C20 C21 1.388(7) . ?
C20 H20 0.9300 . ?
C21 C24 1.509(6) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C30 1.401(5) . ?
C25 C26 1.405(5) . ?
C26 C27 1.400(6) . ?
C26 C31 1.489(6) . ?
C27 C28 1.379(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.389(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.394(6) . ?
C29 H29 0.9300 . ?
C30 C40 1.492(6) . ?
C31 C36 1.406(7) . ?
C31 C32 1.417(6) . ?
C32 C33 1.388(6) . ?
C32 C37 1.483(7) . ?
C33 C34 1.385(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.384(7) . ?
C34 C38 1.502(6) . ?
C35 C36 1.398(6) . ?
C35 H35 0.9300 . ?
C36 C39 1.495(7) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 C41 1.398(6) . ?
C40 C45 1.403(6) . ?
C41 C42 1.393(6) . ?
C41 C46 1.504(7) . ?
C42 C43 1.399(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.377(7) . ?
C43 C47 1.506(6) . ?
C44 C45 1.394(6) . ?
C44 H44 0.9300 . ?
C45 C48 1.507(6) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49A C50A 1.3900 . ?
C49A C54A 1.3900 . ?
C49A H49A 0.9300 . ?
C50A C51A 1.3900 . ?
C50A H50A 0.9300 . ?
C51A C52A 1.3900 . ?
C51A H51A 0.9300 . ?
C52A C53A 1.3900 . ?
C52A H52A 0.9300 . ?
C53A C54A 1.3900 . ?
C53A H53A 0.9300 . ?
C54A H54A 0.9300 . ?
C49B C50B 1.3900 . ?
C49B C54B 1.3900 . ?
C49B H49B 0.9300 . ?
C50B C51B 1.3900 . ?
C50B H50B 0.9300 . ?
C51B C52B 1.3900 . ?
C51B H51B 0.9300 . ?
C52B C53B 1.3900 . ?
C52B H52B 0.9300 . ?
C53B C54B 1.3900 . ?
C53B H53B 0.9300 . ?
C54B H54B 0.9300 . ?
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 P1 N2 78.05(16) . . ?
N1 P1 Au2 130.35(13) . . ?
N2 P1 Au2 104.39(12) . . ?
N1 P1 Au1 105.35(12) . . ?
N2 P1 Au1 111.44(12) . . ?
Au2 P1 Au1 118.50(5) . . ?
N1 P1 P2 39.28(11) . . ?
N2 P1 P2 38.84(11) . . ?
Au2 P1 P2 123.39(5) . . ?
Au1 P1 P2 115.83(6) . . ?
N2 P2 N1 85.33(17) . . ?
N2 P2 P1 42.77(12) . . ?
N1 P2 P1 42.64(12) . . ?
P1 Au1 Cl1 175.80(5) . . ?
P1 Au2 Cl2 175.85(12) . . ?
C1 N1 P2 130.1(3) . . ?
C1 N1 P1 131.0(3) . . ?
P2 N1 P1 98.07(17) . . ?
C25 N2 P2 128.0(3) . . ?
C25 N2 P1 128.2(3) . . ?
P2 N2 P1 98.38(17) . . ?
C2 C1 C6 121.2(4) . . ?
C2 C1 N1 120.4(4) . . ?
C6 C1 N1 118.4(4) . . ?
C3 C2 C1 118.1(5) . . ?
C3 C2 C7 119.1(4) . . ?
C1 C2 C7 122.8(4) . . ?
C4 C3 C2 121.7(5) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 121.0(5) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 118.1(4) . . ?
C5 C6 C16 122.1(4) . . ?
C1 C6 C16 119.8(3) . . ?
C12 C7 C8 119.5(5) . . ?
C12 C7 C2 120.3(4) . . ?
C8 C7 C2 120.1(4) . . ?
C9 C8 C7 119.4(5) . . ?
C9 C8 C13 120.5(5) . . ?
C7 C8 C13 120.1(5) . . ?
C8 C9 C10 122.1(5) . . ?
C8 C9 H9 118.9 . . ?
C10 C9 H9 118.9 . . ?
C11 C10 C9 117.9(6) . . ?
C11 C10 C14 121.5(6) . . ?
C9 C10 C14 120.6(6) . . ?
C10 C11 C12 122.3(5) . . ?
C10 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C11 C12 C7 118.7(5) . . ?
C11 C12 C15 119.7(4) . . ?
C7 C12 C15 121.6(5) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 119.5(4) . . ?
C17 C16 C6 120.8(4) . . ?
C21 C16 C6 119.5(4) . . ?
C18 C17 C16 119.2(4) . . ?
C18 C17 C22 119.7(4) . . ?
C16 C17 C22 120.9(4) . . ?
C19 C18 C17 121.5(4) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C19 C20 118.8(5) . . ?
C18 C19 C23 120.9(4) . . ?
C20 C19 C23 120.2(5) . . ?
C21 C20 C19 121.8(5) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C20 C21 C16 119.0(4) . . ?
C20 C21 C24 120.3(4) . . ?
C16 C21 C24 120.6(4) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 121.6(3) . . ?
C30 C25 N2 118.9(3) . . ?
C26 C25 N2 119.6(3) . . ?
C27 C26 C25 118.0(4) . . ?
C27 C26 C31 119.6(4) . . ?
C25 C26 C31 122.3(3) . . ?
C28 C27 C26 121.2(4) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C27 C28 C29 119.6(4) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C28 C29 C30 121.5(4) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C29 C30 C25 117.9(4) . . ?
C29 C30 C40 118.4(4) . . ?
C25 C30 C40 123.6(3) . . ?
C36 C31 C32 119.4(4) . . ?
C36 C31 C26 119.0(4) . . ?
C32 C31 C26 121.5(4) . . ?
C33 C32 C31 118.5(4) . . ?
C33 C32 C37 121.1(4) . . ?
C31 C32 C37 120.4(4) . . ?
C34 C33 C32 122.9(4) . . ?
C34 C33 H33 118.6 . . ?
C32 C33 H33 118.6 . . ?
C35 C34 C33 118.1(4) . . ?
C35 C34 C38 120.4(5) . . ?
C33 C34 C38 121.5(5) . . ?
C34 C35 C36 121.6(5) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C35 C36 C31 119.5(4) . . ?
C35 C36 C39 119.6(4) . . ?
C31 C36 C39 120.9(4) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C45 120.3(4) . . ?
C41 C40 C30 121.1(4) . . ?
C45 C40 C30 118.4(4) . . ?
C42 C41 C40 119.1(4) . . ?
C42 C41 C46 119.4(4) . . ?
C40 C41 C46 121.6(4) . . ?
C41 C42 C43 121.8(4) . . ?
C41 C42 H42 119.1 . . ?
C43 C42 H42 119.1 . . ?
C44 C43 C42 117.7(4) . . ?
C44 C43 C47 122.0(5) . . ?
C42 C43 C47 120.2(4) . . ?
C43 C44 C45 122.7(5) . . ?
C43 C44 H44 118.7 . . ?
C45 C44 H44 118.7 . . ?
C44 C45 C40 118.5(4) . . ?
C44 C45 C48 120.1(4) . . ?
C40 C45 C48 121.4(4) . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50A C49A C54A 120.0 . . ?
C50A C49A H49A 120.0 . . ?
C54A C49A H49A 120.0 . . ?
C51A C50A C49A 120.0 . . ?
C51A C50A H50A 120.0 . . ?
C49A C50A H50A 120.0 . . ?
C52A C51A C50A 120.0 . . ?
C52A C51A H51A 120.0 . . ?
C50A C51A H51A 120.0 . . ?
C51A C52A C53A 120.0 . . ?
C51A C52A H52A 120.0 . . ?
C53A C52A H52A 120.0 . . ?
C54A C53A C52A 120.0 . . ?
C54A C53A H53A 120.0 . . ?
C52A C53A H53A 120.0 . . ?
C53A C54A C49A 120.0 . . ?
C53A C54A H54A 120.0 . . ?
C49A C54A H54A 120.0 . . ?
C50B C49B C54B 120.0 . . ?
C50B C49B H49B 120.0 . . ?
C54B C49B H49B 120.0 . . ?
C49B C50B C51B 120.0 . . ?
C49B C50B H50B 120.0 . . ?
C51B C50B H50B 120.0 . . ?
C50B C51B C52B 120.0 . . ?
C50B C51B H51B 120.0 . . ?
C52B C51B H51B 120.0 . . ?
C53B C52B C51B 120.0 . . ?
C53B C52B H52B 120.0 . . ?
C51B C52B H52B 120.0 . . ?
C52B C53B C54B 120.0 . . ?
C52B C53B H53B 120.0 . . ?
C54B C53B H53B 120.0 . . ?
C53B C54B C49B 120.0 . . ?
C53B C54B H54B 120.0 . . ?
C49B C54B H54B 120.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P2 N1 C1 -166.9(4) . . . . ?
P1 P2 N1 C1 -170.1(5) . . . . ?
N2 P2 N1 P1 3.16(18) . . . . ?
N2 P1 N1 C1 167.0(4) . . . . ?
Au2 P1 N1 C1 -94.2(4) . . . . ?
Au1 P1 N1 C1 57.8(4) . . . . ?
P2 P1 N1 C1 170.0(5) . . . . ?
N2 P1 N1 P2 -2.97(17) . . . . ?
Au2 P1 N1 P2 95.86(19) . . . . ?
Au1 P1 N1 P2 -112.20(14) . . . . ?
N1 P2 N2 C25 -158.5(4) . . . . ?
P1 P2 N2 C25 -155.4(4) . . . . ?
N1 P2 N2 P1 -3.15(18) . . . . ?
N1 P1 N2 C25 158.3(4) . . . . ?
Au2 P1 N2 C25 29.3(3) . . . . ?
Au1 P1 N2 C25 -99.7(3) . . . . ?
P2 P1 N2 C25 155.3(4) . . . . ?
N1 P1 N2 P2 3.00(17) . . . . ?
Au2 P1 N2 P2 -125.97(13) . . . . ?
Au1 P1 N2 P2 104.99(14) . . . . ?
P2 N1 C1 C2 -158.2(3) . . . . ?
P1 N1 C1 C2 34.8(6) . . . . ?
P2 N1 C1 C6 21.6(5) . . . . ?
P1 N1 C1 C6 -145.3(3) . . . . ?
C6 C1 C2 C3 1.3(6) . . . . ?
N1 C1 C2 C3 -178.9(4) . . . . ?
C6 C1 C2 C7 -176.5(4) . . . . ?
N1 C1 C2 C7 3.3(6) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
C7 C2 C3 C4 177.5(4) . . . . ?
C2 C3 C4 C5 -0.4(7) . . . . ?
C3 C4 C5 C6 0.1(7) . . . . ?
C4 C5 C6 C1 0.8(6) . . . . ?
C4 C5 C6 C16 -178.6(4) . . . . ?
C2 C1 C6 C5 -1.5(6) . . . . ?
N1 C1 C6 C5 178.7(4) . . . . ?
C2 C1 C6 C16 177.9(4) . . . . ?
N1 C1 C6 C16 -1.9(5) . . . . ?
C3 C2 C7 C12 71.0(5) . . . . ?
C1 C2 C7 C12 -111.3(5) . . . . ?
C3 C2 C7 C8 -105.8(5) . . . . ?
C1 C2 C7 C8 71.8(6) . . . . ?
C12 C7 C8 C9 2.2(7) . . . . ?
C2 C7 C8 C9 179.0(4) . . . . ?
C12 C7 C8 C13 -176.3(4) . . . . ?
C2 C7 C8 C13 0.6(7) . . . . ?
C7 C8 C9 C10 -1.6(8) . . . . ?
C13 C8 C9 C10 176.8(5) . . . . ?
C8 C9 C10 C11 0.0(8) . . . . ?
C8 C9 C10 C14 -177.5(6) . . . . ?
C9 C10 C11 C12 1.1(8) . . . . ?
C14 C10 C11 C12 178.5(6) . . . . ?
C10 C11 C12 C7 -0.5(7) . . . . ?
C10 C11 C12 C15 -178.0(5) . . . . ?
C8 C7 C12 C11 -1.1(6) . . . . ?
C2 C7 C12 C11 -178.0(4) . . . . ?
C8 C7 C12 C15 176.3(4) . . . . ?
C2 C7 C12 C15 -0.5(6) . . . . ?
C5 C6 C16 C17 85.4(5) . . . . ?
C1 C6 C16 C17 -94.0(5) . . . . ?
C5 C6 C16 C21 -98.8(5) . . . . ?
C1 C6 C16 C21 81.8(5) . . . . ?
C21 C16 C17 C18 -2.9(6) . . . . ?
C6 C16 C17 C18 172.8(4) . . . . ?
C21 C16 C17 C22 -177.2(4) . . . . ?
C6 C16 C17 C22 -1.4(6) . . . . ?
C16 C17 C18 C19 0.7(6) . . . . ?
C22 C17 C18 C19 175.1(4) . . . . ?
C17 C18 C19 C20 2.2(7) . . . . ?
C17 C18 C19 C23 -177.4(4) . . . . ?
C18 C19 C20 C21 -3.0(7) . . . . ?
C23 C19 C20 C21 176.6(5) . . . . ?
C19 C20 C21 C16 0.8(7) . . . . ?
C19 C20 C21 C24 -176.9(5) . . . . ?
C17 C16 C21 C20 2.1(6) . . . . ?
C6 C16 C21 C20 -173.7(4) . . . . ?
C17 C16 C21 C24 179.8(4) . . . . ?
C6 C16 C21 C24 4.0(6) . . . . ?
P2 N2 C25 C30 -141.0(4) . . . . ?
P1 N2 C25 C30 70.7(5) . . . . ?
P2 N2 C25 C26 38.3(6) . . . . ?
P1 N2 C25 C26 -110.0(4) . . . . ?
C30 C25 C26 C27 -5.1(7) . . . . ?
N2 C25 C26 C27 175.6(5) . . . . ?
C30 C25 C26 C31 172.7(4) . . . . ?
N2 C25 C26 C31 -6.6(7) . . . . ?
C25 C26 C27 C28 -0.1(9) . . . . ?
C31 C26 C27 C28 -177.9(5) . . . . ?
C26 C27 C28 C29 3.2(10) . . . . ?
C27 C28 C29 C30 -1.3(9) . . . . ?
C28 C29 C30 C25 -3.6(8) . . . . ?
C28 C29 C30 C40 172.4(5) . . . . ?
C26 C25 C30 C29 6.9(7) . . . . ?
N2 C25 C30 C29 -173.9(4) . . . . ?
C26 C25 C30 C40 -168.9(4) . . . . ?
N2 C25 C30 C40 10.4(7) . . . . ?
C27 C26 C31 C36 86.9(6) . . . . ?
C25 C26 C31 C36 -90.9(5) . . . . ?
C27 C26 C31 C32 -91.7(6) . . . . ?
C25 C26 C31 C32 90.6(5) . . . . ?
C36 C31 C32 C33 1.2(6) . . . . ?
C26 C31 C32 C33 179.8(4) . . . . ?
C36 C31 C32 C37 -177.0(5) . . . . ?
C26 C31 C32 C37 1.5(7) . . . . ?
C31 C32 C33 C34 0.1(7) . . . . ?
C37 C32 C33 C34 178.4(5) . . . . ?
C32 C33 C34 C35 -0.8(7) . . . . ?
C32 C33 C34 C38 178.6(4) . . . . ?
C33 C34 C35 C36 0.1(6) . . . . ?
C38 C34 C35 C36 -179.3(4) . . . . ?
C34 C35 C36 C31 1.2(6) . . . . ?
C34 C35 C36 C39 -179.4(4) . . . . ?
C32 C31 C36 C35 -1.9(6) . . . . ?
C26 C31 C36 C35 179.5(4) . . . . ?
C32 C31 C36 C39 178.8(4) . . . . ?
C26 C31 C36 C39 0.2(6) . . . . ?
C29 C30 C40 C41 73.1(6) . . . . ?
C25 C30 C40 C41 -111.2(5) . . . . ?
C29 C30 C40 C45 -101.4(5) . . . . ?
C25 C30 C40 C45 74.3(6) . . . . ?
C45 C40 C41 C42 1.2(6) . . . . ?
C30 C40 C41 C42 -173.2(4) . . . . ?
C45 C40 C41 C46 -177.3(4) . . . . ?
C30 C40 C41 C46 8.3(6) . . . . ?
C40 C41 C42 C43 -0.9(6) . . . . ?
C46 C41 C42 C43 177.7(4) . . . . ?
C41 C42 C43 C44 0.0(6) . . . . ?
C41 C42 C43 C47 -178.2(4) . . . . ?
C42 C43 C44 C45 0.7(6) . . . . ?
C47 C43 C44 C45 178.8(4) . . . . ?
C43 C44 C45 C40 -0.3(7) . . . . ?
C43 C44 C45 C48 179.0(4) . . . . ?
C41 C40 C45 C44 -0.7(6) . . . . ?
C30 C40 C45 C44 173.9(4) . . . . ?
C41 C40 C45 C48 -180.0(4) . . . . ?
C30 C40 C45 C48 -5.4(6) . . . . ?
C54A C49A C50A C51A 0.0 . . . . ?
C49A C50A C51A C52A 0.0 . . . . ?
C50A C51A C52A C53A 0.0 . . . . ?
C51A C52A C53A C54A 0.0 . . . . ?
C52A C53A C54A C49A 0.0 . . . . ?
C50A C49A C54A C53A 0.0 . . . . ?
C54B C49B C50B C51B 0.0 . . . . ?
C49B C50B C51B C52B 0.0 . . . . ?
C50B C51B C52B C53B 0.0 . . . . ?
C51B C52B C53B C54B 0.0 . . . . ?
C52B C53B C54B C49B 0.0 . . . . ?
C50B C49B C54B C53B 0.0 . . . . ?
_refine_diff_density_max 1.676
_refine_diff_density_min -2.740
_refine_diff_density_rms 0.139
_shelxl_version_number 2013-4
_shelx_res_file
;
TITL ah172e in P-1
CELL 0.71069 11.168 12.029 18.686 94.538 94.411 114.833
ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005
LATT 1
SFAC C H N P CL AU
UNIT 102 106 4 4 2.665 2.665
MERG 2
OMIT -3 65
OMIT 0 1 0
OMIT -1 0 1
OMIT -1 -2 2
OMIT -3 2 2
OMIT -1 -1 1
OMIT 2 -2 2
OMIT 2 -2 1
OMIT -1 4 2
OMIT 2 -3 3
OMIT 0 -1 1
OMIT -1 1 0
L.S. 8
LIST 4
FMAP 2
SIZE 0.07 0.12 0.22
PLAN 25
ACTA
CONF
BOND $H
EQIV $1 -1-x, -y, -z
FREE C49A C49A_$1
FREE C49A C50A_$1
FREE C49A C51A_$1
FREE C49A C52A_$1
FREE C49A C53A_$1
FREE C49A C54A_$1
FREE C50A C49A_$1
FREE C50A C50A_$1
FREE C50A C51A_$1
FREE C50A C52A_$1
FREE C50A C53A_$1
FREE C50A C54A_$1
FREE C51A C49A_$1
FREE C51A C50A_$1
FREE C51A C51A_$1
FREE C51A C52A_$1
FREE C51A C53A_$1
FREE C51A C54A_$1
FREE C52A C49A_$1
FREE C52A C50A_$1
FREE C52A C51A_$1
FREE C52A C52A_$1
FREE C52A C53A_$1
FREE C52A C54A_$1
FREE C53A C49A_$1
FREE C53A C50A_$1
FREE C53A C51A_$1
FREE C53A C52A_$1
FREE C53A C53A_$1
FREE C53A C54A_$1
FREE C54A C49A_$1
FREE C54A C50A_$1
FREE C54A C51A_$1
FREE C54A C52A_$1
FREE C54A C53A_$1
FREE C54A C54A_$1
FREE C49B C49B_$1
FREE C49B C50B_$1
FREE C49B C51B_$1
FREE C49B C52B_$1
FREE C49B C53B_$1
FREE C49B C54B_$1
FREE C50B C49B_$1
FREE C50B C50B_$1
FREE C50B C51B_$1
FREE C50B C52B_$1
FREE C50B C53B_$1
FREE C50B C54B_$1
FREE C51B C49B_$1
FREE C51B C50B_$1
FREE C51B C51B_$1
FREE C51B C52B_$1
FREE C51B C53B_$1
FREE C51B C54B_$1
FREE C52B C49B_$1
FREE C52B C50B_$1
FREE C52B C51B_$1
FREE C52B C52B_$1
FREE C52B C53B_$1
FREE C52B C54B_$1
FREE C53B C49B_$1
FREE C53B C50B_$1
FREE C53B C51B_$1
FREE C53B C52B_$1
FREE C53B C53B_$1
FREE C53B C54B_$1
FREE C54B C49B_$1
FREE C54B C50B_$1
FREE C54B C51B_$1
FREE C54B C52B_$1
FREE C54B C53B_$1
FREE C54B C54B_$1
EADP C49A C52A C49B C52B
EADP C50A C53A C50B C53B
EADP C51A C54A C51B C54B
WGHT 0.000000 9.433900
FVAR 0.07634 0.33199 0.49485
P1 4 0.210563 0.354145 0.223219 11.00000 0.01707 0.01692 =
0.03369 0.00286 0.00291 0.00719
P2 4 0.260706 0.570320 0.288555 11.00000 0.01521 0.01876 =
0.04006 -0.00253 0.00824 0.00448
AU1 6 0.295517 0.244522 0.281945 11.00000 0.01692 0.01716 =
0.03373 0.00862 0.00772 0.00834
CL1 5 0.389581 0.128622 0.335072 11.00000 0.02442 0.03209 =
0.05427 0.02236 0.01139 0.01647
PART 3
AU2 6 0.056502 0.261316 0.136363 21.00000 0.02312 0.01899 =
0.02080 -0.00047 0.00017 0.00778
CL2 5 -0.119508 0.164675 0.047714 21.00000 0.04379 0.03530 =
0.03501 -0.01085 -0.01288 0.01300
PART 0
N1 3 0.336689 0.507939 0.237080 11.00000 0.01739 0.01574 =
0.03296 0.00639 0.00988 0.00684
N2 3 0.142425 0.429062 0.282687 11.00000 0.01384 0.01832 =
0.02433 0.00584 0.00522 0.00525
C1 1 0.470239 0.558084 0.220657 11.00000 0.01680 0.01968 =
0.03645 0.01482 0.01176 0.00947
C2 1 0.503325 0.509279 0.158479 11.00000 0.02577 0.02444 =
0.03870 0.01785 0.01760 0.01479
C3 1 0.636450 0.560593 0.145508 11.00000 0.03192 0.04019 =
0.05116 0.02638 0.02623 0.02444
AFIX 43
H3 2 0.660130 0.529100 0.104681 11.00000 -1.20000
AFIX 0
C4 1 0.732990 0.656276 0.191548 11.00000 0.02205 0.03940 =
0.07181 0.03240 0.02429 0.01799
AFIX 43
H4 2 0.820868 0.688461 0.181880 11.00000 -1.20000
AFIX 0
C5 1 0.699231 0.705146 0.252777 11.00000 0.01762 0.02390 =
0.06497 0.01850 0.00743 0.00738
AFIX 43
H5 2 0.765140 0.770017 0.283672 11.00000 -1.20000
AFIX 0
C6 1 0.568211 0.658299 0.268427 11.00000 0.01872 0.02113 =
0.04308 0.01607 0.00911 0.01008
C7 1 0.402986 0.409652 0.105230 11.00000 0.03309 0.03233 =
0.03003 0.01396 0.01691 0.02051
C8 1 0.313234 0.434679 0.058768 11.00000 0.03652 0.04069 =
0.03699 0.02289 0.01671 0.02201
C9 1 0.222454 0.342093 0.009148 11.00000 0.04202 0.05406 =
0.03799 0.02526 0.00825 0.01817
AFIX 43
H9 2 0.162396 0.358602 -0.020321 11.00000 -1.20000
AFIX 0
C10 1 0.217039 0.223379 0.001297 11.00000 0.05467 0.04306 =
0.03490 0.01679 0.00858 0.01376
C11 1 0.307441 0.200935 0.045793 11.00000 0.05347 0.03487 =
0.03345 0.01167 0.01482 0.01547
AFIX 43
H11 2 0.305941 0.122812 0.040607 11.00000 -1.20000
AFIX 0
C12 1 0.400310 0.291001 0.097912 11.00000 0.03798 0.03220 =
0.03051 0.01615 0.01961 0.02065
C13 1 0.320498 0.563105 0.062953 11.00000 0.05225 0.04433 =
0.05011 0.02232 0.01132 0.03173
AFIX 137
H13A 2 0.265918 0.568334 0.022282 11.00000 -1.50000
H13B 2 0.410883 0.621730 0.062322 11.00000 -1.50000
H13C 2 0.289319 0.581011 0.106920 11.00000 -1.50000
AFIX 0
C14 1 0.118736 0.124654 -0.056406 11.00000 0.08713 0.04905 =
0.06238 0.01404 -0.01265 0.00911
AFIX 137
H14A 2 0.146878 0.060119 -0.065304 11.00000 -1.50000
H14B 2 0.114711 0.160266 -0.100213 11.00000 -1.50000
H14C 2 0.032371 0.091062 -0.040240 11.00000 -1.50000
AFIX 0
C15 1 0.498864 0.261779 0.142908 11.00000 0.04545 0.03338 =
0.03980 0.01562 0.01999 0.02785
AFIX 137
H15A 2 0.464741 0.174092 0.143237 11.00000 -1.50000
H15B 2 0.513097 0.301241 0.191511 11.00000 -1.50000
H15C 2 0.581532 0.291391 0.122639 11.00000 -1.50000
AFIX 0
C16 1 0.529494 0.710044 0.331715 11.00000 0.01577 0.01551 =
0.04335 0.00474 -0.00133 0.00448
C17 1 0.499681 0.812542 0.328272 11.00000 0.01661 0.01483 =
0.04467 0.00381 -0.00361 0.00443
C18 1 0.449062 0.850513 0.386422 11.00000 0.02742 0.01874 =
0.05027 -0.00232 -0.00941 0.01170
AFIX 43
H18 2 0.428458 0.917521 0.383931 11.00000 -1.20000
AFIX 0
C19 1 0.428765 0.790952 0.447690 11.00000 0.03139 0.02907 =
0.03797 -0.00553 -0.01131 0.01527
C20 1 0.464128 0.693586 0.451968 11.00000 0.04026 0.02891 =
0.03466 0.00020 -0.00566 0.01790
AFIX 43
H20 2 0.454539 0.655742 0.494025 11.00000 -1.20000
AFIX 0
C21 1 0.513359 0.651336 0.395167 11.00000 0.02856 0.01820 =
0.03828 0.00019 -0.00464 0.01016
C22 1 0.509826 0.873682 0.260131 11.00000 0.02939 0.02545 =
0.06163 0.01710 0.00883 0.01354
AFIX 137
H22A 2 0.514137 0.954651 0.271339 11.00000 -1.50000
H22B 2 0.433184 0.825129 0.225802 11.00000 -1.50000
H22C 2 0.588614 0.880176 0.239885 11.00000 -1.50000
AFIX 0
C23 1 0.368308 0.829783 0.509036 11.00000 0.05486 0.05047 =
0.03449 -0.00244 -0.00722 0.03493
AFIX 137
H23A 2 0.427246 0.849825 0.553112 11.00000 -1.50000
H23B 2 0.284576 0.763348 0.514295 11.00000 -1.50000
H23C 2 0.354726 0.900824 0.498642 11.00000 -1.50000
AFIX 0
C24 1 0.544160 0.541325 0.400243 11.00000 0.04995 0.02675 =
0.03674 0.00294 -0.00708 0.02256
AFIX 137
H24A 2 0.562786 0.533683 0.450162 11.00000 -1.50000
H24B 2 0.620181 0.552363 0.375800 11.00000 -1.50000
H24C 2 0.469115 0.467921 0.377998 11.00000 -1.50000
AFIX 0
C25 1 0.005813 0.391471 0.293627 11.00000 0.01363 0.02380 =
0.02867 0.00971 0.00510 0.00675
C26 1 -0.061502 0.459745 0.269170 11.00000 0.01650 0.02952 =
0.03412 0.01633 0.00600 0.00890
C27 1 -0.197145 0.415582 0.276226 11.00000 0.01796 0.04245 =
0.06196 0.02961 0.00956 0.01416
AFIX 43
H27 2 -0.243572 0.459430 0.260435 11.00000 -1.20000
AFIX 0
C28 1 -0.263173 0.308222 0.306174 11.00000 0.01727 0.04912 =
0.06933 0.03516 0.01546 0.01341
AFIX 43
H28 2 -0.354197 0.277829 0.308291 11.00000 -1.20000
AFIX 0
C29 1 -0.192815 0.245777 0.333158 11.00000 0.01971 0.03500 =
0.04770 0.02328 0.01343 0.00873
AFIX 43
H29 2 -0.237401 0.174379 0.354220 11.00000 -1.20000
AFIX 0
C30 1 -0.056879 0.287784 0.329356 11.00000 0.01933 0.02514 =
0.03336 0.01187 0.00901 0.00900
C31 1 0.007369 0.578217 0.238846 11.00000 0.01399 0.02719 =
0.03232 0.01451 0.00397 0.00787
C32 1 0.017833 0.581381 0.163892 11.00000 0.02219 0.02761 =
0.02203 0.01009 -0.00358 0.00606
C33 1 0.082937 0.695055 0.139295 11.00000 0.02850 0.04025 =
0.02967 0.01915 0.00792 0.01406
AFIX 43
H33 2 0.089697 0.697276 0.090083 11.00000 -1.20000
AFIX 0
C34 1 0.138293 0.805361 0.184842 11.00000 0.02247 0.02893 =
0.03930 0.01772 0.00903 0.01141
C35 1 0.126192 0.801187 0.257829 11.00000 0.02841 0.02881 =
0.03798 0.01064 0.00890 0.01648
AFIX 43
H35 2 0.162651 0.874438 0.289139 11.00000 -1.20000
AFIX 0
C36 1 0.060473 0.689502 0.285647 11.00000 0.02742 0.03205 =
0.03058 0.01273 0.01080 0.01889
C37 1 -0.043148 0.465721 0.112956 11.00000 0.05862 0.04420 =
0.02781 0.00497 -0.00871 -0.00127
AFIX 137
H37A 2 -0.016769 0.482919 0.065858 11.00000 -1.50000
H37B 2 -0.138203 0.432614 0.110277 11.00000 -1.50000
H37C 2 -0.013939 0.406776 0.129767 11.00000 -1.50000
AFIX 0
C38 1 0.210885 0.926681 0.156681 11.00000 0.03745 0.03383 =
0.05064 0.02120 0.00719 0.01046
AFIX 137
H38A 2 0.174133 0.982562 0.171999 11.00000 -1.50000
H38B 2 0.201541 0.914011 0.104801 11.00000 -1.50000
H38C 2 0.303365 0.960990 0.175248 11.00000 -1.50000
AFIX 0
C39 1 0.048939 0.689949 0.364846 11.00000 0.06020 0.03651 =
0.03765 0.01218 0.01925 0.02861
AFIX 137
H39A 2 0.104989 0.770651 0.389555 11.00000 -1.50000
H39B 2 0.076086 0.630723 0.383230 11.00000 -1.50000
H39C 2 -0.041662 0.668760 0.372606 11.00000 -1.50000
AFIX 0
C40 1 0.015225 0.225389 0.367624 11.00000 0.01842 0.02282 =
0.02689 0.01222 0.00912 0.00867
C41 1 -0.001250 0.107280 0.341066 11.00000 0.02038 0.02021 =
0.03666 0.00893 0.00725 0.00310
C42 1 0.056646 0.047326 0.382500 11.00000 0.02357 0.01932 =
0.04378 0.00991 0.01322 0.00696
AFIX 43
H42 2 0.044695 -0.031728 0.365178 11.00000 -1.20000
AFIX 0
C43 1 0.132310 0.102890 0.449492 11.00000 0.02141 0.02988 =
0.03686 0.01686 0.01258 0.01282
C44 1 0.148240 0.220044 0.473623 11.00000 0.02704 0.03249 =
0.03224 0.00888 0.00693 0.01323
AFIX 43
H44 2 0.199048 0.258457 0.517822 11.00000 -1.20000
AFIX 0
C45 1 0.091271 0.283369 0.434464 11.00000 0.02821 0.02304 =
0.02737 0.00694 0.00994 0.01274
C46 1 -0.077158 0.044865 0.268174 11.00000 0.04963 0.02038 =
0.05152 0.00371 -0.01222 0.00384
AFIX 137
H46A 2 -0.070976 -0.031810 0.257524 11.00000 -1.50000
H46B 2 -0.040178 0.097388 0.231873 11.00000 -1.50000
H46C 2 -0.168756 0.029189 0.268614 11.00000 -1.50000
AFIX 0
C47 1 0.196687 0.036701 0.491760 11.00000 0.02880 0.03783 =
0.05294 0.02225 0.00923 0.01806
AFIX 137
H47A 2 0.225122 0.076828 0.540535 11.00000 -1.50000
H47B 2 0.272162 0.038497 0.469635 11.00000 -1.50000
H47C 2 0.133817 -0.047416 0.492057 11.00000 -1.50000
AFIX 0
C48 1 0.110606 0.410647 0.464377 11.00000 0.05366 0.03240 =
0.02827 0.00298 0.00570 0.02361
AFIX 137
H48A 2 0.145594 0.426771 0.514584 11.00000 -1.50000
H48B 2 0.026782 0.415484 0.459424 11.00000 -1.50000
H48C 2 0.171758 0.470759 0.438177 11.00000 -1.50000
AFIX 66
MOLE 2
PART 1
C49A 1 -0.443467 -0.043909 0.076028 30.50000 0.08356 0.05172 =
0.06711 0.02359 0.03963 0.03337
AFIX 43
H49A 2 -0.457715 -0.098310 0.110554 30.50000 -1.20000
AFIX 65
C50A 1 -0.540474 -0.069174 0.018008 30.50000 0.10593 0.05629 =
0.05999 0.02625 0.04638 0.05582
AFIX 43
H50A 2 -0.619626 -0.140480 0.013715 30.50000 -1.20000
AFIX 65
C51A 1 -0.519178 0.012135 -0.033594 30.50000 0.08825 0.05764 =
0.07003 0.00654 0.03584 0.04301
AFIX 43
H51A 2 -0.584082 -0.004769 -0.072413 30.50000 -1.20000
AFIX 65
C52A 1 -0.400875 0.118711 -0.027178 30.50000 0.08356 0.05172 =
0.06711 0.02359 0.03963 0.03337
AFIX 43
H52A 2 -0.386628 0.173112 -0.061703 30.50000 -1.20000
AFIX 65
C53A 1 -0.303867 0.143977 0.030842 30.50000 0.10593 0.05629 =
0.05999 0.02625 0.04638 0.05582
AFIX 43
H53A 2 -0.224715 0.215284 0.035134 30.50000 -1.20000
AFIX 65
C54A 1 -0.325161 0.062669 0.082445 30.50000 0.08825 0.05764 =
0.07003 0.00654 0.03584 0.04301
AFIX 43
H54A 2 -0.260256 0.079574 0.121263 30.50000 -1.20000
AFIX 66
PART 2
C49B 1 -0.366869 0.007736 0.100379 -30.50000 0.08356 0.05172 =
0.06711 0.02359 0.03963 0.03337
AFIX 43
H49B 2 -0.342677 -0.019801 0.141784 -30.50000 -1.20000
AFIX 65
C50B 1 -0.490851 -0.060560 0.060701 -30.50000 0.10593 0.05629 =
0.05999 0.02625 0.04638 0.05582
AFIX 43
H50B 2 -0.549612 -0.133793 0.075559 -30.50000 -1.20000
AFIX 65
C51B 1 -0.527009 -0.019403 -0.001185 -30.50000 0.08825 0.05764 =
0.07003 0.00654 0.03584 0.04301
AFIX 43
H51B 2 -0.609961 -0.065099 -0.027732 -30.50000 -1.20000
AFIX 65
C52B 1 -0.439184 0.090051 -0.023392 -30.50000 0.08356 0.05172 =
0.06711 0.02359 0.03963 0.03337
AFIX 43
H52B 2 -0.463376 0.117587 -0.064798 -30.50000 -1.20000
AFIX 65
C53B 1 -0.315201 0.158349 0.016286 -30.50000 0.10593 0.05629 =
0.05999 0.02625 0.04638 0.05582
AFIX 43
H53B 2 -0.256441 0.231581 0.001427 -30.50000 -1.20000
AFIX 65
C54B 1 -0.279042 0.117193 0.078171 -30.50000 0.08825 0.05764 =
0.07003 0.00654 0.03584 0.04301
AFIX 43
H54B 2 -0.196089 0.162889 0.104718 -30.50000 -1.20000
AFIX 0
HKLF 4
REM ah172e in P-1
REM R1 = 0.0434 for 14357 Fo > 4sig(Fo) and 0.0522 for all 16144 data
REM 549 parameters refined using 0 restraints
END
WGHT 0.0000 9.4413
REM Highest difference peak 1.676, deepest hole -2.740, 1-sigma level 0.139
Q1 1 0.2232 0.7845 0.4270 11.00000 0.05 1.68
Q2 1 0.1167 0.2718 0.1238 11.00000 0.05 1.61
Q3 1 -0.1217 0.2876 0.0110 11.00000 0.05 1.45
Q4 1 0.4466 0.7415 0.5471 11.00000 0.05 1.17
Q5 1 0.2207 0.2352 0.2781 11.00000 0.05 1.15
Q6 1 0.4650 0.2145 0.4109 11.00000 0.05 1.12
Q7 1 0.4261 0.7140 0.1577 11.00000 0.05 1.03
Q8 1 -0.0150 0.2439 0.1123 11.00000 0.05 0.81
Q9 1 0.3778 0.2718 0.3008 11.00000 0.05 0.77
Q10 1 0.3045 0.2810 0.3208 11.00000 0.05 0.74
Q11 1 0.4845 0.5520 0.4169 11.00000 0.05 0.72
Q12 1 0.0764 0.6115 0.1492 11.00000 0.05 0.69
Q13 1 -0.2455 0.2687 -0.0319 11.00000 0.05 0.66
Q14 1 0.1329 0.1592 0.1852 11.00000 0.05 0.63
Q15 1 0.4372 0.3299 0.3783 11.00000 0.05 0.63
Q16 1 0.3560 0.2456 0.2615 11.00000 0.05 0.61
Q17 1 0.5998 0.7758 0.5537 11.00000 0.05 0.61
Q18 1 0.0826 0.9190 0.1417 11.00000 0.05 0.59
Q19 1 0.5710 0.8914 0.4311 11.00000 0.05 0.58
Q20 1 0.4620 0.7755 0.6083 11.00000 0.05 0.57
Q21 1 0.1424 0.2978 0.1900 11.00000 0.05 0.55
Q22 1 0.6350 0.7147 0.2740 11.00000 0.05 0.55
Q23 1 -0.0517 0.1660 0.0239 11.00000 0.05 0.55
Q24 1 0.4641 0.4580 0.1386 11.00000 0.05 0.54
Q25 1 0.2593 0.8100 0.4902 11.00000 0.05 0.54
;
_shelx_res_checksum 31195
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_AH172A
_database_code_depnum_ccdc_archive 'CCDC 1457708'
_audit_update_record
;
2016-03-03 deposited with the CCDC.
2016-04-07 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2013
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'0.44(C48 H50 Au2 Cl2 N2 P2), 0.56(C48 H50 Au Cl N2 P2), 0.5(C6 H6)'
_chemical_formula_sum 'C51 H53 Au1.44 Cl1.44 N2 P2'
_chemical_formula_weight 1090.92
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'
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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.2430(7)
_cell_length_b 12.0524(7)
_cell_length_c 18.7795(11)
_cell_angle_alpha 94.113(3)
_cell_angle_beta 94.288(3)
_cell_angle_gamma 114.879(3)
_cell_volume 2287.1(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 6476
_cell_measurement_theta_min 2.28
_cell_measurement_theta_max 21.77
_exptl_crystal_description rod
_exptl_crystal_colour yellow
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.584
_exptl_crystal_F_000 1083
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.310
_exptl_crystal_size_mid 0.060
_exptl_crystal_size_min 0.040
_exptl_absorpt_coefficient_mu 4.816
_shelx_estimated_absorpt_T_min 0.317
_shelx_estimated_absorpt_T_max 0.831
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6198
_exptl_absorpt_correction_T_max 0.7460
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 45356
_diffrn_reflns_av_unetI/netI 0.0672
_diffrn_reflns_av_R_equivalents 0.0649
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 1.094
_diffrn_reflns_theta_max 27.500
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total 10457
_reflns_number_gt 7898
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-2013
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
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^ > 2\s(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
'w=1/[\s^2^(Fo^2^)+10.3427P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 10457
_refine_ls_number_parameters 530
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0765
_refine_ls_R_factor_gt 0.0498
_refine_ls_wR_factor_ref 0.0932
_refine_ls_wR_factor_gt 0.0861
_refine_ls_goodness_of_fit_ref 1.095
_refine_ls_restrained_S_all 1.095
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.29788(2) 0.24808(2) 0.28424(2) 0.03287(8) Uani 1 1 d . . . . .
Au2 Au 0.06536(6) 0.26545(5) 0.13694(3) 0.0389(2) Uani 0.4413(11) 1 d . . P . .
Cl2 Cl -0.1037(6) 0.1698(4) 0.0473(3) 0.0804(17) Uani 0.4413(11) 1 d . . P . .
Cl1 Cl 0.39247(16) 0.13268(15) 0.33670(10) 0.0463(5) Uani 1 1 d . . . . .
P1 P 0.21201(15) 0.35586(14) 0.22534(10) 0.0328(4) Uani 1 1 d . . . . .
P2 P 0.25989(15) 0.57304(15) 0.28661(10) 0.0371(4) Uani 1 1 d . . . . .
N1 N 0.1434(4) 0.4316(4) 0.2826(3) 0.0280(11) Uani 1 1 d . . . . .
N2 N 0.3364(5) 0.5102(4) 0.2367(3) 0.0303(12) Uani 1 1 d . . . . .
C1 C -0.1941(6) 0.4159(7) 0.2761(4) 0.052(2) Uani 1 1 d . . . . .
H1 H -0.2417 0.4598 0.2592 0.062 Uiso 1 1 calc R U . . .
C2 C 0.3687(8) 0.8310(7) 0.5081(4) 0.057(2) Uani 1 1 d . . . . .
H2A H 0.3549 0.9032 0.4969 0.085 Uiso 1 1 calc R U . . .
H2B H 0.4290 0.8519 0.5525 0.085 Uiso 1 1 calc R U . . .
H2C H 0.2839 0.7637 0.5144 0.085 Uiso 1 1 calc R U . . .
C3 C 0.4273(7) 0.7912(6) 0.4473(4) 0.0449(17) Uani 1 1 d . . . . .
C4 C 0.4487(6) 0.8508(6) 0.3862(4) 0.0424(17) Uani 1 1 d . . . . .
H4 H 0.4289 0.9198 0.3835 0.051 Uiso 1 1 calc R U . . .
C5 C 0.4980(6) 0.8127(5) 0.3286(4) 0.0367(15) Uani 1 1 d . . . . .
C6 C 0.5267(6) 0.7109(5) 0.3324(4) 0.0343(15) Uani 1 1 d . . . . .
C7 C 0.5657(6) 0.6587(5) 0.2688(4) 0.0367(16) Uani 1 1 d . . . . .
C8 C 0.6972(6) 0.7054(6) 0.2548(4) 0.0455(18) Uani 1 1 d . . . . .
H8 H 0.7630 0.7701 0.2870 0.055 Uiso 1 1 calc R U . . .
C9 C 0.7330(7) 0.6594(7) 0.1952(5) 0.054(2) Uani 1 1 d . . . . .
H9 H 0.8227 0.6926 0.1861 0.065 Uiso 1 1 calc R U . . .
C10 C 0.5045(6) 0.5126(6) 0.1595(4) 0.0375(16) Uani 1 1 d . . . . .
C11 C 0.4064(7) 0.4149(6) 0.1071(4) 0.0416(17) Uani 1 1 d . . . . .
C12 C 0.4045(7) 0.2960(6) 0.0997(4) 0.0430(18) Uani 1 1 d . . . . .
C13 C 0.2233(9) 0.2297(8) 0.0021(5) 0.066(2) Uani 1 1 d . . . . .
C14 C 0.2290(8) 0.3476(8) 0.0101(4) 0.059(2) Uani 1 1 d . . . . .
H14 H 0.1690 0.3651 -0.0201 0.071 Uiso 1 1 calc R U . . .
C15 C 0.3195(8) 0.4410(7) 0.0609(4) 0.0467(18) Uani 1 1 d . . . . .
C16 C 0.3261(8) 0.5678(7) 0.0643(4) 0.060(2) Uani 1 1 d . . . . .
H16A H 0.3074 0.5908 0.1119 0.089 Uiso 1 1 calc R U . . .
H16B H 0.2608 0.5696 0.0274 0.089 Uiso 1 1 calc R U . . .
H16C H 0.4146 0.6262 0.0559 0.089 Uiso 1 1 calc R U . . .
C17 C 0.5011(7) 0.2665(6) 0.1446(4) 0.0496(19) Uani 1 1 d . . . . .
H17A H 0.4660 0.1772 0.1455 0.074 Uiso 1 1 calc R U . . .
H17B H 0.5155 0.3069 0.1937 0.074 Uiso 1 1 calc R U . . .
H17C H 0.5851 0.2961 0.1239 0.074 Uiso 1 1 calc R U . . .
C18 C 0.4699(6) 0.5606(5) 0.2213(4) 0.0321(15) Uani 1 1 d . . . . .
C20 C 0.5110(7) 0.8758(6) 0.2607(4) 0.0490(19) Uani 1 1 d . . . . .
H20A H 0.5963 0.8911 0.2438 0.073 Uiso 1 1 calc R U . . .
H20B H 0.5053 0.9543 0.2709 0.073 Uiso 1 1 calc R U . . .
H20C H 0.4396 0.8229 0.2235 0.073 Uiso 1 1 calc R U . . .
C22 C -0.2597(6) 0.3095(7) 0.3063(5) 0.058(2) Uani 1 1 d . . . . .
H22 H -0.3520 0.2787 0.3090 0.070 Uiso 1 1 calc R U . . .
C23 C -0.0770(8) 0.0471(6) 0.2696(4) 0.059(2) Uani 1 1 d . . . . .
H23A H -0.1710 0.0244 0.2724 0.088 Uiso 1 1 calc R U . . .
H23B H -0.0645 -0.0271 0.2563 0.088 Uiso 1 1 calc R U . . .
H23C H -0.0459 0.1039 0.2332 0.088 Uiso 1 1 calc R U . . .
C25 C -0.0448(8) 0.4710(7) 0.1139(4) 0.062(2) Uani 1 1 d . . . . .
H25A H -0.0294 0.4049 0.1343 0.093 Uiso 1 1 calc R U . . .
H25B H -0.0059 0.4864 0.0686 0.093 Uiso 1 1 calc R U . . .
H25C H -0.1399 0.4466 0.1050 0.093 Uiso 1 1 calc R U . . .
C26 C 0.0168(6) 0.5840(6) 0.1649(4) 0.0350(15) Uani 1 1 d . . . . .
C27 C 0.0076(5) 0.5805(6) 0.2397(3) 0.0313(14) Uani 1 1 d . . . . .
C28 C 0.0609(6) 0.6904(6) 0.2860(4) 0.0357(15) Uani 1 1 d . . . . .
C29 C 0.1263(6) 0.8028(6) 0.2588(4) 0.0372(15) Uani 1 1 d . . . . .
H29 H 0.1635 0.8767 0.2908 0.045 Uiso 1 1 calc R U . . .
C30 C 0.1379(6) 0.8086(6) 0.1858(4) 0.0392(16) Uani 1 1 d . . . . .
C32 C 0.0817(6) 0.6999(6) 0.1409(4) 0.0412(16) Uani 1 1 d . . . . .
H32 H 0.0871 0.7036 0.0908 0.049 Uiso 1 1 calc R U . . .
C33 C -0.0605(6) 0.4611(6) 0.2696(3) 0.0351(15) Uani 1 1 d . . . . .
C34 C 0.0081(5) 0.3948(5) 0.2942(3) 0.0278(13) Uani 1 1 d . . . . .
C35 C -0.0557(6) 0.2888(6) 0.3291(4) 0.0359(15) Uani 1 1 d . . . . .
C36 C -0.1897(6) 0.2478(6) 0.3329(4) 0.0445(18) Uani 1 1 d . . . . .
H36 H -0.2350 0.1749 0.3546 0.053 Uiso 1 1 calc R U . . .
C37 C 0.0156(5) 0.2265(5) 0.3672(3) 0.0309(14) Uani 1 1 d . . . . .
C38 C 0.0923(6) 0.2840(6) 0.4341(4) 0.0347(15) Uani 1 1 d . . . . .
C39 C 0.1104(8) 0.4099(6) 0.4641(4) 0.0523(19) Uani 1 1 d . . . . .
H39A H 0.1515 0.4278 0.5140 0.078 Uiso 1 1 calc R U . . .
H39B H 0.0243 0.4125 0.4624 0.078 Uiso 1 1 calc R U . . .
H39C H 0.1673 0.4715 0.4354 0.078 Uiso 1 1 calc R U . . .
C40 C 0.1485(6) 0.2205(6) 0.4728(4) 0.0426(17) Uani 1 1 d . . . . .
H40 H 0.1999 0.2593 0.5175 0.051 Uiso 1 1 calc R U . . .
C41 C 0.1329(6) 0.1035(6) 0.4490(4) 0.0421(18) Uani 1 1 d . . . . .
C42 C 0.1966(7) 0.0385(7) 0.4905(5) 0.059(2) Uani 1 1 d . . . . .
H42A H 0.2268 0.0801 0.5396 0.088 Uiso 1 1 calc R U . . .
H42B H 0.2723 0.0396 0.4674 0.088 Uiso 1 1 calc R U . . .
H42C H 0.1328 -0.0469 0.4920 0.088 Uiso 1 1 calc R U . . .
C43 C 0.0582(6) 0.0509(6) 0.3840(4) 0.0426(17) Uani 1 1 d . . . . .
H43 H 0.0453 -0.0300 0.3670 0.051 Uiso 1 1 calc R U . . .
C44 C 0.0004(6) 0.1086(5) 0.3416(4) 0.0372(16) Uani 1 1 d . . . . .
C45 C 0.5100(7) 0.6513(6) 0.3953(4) 0.0408(17) Uani 1 1 d . . . . .
C46 C 0.4603(7) 0.6925(6) 0.4518(4) 0.0444(17) Uani 1 1 d . . . . .
H46 H 0.4486 0.6527 0.4943 0.053 Uiso 1 1 calc R U . . .
C48 C 0.3128(8) 0.2062(7) 0.0469(4) 0.055(2) Uani 1 1 d . . . . .
H48 H 0.3117 0.1267 0.0414 0.066 Uiso 1 1 calc R U . . .
C49 C 0.1254(11) 0.1304(8) -0.0545(5) 0.102(4) Uani 1 1 d . . . . .
H49A H 0.1286 0.1636 -0.1008 0.153 Uiso 1 1 calc R U . . .
H49B H 0.0362 0.1032 -0.0403 0.153 Uiso 1 1 calc R U . . .
H49C H 0.1483 0.0604 -0.0589 0.153 Uiso 1 1 calc R U . . .
C50 C 0.6370(7) 0.5637(7) 0.1483(5) 0.052(2) Uani 1 1 d . . . . .
H50 H 0.6627 0.5323 0.1073 0.063 Uiso 1 1 calc R U . . .
C51 C 0.2103(8) 0.9320(7) 0.1576(4) 0.060(2) Uani 1 1 d . . . . .
H51A H 0.3002 0.9736 0.1825 0.090 Uiso 1 1 calc R U . . .
H51B H 0.1633 0.9832 0.1662 0.090 Uiso 1 1 calc R U . . .
H51C H 0.2142 0.9186 0.1059 0.090 Uiso 1 1 calc R U . . .
C52 C 0.0520(8) 0.6900(7) 0.3651(4) 0.053(2) Uani 1 1 d . . . . .
H52A H 0.1175 0.7686 0.3904 0.079 Uiso 1 1 calc R U . . .
H52B H 0.0693 0.6225 0.3820 0.079 Uiso 1 1 calc R U . . .
H52C H -0.0366 0.6786 0.3748 0.079 Uiso 1 1 calc R U . . .
C54 C 0.5388(7) 0.5400(6) 0.4006(4) 0.0482(18) Uani 1 1 d . . . . .
H54A H 0.4622 0.4660 0.3782 0.072 Uiso 1 1 calc R U . . .
H54B H 0.5571 0.5315 0.4512 0.072 Uiso 1 1 calc R U . . .
H54C H 0.6158 0.5505 0.3757 0.072 Uiso 1 1 calc R U . . .
C100 C 0.5287(14) -0.0082(16) 0.0330(9) 0.115(8) Uiso 0.5 1 d G . P . .
H100 H 0.5953 0.0101 0.0720 0.138 Uiso 0.5 1 calc R U P . .
C101 C 0.4117(15) -0.1147(14) 0.0282(8) 0.113(9) Uiso 0.5 1 d G . P . .
H101 H 0.3983 -0.1692 0.0641 0.136 Uiso 0.5 1 calc R U P . .
C102 C 0.3144(11) -0.1416(11) -0.0289(9) 0.098(7) Uiso 0.5 1 d G . P . .
H102 H 0.2344 -0.2144 -0.0322 0.118 Uiso 0.5 1 calc R U P . .
C103 C 0.3341(13) -0.0619(14) -0.0814(7) 0.133(9) Uiso 0.5 1 d G . P . .
H103 H 0.2675 -0.0802 -0.1205 0.159 Uiso 0.5 1 calc R U P . .
C104 C 0.4511(15) 0.0447(13) -0.0767(8) 0.106(7) Uiso 0.5 1 d G . P . .
H104 H 0.4646 0.0991 -0.1126 0.127 Uiso 0.5 1 calc R U P . .
C105 C 0.5484(12) 0.0715(13) -0.0195(10) 0.078(6) Uiso 0.5 1 d G . P . .
H105 H 0.6284 0.1443 -0.0163 0.093 Uiso 0.5 1 calc R U P . .
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 0.02742(12) 0.02728(13) 0.04880(17) 0.01334(11) 0.01293(11) 0.01368(10)
Au2 0.0510(4) 0.0302(3) 0.0343(4) 0.0015(3) 0.0024(3) 0.0172(3)
Cl2 0.112(4) 0.053(3) 0.059(3) -0.017(2) -0.036(3) 0.030(3)
Cl1 0.0342(8) 0.0454(10) 0.0692(13) 0.0257(9) 0.0128(8) 0.0226(8)
P1 0.0277(8) 0.0255(8) 0.0470(11) 0.0064(8) 0.0088(7) 0.0120(7)
P2 0.0240(8) 0.0273(9) 0.0569(12) -0.0011(8) 0.0125(8) 0.0079(7)
N1 0.028(3) 0.028(3) 0.032(3) 0.008(2) 0.011(2) 0.013(2)
N2 0.027(3) 0.024(3) 0.043(3) 0.009(2) 0.011(2) 0.012(2)
C1 0.026(3) 0.059(5) 0.078(6) 0.032(4) 0.012(4) 0.021(3)
C2 0.077(6) 0.067(5) 0.041(5) -0.006(4) -0.005(4) 0.048(5)
C3 0.049(4) 0.043(4) 0.043(5) -0.007(3) -0.011(3) 0.024(3)
C4 0.036(4) 0.025(3) 0.061(5) -0.006(3) -0.018(3) 0.014(3)
C5 0.028(3) 0.024(3) 0.053(5) 0.007(3) -0.004(3) 0.007(3)
C6 0.024(3) 0.021(3) 0.052(4) 0.004(3) -0.005(3) 0.005(3)
C7 0.025(3) 0.028(3) 0.061(5) 0.015(3) 0.011(3) 0.012(3)
C8 0.023(3) 0.034(4) 0.077(6) 0.018(4) 0.007(3) 0.007(3)
C9 0.031(4) 0.047(4) 0.098(7) 0.040(5) 0.035(4) 0.020(4)
C10 0.036(3) 0.033(4) 0.054(5) 0.021(3) 0.020(3) 0.020(3)
C11 0.051(4) 0.049(4) 0.040(4) 0.021(4) 0.027(3) 0.031(4)
C12 0.051(4) 0.051(4) 0.044(5) 0.024(4) 0.032(4) 0.031(4)
C13 0.087(6) 0.054(5) 0.049(5) 0.020(4) 0.014(5) 0.020(5)
C14 0.077(6) 0.063(5) 0.044(5) 0.030(4) 0.010(4) 0.033(5)
C15 0.059(5) 0.053(5) 0.041(5) 0.020(4) 0.022(4) 0.032(4)
C16 0.080(6) 0.062(5) 0.060(6) 0.031(4) 0.019(4) 0.047(5)
C17 0.065(5) 0.043(4) 0.060(5) 0.022(4) 0.031(4) 0.035(4)
C18 0.025(3) 0.025(3) 0.052(4) 0.018(3) 0.017(3) 0.012(3)
C20 0.044(4) 0.029(4) 0.077(6) 0.015(4) 0.011(4) 0.016(3)
C22 0.023(3) 0.061(5) 0.097(7) 0.041(5) 0.026(4) 0.016(3)
C23 0.060(5) 0.028(4) 0.071(6) 0.002(4) -0.007(4) 0.005(4)
C25 0.074(6) 0.049(5) 0.037(5) 0.004(4) -0.007(4) 0.005(4)
C26 0.028(3) 0.034(4) 0.038(4) 0.009(3) -0.003(3) 0.009(3)
C27 0.024(3) 0.036(4) 0.038(4) 0.014(3) 0.005(3) 0.016(3)
C28 0.035(3) 0.040(4) 0.042(4) 0.017(3) 0.012(3) 0.022(3)
C29 0.036(3) 0.038(4) 0.042(4) 0.003(3) 0.004(3) 0.021(3)
C30 0.031(3) 0.037(4) 0.053(5) 0.017(3) 0.010(3) 0.014(3)
C32 0.038(4) 0.052(4) 0.040(4) 0.019(4) 0.010(3) 0.021(3)
C33 0.027(3) 0.041(4) 0.038(4) 0.019(3) 0.008(3) 0.013(3)
C34 0.020(3) 0.028(3) 0.032(4) 0.009(3) 0.007(2) 0.005(2)
C35 0.028(3) 0.034(3) 0.046(4) 0.014(3) 0.011(3) 0.011(3)
C36 0.027(3) 0.040(4) 0.066(5) 0.026(4) 0.016(3) 0.009(3)
C37 0.024(3) 0.033(3) 0.037(4) 0.015(3) 0.015(3) 0.010(3)
C38 0.033(3) 0.037(4) 0.036(4) 0.012(3) 0.013(3) 0.014(3)
C39 0.070(5) 0.050(5) 0.045(5) 0.012(4) 0.015(4) 0.032(4)
C40 0.038(4) 0.047(4) 0.043(4) 0.018(3) 0.010(3) 0.017(3)
C41 0.031(3) 0.046(4) 0.058(5) 0.029(4) 0.022(3) 0.018(3)
C42 0.044(4) 0.056(5) 0.082(6) 0.033(5) 0.012(4) 0.023(4)
C43 0.034(4) 0.034(4) 0.062(5) 0.015(4) 0.019(4) 0.014(3)
C44 0.034(3) 0.025(3) 0.050(5) 0.010(3) 0.013(3) 0.008(3)
C45 0.046(4) 0.033(4) 0.045(4) -0.004(3) -0.012(3) 0.022(3)
C46 0.053(4) 0.038(4) 0.041(4) 0.003(3) -0.007(3) 0.020(3)
C48 0.084(6) 0.043(4) 0.041(5) 0.012(4) 0.018(4) 0.028(4)
C49 0.146(10) 0.058(6) 0.069(7) -0.001(5) -0.027(7) 0.021(7)
C50 0.045(4) 0.054(5) 0.078(6) 0.036(4) 0.039(4) 0.030(4)
C51 0.056(5) 0.058(5) 0.061(6) 0.024(4) 0.009(4) 0.017(4)
C52 0.074(5) 0.050(5) 0.043(5) 0.010(4) 0.019(4) 0.032(4)
C54 0.059(5) 0.037(4) 0.055(5) 0.011(4) 0.000(4) 0.026(4)
#==============================================================================
# MOLECULAR GEOMETRY
_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 P1 2.2238(16) . ?
Au1 Cl1 2.3066(15) . ?
Au2 P1 2.1169(19) . ?
Au2 Cl2 2.275(5) . ?
Cl2 C102 2.24(4) 2 ?
P1 N1 1.777(5) . ?
P1 N2 1.781(5) . ?
P1 P2 2.599(2) . ?
P2 N1 1.648(5) . ?
P2 N2 1.660(5) . ?
N1 C34 1.434(7) . ?
N2 C18 1.425(7) . ?
C1 C22 1.372(9) . ?
C1 C33 1.385(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.505(10) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.381(10) . ?
C3 C46 1.392(9) . ?
C4 C5 1.385(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(8) . ?
C5 C20 1.518(9) . ?
C6 C45 1.410(9) . ?
C6 C7 1.489(9) . ?
C7 C8 1.396(8) . ?
C7 C18 1.411(9) . ?
C8 C9 1.375(10) . ?
C8 H8 0.9500 . ?
C9 C50 1.391(11) . ?
C9 H9 0.9500 . ?
C10 C50 1.392(8) . ?
C10 C18 1.411(9) . ?
C10 C11 1.466(10) . ?
C11 C15 1.407(9) . ?
C11 C12 1.422(9) . ?
C12 C48 1.405(10) . ?
C12 C17 1.499(9) . ?
C13 C14 1.391(11) . ?
C13 C48 1.397(11) . ?
C13 C49 1.518(12) . ?
C14 C15 1.396(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.494(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C22 C36 1.382(9) . ?
C22 H22 0.9500 . ?
C23 C44 1.508(10) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C25 C26 1.473(9) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C32 1.403(8) . ?
C26 C27 1.419(9) . ?
C27 C28 1.399(9) . ?
C27 C33 1.491(8) . ?
C28 C29 1.398(8) . ?
C28 C52 1.497(9) . ?
C29 C30 1.391(9) . ?
C29 H29 0.9500 . ?
C30 C32 1.375(9) . ?
C30 C51 1.521(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.403(8) . ?
C34 C35 1.412(8) . ?
C35 C36 1.383(8) . ?
C35 C37 1.488(8) . ?
C36 H36 0.9500 . ?
C37 C44 1.401(8) . ?
C37 C38 1.419(9) . ?
C38 C40 1.390(8) . ?
C38 C39 1.503(9) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.382(9) . ?
C40 H40 0.9500 . ?
C41 C43 1.374(10) . ?
C41 C42 1.486(9) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.386(9) . ?
C43 H43 0.9500 . ?
C45 C46 1.390(9) . ?
C45 C54 1.514(8) . ?
C46 H46 0.9500 . ?
C48 H48 0.9500 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C100 C101 1.3900 . ?
C100 C105 1.3900 . ?
C100 H100 0.9500 . ?
C101 C102 1.3900 . ?
C101 H101 0.9500 . ?
C102 C103 1.3900 . ?
C102 Cl2 2.242(14) 2 ?
C102 H102 0.9500 . ?
C103 C104 1.3900 . ?
C103 H103 0.9500 . ?
C104 C105 1.3900 . ?
C104 H104 0.9500 . ?
C105 H105 0.9500 . ?
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
P1 Au1 Cl1 175.36(7) . . ?
P1 Au2 Cl2 175.58(17) . . ?
C102 Cl2 Au2 135(2) 2 . ?
N1 P1 N2 78.0(2) . . ?
N1 P1 Au2 105.39(17) . . ?
N2 P1 Au2 127.95(18) . . ?
N1 P1 Au1 112.60(17) . . ?
N2 P1 Au1 105.84(17) . . ?
Au2 P1 Au1 119.01(7) . . ?
N1 P1 P2 38.83(15) . . ?
N2 P1 P2 39.22(15) . . ?
Au2 P1 P2 122.76(8) . . ?
Au1 P1 P2 116.79(9) . . ?
N1 P2 N2 85.2(2) . . ?
N1 P2 P1 42.55(16) . . ?
N2 P2 P1 42.73(17) . . ?
C34 N1 P2 127.4(4) . . ?
C34 N1 P1 128.9(4) . . ?
P2 N1 P1 98.6(2) . . ?
C18 N2 P2 129.7(4) . . ?
C18 N2 P1 131.1(4) . . ?
P2 N2 P1 98.1(2) . . ?
C22 C1 C33 121.8(6) . . ?
C22 C1 H1 119.1 . . ?
C33 C1 H1 119.1 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C46 118.8(7) . . ?
C4 C3 C2 121.0(6) . . ?
C46 C3 C2 120.3(7) . . ?
C3 C4 C5 121.8(6) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C4 C5 C6 119.2(6) . . ?
C4 C5 C20 119.7(6) . . ?
C6 C5 C20 121.0(6) . . ?
C5 C6 C45 120.0(6) . . ?
C5 C6 C7 120.8(6) . . ?
C45 C6 C7 119.1(5) . . ?
C8 C7 C18 118.5(6) . . ?
C8 C7 C6 121.1(6) . . ?
C18 C7 C6 120.3(5) . . ?
C9 C8 C7 121.2(7) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C50 119.5(6) . . ?
C8 C9 H9 120.2 . . ?
C50 C9 H9 120.2 . . ?
C50 C10 C18 117.5(7) . . ?
C50 C10 C11 119.9(6) . . ?
C18 C10 C11 122.5(5) . . ?
C15 C11 C12 119.8(7) . . ?
C15 C11 C10 119.9(6) . . ?
C12 C11 C10 120.1(6) . . ?
C48 C12 C11 118.6(7) . . ?
C48 C12 C17 119.7(6) . . ?
C11 C12 C17 121.6(7) . . ?
C14 C13 C48 117.7(8) . . ?
C14 C13 C49 121.5(8) . . ?
C48 C13 C49 120.8(8) . . ?
C13 C14 C15 122.6(8) . . ?
C13 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C14 C15 C11 119.1(7) . . ?
C14 C15 C16 120.2(7) . . ?
C11 C15 C16 120.7(7) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C7 C18 C10 121.1(5) . . ?
C7 C18 N2 118.6(5) . . ?
C10 C18 N2 120.2(6) . . ?
C5 C20 H20A 109.5 . . ?
C5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C1 C22 C36 119.1(6) . . ?
C1 C22 H22 120.5 . . ?
C36 C22 H22 120.5 . . ?
C44 C23 H23A 109.5 . . ?
C44 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C44 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C32 C26 C27 117.3(6) . . ?
C32 C26 C25 121.2(6) . . ?
C27 C26 C25 121.4(6) . . ?
C28 C27 C26 119.8(5) . . ?
C28 C27 C33 119.5(6) . . ?
C26 C27 C33 120.8(6) . . ?
C29 C28 C27 120.0(6) . . ?
C29 C28 C52 118.9(6) . . ?
C27 C28 C52 121.1(6) . . ?
C30 C29 C28 121.3(6) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C32 C30 C29 117.8(6) . . ?
C32 C30 C51 121.9(7) . . ?
C29 C30 C51 120.3(7) . . ?
C30 C32 C26 123.7(6) . . ?
C30 C32 H32 118.1 . . ?
C26 C32 H32 118.1 . . ?
C1 C33 C34 118.4(5) . . ?
C1 C33 C27 119.7(5) . . ?
C34 C33 C27 121.8(5) . . ?
C33 C34 C35 120.8(5) . . ?
C33 C34 N1 120.4(5) . . ?
C35 C34 N1 118.8(5) . . ?
C36 C35 C34 117.6(5) . . ?
C36 C35 C37 118.8(5) . . ?
C34 C35 C37 123.4(5) . . ?
C22 C36 C35 122.1(6) . . ?
C22 C36 H36 118.9 . . ?
C35 C36 H36 118.9 . . ?
C44 C37 C38 119.3(6) . . ?
C44 C37 C35 121.7(6) . . ?
C38 C37 C35 118.8(5) . . ?
C40 C38 C37 118.7(6) . . ?
C40 C38 C39 120.1(6) . . ?
C37 C38 C39 121.2(6) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C38 122.9(7) . . ?
C41 C40 H40 118.5 . . ?
C38 C40 H40 118.5 . . ?
C43 C41 C40 116.7(6) . . ?
C43 C41 C42 121.4(7) . . ?
C40 C41 C42 121.9(7) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 C44 124.0(6) . . ?
C41 C43 H43 118.0 . . ?
C44 C43 H43 118.0 . . ?
C43 C44 C37 118.4(7) . . ?
C43 C44 C23 121.3(6) . . ?
C37 C44 C23 120.3(6) . . ?
C46 C45 C6 118.9(6) . . ?
C46 C45 C54 119.9(6) . . ?
C6 C45 C54 121.1(6) . . ?
C45 C46 C3 121.3(7) . . ?
C45 C46 H46 119.4 . . ?
C3 C46 H46 119.4 . . ?
C13 C48 C12 122.2(7) . . ?
C13 C48 H48 118.9 . . ?
C12 C48 H48 118.9 . . ?
C13 C49 H49A 109.5 . . ?
C13 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C13 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C9 C50 C10 122.0(7) . . ?
C9 C50 H50 119.0 . . ?
C10 C50 H50 119.0 . . ?
C30 C51 H51A 109.5 . . ?
C30 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C30 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C28 C52 H52A 109.5 . . ?
C28 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C28 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C45 C54 H54A 109.5 . . ?
C45 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C45 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C101 C100 C105 120.0 . . ?
C101 C100 H100 120.0 . . ?
C105 C100 H100 120.0 . . ?
C100 C101 C102 120.0 . . ?
C100 C101 H101 120.0 . . ?
C102 C101 H101 120.0 . . ?
C101 C102 C103 120.0 . . ?
C101 C102 Cl2 138.7(8) . 2 ?
C103 C102 Cl2 84.3(8) . 2 ?
C101 C102 H102 120.0 . . ?
C103 C102 H102 120.0 . . ?
Cl2 C102 H102 49.3 2 . ?
C104 C103 C102 120.0 . . ?
C104 C103 H103 120.0 . . ?
C102 C103 H103 120.0 . . ?
C105 C104 C103 120.0 . . ?
C105 C104 H104 120.0 . . ?
C103 C104 H104 120.0 . . ?
C104 C105 C100 120.0 . . ?
C104 C105 H105 120.0 . . ?
C100 C105 H105 120.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P2 N1 C34 -159.1(5) . . . . ?
P1 P2 N1 C34 -156.1(6) . . . . ?
N2 P2 N1 P1 -3.0(3) . . . . ?
N2 P1 N1 C34 158.4(5) . . . . ?
Au2 P1 N1 C34 32.0(5) . . . . ?
Au1 P1 N1 C34 -99.2(5) . . . . ?
P2 P1 N1 C34 155.6(6) . . . . ?
N2 P1 N1 P2 2.8(2) . . . . ?
Au2 P1 N1 P2 -123.59(19) . . . . ?
Au1 P1 N1 P2 105.2(2) . . . . ?
N1 P2 N2 C18 -165.8(5) . . . . ?
P1 P2 N2 C18 -168.7(7) . . . . ?
N1 P2 N2 P1 3.0(3) . . . . ?
N1 P1 N2 C18 165.7(6) . . . . ?
Au2 P1 N2 C18 -94.0(5) . . . . ?
Au1 P1 N2 C18 55.3(6) . . . . ?
P2 P1 N2 C18 168.5(7) . . . . ?
N1 P1 N2 P2 -2.8(2) . . . . ?
Au2 P1 N2 P2 97.5(3) . . . . ?
Au1 P1 N2 P2 -113.2(2) . . . . ?
C46 C3 C4 C5 2.0(10) . . . . ?
C2 C3 C4 C5 -177.6(6) . . . . ?
C3 C4 C5 C6 0.2(10) . . . . ?
C3 C4 C5 C20 175.9(6) . . . . ?
C4 C5 C6 C45 -2.4(9) . . . . ?
C20 C5 C6 C45 -178.0(6) . . . . ?
C4 C5 C6 C7 173.2(6) . . . . ?
C20 C5 C6 C7 -2.4(9) . . . . ?
C5 C6 C7 C8 86.4(8) . . . . ?
C45 C6 C7 C8 -97.8(7) . . . . ?
C5 C6 C7 C18 -93.6(7) . . . . ?
C45 C6 C7 C18 82.2(8) . . . . ?
C18 C7 C8 C9 1.6(9) . . . . ?
C6 C7 C8 C9 -178.4(6) . . . . ?
C7 C8 C9 C50 -0.7(10) . . . . ?
C50 C10 C11 C15 -106.2(7) . . . . ?
C18 C10 C11 C15 72.2(8) . . . . ?
C50 C10 C11 C12 69.7(8) . . . . ?
C18 C10 C11 C12 -112.0(7) . . . . ?
C15 C11 C12 C48 -1.4(9) . . . . ?
C10 C11 C12 C48 -177.3(6) . . . . ?
C15 C11 C12 C17 176.0(6) . . . . ?
C10 C11 C12 C17 0.1(9) . . . . ?
C48 C13 C14 C15 -0.3(12) . . . . ?
C49 C13 C14 C15 -178.9(8) . . . . ?
C13 C14 C15 C11 -1.7(11) . . . . ?
C13 C14 C15 C16 176.5(7) . . . . ?
C12 C11 C15 C14 2.5(10) . . . . ?
C10 C11 C15 C14 178.4(6) . . . . ?
C12 C11 C15 C16 -175.7(6) . . . . ?
C10 C11 C15 C16 0.2(10) . . . . ?
C8 C7 C18 C10 -2.1(9) . . . . ?
C6 C7 C18 C10 177.9(5) . . . . ?
C8 C7 C18 N2 178.1(5) . . . . ?
C6 C7 C18 N2 -1.9(8) . . . . ?
C50 C10 C18 C7 1.6(9) . . . . ?
C11 C10 C18 C7 -176.8(5) . . . . ?
C50 C10 C18 N2 -178.5(5) . . . . ?
C11 C10 C18 N2 3.1(9) . . . . ?
P2 N2 C18 C7 22.5(8) . . . . ?
P1 N2 C18 C7 -142.6(5) . . . . ?
P2 N2 C18 C10 -157.4(5) . . . . ?
P1 N2 C18 C10 37.5(8) . . . . ?
C33 C1 C22 C36 2.0(13) . . . . ?
C32 C26 C27 C28 0.8(8) . . . . ?
C25 C26 C27 C28 -176.4(6) . . . . ?
C32 C26 C27 C33 179.6(5) . . . . ?
C25 C26 C27 C33 2.4(9) . . . . ?
C26 C27 C28 C29 -1.8(8) . . . . ?
C33 C27 C28 C29 179.3(5) . . . . ?
C26 C27 C28 C52 179.5(6) . . . . ?
C33 C27 C28 C52 0.7(8) . . . . ?
C27 C28 C29 C30 1.1(9) . . . . ?
C52 C28 C29 C30 179.8(6) . . . . ?
C28 C29 C30 C32 0.7(9) . . . . ?
C28 C29 C30 C51 -179.6(6) . . . . ?
C29 C30 C32 C26 -1.8(9) . . . . ?
C51 C30 C32 C26 178.4(6) . . . . ?
C27 C26 C32 C30 1.1(9) . . . . ?
C25 C26 C32 C30 178.3(6) . . . . ?
C22 C1 C33 C34 0.6(12) . . . . ?
C22 C1 C33 C27 -176.9(7) . . . . ?
C28 C27 C33 C1 88.2(8) . . . . ?
C26 C27 C33 C1 -90.6(8) . . . . ?
C28 C27 C33 C34 -89.2(8) . . . . ?
C26 C27 C33 C34 92.0(8) . . . . ?
C1 C33 C34 C35 -4.1(10) . . . . ?
C27 C33 C34 C35 173.3(6) . . . . ?
C1 C33 C34 N1 174.2(6) . . . . ?
C27 C33 C34 N1 -8.4(10) . . . . ?
P2 N1 C34 C33 38.3(8) . . . . ?
P1 N1 C34 C33 -110.8(6) . . . . ?
P2 N1 C34 C35 -143.4(5) . . . . ?
P1 N1 C34 C35 67.5(7) . . . . ?
C33 C34 C35 C36 5.0(10) . . . . ?
N1 C34 C35 C36 -173.3(6) . . . . ?
C33 C34 C35 C37 -169.5(6) . . . . ?
N1 C34 C35 C37 12.2(10) . . . . ?
C1 C22 C36 C35 -1.0(13) . . . . ?
C34 C35 C36 C22 -2.4(11) . . . . ?
C37 C35 C36 C22 172.3(7) . . . . ?
C36 C35 C37 C44 73.2(9) . . . . ?
C34 C35 C37 C44 -112.4(7) . . . . ?
C36 C35 C37 C38 -101.4(7) . . . . ?
C34 C35 C37 C38 72.9(8) . . . . ?
C44 C37 C38 C40 -0.9(8) . . . . ?
C35 C37 C38 C40 173.9(5) . . . . ?
C44 C37 C38 C39 -179.4(6) . . . . ?
C35 C37 C38 C39 -4.6(8) . . . . ?
C37 C38 C40 C41 -0.1(9) . . . . ?
C39 C38 C40 C41 178.4(6) . . . . ?
C38 C40 C41 C43 0.2(9) . . . . ?
C38 C40 C41 C42 178.5(6) . . . . ?
C40 C41 C43 C44 0.8(9) . . . . ?
C42 C41 C43 C44 -177.6(6) . . . . ?
C41 C43 C44 C37 -1.8(9) . . . . ?
C41 C43 C44 C23 178.1(6) . . . . ?
C38 C37 C44 C43 1.8(9) . . . . ?
C35 C37 C44 C43 -172.9(5) . . . . ?
C38 C37 C44 C23 -178.1(6) . . . . ?
C35 C37 C44 C23 7.3(9) . . . . ?
C5 C6 C45 C46 2.4(10) . . . . ?
C7 C6 C45 C46 -173.3(6) . . . . ?
C5 C6 C45 C54 179.3(6) . . . . ?
C7 C6 C45 C54 3.6(9) . . . . ?
C6 C45 C46 C3 -0.2(10) . . . . ?
C54 C45 C46 C3 -177.1(6) . . . . ?
C4 C3 C46 C45 -2.0(11) . . . . ?
C2 C3 C46 C45 177.6(7) . . . . ?
C14 C13 C48 C12 1.4(12) . . . . ?
C49 C13 C48 C12 -180.0(8) . . . . ?
C11 C12 C48 C13 -0.5(10) . . . . ?
C17 C12 C48 C13 -178.0(7) . . . . ?
C8 C9 C50 C10 0.2(10) . . . . ?
C18 C10 C50 C9 -0.7(9) . . . . ?
C11 C10 C50 C9 177.8(6) . . . . ?
C105 C100 C101 C102 0.0 . . . . ?
C100 C101 C102 C103 0.0 . . . . ?
C100 C101 C102 Cl2 -118.9(11) . . . 2 ?
C101 C102 C103 C104 0.0 . . . . ?
Cl2 C102 C103 C104 144.5(8) 2 . . . ?
C102 C103 C104 C105 0.0 . . . . ?
C103 C104 C105 C100 0.0 . . . . ?
C101 C100 C105 C104 0.0 . . . . ?
_refine_diff_density_max 1.135
_refine_diff_density_min -1.108
_refine_diff_density_rms 0.131
_shelxl_version_number 2013-4
_shelx_res_file
;
TITL a1 in P-1
CELL 0.71073 11.2430 12.0524 18.7795 94.113 94.288 114.879
ZERR 2.00 0.0007 0.0007 0.0011 0.003 0.003 0.003
LATT 1
SFAC C N P CL AU H
UNIT 102 4 4 2.883 2.883 106
LIST 4
TEMP -99.960
SIZE 0.040 0.060 0.310
OMIT -3 55
OMIT -1 -2 2
OMIT -1 -1 1
OMIT 2 3 3
OMIT 2 -2 1
OMIT 3 3 2
OMIT 2 -2 2
OMIT 0 4 6
OMIT 2 4 4
OMIT 2 5 3
OMIT -3 4 2
ACTA
L.S. 8
FMAP 2
PLAN 40
HTAB
BOND $H
CONF
EQIV $1 1-x, -y, -z
FREE C100 C100_$1
FREE C100 C101_$1
FREE C100 C102_$1
FREE C100 C103_$1
FREE C100 C104_$1
FREE C100 C105_$1
FREE C101 C100_$1
FREE C101 C101_$1
FREE C101 C102_$1
FREE C101 C103_$1
FREE C101 C104_$1
FREE C101 C105_$1
FREE C102 C100_$1
FREE C102 C101_$1
FREE C102 C102_$1
FREE C102 C103_$1
FREE C102 C104_$1
FREE C102 C105_$1
FREE C103 C100_$1
FREE C103 C101_$1
FREE C103 C102_$1
FREE C103 C103_$1
FREE C103 C104_$1
FREE C103 C105_$1
FREE C104 C100_$1
FREE C104 C101_$1
FREE C104 C102_$1
FREE C104 C103_$1
FREE C104 C104_$1
FREE C104 C105_$1
FREE C105 C100_$1
FREE C105 C101_$1
FREE C105 C102_$1
FREE C105 C103_$1
FREE C105 C104_$1
FREE C105 C105_$1
ACTA
WGHT 0.000000 10.342700
FVAR 0.07661 0.44129
AU1 5 0.297883 0.248078 0.284241 11.00000 0.02742 0.02728 =
0.04880 0.01334 0.01293 0.01368
AU2 5 0.065363 0.265448 0.136940 21.00000 0.05099 0.03023 =
0.03432 0.00147 0.00238 0.01716
CL2 4 -0.103728 0.169804 0.047292 21.00000 0.11188 0.05299 =
0.05926 -0.01685 -0.03565 0.02989
CL1 4 0.392472 0.132678 0.336700 11.00000 0.03422 0.04536 =
0.06916 0.02566 0.01280 0.02259
P1 3 0.212012 0.355864 0.225337 11.00000 0.02769 0.02545 =
0.04704 0.00637 0.00876 0.01198
P2 3 0.259892 0.573038 0.286606 11.00000 0.02401 0.02732 =
0.05692 -0.00115 0.01247 0.00785
N1 2 0.143382 0.431556 0.282591 11.00000 0.02767 0.02760 =
0.03200 0.00837 0.01139 0.01287
N2 2 0.336355 0.510247 0.236743 11.00000 0.02720 0.02419 =
0.04251 0.00863 0.01057 0.01206
C1 1 -0.194119 0.415931 0.276111 11.00000 0.02633 0.05910 =
0.07809 0.03202 0.01218 0.02077
AFIX 43
H1 6 -0.241670 0.459785 0.259198 11.00000 -1.20000
AFIX 0
C2 1 0.368679 0.830968 0.508067 11.00000 0.07666 0.06687 =
0.04117 -0.00630 -0.00545 0.04791
AFIX 137
H2A 6 0.354918 0.903190 0.496884 11.00000 -1.50000
H2B 6 0.429042 0.851937 0.552463 11.00000 -1.50000
H2C 6 0.283905 0.763703 0.514395 11.00000 -1.50000
AFIX 0
C3 1 0.427299 0.791157 0.447347 11.00000 0.04873 0.04297 =
0.04328 -0.00716 -0.01105 0.02440
C4 1 0.448654 0.850761 0.386171 11.00000 0.03629 0.02533 =
0.06073 -0.00604 -0.01837 0.01412
AFIX 43
H4 6 0.428945 0.919753 0.383473 11.00000 -1.20000
AFIX 0
C5 1 0.498034 0.812657 0.328642 11.00000 0.02784 0.02422 =
0.05288 0.00740 -0.00437 0.00705
C6 1 0.526687 0.710875 0.332406 11.00000 0.02401 0.02075 =
0.05184 0.00396 -0.00530 0.00498
C7 1 0.565741 0.658738 0.268833 11.00000 0.02459 0.02800 =
0.06121 0.01517 0.01080 0.01225
C8 1 0.697150 0.705373 0.254800 11.00000 0.02271 0.03370 =
0.07738 0.01829 0.00678 0.00736
AFIX 43
H8 6 0.763007 0.770094 0.287039 11.00000 -1.20000
AFIX 0
C9 1 0.733010 0.659355 0.195179 11.00000 0.03083 0.04659 =
0.09750 0.04001 0.03451 0.01996
AFIX 43
H9 6 0.822716 0.692650 0.186079 11.00000 -1.20000
AFIX 0
C10 1 0.504465 0.512629 0.159538 11.00000 0.03590 0.03257 =
0.05405 0.02061 0.01982 0.01952
C11 1 0.406365 0.414944 0.107126 11.00000 0.05118 0.04898 =
0.04035 0.02087 0.02677 0.03064
C12 1 0.404513 0.295971 0.099725 11.00000 0.05114 0.05063 =
0.04373 0.02403 0.03177 0.03068
C13 1 0.223256 0.229676 0.002065 11.00000 0.08717 0.05404 =
0.04856 0.02021 0.01399 0.02016
C14 1 0.229002 0.347562 0.010134 11.00000 0.07750 0.06302 =
0.04412 0.02971 0.01050 0.03282
AFIX 43
H14 6 0.168985 0.365129 -0.020091 11.00000 -1.20000
AFIX 0
C15 1 0.319466 0.441043 0.060882 11.00000 0.05927 0.05295 =
0.04074 0.01970 0.02230 0.03162
C16 1 0.326141 0.567823 0.064321 11.00000 0.07957 0.06226 =
0.06019 0.03147 0.01858 0.04738
AFIX 137
H16A 6 0.307417 0.590785 0.111884 11.00000 -1.50000
H16B 6 0.260750 0.569609 0.027422 11.00000 -1.50000
H16C 6 0.414634 0.626216 0.055912 11.00000 -1.50000
AFIX 0
C17 1 0.501128 0.266472 0.144573 11.00000 0.06496 0.04287 =
0.06014 0.02177 0.03118 0.03515
AFIX 137
H17A 6 0.465987 0.177185 0.145496 11.00000 -1.50000
H17B 6 0.515498 0.306868 0.193670 11.00000 -1.50000
H17C 6 0.585065 0.296075 0.123875 11.00000 -1.50000
AFIX 0
C18 1 0.469881 0.560556 0.221312 11.00000 0.02478 0.02530 =
0.05155 0.01787 0.01655 0.01194
C20 1 0.510960 0.875830 0.260681 11.00000 0.04361 0.02905 =
0.07656 0.01473 0.01064 0.01577
AFIX 137
H20A 6 0.596295 0.891138 0.243772 11.00000 -1.50000
H20B 6 0.505339 0.954258 0.270906 11.00000 -1.50000
H20C 6 0.439592 0.822883 0.223485 11.00000 -1.50000
AFIX 0
C22 1 -0.259694 0.309548 0.306341 11.00000 0.02327 0.06109 =
0.09667 0.04124 0.02556 0.01606
AFIX 43
H22 6 -0.351960 0.278725 0.308957 11.00000 -1.20000
AFIX 0
C23 1 -0.077028 0.047059 0.269576 11.00000 0.06027 0.02801 =
0.07055 0.00245 -0.00672 0.00488
AFIX 137
H23A 6 -0.170953 0.024373 0.272433 11.00000 -1.50000
H23B 6 -0.064522 -0.027124 0.256295 11.00000 -1.50000
H23C 6 -0.045910 0.103940 0.233191 11.00000 -1.50000
AFIX 0
C25 1 -0.044754 0.471028 0.113936 11.00000 0.07419 0.04945 =
0.03733 0.00413 -0.00714 0.00546
AFIX 137
H25A 6 -0.029411 0.404924 0.134311 11.00000 -1.50000
H25B 6 -0.005879 0.486394 0.068598 11.00000 -1.50000
H25C 6 -0.139908 0.446600 0.105001 11.00000 -1.50000
AFIX 0
C26 1 0.016765 0.583985 0.164876 11.00000 0.02781 0.03412 =
0.03791 0.00897 -0.00290 0.00853
C27 1 0.007635 0.580521 0.239722 11.00000 0.02398 0.03631 =
0.03835 0.01373 0.00495 0.01574
C28 1 0.060931 0.690361 0.286015 11.00000 0.03507 0.03964 =
0.04197 0.01697 0.01224 0.02196
C29 1 0.126258 0.802778 0.258802 11.00000 0.03552 0.03847 =
0.04210 0.00297 0.00419 0.02061
AFIX 43
H29 6 0.163452 0.876711 0.290823 11.00000 -1.20000
AFIX 0
C30 1 0.137899 0.808569 0.185793 11.00000 0.03061 0.03671 =
0.05275 0.01730 0.01028 0.01394
C32 1 0.081709 0.699947 0.140914 11.00000 0.03774 0.05171 =
0.03951 0.01940 0.01000 0.02130
AFIX 43
H32 6 0.087144 0.703579 0.090831 11.00000 -1.20000
AFIX 0
C33 1 -0.060493 0.461143 0.269574 11.00000 0.02687 0.04128 =
0.03795 0.01925 0.00751 0.01252
C34 1 0.008057 0.394750 0.294222 11.00000 0.02035 0.02765 =
0.03182 0.00890 0.00664 0.00543
C35 1 -0.055694 0.288785 0.329140 11.00000 0.02822 0.03376 =
0.04571 0.01354 0.01071 0.01082
C36 1 -0.189658 0.247811 0.332948 11.00000 0.02740 0.03960 =
0.06567 0.02553 0.01590 0.00893
AFIX 43
H36 6 -0.235020 0.174865 0.354552 11.00000 -1.20000
AFIX 0
C37 1 0.015648 0.226504 0.367168 11.00000 0.02408 0.03302 =
0.03736 0.01457 0.01490 0.01046
C38 1 0.092274 0.284036 0.434097 11.00000 0.03325 0.03662 =
0.03599 0.01158 0.01307 0.01392
C39 1 0.110444 0.409909 0.464069 11.00000 0.07022 0.05027 =
0.04494 0.01201 0.01498 0.03178
AFIX 137
H39A 6 0.151496 0.427780 0.513972 11.00000 -1.50000
H39B 6 0.024340 0.412520 0.462423 11.00000 -1.50000
H39C 6 0.167341 0.471488 0.435352 11.00000 -1.50000
AFIX 0
C40 1 0.148478 0.220511 0.472784 11.00000 0.03815 0.04745 =
0.04343 0.01779 0.01017 0.01663
AFIX 43
H40 6 0.199874 0.259268 0.517541 11.00000 -1.20000
AFIX 0
C41 1 0.132920 0.103453 0.449034 11.00000 0.03060 0.04554 =
0.05836 0.02944 0.02152 0.01789
C42 1 0.196610 0.038526 0.490525 11.00000 0.04354 0.05622 =
0.08213 0.03272 0.01231 0.02265
AFIX 137
H42A 6 0.226797 0.080068 0.539635 11.00000 -1.50000
H42B 6 0.272273 0.039553 0.467356 11.00000 -1.50000
H42C 6 0.132766 -0.046866 0.491951 11.00000 -1.50000
AFIX 0
C43 1 0.058162 0.050879 0.383956 11.00000 0.03437 0.03409 =
0.06222 0.01495 0.01947 0.01386
AFIX 43
H43 6 0.045308 -0.029980 0.366958 11.00000 -1.20000
AFIX 0
C44 1 0.000374 0.108592 0.341603 11.00000 0.03359 0.02517 =
0.05032 0.00964 0.01279 0.00812
C45 1 0.510039 0.651299 0.395340 11.00000 0.04566 0.03310 =
0.04486 -0.00433 -0.01153 0.02225
C46 1 0.460274 0.692542 0.451839 11.00000 0.05284 0.03759 =
0.04065 0.00252 -0.00695 0.01965
AFIX 43
H46 6 0.448550 0.652656 0.494325 11.00000 -1.20000
AFIX 0
C48 1 0.312819 0.206156 0.046879 11.00000 0.08441 0.04345 =
0.04060 0.01160 0.01806 0.02803
AFIX 43
H48 6 0.311699 0.126734 0.041443 11.00000 -1.20000
AFIX 0
C49 1 0.125415 0.130419 -0.054485 11.00000 0.14634 0.05841 =
0.06918 -0.00056 -0.02655 0.02062
AFIX 137
H49A 6 0.128596 0.163623 -0.100798 11.00000 -1.50000
H49B 6 0.036222 0.103150 -0.040255 11.00000 -1.50000
H49C 6 0.148269 0.060412 -0.058907 11.00000 -1.50000
AFIX 0
C50 1 0.637014 0.563702 0.148275 11.00000 0.04494 0.05387 =
0.07801 0.03638 0.03895 0.03031
AFIX 43
H50 6 0.662686 0.532259 0.107299 11.00000 -1.20000
AFIX 0
C51 1 0.210330 0.931957 0.157578 11.00000 0.05612 0.05783 =
0.06127 0.02447 0.00879 0.01693
AFIX 137
H51A 6 0.300158 0.973573 0.182529 11.00000 -1.50000
H51B 6 0.163264 0.983179 0.166152 11.00000 -1.50000
H51C 6 0.214229 0.918610 0.105876 11.00000 -1.50000
AFIX 0
C52 1 0.052010 0.690002 0.365130 11.00000 0.07356 0.04997 =
0.04336 0.01013 0.01931 0.03236
AFIX 137
H52A 6 0.117487 0.768574 0.390382 11.00000 -1.50000
H52B 6 0.069322 0.622549 0.382026 11.00000 -1.50000
H52C 6 -0.036622 0.678648 0.374782 11.00000 -1.50000
REM #####
REM #####
REM #####
REM #####
AFIX 0
C54 1 0.538809 0.540024 0.400581 11.00000 0.05885 0.03708 =
0.05451 0.01096 -0.00012 0.02623
AFIX 137
H54A 6 0.462191 0.465981 0.378191 11.00000 -1.50000
H54B 6 0.557068 0.531545 0.451250 11.00000 -1.50000
H54C 6 0.615792 0.550517 0.375694 11.00000 -1.50000
AFIX 66
C100 1 0.528744 -0.008230 0.032954 10.50000 0.11511
AFIX 43
H100 6 0.595269 0.010095 0.072035 10.50000 -1.20000
AFIX 65
C101 1 0.411716 -0.114743 0.028241 10.50000 0.11315
AFIX 43
H101 6 0.398259 -0.169217 0.064100 10.50000 -1.20000
AFIX 65
C102 1 0.314379 -0.141554 -0.028940 10.50000 0.09826
AFIX 43
H102 6 0.234396 -0.214352 -0.032161 10.50000 -1.20000
AFIX 65
C103 1 0.334068 -0.061852 -0.081407 10.50000 0.13273
AFIX 43
H103 6 0.267542 -0.080176 -0.120487 10.50000 -1.20000
AFIX 65
C104 1 0.451095 0.044662 -0.076695 10.50000 0.10618
AFIX 43
H104 6 0.464551 0.099135 -0.112554 10.50000 -1.20000
AFIX 65
C105 1 0.548433 0.071475 -0.019515 10.50000 0.07765
AFIX 43
H105 6 0.628416 0.144272 -0.016294 10.50000 -1.20000
AFIX 0
HKLF 4
REM a1 in P-1
REM R1 = 0.0498 for 7898 Fo > 4sig(Fo) and 0.0765 for all 10457 data
REM 530 parameters refined using 0 restraints
END
WGHT 0.0000 10.3431
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 1.135, deepest hole -1.108, 1-sigma level 0.131
Q1 1 0.5059 0.0674 -0.0536 11.00000 0.05 1.13
Q2 1 0.5000 0.0000 0.0000 10.50000 0.05 0.98
Q3 1 0.3057 0.1832 0.3397 11.00000 0.05 0.84
Q4 1 0.2820 -0.1183 -0.0792 11.00000 0.05 0.73
Q5 1 0.1389 0.2940 0.1325 11.00000 0.05 0.72
Q6 1 0.1270 0.3576 0.1375 11.00000 0.05 0.69
Q7 1 0.6345 0.0050 0.1024 11.00000 0.05 0.67
Q8 1 -0.0462 0.2733 0.1269 11.00000 0.05 0.63
Q9 1 0.4799 0.7631 0.5455 11.00000 0.05 0.60
Q10 1 -0.0167 0.1702 0.0689 11.00000 0.05 0.59
Q11 1 0.0371 0.2936 0.1273 11.00000 0.05 0.59
Q12 1 0.1001 0.6982 0.0064 11.00000 0.05 0.58
Q13 1 -0.0246 0.1981 0.0335 11.00000 0.05 0.55
Q14 1 0.1575 0.6827 0.3793 11.00000 0.05 0.53
Q15 1 0.2313 0.5360 0.3522 11.00000 0.05 0.53
Q16 1 0.1334 0.1657 0.1877 11.00000 0.05 0.52
Q17 1 0.3972 0.3628 0.3477 11.00000 0.05 0.52
Q18 1 0.2027 0.2726 0.2766 11.00000 0.05 0.51
Q19 1 0.2583 0.1793 0.2800 11.00000 0.05 0.50
Q20 1 -0.1201 0.4508 0.0575 11.00000 0.05 0.50
Q21 1 0.3375 0.2708 0.3090 11.00000 0.05 0.50
Q22 1 0.3035 0.1307 0.2904 11.00000 0.05 0.50
Q23 1 0.2432 0.3085 0.2652 11.00000 0.05 0.49
Q24 1 0.3813 0.2963 0.3593 11.00000 0.05 0.49
Q25 1 -0.0043 0.1384 0.1202 11.00000 0.05 0.49
Q26 1 0.2131 0.3046 0.1871 11.00000 0.05 0.48
Q27 1 0.1252 0.2661 0.2017 11.00000 0.05 0.48
Q28 1 0.4388 0.2796 0.3396 11.00000 0.05 0.48
Q29 1 0.0500 0.1806 0.1836 11.00000 0.05 0.47
Q30 1 0.4193 0.3377 0.3887 11.00000 0.05 0.47
Q31 1 0.4869 0.2688 0.3899 11.00000 0.05 0.47
Q32 1 0.3961 0.8650 0.2482 11.00000 0.05 0.47
Q33 1 0.4227 0.0690 0.3524 11.00000 0.05 0.45
Q34 1 -0.0593 0.3341 0.4388 11.00000 0.05 0.45
Q35 1 -0.0818 0.0330 0.1913 11.00000 0.05 0.45
Q36 1 0.0801 0.3418 0.0809 11.00000 0.05 0.45
Q37 1 0.0643 0.0644 0.4590 11.00000 0.05 0.45
Q38 1 0.1418 0.1321 0.0706 11.00000 0.05 0.44
Q39 1 0.4819 0.5669 0.4110 11.00000 0.05 0.44
Q40 1 0.1208 0.1004 0.4035 11.00000 0.05 0.44
;
_shelx_res_checksum 73500