##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
# http://www.iucr.org/resources/cif/software. #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
# article from which it was obtained. #
# #
##############################################################################
data_global
_audit_creation_method
;
manual editing of the CIF file
created by SHELXTL Ver. 6.10
and processed with modiCIfer-03272007.
;
_journal_date_recd_electronic 2011-10-18
_journal_date_accepted 2011-10-24
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2011
_journal_volume 67
_journal_issue 11
_journal_page_first m1629
_journal_page_last m1630
_journal_paper_category QM
_journal_coeditor_code NG5253
_publ_contact_author_name
;
Guzei, Ilia A.
;
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI 53706
USA
;
_publ_contact_author_email iguzei@chem.wisc.edu
_publ_contact_author_fax '608-262-0381'
_publ_contact_author_phone '608-263-4694'
_publ_section_title
;\
(\m-Piperazine-1,4-dicarbodithioato-\k^4^S^1^,S^1'^:S^4^,\
S^4'^)bis[bis(triphenylphosphane-\kP)gold(I)] chloroform
disolvate
;
loop_
_publ_author_name
_publ_author_address
'Guzei, Ilia A.'
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI 53706
USA
;
'Spencer, Lara C.'
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI 53706
USA
;
'Lillywhite, Stacy'
;
Department of Chemistry
University of Johannesburg
Auckland Park Kingsway Campus
Johannesburg 2006
South Africa
;
'Darkwa, James'
;
Department of Chemistry
University of Johannesburg
Auckland Park Kingsway Campus
Johannesburg 2006
South Africa
;
data_I
_chemical_name_systematic
;
(\m-Piperazine-1,4-dicarbodithioato-
\k^4^S^1^,S^1'^:S^4^,S^4'^)
bis[bis(triphenylphosphane-\kP)gold(I)] chloroform disolvate
;
_chemical_name_common ?
_chemical_formula_moiety 'C78 H68 Au2 N2 P4 S4, 2(C H Cl3)'
_chemical_formula_sum 'C80 H70 Au2 Cl6 N2 P4 S4'
_chemical_formula_iupac '[Au2 (C6 H8 N2 S4) (C18 H15 P)4], 2C H Cl3'
_chemical_formula_weight 1918.13
_chemical_melting_point ?
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.8455(17)
_cell_length_b 13.2879(10)
_cell_length_c 13.4197(9)
_cell_angle_alpha 119.572(2)
_cell_angle_beta 101.544(2)
_cell_angle_gamma 96.039(2)
_cell_volume 1895.2(3)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 9936
_cell_measurement_theta_min 3.6156
_cell_measurement_theta_max 71.6517
_cell_measurement_temperature 100(2)
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.44
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.29
_exptl_crystal_density_diffrn 1.681
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 948
_exptl_absorpt_coefficient_mu 11.304
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_absorpt_correction_T_min 0.0833
_exptl_absorpt_correction_T_max 0.1398
_exptl_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_type Cu-K\a
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART APEXII'
_diffrn_measurement_method '0.50\% \w and 0.5 \% \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 30338
_diffrn_reflns_av_R_equivalents 0.0314
_diffrn_reflns_av_sigmaI/netI 0.0215
_diffrn_reflns_theta_min 3.62
_diffrn_reflns_theta_max 72.25
_diffrn_reflns_theta_full 67.00
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F^2^, conventional
R-factors R are based on F, with F set to zero for
negative F^2^. The threshold expression of F^2^ >
\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.
;
_reflns_number_total 7089
_reflns_number_gt 7080
_reflns_threshold_expression I>2\s(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0281
_refine_ls_R_factor_gt 0.0281
_refine_ls_wR_factor_gt 0.0739
_refine_ls_wR_factor_ref 0.0740
_refine_ls_goodness_of_fit_ref 1.152
_refine_ls_restrained_S_all 1.152
_refine_ls_number_reflns 7089
_refine_ls_number_parameters 442
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+3.5159P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 2.398
_refine_diff_density_min -1.349
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.3639 0.7018
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Au' 'Au' -4.4197 7.2980
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S' 'S' 0.3331 0.5567
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P' 'P' 0.2955 0.4335
'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'
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'SAINT (Bruker, 2007)'
_computing_data_reduction 'SAINT (Bruker, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008), FCF_filter (Guzei, 2007) and INSerter
(Guzei, 2007)
;
_computing_molecular_graphics
'SHELXTL(Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2010) and modiCIFer
(Guzei, 2007)
;
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Au Au1 0.234436(10) 0.776500(10) 0.653197(10) 0.01426(6) Uani d . 1 1 . .
S S1 0.25387(6) 0.94442(7) 0.88645(7) 0.01770(16) Uani d . 1 1 . .
S S2 0.04873(6) 0.82819(7) 0.68645(7) 0.01689(16) Uani d . 1 1 . .
P P1 0.24564(7) 0.61270(7) 0.67150(7) 0.01428(16) Uani d . 1 1 . .
P P2 0.32654(7) 0.86933(7) 0.57904(7) 0.01350(16) Uani d . 1 1 . .
N N1 0.0585(2) 0.9761(2) 0.9150(2) 0.0168(5) Uani d . 1 1 . .
C C1 0.1155(3) 0.9217(3) 0.8365(3) 0.0156(6) Uani d . 1 1 . .
C C2 0.1115(3) 1.0645(3) 1.0418(3) 0.0195(7) Uani d . 1 1 . .
H H2AB 0.1051 1.1446 1.0584 0.023 Uiso calc R 1 1 . .
H H2AA 0.1903 1.0655 1.0614 0.023 Uiso calc R 1 1 . .
C C3 0.0590(3) 1.0359(3) 1.1199(3) 0.0192(7) Uani d . 1 1 . .
H H3AA 0.0737 0.9608 1.1113 0.023 Uiso calc R 1 1 . .
H H3AB 0.0913 1.1005 1.2050 0.023 Uiso calc R 1 1 . .
C C4 0.3628(3) 0.6456(3) 0.7941(3) 0.0183(7) Uani d . 1 1 . .
C C5 0.4568(3) 0.7301(3) 0.8254(3) 0.0215(7) Uani d . 1 1 . .
H H5AA 0.4581 0.7723 0.7854 0.026 Uiso calc R 1 1 . .
C C6 0.5488(3) 0.7527(4) 0.9152(3) 0.0285(8) Uani d . 1 1 . .
H H6AA 0.6130 0.8098 0.9357 0.034 Uiso calc R 1 1 . .
C C7 0.5471(3) 0.6927(4) 0.9744(3) 0.0311(9) Uani d . 1 1 . .
H H7AA 0.6101 0.7085 1.0357 0.037 Uiso calc R 1 1 . .
C C8 0.4537(3) 0.6093(4) 0.9447(3) 0.0301(8) Uani d . 1 1 . .
H H8AA 0.4526 0.5687 0.9863 0.036 Uiso calc R 1 1 . .
C C9 0.3620(3) 0.5849(3) 0.8550(3) 0.0238(7) Uani d . 1 1 . .
H H9AA 0.2985 0.5270 0.8346 0.029 Uiso calc R 1 1 . .
C C10 0.2675(3) 0.4871(3) 0.5424(3) 0.0159(6) Uani d . 1 1 . .
C C11 0.3632(3) 0.4487(3) 0.5474(3) 0.0203(7) Uani d . 1 1 . .
H H11A 0.4171 0.4825 0.6223 0.024 Uiso calc R 1 1 . .
C C12 0.3813(3) 0.3601(3) 0.4429(3) 0.0245(7) Uani d . 1 1 . .
H H12A 0.4475 0.3346 0.4470 0.029 Uiso calc R 1 1 . .
C C13 0.3025(3) 0.3101(3) 0.3339(3) 0.0229(7) Uani d . 1 1 . .
H H13A 0.3145 0.2498 0.2631 0.027 Uiso calc R 1 1 . .
C C14 0.2067(3) 0.3477(3) 0.3280(3) 0.0215(7) Uani d . 1 1 . .
H H14A 0.1527 0.3128 0.2530 0.026 Uiso calc R 1 1 . .
C C15 0.1887(3) 0.4362(3) 0.4311(3) 0.0190(7) Uani d . 1 1 . .
H H15A 0.1228 0.4624 0.4262 0.023 Uiso calc R 1 1 . .
C C16 0.1298(3) 0.5531(3) 0.7022(3) 0.0168(6) Uani d . 1 1 . .
C C17 0.0658(3) 0.4376(3) 0.6282(3) 0.0187(7) Uani d . 1 1 . .
H H17A 0.0823 0.3836 0.5574 0.022 Uiso calc R 1 1 . .
C C18 -0.0229(3) 0.4005(3) 0.6578(3) 0.0236(7) Uani d . 1 1 . .
H H18A -0.0670 0.3215 0.6065 0.028 Uiso calc R 1 1 . .
C C19 -0.0467(3) 0.4788(3) 0.7617(3) 0.0243(7) Uani d . 1 1 . .
H H19A -0.1067 0.4534 0.7820 0.029 Uiso calc R 1 1 . .
C C20 0.0174(3) 0.5941(3) 0.8355(3) 0.0248(7) Uani d . 1 1 . .
H H20A 0.0017 0.6474 0.9072 0.030 Uiso calc R 1 1 . .
C C21 0.1042(3) 0.6322(3) 0.8060(3) 0.0204(7) Uani d . 1 1 . .
H H21A 0.1464 0.7121 0.8561 0.025 Uiso calc R 1 1 . .
C C22 0.2798(3) 0.9894(3) 0.5672(3) 0.0169(6) Uani d . 1 1 . .
C C23 0.1719(3) 0.9678(3) 0.5049(3) 0.0218(7) Uani d . 1 1 . .
H H23A 0.1233 0.8929 0.4726 0.026 Uiso calc R 1 1 . .
C C24 0.1338(3) 1.0550(3) 0.4894(3) 0.0269(8) Uani d . 1 1 . .
H H24A 0.0604 1.0382 0.4438 0.032 Uiso calc R 1 1 . .
C C25 0.2025(3) 1.1658(3) 0.5399(3) 0.0262(8) Uani d . 1 1 . .
H H25A 0.1764 1.2252 0.5293 0.031 Uiso calc R 1 1 . .
C C26 0.3099(3) 1.1904(3) 0.6063(3) 0.0242(7) Uani d . 1 1 . .
H H26A 0.3567 1.2672 0.6431 0.029 Uiso calc R 1 1 . .
C C27 0.3491(3) 1.1018(3) 0.6189(3) 0.0207(7) Uani d . 1 1 . .
H H27A 0.4230 1.1181 0.6628 0.025 Uiso calc R 1 1 . .
C C28 0.4678(3) 0.9384(3) 0.6736(3) 0.0157(6) Uani d . 1 1 . .
C C29 0.4856(3) 1.0177(3) 0.7967(3) 0.0187(7) Uani d . 1 1 . .
H H29A 0.4249 1.0341 0.8276 0.022 Uiso calc R 1 1 . .
C C30 0.5910(3) 1.0720(3) 0.8732(3) 0.0214(7) Uani d . 1 1 . .
H H30A 0.6027 1.1262 0.9563 0.026 Uiso calc R 1 1 . .
C C31 0.6797(3) 1.0473(3) 0.8284(3) 0.0208(7) Uani d . 1 1 . .
H H31A 0.7520 1.0844 0.8812 0.025 Uiso calc R 1 1 . .
C C32 0.6637(3) 0.9691(3) 0.7077(3) 0.0206(7) Uani d . 1 1 . .
H H32A 0.7247 0.9524 0.6776 0.025 Uiso calc R 1 1 . .
C C33 0.5574(3) 0.9145(3) 0.6298(3) 0.0177(6) Uani d . 1 1 . .
H H33A 0.5464 0.8610 0.5467 0.021 Uiso calc R 1 1 . .
C C34 0.3386(3) 0.7666(3) 0.4312(3) 0.0154(6) Uani d . 1 1 . .
C C35 0.3435(3) 0.7995(3) 0.3476(3) 0.0205(7) Uani d . 1 1 . .
H H35A 0.3372 0.8769 0.3657 0.025 Uiso calc R 1 1 . .
C C36 0.3575(3) 0.7189(3) 0.2381(3) 0.0247(7) Uani d . 1 1 . .
H H36A 0.3597 0.7410 0.1810 0.030 Uiso calc R 1 1 . .
C C37 0.3683(3) 0.6067(3) 0.2119(3) 0.0220(7) Uani d . 1 1 . .
H H37A 0.3790 0.5524 0.1374 0.026 Uiso calc R 1 1 . .
C C38 0.3635(3) 0.5729(3) 0.2941(3) 0.0220(7) Uani d . 1 1 . .
H H38A 0.3715 0.4960 0.2763 0.026 Uiso calc R 1 1 . .
C C39 0.3470(3) 0.6526(3) 0.4026(3) 0.0184(7) Uani d . 1 1 . .
H H39A 0.3413 0.6288 0.4578 0.022 Uiso calc R 1 1 . .
Cl Cl1 0.15739(10) 0.41053(9) 0.95175(11) 0.0451(3) Uani d . 1 1 . .
Cl Cl2 0.14677(11) 0.15846(10) 0.81701(11) 0.0455(3) Uani d . 1 1 . .
Cl Cl3 -0.05265(9) 0.24127(10) 0.82114(9) 0.0383(2) Uani d . 1 1 . .
C C40 0.0848(3) 0.2721(4) 0.8232(4) 0.0305(8) Uani d . 1 1 . .
H H40A 0.0863 0.2762 0.7511 0.037 Uiso calc R 1 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Au1 0.01735(9) 0.01435(8) 0.01405(8) 0.00500(5) 0.00798(6) 0.00817(6)
S1 0.0143(4) 0.0222(4) 0.0133(3) 0.0047(3) 0.0051(3) 0.0065(3)
S2 0.0149(4) 0.0209(4) 0.0123(3) 0.0050(3) 0.0044(3) 0.0066(3)
P1 0.0157(4) 0.0147(4) 0.0139(4) 0.0043(3) 0.0058(3) 0.0080(3)
P2 0.0156(4) 0.0141(4) 0.0136(4) 0.0045(3) 0.0063(3) 0.0084(3)
N1 0.0135(14) 0.0212(14) 0.0138(13) 0.0050(11) 0.0049(10) 0.0073(11)
C1 0.0168(16) 0.0153(15) 0.0155(15) 0.0025(12) 0.0057(12) 0.0085(13)
C2 0.0175(17) 0.0210(16) 0.0151(16) 0.0036(13) 0.0056(13) 0.0058(14)
C3 0.0156(17) 0.0260(17) 0.0147(15) 0.0079(13) 0.0062(12) 0.0086(14)
C4 0.0197(17) 0.0199(16) 0.0145(15) 0.0068(13) 0.0062(13) 0.0077(13)
C5 0.0224(18) 0.0199(16) 0.0170(16) 0.0042(13) 0.0077(13) 0.0054(14)
C6 0.0201(19) 0.0315(19) 0.0225(18) 0.0079(15) 0.0067(14) 0.0057(16)
C7 0.028(2) 0.041(2) 0.0168(17) 0.0185(17) 0.0045(15) 0.0091(16)
C8 0.035(2) 0.043(2) 0.0243(19) 0.0203(18) 0.0115(16) 0.0225(18)
C9 0.027(2) 0.0289(18) 0.0237(18) 0.0109(15) 0.0102(15) 0.0175(16)
C10 0.0218(18) 0.0128(14) 0.0159(15) 0.0054(12) 0.0090(13) 0.0080(12)
C11 0.0209(18) 0.0190(16) 0.0211(17) 0.0069(13) 0.0052(14) 0.0105(14)
C12 0.0243(19) 0.0223(17) 0.0285(19) 0.0087(14) 0.0117(15) 0.0124(15)
C13 0.030(2) 0.0157(15) 0.0219(17) 0.0062(14) 0.0130(15) 0.0071(14)
C14 0.0243(19) 0.0198(16) 0.0166(16) 0.0027(14) 0.0037(13) 0.0084(14)
C15 0.0199(18) 0.0184(16) 0.0200(16) 0.0053(13) 0.0060(13) 0.0108(14)
C16 0.0155(17) 0.0200(16) 0.0204(16) 0.0062(13) 0.0053(12) 0.0143(14)
C17 0.0193(18) 0.0195(16) 0.0206(16) 0.0062(13) 0.0061(13) 0.0125(14)
C18 0.0196(18) 0.0260(18) 0.0286(19) 0.0013(14) 0.0043(14) 0.0185(16)
C19 0.0173(18) 0.037(2) 0.0321(19) 0.0067(15) 0.0089(14) 0.0270(17)
C20 0.026(2) 0.0334(19) 0.0237(18) 0.0115(15) 0.0123(15) 0.0189(16)
C21 0.0233(18) 0.0206(16) 0.0202(16) 0.0052(13) 0.0079(13) 0.0122(14)
C22 0.0216(18) 0.0187(15) 0.0169(15) 0.0095(13) 0.0105(13) 0.0113(13)
C23 0.0222(18) 0.0218(17) 0.0239(17) 0.0069(14) 0.0073(14) 0.0132(15)
C24 0.027(2) 0.032(2) 0.0281(19) 0.0129(16) 0.0090(15) 0.0191(17)
C25 0.032(2) 0.0299(19) 0.0308(19) 0.0190(16) 0.0162(16) 0.0216(17)
C26 0.030(2) 0.0188(16) 0.0276(18) 0.0067(14) 0.0125(15) 0.0134(15)
C27 0.0203(18) 0.0218(17) 0.0244(17) 0.0077(14) 0.0080(14) 0.0142(15)
C28 0.0176(17) 0.0152(14) 0.0173(15) 0.0045(12) 0.0047(12) 0.0108(13)
C29 0.0180(17) 0.0222(16) 0.0182(16) 0.0062(13) 0.0068(13) 0.0114(14)
C30 0.0228(18) 0.0239(17) 0.0165(16) 0.0060(14) 0.0044(13) 0.0104(14)
C31 0.0158(17) 0.0238(17) 0.0240(17) 0.0056(13) 0.0027(13) 0.0143(15)
C32 0.0203(18) 0.0236(17) 0.0252(18) 0.0114(14) 0.0110(14) 0.0154(15)
C33 0.0199(17) 0.0192(15) 0.0199(16) 0.0070(13) 0.0080(13) 0.0132(14)
C34 0.0129(16) 0.0172(15) 0.0152(15) 0.0041(12) 0.0048(12) 0.0075(13)
C35 0.0275(19) 0.0193(16) 0.0176(16) 0.0062(13) 0.0086(14) 0.0109(14)
C36 0.031(2) 0.0309(19) 0.0186(17) 0.0078(15) 0.0111(14) 0.0162(15)
C37 0.0231(18) 0.0237(17) 0.0152(16) 0.0053(14) 0.0097(13) 0.0059(14)
C38 0.0239(19) 0.0192(16) 0.0224(17) 0.0064(13) 0.0102(14) 0.0093(14)
C39 0.0196(17) 0.0208(16) 0.0169(15) 0.0051(13) 0.0068(13) 0.0109(14)
Cl1 0.0397(6) 0.0299(5) 0.0451(6) -0.0012(4) 0.0001(5) 0.0112(5)
Cl2 0.0608(7) 0.0342(5) 0.0547(7) 0.0180(5) 0.0278(6) 0.0276(5)
Cl3 0.0355(5) 0.0420(5) 0.0346(5) -0.0020(4) 0.0028(4) 0.0230(4)
C40 0.035(2) 0.030(2) 0.0264(19) 0.0009(16) 0.0048(16) 0.0183(17)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Au1 P2 . 2.2994(8) yes
Au1 P1 . 2.3233(8) yes
Au1 S2 . 2.6133(8) yes
Au1 S1 . 2.7414(8) yes
S1 C1 . 1.706(3) ?
S2 C1 . 1.718(3) ?
P1 C10 . 1.818(3) ?
P1 C4 . 1.823(4) ?
P1 C16 . 1.825(3) ?
P2 C34 . 1.822(3) ?
P2 C28 . 1.823(3) ?
P2 C22 . 1.829(3) ?
N1 C1 . 1.354(4) ?
N1 C3 2_577 1.454(4) ?
N1 C2 . 1.460(4) ?
C2 C3 . 1.524(5) ?
C2 H2AB . 0.9900 ?
C2 H2AA . 0.9900 ?
C3 N1 2_577 1.454(4) ?
C3 H3AA . 0.9900 ?
C3 H3AB . 0.9900 ?
C4 C5 . 1.393(5) ?
C4 C9 . 1.405(5) ?
C5 C6 . 1.392(5) ?
C5 H5AA . 0.9500 ?
C6 C7 . 1.378(6) ?
C6 H6AA . 0.9500 ?
C7 C8 . 1.386(6) ?
C7 H7AA . 0.9500 ?
C8 C9 . 1.380(5) ?
C8 H8AA . 0.9500 ?
C9 H9AA . 0.9500 ?
C10 C11 . 1.381(5) ?
C10 C15 . 1.403(5) ?
C11 C12 . 1.402(5) ?
C11 H11A . 0.9500 ?
C12 C13 . 1.382(5) ?
C12 H12A . 0.9500 ?
C13 C14 . 1.378(5) ?
C13 H13A . 0.9500 ?
C14 C15 . 1.390(5) ?
C14 H14A . 0.9500 ?
C15 H15A . 0.9500 ?
C16 C17 . 1.386(5) ?
C16 C21 . 1.402(5) ?
C17 C18 . 1.398(5) ?
C17 H17A . 0.9500 ?
C18 C19 . 1.388(6) ?
C18 H18A . 0.9500 ?
C19 C20 . 1.384(5) ?
C19 H19A . 0.9500 ?
C20 C21 . 1.383(5) ?
C20 H20A . 0.9500 ?
C21 H21A . 0.9500 ?
C22 C23 . 1.386(5) ?
C22 C27 . 1.398(5) ?
C23 C24 . 1.393(5) ?
C23 H23A . 0.9500 ?
C24 C25 . 1.382(6) ?
C24 H24A . 0.9500 ?
C25 C26 . 1.389(6) ?
C25 H25A . 0.9500 ?
C26 C27 . 1.397(5) ?
C26 H26A . 0.9500 ?
C27 H27A . 0.9500 ?
C28 C33 . 1.392(5) ?
C28 C29 . 1.403(5) ?
C29 C30 . 1.385(5) ?
C29 H29A . 0.9500 ?
C30 C31 . 1.387(5) ?
C30 H30A . 0.9500 ?
C31 C32 . 1.381(5) ?
C31 H31A . 0.9500 ?
C32 C33 . 1.397(5) ?
C32 H32A . 0.9500 ?
C33 H33A . 0.9500 ?
C34 C39 . 1.390(5) ?
C34 C35 . 1.400(5) ?
C35 C36 . 1.390(5) ?
C35 H35A . 0.9500 ?
C36 C37 . 1.383(5) ?
C36 H36A . 0.9500 ?
C37 C38 . 1.389(5) ?
C37 H37A . 0.9500 ?
C38 C39 . 1.392(5) ?
C38 H38A . 0.9500 ?
C39 H39A . 0.9500 ?
Cl1 C40 . 1.758(4) ?
Cl2 C40 . 1.754(4) ?
Cl3 C40 . 1.762(4) ?
C40 H40A . 1.0000 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P2 Au1 P1 . . 134.65(3) yes
P2 Au1 S2 . . 116.81(3) yes
P1 Au1 S2 . . 107.10(3) yes
P2 Au1 S1 . . 107.34(3) yes
P1 Au1 S1 . . 99.39(3) yes
S2 Au1 S1 . . 67.03(2) yes
C1 S1 Au1 . . 84.64(11) ?
C1 S2 Au1 . . 88.55(12) ?
C10 P1 C4 . . 103.04(16) ?
C10 P1 C16 . . 106.19(15) ?
C4 P1 C16 . . 103.85(15) ?
C10 P1 Au1 . . 113.94(10) ?
C4 P1 Au1 . . 112.18(11) ?
C16 P1 Au1 . . 116.33(11) ?
C34 P2 C28 . . 104.10(15) ?
C34 P2 C22 . . 104.72(15) ?
C28 P2 C22 . . 103.69(15) ?
C34 P2 Au1 . . 113.39(11) ?
C28 P2 Au1 . . 109.59(10) ?
C22 P2 Au1 . . 119.85(11) ?
C1 N1 C3 . 2_577 123.8(3) ?
C1 N1 C2 . . 122.7(3) ?
C3 N1 C2 2_577 . 113.0(3) ?
N1 C1 S1 . . 120.2(2) ?
N1 C1 S2 . . 120.3(3) ?
S1 C1 S2 . . 119.56(19) ?
N1 C2 C3 . . 110.7(3) ?
N1 C2 H2AB . . 109.5 ?
C3 C2 H2AB . . 109.5 ?
N1 C2 H2AA . . 109.5 ?
C3 C2 H2AA . . 109.5 ?
H2AB C2 H2AA . . 108.1 ?
N1 C3 C2 2_577 . 110.2(3) ?
N1 C3 H3AA 2_577 . 109.6 ?
C2 C3 H3AA . . 109.6 ?
N1 C3 H3AB 2_577 . 109.6 ?
C2 C3 H3AB . . 109.6 ?
H3AA C3 H3AB . . 108.1 ?
C5 C4 C9 . . 119.1(3) ?
C5 C4 P1 . . 119.3(3) ?
C9 C4 P1 . . 121.6(3) ?
C6 C5 C4 . . 120.2(3) ?
C6 C5 H5AA . . 119.9 ?
C4 C5 H5AA . . 119.9 ?
C7 C6 C5 . . 120.2(4) ?
C7 C6 H6AA . . 119.9 ?
C5 C6 H6AA . . 119.9 ?
C6 C7 C8 . . 120.0(4) ?
C6 C7 H7AA . . 120.0 ?
C8 C7 H7AA . . 120.0 ?
C9 C8 C7 . . 120.5(4) ?
C9 C8 H8AA . . 119.8 ?
C7 C8 H8AA . . 119.8 ?
C8 C9 C4 . . 119.9(4) ?
C8 C9 H9AA . . 120.0 ?
C4 C9 H9AA . . 120.0 ?
C11 C10 C15 . . 119.0(3) ?
C11 C10 P1 . . 122.6(3) ?
C15 C10 P1 . . 118.0(3) ?
C10 C11 C12 . . 120.6(3) ?
C10 C11 H11A . . 119.7 ?
C12 C11 H11A . . 119.7 ?
C13 C12 C11 . . 119.8(3) ?
C13 C12 H12A . . 120.1 ?
C11 C12 H12A . . 120.1 ?
C14 C13 C12 . . 120.1(3) ?
C14 C13 H13A . . 120.0 ?
C12 C13 H13A . . 120.0 ?
C13 C14 C15 . . 120.4(3) ?
C13 C14 H14A . . 119.8 ?
C15 C14 H14A . . 119.8 ?
C14 C15 C10 . . 120.1(3) ?
C14 C15 H15A . . 120.0 ?
C10 C15 H15A . . 120.0 ?
C17 C16 C21 . . 119.4(3) ?
C17 C16 P1 . . 124.1(3) ?
C21 C16 P1 . . 116.5(3) ?
C16 C17 C18 . . 120.1(3) ?
C16 C17 H17A . . 120.0 ?
C18 C17 H17A . . 120.0 ?
C19 C18 C17 . . 120.2(3) ?
C19 C18 H18A . . 119.9 ?
C17 C18 H18A . . 119.9 ?
C20 C19 C18 . . 119.6(3) ?
C20 C19 H19A . . 120.2 ?
C18 C19 H19A . . 120.2 ?
C21 C20 C19 . . 120.6(3) ?
C21 C20 H20A . . 119.7 ?
C19 C20 H20A . . 119.7 ?
C20 C21 C16 . . 120.1(3) ?
C20 C21 H21A . . 120.0 ?
C16 C21 H21A . . 120.0 ?
C23 C22 C27 . . 119.1(3) ?
C23 C22 P2 . . 118.6(3) ?
C27 C22 P2 . . 122.3(3) ?
C22 C23 C24 . . 120.6(3) ?
C22 C23 H23A . . 119.7 ?
C24 C23 H23A . . 119.7 ?
C25 C24 C23 . . 120.2(4) ?
C25 C24 H24A . . 119.9 ?
C23 C24 H24A . . 119.9 ?
C24 C25 C26 . . 119.9(3) ?
C24 C25 H25A . . 120.1 ?
C26 C25 H25A . . 120.1 ?
C25 C26 C27 . . 119.9(3) ?
C25 C26 H26A . . 120.0 ?
C27 C26 H26A . . 120.0 ?
C26 C27 C22 . . 120.2(3) ?
C26 C27 H27A . . 119.9 ?
C22 C27 H27A . . 119.9 ?
C33 C28 C29 . . 119.1(3) ?
C33 C28 P2 . . 123.2(3) ?
C29 C28 P2 . . 117.7(3) ?
C30 C29 C28 . . 120.4(3) ?
C30 C29 H29A . . 119.8 ?
C28 C29 H29A . . 119.8 ?
C29 C30 C31 . . 119.9(3) ?
C29 C30 H30A . . 120.0 ?
C31 C30 H30A . . 120.0 ?
C32 C31 C30 . . 120.5(3) ?
C32 C31 H31A . . 119.8 ?
C30 C31 H31A . . 119.8 ?
C31 C32 C33 . . 119.9(3) ?
C31 C32 H32A . . 120.0 ?
C33 C32 H32A . . 120.0 ?
C28 C33 C32 . . 120.2(3) ?
C28 C33 H33A . . 119.9 ?
C32 C33 H33A . . 119.9 ?
C39 C34 C35 . . 119.2(3) ?
C39 C34 P2 . . 118.2(2) ?
C35 C34 P2 . . 122.6(2) ?
C36 C35 C34 . . 120.0(3) ?
C36 C35 H35A . . 120.0 ?
C34 C35 H35A . . 120.0 ?
C37 C36 C35 . . 120.2(3) ?
C37 C36 H36A . . 119.9 ?
C35 C36 H36A . . 119.9 ?
C36 C37 C38 . . 120.3(3) ?
C36 C37 H37A . . 119.8 ?
C38 C37 H37A . . 119.8 ?
C37 C38 C39 . . 119.5(3) ?
C37 C38 H38A . . 120.2 ?
C39 C38 H38A . . 120.2 ?
C34 C39 C38 . . 120.7(3) ?
C34 C39 H39A . . 119.6 ?
C38 C39 H39A . . 119.6 ?
Cl2 C40 Cl1 . . 110.6(2) ?
Cl2 C40 Cl3 . . 110.7(2) ?
Cl1 C40 Cl3 . . 110.3(2) ?
Cl2 C40 H40A . . 108.4 ?
Cl1 C40 H40A . . 108.4 ?
Cl3 C40 H40A . . 108.4 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
P2 Au1 S1 C1 . . . . 115.18(11) ?
P1 Au1 S1 C1 . . . . -101.89(11) ?
S2 Au1 S1 C1 . . . . 2.79(11) ?
P2 Au1 S2 C1 . . . . -101.30(11) ?
P1 Au1 S2 C1 . . . . 90.39(11) ?
S1 Au1 S2 C1 . . . . -2.76(11) ?
P2 Au1 P1 C10 . . . . -40.63(13) ?
S2 Au1 P1 C10 . . . . 124.64(13) ?
S1 Au1 P1 C10 . . . . -166.64(13) ?
P2 Au1 P1 C4 . . . . 75.96(12) ?
S2 Au1 P1 C4 . . . . -118.77(12) ?
S1 Au1 P1 C4 . . . . -50.05(12) ?
P2 Au1 P1 C16 . . . . -164.70(12) ?
S2 Au1 P1 C16 . . . . 0.57(13) ?
S1 Au1 P1 C16 . . . . 69.29(13) ?
P1 Au1 P2 C34 . . . . 48.64(13) ?
S2 Au1 P2 C34 . . . . -115.56(12) ?
S1 Au1 P2 C34 . . . . 171.92(12) ?
P1 Au1 P2 C28 . . . . -67.20(12) ?
S2 Au1 P2 C28 . . . . 128.61(11) ?
S1 Au1 P2 C28 . . . . 56.08(11) ?
P1 Au1 P2 C22 . . . . 173.21(13) ?
S2 Au1 P2 C22 . . . . 9.01(13) ?
S1 Au1 P2 C22 . . . . -63.52(13) ?
C3 N1 C1 S1 2_577 . . . 178.5(2) ?
C2 N1 C1 S1 . . . . 6.3(4) ?
C3 N1 C1 S2 2_577 . . . -2.2(4) ?
C2 N1 C1 S2 . . . . -174.4(2) ?
Au1 S1 C1 N1 . . . . 174.8(3) ?
Au1 S1 C1 S2 . . . . -4.50(17) ?
Au1 S2 C1 N1 . . . . -174.6(3) ?
Au1 S2 C1 S1 . . . . 4.70(18) ?
C1 N1 C2 C3 . . . . -131.2(3) ?
C3 N1 C2 C3 2_577 . . . 55.8(4) ?
N1 C2 C3 N1 . . . 2_577 -54.2(4) ?
C10 P1 C4 C5 . . . . 92.7(3) ?
C16 P1 C4 C5 . . . . -156.7(3) ?
Au1 P1 C4 C5 . . . . -30.2(3) ?
C10 P1 C4 C9 . . . . -85.0(3) ?
C16 P1 C4 C9 . . . . 25.6(3) ?
Au1 P1 C4 C9 . . . . 152.0(3) ?
C9 C4 C5 C6 . . . . 0.6(5) ?
P1 C4 C5 C6 . . . . -177.2(3) ?
C4 C5 C6 C7 . . . . -0.7(5) ?
C5 C6 C7 C8 . . . . 0.1(6) ?
C6 C7 C8 C9 . . . . 0.6(6) ?
C7 C8 C9 C4 . . . . -0.6(6) ?
C5 C4 C9 C8 . . . . 0.0(5) ?
P1 C4 C9 C8 . . . . 177.8(3) ?
C4 P1 C10 C11 . . . . -8.8(3) ?
C16 P1 C10 C11 . . . . -117.7(3) ?
Au1 P1 C10 C11 . . . . 113.0(3) ?
C4 P1 C10 C15 . . . . 178.2(3) ?
C16 P1 C10 C15 . . . . 69.4(3) ?
Au1 P1 C10 C15 . . . . -60.0(3) ?
C15 C10 C11 C12 . . . . 0.0(5) ?
P1 C10 C11 C12 . . . . -172.9(3) ?
C10 C11 C12 C13 . . . . -0.5(5) ?
C11 C12 C13 C14 . . . . 0.3(5) ?
C12 C13 C14 C15 . . . . 0.3(5) ?
C13 C14 C15 C10 . . . . -0.8(5) ?
C11 C10 C15 C14 . . . . 0.7(5) ?
P1 C10 C15 C14 . . . . 173.9(3) ?
C10 P1 C16 C17 . . . . -7.7(3) ?
C4 P1 C16 C17 . . . . -116.0(3) ?
Au1 P1 C16 C17 . . . . 120.2(3) ?
C10 P1 C16 C21 . . . . 174.0(3) ?
C4 P1 C16 C21 . . . . 65.7(3) ?
Au1 P1 C16 C21 . . . . -58.0(3) ?
C21 C16 C17 C18 . . . . -0.4(5) ?
P1 C16 C17 C18 . . . . -178.6(3) ?
C16 C17 C18 C19 . . . . -0.6(5) ?
C17 C18 C19 C20 . . . . 0.4(5) ?
C18 C19 C20 C21 . . . . 0.7(5) ?
C19 C20 C21 C16 . . . . -1.7(5) ?
C17 C16 C21 C20 . . . . 1.6(5) ?
P1 C16 C21 C20 . . . . 179.9(3) ?
C34 P2 C22 C23 . . . . 74.3(3) ?
C28 P2 C22 C23 . . . . -176.8(3) ?
Au1 P2 C22 C23 . . . . -54.3(3) ?
C34 P2 C22 C27 . . . . -105.8(3) ?
C28 P2 C22 C27 . . . . 3.1(3) ?
Au1 P2 C22 C27 . . . . 125.6(3) ?
C27 C22 C23 C24 . . . . 2.8(5) ?
P2 C22 C23 C24 . . . . -177.3(3) ?
C22 C23 C24 C25 . . . . -2.4(6) ?
C23 C24 C25 C26 . . . . 0.1(6) ?
C24 C25 C26 C27 . . . . 1.8(5) ?
C25 C26 C27 C22 . . . . -1.5(5) ?
C23 C22 C27 C26 . . . . -0.8(5) ?
P2 C22 C27 C26 . . . . 179.3(3) ?
C34 P2 C28 C33 . . . . 2.9(3) ?
C22 P2 C28 C33 . . . . -106.4(3) ?
Au1 P2 C28 C33 . . . . 124.5(2) ?
C34 P2 C28 C29 . . . . -175.9(2) ?
C22 P2 C28 C29 . . . . 74.8(3) ?
Au1 P2 C28 C29 . . . . -54.3(3) ?
C33 C28 C29 C30 . . . . 0.5(5) ?
P2 C28 C29 C30 . . . . 179.4(3) ?
C28 C29 C30 C31 . . . . -0.6(5) ?
C29 C30 C31 C32 . . . . 0.3(5) ?
C30 C31 C32 C33 . . . . 0.1(5) ?
C29 C28 C33 C32 . . . . -0.1(5) ?
P2 C28 C33 C32 . . . . -178.9(2) ?
C31 C32 C33 C28 . . . . -0.2(5) ?
C28 P2 C34 C39 . . . . 86.8(3) ?
C22 P2 C34 C39 . . . . -164.7(3) ?
Au1 P2 C34 C39 . . . . -32.3(3) ?
C28 P2 C34 C35 . . . . -91.1(3) ?
C22 P2 C34 C35 . . . . 17.5(3) ?
Au1 P2 C34 C35 . . . . 149.9(3) ?
C39 C34 C35 C36 . . . . -0.6(5) ?
P2 C34 C35 C36 . . . . 177.2(3) ?
C34 C35 C36 C37 . . . . -0.9(6) ?
C35 C36 C37 C38 . . . . 1.0(6) ?
C36 C37 C38 C39 . . . . 0.5(6) ?
C35 C34 C39 C38 . . . . 2.1(5) ?
P2 C34 C39 C38 . . . . -175.8(3) ?
C37 C38 C39 C34 . . . . -2.0(5) ?
_iucr_refine_instructions_details
;
TITL DARKWA116 IN P-1 #1
CELL 1.54178 12.8455 13.2879 13.4197 119.572 101.544 96.039
ZERR 1 0.0017 0.001 0.0009 0.002 0.002 0.002
LATT 1
SFAC C N Cl Au S P H
UNIT 80 2 6 2 4 4 70
L.S. 12
PLAN 12
SIZE 0.287 0.346 0.437
TEMP -173.13
REM FCF_FILTER (MSL, UW-MADISON) INSERTED 1 OMIT INSTRUCTIONS
REM FOR OUTLIER REFLECTIONS WITH THE CUTOFF VALUE OF 5.20677.
CONF
HTAB
more -1
BOND $H
REM RESET TO P1 #1
REM The weighting scheme has been updated.
fmap 2.0
acta 134
OMIT -4 1 3
REM C:\Documents%20and%20Settings\Administrator\My%20Documents\Scientific
REM %20papers\Darkwa\darkwa116paper\Refinement\darkwa116.hkl
WGHT 0.041600 3.515900
FVAR 0.10472
AU1 4 0.234436 0.776500 0.653197 11.00000 0.01735 0.01435 =
0.01405 0.00817 0.00798 0.00500
S1 5 0.253869 0.944415 0.886447 11.00000 0.01430 0.02218 =
0.01329 0.00652 0.00515 0.00471
S2 5 0.048734 0.828193 0.686452 11.00000 0.01490 0.02095 =
0.01227 0.00664 0.00443 0.00502
P1 6 0.245641 0.612698 0.671497 11.00000 0.01574 0.01475 =
0.01389 0.00800 0.00582 0.00427
P2 6 0.326539 0.869330 0.579045 11.00000 0.01559 0.01415 =
0.01361 0.00845 0.00629 0.00448
N1 2 0.058525 0.976112 0.914989 11.00000 0.01346 0.02121 =
0.01376 0.00734 0.00491 0.00496
C1 1 0.115459 0.921705 0.836543 11.00000 0.01676 0.01526 =
0.01550 0.00849 0.00575 0.00246
C2 1 0.111502 1.064497 1.041759 11.00000 0.01747 0.02100 =
0.01515 0.00584 0.00563 0.00360
AFIX 23
H2A 7 0.105119 1.144582 1.058406 11.00000 -1.20000
H2B 7 0.190255 1.065492 1.061425 11.00000 -1.20000
AFIX 0
C3 1 0.058979 1.035949 1.119945 11.00000 0.01564 0.02596 =
0.01471 0.00863 0.00617 0.00790
AFIX 23
H3A 7 0.073684 0.960822 1.111331 11.00000 -1.20000
H3B 7 0.091293 1.100479 1.205017 11.00000 -1.20000
AFIX 0
C4 1 0.362815 0.645634 0.794061 11.00000 0.01968 0.01993 =
0.01454 0.00767 0.00623 0.00682
C5 1 0.456806 0.730066 0.825415 11.00000 0.02235 0.01986 =
0.01702 0.00540 0.00772 0.00415
AFIX 43
H5 7 0.458105 0.772304 0.785411 11.00000 -1.20000
AFIX 0
C6 1 0.548833 0.752736 0.915189 11.00000 0.02010 0.03150 =
0.02247 0.00570 0.00671 0.00789
AFIX 43
H6 7 0.613042 0.809790 0.935685 11.00000 -1.20000
AFIX 0
C7 1 0.547139 0.692716 0.974445 11.00000 0.02799 0.04139 =
0.01680 0.00913 0.00446 0.01849
AFIX 43
H7 7 0.610099 0.708498 1.035744 11.00000 -1.20000
AFIX 0
C8 1 0.453657 0.609337 0.944691 11.00000 0.03452 0.04264 =
0.02432 0.02252 0.01153 0.02026
AFIX 43
H8 7 0.452628 0.568704 0.986299 11.00000 -1.20000
AFIX 0
C9 1 0.362015 0.584887 0.855033 11.00000 0.02652 0.02890 =
0.02366 0.01748 0.01019 0.01095
AFIX 43
H9 7 0.298465 0.527045 0.834572 11.00000 -1.20000
AFIX 0
C10 1 0.267507 0.487085 0.542366 11.00000 0.02176 0.01280 =
0.01593 0.00804 0.00895 0.00545
C11 1 0.363156 0.448655 0.547381 11.00000 0.02090 0.01902 =
0.02112 0.01053 0.00522 0.00691
AFIX 43
H11 7 0.417113 0.482519 0.622293 11.00000 -1.20000
AFIX 0
C12 1 0.381296 0.360125 0.442897 11.00000 0.02425 0.02231 =
0.02846 0.01237 0.01166 0.00869
AFIX 43
H12 7 0.447526 0.334575 0.446954 11.00000 -1.20000
AFIX 0
C13 1 0.302540 0.310111 0.333948 11.00000 0.02999 0.01569 =
0.02190 0.00713 0.01299 0.00616
AFIX 43
H13 7 0.314470 0.249783 0.263063 11.00000 -1.20000
AFIX 0
C14 1 0.206706 0.347662 0.328022 11.00000 0.02433 0.01984 =
0.01662 0.00839 0.00369 0.00267
AFIX 43
H14 7 0.152651 0.312767 0.252996 11.00000 -1.20000
AFIX 0
C15 1 0.188655 0.436237 0.431094 11.00000 0.01989 0.01842 =
0.02000 0.01085 0.00598 0.00534
AFIX 43
H15 7 0.122813 0.462383 0.426177 11.00000 -1.20000
AFIX 0
C16 1 0.129785 0.553121 0.702170 11.00000 0.01555 0.01998 =
0.02042 0.01426 0.00532 0.00619
C17 1 0.065808 0.437583 0.628215 11.00000 0.01930 0.01945 =
0.02058 0.01250 0.00608 0.00624
AFIX 43
H17 7 0.082271 0.383550 0.557384 11.00000 -1.20000
AFIX 0
C18 1 -0.022921 0.400488 0.657753 11.00000 0.01960 0.02598 =
0.02861 0.01852 0.00428 0.00126
AFIX 43
H18 7 -0.067042 0.321477 0.606550 11.00000 -1.20000
AFIX 0
C19 1 -0.046724 0.478789 0.761693 11.00000 0.01728 0.03673 =
0.03213 0.02698 0.00894 0.00668
AFIX 43
H19 7 -0.106707 0.453415 0.782049 11.00000 -1.20000
AFIX 0
C20 1 0.017426 0.594063 0.835533 11.00000 0.02633 0.03339 =
0.02365 0.01888 0.01229 0.01155
AFIX 43
H20 7 0.001709 0.647436 0.907153 11.00000 -1.20000
AFIX 0
C21 1 0.104169 0.632228 0.805995 11.00000 0.02331 0.02059 =
0.02023 0.01222 0.00790 0.00525
AFIX 43
H21 7 0.146449 0.712145 0.856118 11.00000 -1.20000
AFIX 0
C22 1 0.279825 0.989407 0.567247 11.00000 0.02163 0.01870 =
0.01690 0.01134 0.01047 0.00952
C23 1 0.171850 0.967840 0.504947 11.00000 0.02216 0.02180 =
0.02391 0.01321 0.00735 0.00686
AFIX 43
H23 7 0.123315 0.892923 0.472564 11.00000 -1.20000
AFIX 0
C24 1 0.133814 1.055006 0.489364 11.00000 0.02716 0.03206 =
0.02807 0.01914 0.00897 0.01293
AFIX 43
H24 7 0.060409 1.038184 0.443850 11.00000 -1.20000
AFIX 0
C25 1 0.202533 1.165836 0.539909 11.00000 0.03237 0.02986 =
0.03083 0.02161 0.01623 0.01905
AFIX 43
H25 7 0.176391 1.225176 0.529273 11.00000 -1.20000
AFIX 0
C26 1 0.309941 1.190359 0.606321 11.00000 0.03009 0.01884 =
0.02758 0.01343 0.01245 0.00674
AFIX 43
H26 7 0.356706 1.267236 0.643111 11.00000 -1.20000
AFIX 0
C27 1 0.349102 1.101833 0.618941 11.00000 0.02026 0.02182 =
0.02444 0.01424 0.00804 0.00773
AFIX 43
H27 7 0.423032 1.118082 0.662784 11.00000 -1.20000
AFIX 0
C28 1 0.467777 0.938435 0.673617 11.00000 0.01764 0.01523 =
0.01732 0.01081 0.00474 0.00447
C29 1 0.485572 1.017658 0.796651 11.00000 0.01802 0.02217 =
0.01822 0.01145 0.00678 0.00617
AFIX 43
H29 7 0.424934 1.034087 0.827587 11.00000 -1.20000
AFIX 0
C30 1 0.591040 1.072005 0.873195 11.00000 0.02285 0.02394 =
0.01646 0.01043 0.00443 0.00600
AFIX 43
H30 7 0.602660 1.126179 0.956295 11.00000 -1.20000
AFIX 0
C31 1 0.679698 1.047289 0.828448 11.00000 0.01579 0.02379 =
0.02400 0.01433 0.00269 0.00562
AFIX 43
H31 7 0.751973 1.084402 0.881226 11.00000 -1.20000
AFIX 0
C32 1 0.663655 0.969106 0.707706 11.00000 0.02031 0.02358 =
0.02519 0.01543 0.01102 0.01140
AFIX 43
H32 7 0.724738 0.952436 0.677647 11.00000 -1.20000
AFIX 0
C33 1 0.557448 0.914545 0.629799 11.00000 0.01990 0.01918 =
0.01990 0.01320 0.00804 0.00697
AFIX 43
H33 7 0.546421 0.860994 0.546692 11.00000 -1.20000
AFIX 0
C34 1 0.338628 0.766608 0.431154 11.00000 0.01286 0.01719 =
0.01519 0.00751 0.00476 0.00407
C35 1 0.343458 0.799528 0.347598 11.00000 0.02747 0.01934 =
0.01758 0.01090 0.00863 0.00616
AFIX 43
H35 7 0.337153 0.876948 0.365720 11.00000 -1.20000
AFIX 0
C36 1 0.357485 0.718913 0.238074 11.00000 0.03083 0.03094 =
0.01862 0.01617 0.01111 0.00785
AFIX 43
H36 7 0.359675 0.740995 0.180989 11.00000 -1.20000
AFIX 0
C37 1 0.368263 0.606667 0.211927 11.00000 0.02313 0.02371 =
0.01516 0.00591 0.00965 0.00527
AFIX 43
H37 7 0.378968 0.552406 0.137438 11.00000 -1.20000
AFIX 0
C38 1 0.363508 0.572919 0.294061 11.00000 0.02393 0.01924 =
0.02236 0.00926 0.01016 0.00642
AFIX 43
H38 7 0.371488 0.496030 0.276281 11.00000 -1.20000
AFIX 0
C39 1 0.346962 0.652606 0.402640 11.00000 0.01961 0.02078 =
0.01693 0.01093 0.00677 0.00511
AFIX 43
H39 7 0.341306 0.628788 0.457849 11.00000 -1.20000
AFIX 0
CL1 3 0.157387 0.410534 0.951745 11.00000 0.03973 0.02985 =
0.04509 0.01121 0.00010 -0.00120
CL2 3 0.146768 0.158464 0.817008 11.00000 0.06076 0.03422 =
0.05470 0.02764 0.02784 0.01796
CL3 3 -0.052651 0.241273 0.821143 11.00000 0.03546 0.04198 =
0.03460 0.02300 0.00282 -0.00202
C40 1 0.084833 0.272108 0.823234 11.00000 0.03529 0.03038 =
0.02644 0.01828 0.00480 0.00087
AFIX 13
H40 7 0.086328 0.276218 0.751092 11.00000 -1.20000
HKLF 4
REM DARKWA116 IN P-1 #1
REM R1 = 0.0281 for 7080 Fo > 4sig(Fo) and 0.0281 for all 7089 data
REM 442 parameters refined using 0 restraints
END
WGHT 0.0415 3.5072
REM Highest difference peak 2.398, deepest hole -1.349, 1-sigma level 0.112
Q1 1 0.3010 0.7653 0.6602 11.00000 0.05 2.40
Q2 1 0.1627 0.7805 0.6414 11.00000 0.05 2.20
Q3 1 0.2397 0.7110 0.5941 11.00000 0.05 1.61
Q4 1 0.2585 0.5487 0.6095 11.00000 0.05 0.74
Q5 1 0.3080 0.9267 0.5731 11.00000 0.05 0.60
Q6 1 0.4013 0.8977 0.6146 11.00000 0.05 0.60
Q7 1 0.1795 0.9403 0.8635 11.00000 0.05 0.57
Q8 1 0.1627 0.3624 0.9726 11.00000 0.05 0.54
Q9 1 0.0834 0.7783 0.6585 11.00000 0.05 0.52
Q10 1 0.2535 0.8677 0.5740 11.00000 0.05 0.50
Q11 1 -0.0229 0.8448 0.6889 11.00000 0.05 0.49
Q12 1 0.1622 0.6692 0.5979 11.00000 0.05 0.49
;