# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2015
#######################################################################
#
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1049919'
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PUBL004_GLOBAL
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PROBLEM: _publ_author_name is missing. List of author(s) name(s).
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_vrf_DIFF005_4
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PROBLEM: _diffrn_measurement_method is missing
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# end Validation Reply Form
#Added by publCIF (mar 17. feb 11:28:58 2015)
_publcif_datablock.id {39179c3d-a75c-4c35-9e89-986fe0cc1011}
_audit_creation_method SHELXL-2013
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C25 H20 Au Br F3 P'
_chemical_formula_weight 685.26
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Br Br -0.2901 2.4595 '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'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 8.3781(2)
_cell_length_b 14.3827(2)
_cell_length_c 19.3153(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2327.49(7)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9467
_cell_measurement_theta_min 4.2274
_cell_measurement_theta_max 28.8283
_exptl_crystal_description prismatic
_exptl_crystal_colour colourless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.956
_exptl_crystal_F_000 1304
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.390
_exptl_crystal_size_mid 0.270
_exptl_crystal_size_min 0.160
_exptl_absorpt_coefficient_mu 8.140
_shelx_estimated_absorpt_T_min 0.143
_shelx_estimated_absorpt_T_max 0.356
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.49711
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Xcalibur, Sapphire3'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_reflns_number 14688
_diffrn_reflns_av_unetI/netI 0.0271
_diffrn_reflns_av_R_equivalents 0.0223
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 4.236
_diffrn_reflns_theta_max 28.892
_diffrn_reflns_theta_full 25.000
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_orient_matrix_UB_11 -0.0289143000
_diffrn_orient_matrix_UB_12 0.0093873000
_diffrn_orient_matrix_UB_13 0.0337916000
_diffrn_orient_matrix_UB_21 -0.0199847000
_diffrn_orient_matrix_UB_22 0.0458755000
_diffrn_orient_matrix_UB_23 -0.0102752000
_diffrn_orient_matrix_UB_31 -0.0770721000
_diffrn_orient_matrix_UB_32 -0.0154133000
_diffrn_orient_matrix_UB_33 -0.0100281000
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -31.00 -4.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- -19.9615 77.0000 30.0000 27
#__ type_ start__ end____ width___ exp.time_
2 omega -31.00 86.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 22.1490 19.0000 -180.0000 117
#__ type_ start__ end____ width___ exp.time_
3 omega -48.00 38.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 22.1490 -57.0000 150.0000 86
#__ type_ start__ end____ width___ exp.time_
4 omega -11.00 95.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 22.1490 77.0000 -120.0000 106
;
_reflns_number_total 5377
_reflns_number_gt 5203
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.777
_reflns_Friedel_fraction_max 0.921
_reflns_Friedel_fraction_full 0.998
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution ?
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refined as a 2-component inversion twin.
;
_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^)+(0.0267P)^2^+3.1182P] 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_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.311(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns 5377
_refine_ls_number_parameters 281
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0253
_refine_ls_R_factor_gt 0.0234
_refine_ls_wR_factor_ref 0.0549
_refine_ls_wR_factor_gt 0.0542
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_restrained_S_all 1.067
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Au Au 0.21041(3) 0.57254(2) 0.43384(2) 0.01797(6) Uani 1 1 d . . . . .
Br Br 0.20646(9) 0.40653(4) 0.44858(3) 0.02899(14) Uani 1 1 d . . . . .
F1 F 0.0763(5) 0.7535(3) 0.4516(2) 0.0371(10) Uani 1 1 d . . . . .
F2 F 0.3327(5) 0.7579(3) 0.4482(3) 0.0529(14) Uani 1 1 d . . . . .
F3 F 0.1996(6) 0.7418(3) 0.3551(2) 0.0439(10) Uani 1 1 d . . . . .
C1 C 0.2053(7) 0.7192(4) 0.4234(2) 0.0161(10) Uani 1 1 d . U . . .
P P 0.49930(17) 0.58958(9) 0.17822(7) 0.0134(3) Uani 1 1 d . . . . .
C2 C 0.3725(8) 0.6892(4) 0.1684(3) 0.0158(11) Uani 1 1 d . . . . .
C3 C 0.2164(9) 0.6786(4) 0.1437(3) 0.0220(12) Uani 1 1 d . . . . .
H3 H 0.1764 0.6185 0.1329 0.026 Uiso 1 1 calc R U . . .
C4 C 0.1218(8) 0.7551(5) 0.1351(3) 0.0260(14) Uani 1 1 d . . . . .
H4 H 0.0153 0.7476 0.1192 0.031 Uiso 1 1 calc R U . . .
C5 C 0.1784(8) 0.8429(4) 0.1492(3) 0.0235(14) Uani 1 1 d . . . . .
H5 H 0.1117 0.8955 0.1423 0.028 Uiso 1 1 calc R U . . .
C6 C 0.3335(8) 0.8545(4) 0.1734(3) 0.0221(13) Uani 1 1 d . . . . .
H6 H 0.3729 0.9151 0.1830 0.027 Uiso 1 1 calc R U . . .
C7 C 0.4304(7) 0.7777(4) 0.1835(3) 0.0192(12) Uani 1 1 d . . . . .
H7 H 0.5358 0.7853 0.2007 0.023 Uiso 1 1 calc R U . . .
C8 C 0.3739(7) 0.4894(4) 0.1852(3) 0.0160(11) Uani 1 1 d . . . . .
C9 C 0.3226(8) 0.4441(4) 0.1251(3) 0.0225(13) Uani 1 1 d . . . . .
H9 H 0.3650 0.4621 0.0814 0.027 Uiso 1 1 calc R U . . .
C10 C 0.2120(10) 0.3741(4) 0.1285(3) 0.0263(13) Uani 1 1 d . . . . .
H10 H 0.1798 0.3427 0.0875 0.032 Uiso 1 1 calc R U . . .
C11 C 0.1473(8) 0.3492(4) 0.1917(4) 0.0256(14) Uani 1 1 d . . . . .
H11 H 0.0685 0.3018 0.1939 0.031 Uiso 1 1 calc R U . . .
C12 C 0.1970(8) 0.3933(4) 0.2520(3) 0.0214(12) Uani 1 1 d . . . . .
H12 H 0.1532 0.3756 0.2954 0.026 Uiso 1 1 calc R U . . .
C13 C 0.3113(7) 0.4633(4) 0.2485(3) 0.0169(11) Uani 1 1 d . . . . .
H13 H 0.3464 0.4932 0.2896 0.020 Uiso 1 1 calc R U . . .
C14 C 0.6176(7) 0.6048(4) 0.2549(3) 0.0154(11) Uani 1 1 d . . . . .
C15 C 0.5462(7) 0.6375(4) 0.3156(3) 0.0188(12) Uani 1 1 d . . . . .
H15 H 0.4370 0.6554 0.3153 0.023 Uiso 1 1 calc R U . . .
C16 C 0.6338(9) 0.6440(4) 0.3758(3) 0.0227(13) Uani 1 1 d . . . . .
H16 H 0.5844 0.6656 0.4170 0.027 Uiso 1 1 calc R U . . .
C17 C 0.7933(9) 0.6190(4) 0.3765(3) 0.0221(12) Uani 1 1 d . . . . .
H17 H 0.8529 0.6232 0.4183 0.026 Uiso 1 1 calc R U . . .
C18 C 0.8666(7) 0.5876(4) 0.3161(3) 0.0198(12) Uani 1 1 d . . . . .
H18 H 0.9765 0.5712 0.3165 0.024 Uiso 1 1 calc R U . . .
C19 C 0.7789(7) 0.5805(4) 0.2555(3) 0.0179(10) Uani 1 1 d . . . . .
H19 H 0.8287 0.5591 0.2143 0.021 Uiso 1 1 calc R U . . .
C20 C 0.6335(7) 0.5769(4) 0.1067(2) 0.0148(10) Uani 1 1 d . . . . .
C21 C 0.7058(9) 0.4909(4) 0.0944(3) 0.0238(12) Uani 1 1 d . . . . .
H21 H 0.6746 0.4377 0.1201 0.029 Uiso 1 1 calc R U . . .
C22 C 0.8230(8) 0.4842(5) 0.0445(3) 0.0261(14) Uani 1 1 d . . . . .
H22 H 0.8730 0.4260 0.0359 0.031 Uiso 1 1 calc R U . . .
C23 C 0.8681(8) 0.5618(5) 0.0067(3) 0.0289(14) Uani 1 1 d . . . . .
H23 H 0.9491 0.5564 -0.0274 0.035 Uiso 1 1 calc R U . . .
C24 C 0.7970(10) 0.6466(4) 0.0182(3) 0.0253(13) Uani 1 1 d . . . . .
H24 H 0.8283 0.6994 -0.0080 0.030 Uiso 1 1 calc R U . . .
C25 C 0.6779(7) 0.6545(4) 0.0688(3) 0.0182(11) Uani 1 1 d . . . . .
H25 H 0.6279 0.7127 0.0770 0.022 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
Au 0.01505(10) 0.02227(10) 0.01659(9) -0.00069(8) -0.00174(9) 0.00144(10)
Br 0.0288(3) 0.0252(3) 0.0329(3) -0.0011(2) -0.0051(3) -0.0036(3)
F1 0.028(2) 0.034(2) 0.049(3) -0.007(2) 0.0059(18) 0.0082(18)
F2 0.032(2) 0.027(2) 0.100(4) 0.002(3) -0.025(3) -0.0026(18)
F3 0.050(3) 0.042(2) 0.040(2) 0.0143(18) 0.005(2) 0.014(3)
C1 0.0117(14) 0.0215(14) 0.0152(14) 0.0021(11) 0.0000(12) 0.0012(12)
P 0.0139(7) 0.0127(7) 0.0136(6) -0.0007(5) -0.0004(5) 0.0003(5)
C2 0.016(3) 0.016(3) 0.016(3) -0.001(2) 0.001(2) 0.003(2)
C3 0.019(3) 0.020(3) 0.028(3) -0.002(2) -0.007(3) -0.002(3)
C4 0.015(3) 0.028(3) 0.034(3) -0.003(3) -0.003(3) 0.001(3)
C5 0.022(4) 0.017(3) 0.031(3) -0.004(2) 0.002(3) 0.003(2)
C6 0.024(4) 0.016(3) 0.026(3) -0.003(2) 0.000(3) 0.000(2)
C7 0.016(3) 0.017(3) 0.024(3) -0.003(2) -0.003(2) -0.002(2)
C8 0.016(3) 0.014(2) 0.018(3) -0.001(2) 0.000(2) 0.000(2)
C9 0.030(4) 0.020(3) 0.017(2) -0.001(2) -0.002(2) -0.004(3)
C10 0.033(3) 0.020(3) 0.026(3) -0.003(2) -0.005(3) -0.005(3)
C11 0.024(3) 0.013(3) 0.039(4) -0.002(3) -0.003(3) -0.007(2)
C12 0.020(3) 0.017(2) 0.027(3) 0.004(2) 0.002(3) -0.003(3)
C13 0.014(3) 0.017(2) 0.020(2) 0.002(2) -0.004(2) 0.000(2)
C14 0.017(3) 0.013(2) 0.016(2) 0.004(2) -0.004(2) 0.000(2)
C15 0.017(3) 0.019(3) 0.020(3) 0.000(2) -0.001(2) -0.003(3)
C16 0.023(3) 0.026(3) 0.019(3) -0.001(2) 0.000(3) 0.000(3)
C17 0.024(3) 0.021(3) 0.021(3) 0.002(2) -0.009(3) -0.002(3)
C18 0.014(3) 0.018(3) 0.027(3) 0.003(2) -0.004(2) -0.001(2)
C19 0.018(3) 0.017(2) 0.019(2) -0.001(2) 0.000(2) -0.004(3)
C20 0.015(3) 0.017(2) 0.012(2) -0.001(2) -0.0002(19) 0.002(3)
C21 0.030(3) 0.017(3) 0.025(3) 0.001(2) 0.001(3) 0.005(3)
C22 0.028(4) 0.024(3) 0.026(3) -0.006(2) 0.005(3) 0.005(3)
C23 0.026(3) 0.039(4) 0.022(3) -0.004(3) 0.006(3) 0.003(3)
C24 0.028(3) 0.029(3) 0.019(2) 0.003(2) 0.007(3) -0.009(3)
C25 0.015(3) 0.017(2) 0.022(2) -0.001(2) 0.001(3) 0.000(2)
_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
Au C1 2.119(5) . ?
Au Br 2.4049(6) . ?
F1 C1 1.307(7) . ?
F2 C1 1.296(7) . ?
F3 C1 1.360(6) . ?
P C8 1.789(6) . ?
P C20 1.790(5) . ?
P C2 1.794(6) . ?
P C14 1.796(6) . ?
C2 C7 1.394(8) . ?
C2 C3 1.400(9) . ?
C3 C4 1.366(9) . ?
C4 C5 1.375(9) . ?
C5 C6 1.391(10) . ?
C6 C7 1.384(8) . ?
C8 C13 1.381(8) . ?
C8 C9 1.399(7) . ?
C9 C10 1.371(9) . ?
C10 C11 1.383(9) . ?
C11 C12 1.390(9) . ?
C12 C13 1.392(8) . ?
C14 C19 1.396(8) . ?
C14 C15 1.397(8) . ?
C15 C16 1.379(8) . ?
C16 C17 1.384(10) . ?
C17 C18 1.394(9) . ?
C18 C19 1.386(8) . ?
C20 C25 1.386(8) . ?
C20 C21 1.397(8) . ?
C21 C22 1.379(9) . ?
C22 C23 1.387(9) . ?
C23 C24 1.374(9) . ?
C24 C25 1.401(9) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au Br 177.64(15) . . ?
F2 C1 F1 111.4(5) . . ?
F2 C1 F3 106.6(5) . . ?
F1 C1 F3 106.5(5) . . ?
F2 C1 Au 112.1(4) . . ?
F1 C1 Au 110.6(4) . . ?
F3 C1 Au 109.3(3) . . ?
C8 P C20 110.2(3) . . ?
C8 P C2 107.7(3) . . ?
C20 P C2 111.8(3) . . ?
C8 P C14 111.1(3) . . ?
C20 P C14 107.6(3) . . ?
C2 P C14 108.5(3) . . ?
C7 C2 C3 119.7(6) . . ?
C7 C2 P 120.1(5) . . ?
C3 C2 P 120.2(5) . . ?
C4 C3 C2 119.7(6) . . ?
C3 C4 C5 121.0(6) . . ?
C4 C5 C6 119.9(6) . . ?
C7 C6 C5 120.0(6) . . ?
C6 C7 C2 119.7(5) . . ?
C13 C8 C9 119.5(5) . . ?
C13 C8 P 120.6(4) . . ?
C9 C8 P 119.5(4) . . ?
C10 C9 C8 120.6(5) . . ?
C9 C10 C11 119.9(5) . . ?
C10 C11 C12 120.3(6) . . ?
C11 C12 C13 119.7(5) . . ?
C8 C13 C12 120.1(5) . . ?
C19 C14 C15 119.5(5) . . ?
C19 C14 P 120.7(4) . . ?
C15 C14 P 119.8(5) . . ?
C16 C15 C14 120.2(6) . . ?
C15 C16 C17 120.3(6) . . ?
C16 C17 C18 120.1(6) . . ?
C19 C18 C17 119.8(6) . . ?
C18 C19 C14 120.1(5) . . ?
C25 C20 C21 120.4(5) . . ?
C25 C20 P 119.6(4) . . ?
C21 C20 P 119.6(4) . . ?
C22 C21 C20 119.4(5) . . ?
C21 C22 C23 120.3(6) . . ?
C24 C23 C22 120.8(6) . . ?
C23 C24 C25 119.5(5) . . ?
C20 C25 C24 119.7(5) . . ?
_refine_diff_density_max 1.292
_refine_diff_density_min -1.059
_refine_diff_density_rms 0.117
_shelxl_version_number 2013-4
_shelx_res_file
;
TITL amt731 in P2(1)2(1)2(1)
CELL 0.71073 8.3781 14.3827 19.3153 90.000 90.000 90.000
ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.000 0.000
LATT -1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H F P BR AU
UNIT 100 80 12 4 4 4
L.S. 10
BOND
FMAP 2
PLAN 5
acta 50
temp -173
list 4
size .39 .27 .16
rem colourless prismatic
twin
isor 0.001 c1
WGHT 0.026700 3.118200
BASF 0.31139
FVAR 1.74171
AU 6 0.210412 0.572540 0.433836 11.00000 0.01505 0.02227 =
0.01659 -0.00069 -0.00174 0.00144
BR 5 0.206458 0.406526 0.448575 11.00000 0.02884 0.02524 =
0.03288 -0.00114 -0.00514 -0.00355
F1 3 0.076275 0.753465 0.451574 11.00000 0.02812 0.03420 =
0.04904 -0.00738 0.00592 0.00825
F2 3 0.332684 0.757882 0.448242 11.00000 0.03213 0.02699 =
0.09950 0.00245 -0.02516 -0.00262
F3 3 0.199583 0.741826 0.355093 11.00000 0.04979 0.04236 =
0.03957 0.01427 0.00539 0.01415
C1 1 0.205307 0.719183 0.423405 11.00000 0.01172 0.02148 =
0.01519 0.00210 -0.00004 0.00124
P 4 0.499305 0.589579 0.178219 11.00000 0.01394 0.01271 =
0.01359 -0.00071 -0.00045 0.00028
C2 1 0.372455 0.689152 0.168351 11.00000 0.01588 0.01567 =
0.01579 -0.00111 0.00092 0.00300
C3 1 0.216367 0.678635 0.143664 11.00000 0.01870 0.01974 =
0.02755 -0.00227 -0.00733 -0.00168
AFIX 43
H3 2 0.176390 0.618541 0.132895 11.00000 -1.20000
AFIX 0
C4 1 0.121835 0.755139 0.135130 11.00000 0.01527 0.02832 =
0.03438 -0.00268 -0.00322 0.00095
AFIX 43
H4 2 0.015300 0.747619 0.119246 11.00000 -1.20000
AFIX 0
C5 1 0.178420 0.842873 0.149165 11.00000 0.02235 0.01720 =
0.03106 -0.00395 0.00151 0.00273
AFIX 43
H5 2 0.111702 0.895487 0.142334 11.00000 -1.20000
AFIX 0
C6 1 0.333499 0.854472 0.173382 11.00000 0.02429 0.01566 =
0.02635 -0.00297 -0.00027 -0.00026
AFIX 43
H6 2 0.372913 0.915052 0.182969 11.00000 -1.20000
AFIX 0
C7 1 0.430378 0.777701 0.183505 11.00000 0.01622 0.01732 =
0.02410 -0.00330 -0.00319 -0.00248
AFIX 43
H7 2 0.535810 0.785324 0.200694 11.00000 -1.20000
AFIX 0
C8 1 0.373878 0.489377 0.185233 11.00000 0.01605 0.01404 =
0.01804 -0.00106 -0.00035 0.00029
C9 1 0.322646 0.444125 0.125065 11.00000 0.03036 0.02019 =
0.01699 -0.00122 -0.00187 -0.00362
AFIX 43
H9 2 0.364976 0.462122 0.081450 11.00000 -1.20000
AFIX 0
C10 1 0.211987 0.374090 0.128460 11.00000 0.03251 0.02007 =
0.02642 -0.00319 -0.00489 -0.00529
AFIX 43
H10 2 0.179805 0.342726 0.087487 11.00000 -1.20000
AFIX 0
C11 1 0.147260 0.349173 0.191687 11.00000 0.02422 0.01312 =
0.03939 -0.00178 -0.00337 -0.00708
AFIX 43
H11 2 0.068490 0.301755 0.193906 11.00000 -1.20000
AFIX 0
C12 1 0.197037 0.393252 0.251971 11.00000 0.02029 0.01727 =
0.02668 0.00379 0.00168 -0.00315
AFIX 43
H12 2 0.153221 0.375632 0.295395 11.00000 -1.20000
AFIX 0
C13 1 0.311346 0.463317 0.248457 11.00000 0.01385 0.01729 =
0.01968 0.00243 -0.00384 -0.00010
AFIX 43
H13 2 0.346367 0.493231 0.289592 11.00000 -1.20000
AFIX 0
C14 1 0.617642 0.604834 0.254938 11.00000 0.01727 0.01289 =
0.01611 0.00380 -0.00365 -0.00033
C15 1 0.546213 0.637540 0.315561 11.00000 0.01704 0.01927 =
0.02017 0.00038 -0.00103 -0.00261
AFIX 43
H15 2 0.437046 0.655395 0.315284 11.00000 -1.20000
AFIX 0
C16 1 0.633782 0.643974 0.375820 11.00000 0.02307 0.02646 =
0.01855 -0.00117 -0.00008 0.00002
AFIX 43
H16 2 0.584369 0.665648 0.417042 11.00000 -1.20000
AFIX 0
C17 1 0.793344 0.619005 0.376535 11.00000 0.02436 0.02090 =
0.02090 0.00155 -0.00901 -0.00235
AFIX 43
H17 2 0.852949 0.623249 0.418256 11.00000 -1.20000
AFIX 0
C18 1 0.866646 0.587648 0.316119 11.00000 0.01429 0.01833 =
0.02671 0.00284 -0.00355 -0.00095
AFIX 43
H18 2 0.976455 0.571184 0.316485 11.00000 -1.20000
AFIX 0
C19 1 0.778937 0.580537 0.255479 11.00000 0.01767 0.01699 =
0.01901 -0.00053 0.00032 -0.00395
AFIX 43
H19 2 0.828664 0.559107 0.214258 11.00000 -1.20000
AFIX 0
C20 1 0.633478 0.576882 0.106725 11.00000 0.01533 0.01703 =
0.01207 -0.00138 -0.00019 0.00175
C21 1 0.705805 0.490947 0.094391 11.00000 0.02967 0.01667 =
0.02492 0.00072 0.00141 0.00524
AFIX 43
H21 2 0.674575 0.437685 0.120133 11.00000 -1.20000
AFIX 0
C22 1 0.822994 0.484157 0.044482 11.00000 0.02819 0.02368 =
0.02650 -0.00627 0.00468 0.00478
AFIX 43
H22 2 0.873030 0.426006 0.035935 11.00000 -1.20000
AFIX 0
C23 1 0.868076 0.561847 0.006733 11.00000 0.02573 0.03879 =
0.02225 -0.00350 0.00623 0.00308
AFIX 43
H23 2 0.949077 0.556447 -0.027449 11.00000 -1.20000
AFIX 0
C24 1 0.796952 0.646558 0.018191 11.00000 0.02788 0.02929 =
0.01872 0.00259 0.00687 -0.00948
AFIX 43
H24 2 0.828313 0.699392 -0.008005 11.00000 -1.20000
AFIX 0
C25 1 0.677906 0.654460 0.068759 11.00000 0.01499 0.01727 =
0.02239 -0.00144 0.00110 0.00045
AFIX 43
H25 2 0.627865 0.712690 0.076994 11.00000 -1.20000
AFIX 0
HKLF 4
REM amt731 in P2(1)2(1)2(1)
REM R1 = 0.0234 for 5203 Fo > 4sig(Fo) and 0.0253 for all 5377 data
REM 281 parameters refined using 6 restraints
END
WGHT 0.0270 3.1597
REM Highest difference peak 1.292, deepest hole -1.059, 1-sigma level 0.117
Q1 1 0.2083 0.7554 0.4318 11.00000 0.05 1.29
Q2 1 0.2060 0.6763 0.4262 11.00000 0.05 1.16
Q3 1 0.2057 0.5038 0.4355 11.00000 0.05 1.11
Q4 1 0.2097 0.6442 0.4336 11.00000 0.05 0.97
Q5 1 0.0801 0.3929 0.4410 11.00000 0.05 0.66
;
_shelx_res_checksum 39212
#######################################################################
#
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1049920'
# end Validation Reply Form
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
_publcif_datablock.id {4188dfa1-2432-4abf-a834-4c707628924e}
# start Validation Reply Form
_vrf_PLAT213_3
;
PROBLEM: Atom C14 has ADP max/min Ratio ..... 7.1 oblate
RESPONSE: This is a result of twinning. See the detailed
description in the supporting information.
;
_vrf_PLAT215_3
;
PROBLEM: Disordered F6A has ADP max/min Ratio ..... 9.1
RESPONSE: This is a result of twinning and disorder. There
is a detailed description and a specific comment about this
atom in the supporting information.
;
# publcif _publ_body_element loop end
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C24 H20 P +1, C2 Au2 Br F6 -1, C H2 Cl2 '
_chemical_formula_sum 'C27 H22 Au2 Br Cl2 F6 P'
_chemical_formula_weight 1036.16
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'
F F 0.0171 0.0103 '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'
Br Br -0.2901 2.4595 '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'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/n'
_space_group_name_Hall '-P 2yn'
_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
# Cell from amt770_tw4L_twin1_hklf4.cif_od
_cell_length_a 11.2208(16)
_cell_length_b 16.168(3)
_cell_length_c 17.031(3)
_cell_angle_alpha 90
_cell_angle_beta 108.049(19)
_cell_angle_gamma 90
_cell_volume 2937.7(9)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(1)
_cell_measurement_reflns_used 1637
_cell_measurement_theta_min 8.6080
_cell_measurement_theta_max 27.8550
_exptl_crystal_description needle
_exptl_crystal_colour colourless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 2.343
_exptl_crystal_F_000 1920
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.53
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_exptl_absorpt_coefficient_mu 11.628
#
# Internal note (LRF)
# Data used for refinement from amt770_tw3Lv37_twin1_hklf5
_exptl_absorpt_correction_T_min 0.69916
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Multi-scan absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_diffrn_ambient_temperature 100(1)
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Sapphire3'
_diffrn_detector 'CCD plate'
_diffrn_detector_type Sapphire3
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measurement_method '\w scans'
_diffrn_reflns_number 10326
_diffrn_reflns_av_unetI/netI 0.0954
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 4.236
_diffrn_reflns_theta_max 27.490
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total 10326
_reflns_number_gt 6600
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
See the following loop with _cell_oxdiff_* data items. The
crystal was treated as having three domains.
_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.
;
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -1.0020 0.0008 0.0019 -0.0043 -1.0020 -0.0052 0.9450 -0.0072 0.9997
3 -1.0078 0.0143 -0.0230 0.0281 1.0012 -0.0049 0.0545 -0.0118 -0.9876
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution
;
SIR-92;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
;
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics
;
Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material
;
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920--925.
;
_refine_special_details
;
Refined as a 3-component twin. See the experimental details in the manuscript
and supporting information.
;
_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^)+(0.1652P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_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 10326
_refine_ls_number_parameters 390
_refine_ls_number_restraints 210
_refine_ls_R_factor_all 0.1135
_refine_ls_R_factor_gt 0.0813
_refine_ls_wR_factor_ref 0.2633
_refine_ls_wR_factor_gt 0.2471
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_restrained_S_all 1.081
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Br1 Br 0.4730(2) 0.13127(14) 0.40915(14) 0.0410(6) Uani 0.5 1 d . . P . .
Au1 Au 0.40766(12) 0.09581(10) 0.52807(9) 0.0246(4) Uani 0.5 1 d D . P A -1
C1 C 0.3238(13) 0.0940(11) 0.6147(10) 0.048(3) Uani 0.5 1 d D U P A -1
F1 F 0.2006(9) 0.0891(9) 0.6080(8) 0.056(3) Uani 0.5 1 d D U P A -1
F2 F 0.3728(11) 0.1399(9) 0.6836(7) 0.056(3) Uani 0.5 1 d D U P A -1
F3 F 0.348(2) 0.0137(12) 0.6567(17) 0.071(6) Uani 0.5 1 d D U P A -1
Au2 Au 0.59269(12) -0.00108(10) 0.40616(9) 0.0267(4) Uani 0.5 1 d D . P A -2
C1A C 0.6762(13) -0.0940(11) 0.3853(10) 0.048(3) Uani 0.5 1 d D U P A -2
F1A F 0.7994(9) -0.0891(9) 0.3920(8) 0.056(3) Uani 0.5 1 d D U P A -2
F2A F 0.6272(11) -0.1399(9) 0.3164(7) 0.056(3) Uani 0.5 1 d D U P A -2
F3A F 0.692(2) -0.1594(14) 0.4432(12) 0.050(5) Uani 0.5 1 d D U P A -2
Br1A Br 0.5270(2) -0.13127(14) 0.59085(14) 0.0410(6) Uani 0.5 1 d . . P . .
Au3 Au 0.38462(12) -0.09518(10) 0.46176(9) 0.0271(4) Uani 0.5 1 d D . P A -1
C2 C 0.2335(18) -0.0831(15) 0.3574(13) 0.109(7) Uani 0.5 1 d D U P A -1
F4 F 0.1099(13) -0.0874(16) 0.3418(12) 0.130(7) Uani 0.5 1 d D U P A -1
F5 F 0.2580(17) -0.1149(14) 0.2916(10) 0.127(7) Uani 0.5 1 d D U P A -1
F6 F 0.221(3) 0.0055(14) 0.3378(18) 0.109(8) Uani 0.5 1 d D U P A -1
Au4 Au 0.66095(12) -0.00829(10) 0.61296(9) 0.0277(4) Uani 0.5 1 d D . P A -2
C2A C 0.7665(18) 0.0831(15) 0.6426(13) 0.109(7) Uani 0.5 1 d D U P A -2
F4A F 0.8901(13) 0.0874(16) 0.6582(12) 0.130(7) Uani 0.5 1 d D U P A -2
F5A F 0.7420(17) 0.1149(14) 0.7084(10) 0.127(7) Uani 0.5 1 d D U P A -2
F6A F 0.743(2) 0.1482(16) 0.5841(13) 0.082(7) Uani 0.5 1 d D U P A -2
P1 P 0.7770(4) 0.4425(3) 0.5620(3) 0.0190(9) Uani 1 1 d . U . . .
C3 C 0.6719(13) 0.4037(12) 0.6147(11) 0.022(3) Uani 1 1 d . U . . .
C4 C 0.6593(16) 0.3162(13) 0.6196(11) 0.026(4) Uani 1 1 d . U . . .
H4 H 0.7039 0.2804 0.5964 0.032 Uiso 1 1 calc R U . . .
C5 C 0.5793(18) 0.2867(14) 0.6596(13) 0.036(4) Uani 1 1 d . U . . .
H5 H 0.5657 0.2302 0.6624 0.043 Uiso 1 1 calc R U . . .
C6 C 0.5166(17) 0.3455(16) 0.6972(14) 0.037(5) Uani 1 1 d . U . . .
H6 H 0.4628 0.3257 0.7250 0.045 Uiso 1 1 calc R U . . .
C7 C 0.5324(17) 0.4250(15) 0.6938(14) 0.036(5) Uani 1 1 d . U . . .
H7 H 0.4909 0.4598 0.7202 0.043 Uiso 1 1 calc R U . . .
C8 C 0.6090(14) 0.4601(14) 0.6522(12) 0.028(4) Uani 1 1 d . U . . .
H8 H 0.6184 0.5171 0.6492 0.034 Uiso 1 1 calc R U . . .
C9 C 0.9252(14) 0.3915(10) 0.6072(11) 0.018(3) Uani 1 1 d . U . . .
C10 C 0.9779(14) 0.3886(12) 0.6925(11) 0.024(4) Uani 1 1 d . U . . .
H10 H 0.9371 0.4135 0.7262 0.029 Uiso 1 1 calc R U . . .
C11 C 1.0884(15) 0.3496(12) 0.7265(12) 0.027(4) Uani 1 1 d . U . . .
H11 H 1.1223 0.3487 0.7837 0.033 Uiso 1 1 calc R U . . .
C12 C 1.1513(16) 0.3120(13) 0.6808(13) 0.029(4) Uani 1 1 d . U . . .
H12 H 1.2271 0.2854 0.7057 0.034 Uiso 1 1 calc R U . . .
C13 C 1.0984(15) 0.3141(13) 0.5933(13) 0.028(4) Uani 1 1 d . U . . .
H13 H 1.1398 0.2876 0.5607 0.034 Uiso 1 1 calc R U . . .
C14 C 0.9884(14) 0.3541(11) 0.5563(12) 0.020(3) Uani 1 1 d . U . . .
H14 H 0.9557 0.3568 0.4990 0.024 Uiso 1 1 calc R U . . .
C15 C 0.7918(14) 0.5535(11) 0.5746(11) 0.019(3) Uani 1 1 d . U . . .
C16 C 0.8993(14) 0.5912(12) 0.6294(11) 0.020(3) Uani 1 1 d . U . . .
H16 H 0.9676 0.5591 0.6582 0.024 Uiso 1 1 calc R U . . .
C17 C 0.9021(17) 0.6713(12) 0.6394(13) 0.030(4) Uani 1 1 d . U . . .
H17 H 0.9727 0.6950 0.6764 0.036 Uiso 1 1 calc R U . . .
C18 C 0.8037(15) 0.7225(13) 0.5969(11) 0.026(4) Uani 1 1 d . U . . .
H18 H 0.8082 0.7794 0.6049 0.032 Uiso 1 1 calc R U . . .
C19 C 0.6987(16) 0.6861(13) 0.5421(13) 0.030(4) Uani 1 1 d . U . . .
H19 H 0.6320 0.7189 0.5123 0.036 Uiso 1 1 calc R U . . .
C20 C 0.6927(14) 0.6018(12) 0.5317(12) 0.024(4) Uani 1 1 d . U . . .
H20 H 0.6215 0.5776 0.4957 0.029 Uiso 1 1 calc R U . . .
C21 C 0.7192(14) 0.4202(12) 0.4544(11) 0.022(3) Uani 1 1 d . U . . .
C22 C 0.6207(14) 0.3660(11) 0.4199(11) 0.021(3) Uani 1 1 d . U . . .
H22 H 0.5810 0.3400 0.4537 0.025 Uiso 1 1 calc R U . . .
C23 C 0.5801(15) 0.3497(13) 0.3342(12) 0.027(4) Uani 1 1 d . U . . .
H23 H 0.5123 0.3150 0.3106 0.033 Uiso 1 1 calc R U . . .
C24 C 0.6438(14) 0.3868(12) 0.2871(12) 0.026(4) Uani 1 1 d . U . . .
H24 H 0.6221 0.3732 0.2313 0.031 Uiso 1 1 calc R U . . .
C25 C 0.7359(15) 0.4417(14) 0.3174(11) 0.027(4) Uani 1 1 d . U . . .
H25 H 0.7743 0.4663 0.2822 0.032 Uiso 1 1 calc R U . . .
C26 C 0.7758(16) 0.4631(13) 0.4026(11) 0.025(4) Uani 1 1 d . U . . .
H26 H 0.8365 0.5034 0.4234 0.030 Uiso 1 1 calc R U . . .
C27 C 0.9128(19) 0.1145(16) 0.4617(15) 0.046(6) Uani 1 1 d . . . . .
H27A H 0.9656 0.1279 0.5171 0.055 Uiso 1 1 calc R U . . .
H27B H 0.8523 0.0735 0.4664 0.055 Uiso 1 1 calc R U . . .
Cl1 Cl 1.0039(5) 0.0728(4) 0.4075(4) 0.0497(15) Uani 1 1 d . . . . .
Cl2 Cl 0.8323(5) 0.2045(4) 0.4156(4) 0.0571(18) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0655(13) 0.0302(12) 0.0352(12) 0.0068(11) 0.0271(10) 0.0089(11)
Au1 0.0347(7) 0.0182(7) 0.0239(8) 0.0049(6) 0.0135(6) 0.0087(6)
C1 0.059(6) 0.050(8) 0.039(7) -0.014(6) 0.020(6) -0.012(6)
F1 0.059(5) 0.064(9) 0.049(7) -0.018(6) 0.021(5) -0.012(5)
F2 0.068(6) 0.063(8) 0.040(6) -0.019(6) 0.022(5) -0.019(6)
F3 0.100(12) 0.053(8) 0.078(16) -0.003(8) 0.053(11) 0.009(8)
Au2 0.0358(7) 0.0205(8) 0.0288(8) 0.0071(7) 0.0175(6) 0.0086(6)
C1A 0.059(6) 0.050(8) 0.039(7) -0.014(6) 0.020(6) -0.012(6)
F1A 0.059(5) 0.064(9) 0.049(7) -0.018(6) 0.021(5) -0.012(5)
F2A 0.068(6) 0.063(8) 0.040(6) -0.019(6) 0.022(5) -0.019(6)
F3A 0.066(11) 0.049(12) 0.042(7) -0.013(8) 0.026(8) -0.001(9)
Br1A 0.0655(13) 0.0302(12) 0.0352(12) 0.0068(11) 0.0271(10) 0.0089(11)
Au3 0.0247(6) 0.0302(9) 0.0258(8) -0.0027(7) 0.0067(5) 0.0048(7)
C2 0.104(9) 0.148(16) 0.059(10) -0.032(10) 0.003(9) 0.052(11)
F4 0.105(8) 0.190(19) 0.076(12) -0.025(12) 0.002(8) 0.044(10)
F5 0.129(11) 0.178(18) 0.056(9) -0.028(11) 0.000(8) 0.082(12)
F6 0.097(16) 0.156(16) 0.050(18) -0.020(12) -0.012(14) 0.064(11)
Au4 0.0293(6) 0.0206(8) 0.0298(8) -0.0021(7) 0.0043(5) 0.0051(6)
C2A 0.104(9) 0.148(16) 0.059(10) -0.032(10) 0.003(9) 0.052(11)
F4A 0.105(8) 0.190(19) 0.076(12) -0.025(12) 0.002(8) 0.044(10)
F5A 0.129(11) 0.178(18) 0.056(9) -0.028(11) 0.000(8) 0.082(12)
F6A 0.079(13) 0.097(16) 0.050(10) -0.067(10) -0.011(9) 0.006(12)
P1 0.0205(19) 0.017(2) 0.021(2) 0.001(2) 0.0076(16) 0.0015(18)
C3 0.013(6) 0.027(8) 0.025(8) -0.001(8) 0.005(6) -0.006(7)
C4 0.033(8) 0.029(8) 0.016(9) 0.004(8) 0.007(7) 0.001(8)
C5 0.046(10) 0.028(10) 0.038(12) 0.006(10) 0.020(9) -0.010(9)
C6 0.026(9) 0.047(11) 0.040(12) 0.010(11) 0.013(8) 0.002(9)
C7 0.029(9) 0.045(10) 0.044(13) 0.016(11) 0.025(8) 0.018(9)
C8 0.022(8) 0.036(10) 0.029(10) -0.002(9) 0.010(7) 0.001(8)
C9 0.024(6) 0.006(7) 0.025(7) -0.002(7) 0.009(5) -0.004(6)
C10 0.020(7) 0.024(10) 0.027(7) -0.006(8) 0.005(6) -0.005(6)
C11 0.027(8) 0.019(11) 0.032(9) -0.002(8) 0.005(6) -0.004(7)
C12 0.030(8) 0.019(11) 0.039(9) 0.001(9) 0.013(7) -0.006(7)
C13 0.023(7) 0.031(12) 0.040(9) 0.001(10) 0.022(7) -0.002(7)
C14 0.021(7) 0.006(8) 0.036(9) -0.009(8) 0.013(6) -0.010(6)
C15 0.018(7) 0.011(6) 0.028(9) -0.006(6) 0.008(6) -0.002(5)
C16 0.022(7) 0.018(7) 0.019(9) -0.006(7) 0.003(6) -0.004(7)
C17 0.033(8) 0.010(8) 0.044(13) 0.001(8) 0.009(7) -0.009(7)
C18 0.030(8) 0.021(9) 0.031(11) 0.000(8) 0.015(7) -0.008(6)
C19 0.028(7) 0.024(9) 0.039(12) -0.013(9) 0.011(7) 0.004(7)
C20 0.017(7) 0.021(8) 0.031(11) 0.004(8) 0.003(6) -0.002(6)
C21 0.020(7) 0.022(10) 0.026(7) -0.013(7) 0.013(5) -0.004(7)
C22 0.019(7) 0.013(9) 0.032(8) -0.006(8) 0.012(6) -0.004(6)
C23 0.018(7) 0.024(11) 0.032(8) 0.005(8) -0.003(6) -0.005(7)
C24 0.024(8) 0.028(11) 0.023(8) -0.003(8) 0.003(6) 0.005(7)
C25 0.026(8) 0.035(12) 0.018(8) -0.004(9) 0.005(7) -0.003(7)
C26 0.030(8) 0.026(11) 0.021(7) -0.004(8) 0.012(7) -0.008(7)
C27 0.042(11) 0.053(17) 0.042(14) 0.020(13) 0.013(10) 0.014(11)
Cl1 0.061(3) 0.044(4) 0.048(4) 0.004(3) 0.023(3) 0.000(3)
Cl2 0.046(3) 0.023(3) 0.078(5) -0.004(3) -0.017(3) -0.001(2)
_geom_special_details
;
Care will be needed when calculating geometrical details from the atomic
coordinates used to describe this structure. As detailed in the
experimental description in the supporting information, in order to
facilitate the use of geometrical restraints for the atoms of the
highly disordered anion, some atomic sites were split into symmetry
equivalent components.
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
Br1 Au1 2.426(2) . ?
Br1 Au2 2.536(3) . ?
Au1 C1 1.981(16) . ?
Au1 Au3 3.271(2) . ?
C1 F2 1.353(15) . ?
C1 F1 1.354(14) . ?
C1 F3 1.466(19) . ?
Au2 C1A 1.862(17) . ?
Au2 Au4 3.366(2) . ?
C1A F2A 1.353(15) . ?
C1A F1A 1.354(14) . ?
C1A F3A 1.419(19) . ?
Br1A Au3 2.356(3) . ?
Br1A Au4 2.450(3) . ?
Au3 C2 2.05(2) . ?
C2 F4 1.330(16) . ?
C2 F5 1.338(16) . ?
C2 F6 1.47(2) . ?
Au4 C2A 1.86(2) . ?
Au4 F5A 2.55(2) . ?
C2A F4A 1.330(16) . ?
C2A F5A 1.338(16) . ?
C2A F6A 1.42(2) . ?
P1 C21 1.781(18) . ?
P1 C3 1.801(16) . ?
P1 C9 1.801(16) . ?
P1 C15 1.809(19) . ?
C3 C8 1.42(3) . ?
C3 C4 1.43(3) . ?
C4 C5 1.37(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.45(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.30(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.39(3) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.39(3) . ?
C9 C14 1.41(2) . ?
C10 C11 1.35(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.35(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.42(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.36(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C20 1.37(2) . ?
C15 C16 1.41(2) . ?
C16 C17 1.30(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.39(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.39(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.37(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.39(2) . ?
C21 C26 1.42(2) . ?
C22 C23 1.41(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.37(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.34(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.42(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 Cl1 1.71(2) . ?
C27 Cl2 1.76(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au1 Br1 164.0(5) . . ?
C1 Au1 Au3 103.8(5) . . ?
Br1 Au1 Au3 86.96(7) . . ?
F2 C1 F1 103.6(12) . . ?
F2 C1 F3 95.6(14) . . ?
F1 C1 F3 91.3(13) . . ?
F2 C1 Au1 118.6(10) . . ?
F1 C1 Au1 130.2(11) . . ?
F3 C1 Au1 108.4(13) . . ?
C1A Au2 Br1 170.3(5) . . ?
C1A Au2 Au4 101.9(5) . . ?
Br1 Au2 Au4 87.62(7) . . ?
F2A C1A F1A 103.6(12) . . ?
F2A C1A F3A 97.2(14) . . ?
F1A C1A F3A 94.4(13) . . ?
F2A C1A Au2 121.0(12) . . ?
F1A C1A Au2 119.9(12) . . ?
F3A C1A Au2 115.6(13) . . ?
C2 Au3 Br1A 166.4(7) . . ?
C2 Au3 Au1 99.5(7) . . ?
Br1A Au3 Au1 87.33(8) . . ?
F4 C2 F5 106.5(16) . . ?
F4 C2 F6 89.2(15) . . ?
F5 C2 F6 102.4(17) . . ?
F4 C2 Au3 134.4(14) . . ?
F5 C2 Au3 111.1(13) . . ?
F6 C2 Au3 106.5(16) . . ?
C2A Au4 Br1A 173.5(7) . . ?
C2A Au4 F5A 30.4(6) . . ?
Br1A Au4 F5A 144.2(5) . . ?
C2A Au4 Au2 100.1(6) . . ?
Br1A Au4 Au2 86.41(7) . . ?
F5A Au4 Au2 124.0(5) . . ?
F4A C2A F5A 106.5(16) . . ?
F4A C2A F6A 93.3(16) . . ?
F5A C2A F6A 105.2(16) . . ?
F4A C2A Au4 129.2(16) . . ?
F5A C2A Au4 104.7(14) . . ?
F6A C2A Au4 115.7(16) . . ?
C2A F5A Au4 44.9(11) . . ?
C21 P1 C3 110.9(8) . . ?
C21 P1 C9 109.9(8) . . ?
C3 P1 C9 106.7(8) . . ?
C21 P1 C15 108.3(9) . . ?
C3 P1 C15 109.7(8) . . ?
C9 P1 C15 111.4(8) . . ?
C8 C3 C4 122.5(16) . . ?
C8 C3 P1 119.6(15) . . ?
C4 C3 P1 117.9(13) . . ?
C5 C4 C3 117.8(18) . . ?
C5 C4 H4 121.1 . . ?
C3 C4 H4 121.1 . . ?
C4 C5 C6 118(2) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C7 C6 C5 122.5(18) . . ?
C7 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C6 C7 C8 123(2) . . ?
C6 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C7 C8 C3 116(2) . . ?
C7 C8 H8 122.0 . . ?
C3 C8 H8 122.0 . . ?
C10 C9 C14 119.6(16) . . ?
C10 C9 P1 120.0(13) . . ?
C14 C9 P1 120.4(14) . . ?
C11 C10 C9 120.1(17) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 122.5(19) . . ?
C12 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?
C11 C12 C13 118.2(18) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
C14 C13 C12 121.2(17) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C9 118.3(18) . . ?
C13 C14 H14 120.8 . . ?
C9 C14 H14 120.8 . . ?
C20 C15 C16 119.5(17) . . ?
C20 C15 P1 118.3(13) . . ?
C16 C15 P1 122.2(13) . . ?
C17 C16 C15 119.6(18) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 122.7(19) . . ?
C16 C17 H17 118.6 . . ?
C18 C17 H17 118.6 . . ?
C19 C18 C17 118.0(19) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C20 C19 C18 120.3(18) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C15 C20 C19 119.9(17) . . ?
C15 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C26 119.7(16) . . ?
C22 C21 P1 123.5(13) . . ?
C26 C21 P1 116.8(13) . . ?
C21 C22 C23 120.9(16) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 117.7(16) . . ?
C24 C23 H23 121.1 . . ?
C22 C23 H23 121.1 . . ?
C25 C24 C23 123.0(18) . . ?
C25 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
C24 C25 C26 121.1(17) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C21 C26 C25 117.2(17) . . ?
C21 C26 H26 121.4 . . ?
C25 C26 H26 121.4 . . ?
Cl1 C27 Cl2 113.2(13) . . ?
Cl1 C27 H27A 108.9 . . ?
Cl2 C27 H27A 108.9 . . ?
Cl1 C27 H27B 108.9 . . ?
Cl2 C27 H27B 108.9 . . ?
H27A C27 H27B 107.8 . . ?
_refine_diff_density_max 3.845
_refine_diff_density_min -2.411
_refine_diff_density_rms 0.398
_shelx_res_file
;
shelx.res created by SHELXL-2014/7
TITL amt770_tw4l_twin1_hklf4_a.res in P2(1)/n
REM Old TITL amt770_tw4L_twin1_hklf4 in P2(1)/n
CELL 0.71073 11.220771 16.168437 17.030768 90.0000 108.0494 90.0000
ZERR 4.00 0.001636 0.003243 0.002851 0.0000 0.0187 0.0000
REM SHELXT solution in P2(1)/n
REM R1 0.221, Rweak 0.063, Alpha 0.103, Orientation as input
REM Formula found by SHELXT: C32 O3 F P Cl2 Br5
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H F P Cl Br Au
UNIT 108 88 24 4 8 4 8
omit -2 55
omit 8 -4 -6
omit 6 8 0
omit -5 -1 3
omit -1 1 -5
omit 2 -3 4
L.S. 4
BOND $H
LIST 4
acta
FMAP 2
PLAN 20
rem F3B 4 0.29860 0.16040 0.55720 10.50000 0.05000
rem
delu P1 > C26
rigu 0.004 0.004 C1 > F3 C1A > F3A C2 > F6 C2A > F6A
delu 0.004 0.004 C1 > F3 C1A > F3A C2 > F6 C2A > F6A
isor 0.03 0.03 F6A
eadp Br1 Br1a
eadp C1 C1a
eadp F1 F1a
eadp F2 F2a
eadp C2 C2a
eadp F4 F4a
eadp F5 F5a
rem
sadi 0.05 Au1 C1 Au2 C1A Au3 C2 Au4 C2A
rem
dfix 1.328 C1 F1 C1 F2 C1 F3
dfix 2.125 F1 F2 F1 F3 F2 F3
sadi 0.05 Au1 F1 Au1 F2 Au1 F3
rem
dfix 1.328 C1A F1A C1A F2A C1A F3A
dfix 2.125 F1A F2A F1A F3A F2A F3A
sadi 0.05 Au2 F1A Au2 F2A Au2 F3A
rem
dfix 1.328 C2 F4 C2 F5 C2 F6
dfix 2.125 F4 F5 F4 F6 F5 F6
sadi 0.05 Au3 F4 Au3 F5 Au3 F6
rem
dfix 1.328 C2A F4A C2A F5A C2A F6A
dfix 2.125 F4A F5A F4A F6A F5A F6A
sadi 0.05 Au4 F4A Au4 F5A Au4 F6A
rem
WGHT 0.165200
BASF 0.29873 0.13338
FVAR 1.39916 0.47297 0.13127 0.40915 0.32382 0.09399 0.61471
FVAR 0.20060 0.08911 0.60798 0.37276 0.13989 0.68365 0.23345
FVAR -0.08311 0.35743 0.10986 -0.08741 0.34177 0.25802 -0.11494
FVAR 0.29161
BR1 6 21.000000 31.000000 41.000000 10.50000 0.06553 0.03023 =
0.03520 0.00677 0.02712 0.00892
part -1
AU1 7 0.407656 0.095808 0.528075 10.50000 0.03466 0.01821 =
0.02387 0.00486 0.01352 0.00869
C1 1 51.000000 61.000000 71.000000 10.50000 0.05873 0.05022 =
0.03915 -0.01434 0.01989 -0.01183
F1 3 81.000000 91.000000 101.000000 10.50000 0.05879 0.06409 =
0.04933 -0.01822 0.02111 -0.01221
F2 3 111.000000 121.000000 131.000000 10.50000 0.06756 0.06252 =
0.04036 -0.01895 0.02243 -0.01908
F3 3 0.348418 0.013712 0.656694 10.50000 0.09964 0.05263 =
0.07833 -0.00314 0.05258 0.00917
part -2
AU2 7 0.592692 -0.001076 0.406164 10.50000 0.03578 0.02054 =
0.02884 0.00706 0.01747 0.00856
C1A 1 -51.000000 59.000000 -71.000000 10.50000 0.05873 0.05022 =
0.03915 -0.01434 0.01989 -0.01183
F1A 3 -81.000000 89.000000 -101.000000 10.50000 0.05879 0.06409 =
0.04933 -0.01822 0.02111 -0.01221
F2A 3 -111.000000 119.000000 -131.000000 10.50000 0.06756 0.06252 =
0.04036 -0.01895 0.02243 -0.01908
F3A 3 0.692476 -0.159415 0.443222 10.50000 0.06631 0.04912 =
0.04250 -0.01346 0.02637 -0.00090
part 0
BR1A 6 -21.000000 29.000000 -41.000000 10.50000 0.06553 0.03023 =
0.03520 0.00677 0.02712 0.00892
part -1
AU3 7 0.384621 -0.095184 0.461757 10.50000 0.02465 0.03019 =
0.02583 -0.00268 0.00673 0.00477
C2 1 141.000000 151.000000 161.000000 10.50000 0.10400 0.14844 =
0.05903 -0.03167 0.00311 0.05247
F4 3 171.000000 181.000000 191.000000 10.50000 0.10510 0.19014 =
0.07590 -0.02503 0.00239 0.04375
F5 3 201.000000 211.000000 221.000000 10.50000 0.12877 0.17792 =
0.05600 -0.02826 0.00047 0.08219
F6 3 0.221026 0.005494 0.337848 10.50000 0.09652 0.15648 =
0.05025 -0.02043 -0.01205 0.06352
part -2
AU4 7 0.660953 -0.008289 0.612959 10.50000 0.02930 0.02057 =
0.02977 -0.00206 0.00427 0.00512
C2A 1 -141.000000 149.000000 -161.000000 10.50000 0.10400 0.14844 =
0.05903 -0.03167 0.00311 0.05247
F4A 3 -171.000000 179.000000 -191.000000 10.50000 0.10510 0.19014 =
0.07590 -0.02503 0.00239 0.04375
F5A 3 -201.000000 209.000000 -221.000000 10.50000 0.12877 0.17792 =
0.05600 -0.02826 0.00047 0.08219
F6A 3 0.742951 0.148217 0.584061 10.50000 0.07884 0.09657 =
0.04981 -0.06658 -0.01089 0.00570
part 0
P1 4 0.776988 0.442550 0.562018 11.00000 0.02054 0.01669 =
0.02051 0.00052 0.00755 0.00150
C3 1 0.671928 0.403730 0.614709 11.00000 0.01275 0.02734 =
0.02472 -0.00100 0.00530 -0.00586
C4 1 0.659255 0.316208 0.619622 11.00000 0.03301 0.02946 =
0.01578 0.00386 0.00655 0.00139
AFIX 43
H4 2 0.703872 0.280371 0.596432 11.00000 -1.20000
AFIX 0
C5 1 0.579293 0.286741 0.659579 11.00000 0.04601 0.02761 =
0.03776 0.00599 0.02001 -0.00967
AFIX 43
H5 2 0.565651 0.230241 0.662428 11.00000 -1.20000
AFIX 0
C6 1 0.516553 0.345488 0.697241 11.00000 0.02620 0.04735 =
0.04025 0.00951 0.01308 0.00158
AFIX 43
H6 2 0.462836 0.325736 0.724978 11.00000 -1.20000
AFIX 0
C7 1 0.532412 0.425024 0.693796 11.00000 0.02855 0.04451 =
0.04443 0.01614 0.02511 0.01793
AFIX 43
H7 2 0.490897 0.459810 0.720178 11.00000 -1.20000
AFIX 0
C8 1 0.609030 0.460138 0.652202 11.00000 0.02157 0.03566 =
0.02892 -0.00243 0.01037 0.00103
AFIX 43
H8 2 0.618424 0.517084 0.649169 11.00000 -1.20000
AFIX 0
C9 1 0.925167 0.391490 0.607191 11.00000 0.02391 0.00633 =
0.02488 -0.00232 0.00915 -0.00373
C10 1 0.977920 0.388573 0.692455 11.00000 0.01968 0.02361 =
0.02713 -0.00555 0.00458 -0.00507
AFIX 43
H10 2 0.937113 0.413511 0.726172 11.00000 -1.20000
AFIX 0
C11 1 1.088380 0.349588 0.726513 11.00000 0.02733 0.01932 =
0.03195 -0.00169 0.00492 -0.00388
AFIX 43
H11 2 1.122336 0.348681 0.783732 11.00000 -1.20000
AFIX 0
C12 1 1.151251 0.311965 0.680772 11.00000 0.02974 0.01878 =
0.03908 0.00093 0.01299 -0.00620
AFIX 43
H12 2 1.227051 0.285355 0.705683 11.00000 -1.20000
AFIX 0
C13 1 1.098445 0.314073 0.593251 11.00000 0.02314 0.03080 =
0.03984 0.00060 0.02187 -0.00211
AFIX 43
H13 2 1.139780 0.287633 0.560685 11.00000 -1.20000
AFIX 0
C14 1 0.988359 0.354148 0.556276 11.00000 0.02096 0.00596 =
0.03637 -0.00910 0.01343 -0.01018
AFIX 43
H14 2 0.955683 0.356849 0.499046 11.00000 -1.20000
AFIX 0
C15 1 0.791761 0.553532 0.574556 11.00000 0.01815 0.01096 =
0.02765 -0.00567 0.00839 -0.00197
C16 1 0.899300 0.591186 0.629408 11.00000 0.02178 0.01781 =
0.01915 -0.00581 0.00284 -0.00441
AFIX 43
H16 2 0.967624 0.559067 0.658196 11.00000 -1.20000
AFIX 0
C17 1 0.902059 0.671259 0.639372 11.00000 0.03264 0.00980 =
0.04436 0.00094 0.00897 -0.00901
AFIX 43
H17 2 0.972733 0.695037 0.676433 11.00000 -1.20000
AFIX 0
C18 1 0.803749 0.722481 0.596891 11.00000 0.03039 0.02126 =
0.03134 0.00044 0.01497 -0.00837
AFIX 43
H18 2 0.808243 0.779431 0.604934 11.00000 -1.20000
AFIX 0
C19 1 0.698677 0.686052 0.542107 11.00000 0.02786 0.02390 =
0.03930 -0.01331 0.01134 0.00382
AFIX 43
H19 2 0.631958 0.718890 0.512263 11.00000 -1.20000
AFIX 0
C20 1 0.692730 0.601830 0.531748 11.00000 0.01739 0.02098 =
0.03130 0.00359 0.00302 -0.00179
AFIX 43
H20 2 0.621527 0.577591 0.495698 11.00000 -1.20000
AFIX 0
C21 1 0.719202 0.420246 0.454418 11.00000 0.02008 0.02245 =
0.02613 -0.01340 0.01253 -0.00371
C22 1 0.620659 0.365974 0.419855 11.00000 0.01928 0.01317 =
0.03205 -0.00592 0.01197 -0.00388
AFIX 43
H22 2 0.580959 0.340025 0.453662 11.00000 -1.20000
AFIX 0
C23 1 0.580083 0.349741 0.334192 11.00000 0.01822 0.02417 =
0.03218 0.00487 -0.00291 -0.00527
AFIX 43
H23 2 0.512329 0.315035 0.310622 11.00000 -1.20000
AFIX 0
C24 1 0.643781 0.386776 0.287058 11.00000 0.02376 0.02843 =
0.02285 -0.00279 0.00302 0.00467
AFIX 43
H24 2 0.622149 0.373176 0.231343 11.00000 -1.20000
AFIX 0
C25 1 0.735872 0.441723 0.317399 11.00000 0.02624 0.03475 =
0.01801 -0.00358 0.00515 -0.00287
AFIX 43
H25 2 0.774345 0.466328 0.282179 11.00000 -1.20000
AFIX 0
C26 1 0.775803 0.463067 0.402601 11.00000 0.02981 0.02637 =
0.02116 -0.00446 0.01201 -0.00847
AFIX 43
H26 2 0.836470 0.503403 0.423429 11.00000 -1.20000
AFIX 0
C27 1 0.912837 0.114540 0.461731 11.00000 0.04181 0.05330 =
0.04214 0.01957 0.01288 0.01352
AFIX 23
H27A 2 0.965645 0.127862 0.517117 11.00000 -1.20000
H27B 2 0.852256 0.073545 0.466366 11.00000 -1.20000
AFIX 0
CL1 5 1.003915 0.072804 0.407534 11.00000 0.06069 0.04437 =
0.04824 0.00384 0.02310 0.00044
CL2 5 0.832316 0.204486 0.415566 11.00000 0.04639 0.02269 =
0.07764 -0.00374 -0.01685 -0.00142
HKLF 5
REM amt770_tw4l_twin1_hklf4_a.res in P2(1)/n
REM R1 = 0.0813 for 6600 Fo > 4sig(Fo) and 0.1135 for all 10326 data
REM 390 parameters refined using 210 restraints
END
WGHT 0.1652 0.0000
REM Highest difference peak 3.845, deepest hole -2.411, 1-sigma level 0.398
Q1 1 0.3561 -0.0983 0.4867 11.00000 0.05 3.84
Q2 1 0.3330 0.0969 0.5382 11.00000 0.05 2.76
Q3 1 0.6243 0.0002 0.3847 11.00000 0.05 2.55
Q4 1 0.4971 0.0958 0.5264 11.00000 0.05 2.53
Q5 1 0.4379 0.0963 0.5118 11.00000 0.05 2.48
Q6 1 0.3176 -0.0020 0.6011 11.00000 0.05 2.35
Q7 1 0.6806 -0.0026 0.5977 11.00000 0.05 2.23
Q8 1 0.5156 0.0042 0.4139 11.00000 0.05 2.16
Q9 1 0.5857 -0.0045 0.6236 11.00000 0.05 2.09
Q10 1 0.3888 0.1339 0.4241 11.00000 0.05 1.84
Q11 1 0.2352 0.0166 0.3912 11.00000 0.05 1.84
Q12 1 0.6972 -0.0380 0.4515 11.00000 0.05 1.81
Q13 1 0.5952 0.0413 0.5919 11.00000 0.05 1.80
Q14 1 0.1560 -0.1441 0.3418 11.00000 0.05 1.80
Q15 1 0.3240 0.0970 0.4691 11.00000 0.05 1.78
Q16 1 0.4564 -0.1430 0.4890 11.00000 0.05 1.71
Q17 1 0.5195 -0.0402 0.3770 11.00000 0.05 1.69
Q18 1 0.5734 0.0009 0.4273 11.00000 0.05 1.61
Q19 1 0.3068 -0.0746 0.2835 11.00000 0.05 1.61
Q20 1 0.4189 -0.0979 0.4503 11.00000 0.05 1.60
;
_shelx_res_checksum 40571
#######################################################################
#
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1049921'
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
_publcif_datablock.id {df1a9729-19c7-47f8-838b-d80f565e71a8}
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C56 H40 Au6 Br2 F18 O2 P2'
_chemical_formula_weight 2490.44
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M C2/m
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
_cell_length_a 11.6100(3)
_cell_length_b 23.9064(7)
_cell_length_c 11.1568(3)
_cell_angle_alpha 90.00
_cell_angle_beta 97.975(3)
_cell_angle_gamma 90.00
_cell_volume 3066.66(15)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9990
_cell_measurement_theta_min 4.1152
_cell_measurement_theta_max 28.8141
_exptl_crystal_description 'thin plate'
_exptl_crystal_colour 'translucent blue'
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.01
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.697
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2256
_exptl_absorpt_coefficient_mu 15.749
_exptl_absorpt_correction_T_min 0.0481
_exptl_absorpt_correction_T_max 0.8584
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measurement_method ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 16422
_diffrn_reflns_av_R_equivalents 0.0591
_diffrn_reflns_av_sigmaI/netI 0.0400
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_k_max 30
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 4.13
_diffrn_reflns_theta_max 28.87
_diffrn_orient_matrix_UB_11 0.0516727724
_diffrn_orient_matrix_UB_12 -0.0138218978
_diffrn_orient_matrix_UB_13 -0.0105491043
_diffrn_orient_matrix_UB_21 0.0309106606
_diffrn_orient_matrix_UB_22 0.0256057385
_diffrn_orient_matrix_UB_23 0.0084738331
_diffrn_orient_matrix_UB_31 0.0133123704
_diffrn_orient_matrix_UB_32 -0.0058090823
_diffrn_orient_matrix_UB_33 0.0627721770
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 59.00 102.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 22.1490 179.0000 -180.0000 43
#__ type_ start__ end____ width___ exp.time_
2 omega -10.00 68.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 22.1490 -111.0000 -164.0000 78
#__ type_ start__ end____ width___ exp.time_
3 omega -30.00 87.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 22.1490 0.0000 -30.0000 117
#__ type_ start__ end____ width___ exp.time_
4 omega -102.00 -32.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -19.9615 179.0000 -150.0000 70
#__ type_ start__ end____ width___ exp.time_
5 omega -93.00 12.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -19.9615 -37.0000 -60.0000 105
#__ type_ start__ end____ width___ exp.time_
6 omega -92.00 -14.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -19.9615 -77.0000 -150.0000 78
#__ type_ start__ end____ width___ exp.time_
7 omega -92.00 13.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -19.9615 -77.0000 90.0000 105
;
_reflns_number_total 3746
_reflns_number_gt 3147
_reflns_threshold_expression >2sigma(I)
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3746
_refine_ls_number_parameters 204
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0432
_refine_ls_R_factor_gt 0.0337
_refine_ls_wR_factor_ref 0.0877
_refine_ls_wR_factor_gt 0.0849
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_restrained_S_all 1.016
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.127586(18) 0.072732(10) 0.55929(2) 0.01697(9) Uani 1 1 d . . .
Au2 Au 0.34831(3) 0.0000 0.53119(3) 0.01898(10) Uani 1 2 d S . .
Br Br 0.06132(8) 0.0000 0.68897(8) 0.0265(2) Uani 1 2 d S . .
F1 F 0.1826(4) 0.18597(18) 0.5032(5) 0.0496(13) Uani 1 1 d . . .
F2 F 0.1056(4) 0.1403(2) 0.3469(4) 0.0449(12) Uani 1 1 d . . .
F3 F 0.2843(3) 0.12742(17) 0.4173(4) 0.0321(9) Uani 1 1 d . . .
F4 F 0.3714(5) 0.0000 0.7932(6) 0.054(2) Uani 1 2 d S . .
F5 F 0.5100(4) -0.04456(18) 0.7275(4) 0.0392(10) Uani 1 1 d . . .
O O 0.2307(6) 0.0000 0.2647(6) 0.0329(17) Uani 1 2 d S . .
C1 C 0.1766(5) 0.1340(3) 0.4536(6) 0.0209(13) Uani 1 1 d . . .
C2 C 0.4382(7) 0.0000 0.7024(8) 0.0226(19) Uani 1 2 d S . .
C3 C 0.2711(7) 0.0000 0.3582(10) 0.030(2) Uani 1 2 d S . .
P P 0.0000 0.20569(9) 0.0000 0.0158(4) Uani 1 2 d S . .
C4 C 0.1249(5) 0.1609(2) 0.0113(6) 0.0186(12) Uani 1 1 d . . .
C5 C 0.1281(6) 0.1189(3) -0.0760(6) 0.0264(15) Uani 1 1 d . . .
H5 H 0.0667 0.1156 -0.1414 0.032 Uiso 1 1 calc R . .
C6 C 0.2211(6) 0.0822(3) -0.0665(7) 0.0297(16) Uani 1 1 d . . .
H6 H 0.2238 0.0538 -0.1257 0.036 Uiso 1 1 calc R . .
C7 C 0.3107(6) 0.0869(3) 0.0294(6) 0.0242(14) Uani 1 1 d . . .
H7 H 0.3748 0.0618 0.0355 0.029 Uiso 1 1 calc R . .
C8 C 0.3066(5) 0.1279(3) 0.1160(6) 0.0226(13) Uani 1 1 d . . .
H8 H 0.3676 0.1307 0.1818 0.027 Uiso 1 1 calc R . .
C9 C 0.2143(5) 0.1648(3) 0.1075(5) 0.0170(12) Uani 1 1 d . . .
H9 H 0.2120 0.1929 0.1673 0.020 Uiso 1 1 calc R . .
C10 C -0.0099(5) 0.2500(2) -0.1325(5) 0.0153(11) Uani 1 1 d . . .
C11 C 0.0562(5) 0.2395(3) -0.2244(5) 0.0184(12) Uani 1 1 d . . .
H11 H 0.1114 0.2099 -0.2173 0.022 Uiso 1 1 calc R . .
C12 C 0.0402(5) 0.2731(3) -0.3276(6) 0.0219(13) Uani 1 1 d . . .
H12 H 0.0860 0.2670 -0.3906 0.026 Uiso 1 1 calc R . .
C13 C -0.0414(6) 0.3147(3) -0.3382(6) 0.0244(14) Uani 1 1 d . . .
H13 H -0.0533 0.3366 -0.4098 0.029 Uiso 1 1 calc R . .
C14 C -0.1067(5) 0.3252(3) -0.2460(6) 0.0201(13) Uani 1 1 d . . .
H14 H -0.1626 0.3544 -0.2539 0.024 Uiso 1 1 calc R . .
C15 C -0.0903(5) 0.2928(3) -0.1419(5) 0.0183(12) Uani 1 1 d . . .
H15 H -0.1340 0.3000 -0.0777 0.022 Uiso 1 1 calc R . .
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 0.01489(13) 0.01794(14) 0.01750(14) -0.00077(9) 0.00019(9) 0.00071(8)
Au2 0.01619(17) 0.01816(18) 0.02306(19) 0.000 0.00432(13) 0.000
Br 0.0268(5) 0.0283(5) 0.0235(5) 0.000 0.0009(4) 0.000
F1 0.064(3) 0.018(2) 0.071(4) 0.000(2) 0.024(3) 0.000(2)
F2 0.033(2) 0.060(3) 0.039(3) 0.028(2) -0.0053(19) -0.009(2)
F3 0.0252(19) 0.031(2) 0.042(3) 0.0079(19) 0.0108(17) -0.0056(17)
F4 0.026(3) 0.111(7) 0.028(3) 0.000 0.011(3) 0.000
F5 0.039(2) 0.025(2) 0.049(3) 0.006(2) -0.0072(19) 0.0072(19)
O 0.023(3) 0.050(5) 0.025(4) 0.000 -0.001(3) 0.000
C1 0.022(3) 0.023(3) 0.018(3) 0.000(3) 0.003(2) -0.002(3)
C2 0.009(4) 0.032(5) 0.027(5) 0.000 0.005(3) 0.000
C3 0.010(4) 0.042(6) 0.037(6) 0.000 0.001(4) 0.000
P 0.0167(10) 0.0116(10) 0.0177(11) 0.000 -0.0025(8) 0.000
C4 0.017(3) 0.011(3) 0.028(3) 0.004(3) 0.000(2) 0.000(2)
C5 0.026(3) 0.021(3) 0.028(4) -0.006(3) -0.011(3) 0.004(3)
C6 0.039(4) 0.015(3) 0.032(4) -0.008(3) -0.005(3) 0.006(3)
C7 0.026(3) 0.017(3) 0.028(4) 0.000(3) -0.002(3) 0.006(3)
C8 0.021(3) 0.018(3) 0.027(4) 0.001(3) -0.003(3) -0.001(2)
C9 0.018(3) 0.016(3) 0.016(3) 0.000(2) -0.002(2) -0.001(2)
C10 0.020(3) 0.014(3) 0.011(3) 0.003(2) -0.003(2) -0.003(2)
C11 0.021(3) 0.014(3) 0.021(3) -0.004(2) 0.003(2) -0.002(2)
C12 0.026(3) 0.024(3) 0.016(3) -0.003(3) 0.003(2) 0.001(3)
C13 0.026(3) 0.025(4) 0.018(3) 0.003(3) -0.008(3) -0.001(3)
C14 0.019(3) 0.019(3) 0.021(3) 0.003(2) 0.001(2) 0.001(2)
C15 0.017(3) 0.017(3) 0.021(3) 0.001(2) 0.004(2) -0.001(2)
_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 C1 2.011(6) . ?
Au1 Br 2.4530(7) . ?
Au1 Au1 3.0724(4) 2_556 ?
Au1 Au2 3.1483(3) . ?
Au2 C3 2.012(11) . ?
Au2 C2 2.045(9) . ?
Au2 Au1 3.1483(3) 6 ?
Br Au1 2.4530(7) 6 ?
F1 C1 1.358(8) . ?
F2 C1 1.360(7) . ?
F3 C1 1.376(7) . ?
F4 C2 1.358(10) . ?
F5 C2 1.358(6) . ?
O C3 1.083(11) . ?
C2 F5 1.358(6) 6 ?
P C4 1.794(6) 2 ?
P C4 1.794(6) . ?
P C10 1.810(6) . ?
P C10 1.810(6) 2 ?
C4 C9 1.389(8) . ?
C4 C5 1.402(9) . ?
C5 C6 1.384(9) . ?
C6 C7 1.389(9) . ?
C7 C8 1.381(9) . ?
C8 C9 1.382(8) . ?
C10 C15 1.378(8) . ?
C10 C11 1.386(8) . ?
C11 C12 1.394(9) . ?
C12 C13 1.366(9) . ?
C13 C14 1.383(9) . ?
C14 C15 1.387(8) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au1 Br 177.88(18) . . ?
C1 Au1 Au1 94.71(17) . 2_556 ?
Br Au1 Au1 83.76(2) . 2_556 ?
C1 Au1 Au2 92.49(18) . . ?
Br Au1 Au2 89.63(2) . . ?
Au1 Au1 Au2 134.968(9) 2_556 . ?
C3 Au2 C2 175.8(3) . . ?
C3 Au2 Au1 80.5(2) . 6 ?
C2 Au2 Au1 102.94(19) . 6 ?
C3 Au2 Au1 80.5(2) . . ?
C2 Au2 Au1 102.94(19) . . ?
Au1 Au2 Au1 67.048(10) 6 . ?
Au1 Br Au1 90.28(3) 6 . ?
F1 C1 F2 104.3(5) . . ?
F1 C1 F3 103.1(5) . . ?
F2 C1 F3 102.7(5) . . ?
F1 C1 Au1 115.5(4) . . ?
F2 C1 Au1 114.0(4) . . ?
F3 C1 Au1 115.6(4) . . ?
F5 C2 F5 103.3(7) . 6 ?
F5 C2 F4 104.1(5) . . ?
F5 C2 F4 104.1(5) 6 . ?
F5 C2 Au2 114.3(5) . . ?
F5 C2 Au2 114.3(5) 6 . ?
F4 C2 Au2 115.2(6) . . ?
O C3 Au2 179.2(8) . . ?
C4 P C4 106.6(4) 2 . ?
C4 P C10 109.5(3) 2 . ?
C4 P C10 111.5(3) . . ?
C4 P C10 111.5(3) 2 2 ?
C4 P C10 109.5(3) . 2 ?
C10 P C10 108.3(4) . 2 ?
C9 C4 C5 119.8(5) . . ?
C9 C4 P 121.6(5) . . ?
C5 C4 P 118.6(5) . . ?
C6 C5 C4 119.8(6) . . ?
C5 C6 C7 120.0(6) . . ?
C8 C7 C6 120.1(6) . . ?
C7 C8 C9 120.5(6) . . ?
C8 C9 C4 119.9(6) . . ?
C15 C10 C11 121.1(5) . . ?
C15 C10 P 117.5(4) . . ?
C11 C10 P 121.3(5) . . ?
C10 C11 C12 118.8(6) . . ?
C13 C12 C11 120.1(6) . . ?
C12 C13 C14 120.8(6) . . ?
C13 C14 C15 119.7(6) . . ?
C10 C15 C14 119.4(6) . . ?
_diffrn_measured_fraction_theta_max 0.909
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 3.135
_refine_diff_density_min -2.264
_refine_diff_density_rms 0.275