# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 995723'
_audit_update_record             
;
2014-04-07 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   20.9517(2)
_cell_length_b                   21.1340(2)
_cell_length_c                   22.12610(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9797.29(14)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_space_group_name_Hall  ?
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+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Rh -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062
5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C42 H51 B1 Cl6 N6 O2 P1 Rh1 W1 
# Dc =      1.64 Fooo =   4816.00 Mu =     30.84 M =   1213.16
# Found Formula = C42 H51 B1 Cl6 N6 O2 P1 Rh1 W1 
# Dc =      1.64 FOOO =   4816.00 Mu =     30.84 M =   1213.16

_chemical_formula_sum            'C42 H51 B1 Cl6 N6 O2 P1 Rh1 W1'
_chemical_formula_moiety         'C42 H51 B1 Cl6 N6 O2 P1 Rh1 W1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         1213.16


_cell_measurement_reflns_used    123670
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      30.03
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.140
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.270

_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             4816
_exptl_absorpt_coefficient_mu    3.084

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.100
-1 0 0 0.100
0 1 0 0.080
0 -1 0 0.060
0 0 1 0.120
0 0 -1 0.150
-2 0 -3 0.100
1 1 0 0.090
-1 4 0 0.090


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            157502
_reflns_number_total             14324
_diffrn_reflns_av_R_equivalents  0.073
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 14324 
# Theoretical number of reflections is about 28702 


_diffrn_reflns_theta_min         2.666
_diffrn_reflns_theta_max         30.048
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        30.048
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       31
_reflns_limit_h_min              0
_reflns_limit_h_max              29
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.20
_refine_diff_density_max         2.25


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         14323
_refine_ls_number_restraints     0
_refine_ls_number_parameters     541
_oxford_refine_ls_R_factor_ref   0.0549
_refine_ls_wR_factor_ref         0.1063
_refine_ls_goodness_of_fit_ref   0.9458
_refine_ls_shift/su_max          0.0039986
_refine_ls_shift/su_mean         0.0000373


# The values computed from all data 
_oxford_reflns_number_all        14323
_refine_ls_R_factor_all          0.0549
_refine_ls_wR_factor_all         0.1063

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                11541
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_gt          0.0950

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 57.8 94.7 58.1 25.0 6.13 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.342161(7) 0.668037(7) 0.413349(6) 0.0220 1.0000 Uani . . . . . .
Rh1 Rh 0.538234(14) 0.811109(15) 0.397518(13) 0.0239 1.0000 Uani . . . . . .
P1 P 0.49646(5) 0.73039(5) 0.45654(4) 0.0243 1.0000 Uani . . . . . .
Cl1 Cl 0.52464(6) 0.74748(6) 0.30851(4) 0.0366 1.0000 Uani . . . . . .
Cl2 Cl 0.43190(5) 0.85259(5) 0.39203(5) 0.0362 1.0000 Uani . . . . . .
Cl3 Cl 0.68187(7) 0.36930(7) 0.25467(7) 0.0533 1.0000 Uani . . . . . .
Cl4 Cl 0.56592(11) 0.42256(11) 0.30430(11) 0.0930 1.0000 Uani . . . . . .
Cl5 Cl 0.24375(17) 0.01495(10) 0.22354(11) 0.1057 1.0000 Uani . . . . . .
Cl6 Cl 0.22453(12) 0.14373(10) 0.18276(9) 0.0810 1.0000 Uani . . . . . .
O2 O 0.37047(18) 0.72804(18) 0.28609(15) 0.0428 1.0000 Uani . . . . . .
O3 O 0.29009(18) 0.79983(17) 0.45895(19) 0.0473 1.0000 Uani . . . . . .
N11 N 0.24232(16) 0.64492(16) 0.37404(15) 0.0273 1.0000 Uani . . . . . .
N12 N 0.21909(16) 0.58403(17) 0.37979(16) 0.0288 1.0000 Uani . . . . . .
N21 N 0.36272(17) 0.57126(16) 0.37968(16) 0.0279 1.0000 Uani . . . . . .
N22 N 0.32093(18) 0.52217(17) 0.39072(18) 0.0321 1.0000 Uani . . . . . .
N31 N 0.30287(17) 0.61471(16) 0.49121(15) 0.0279 1.0000 Uani . . . . . .
N32 N 0.26489(17) 0.56225(17) 0.48255(16) 0.0296 1.0000 Uani . . . . . .
C1 C 0.42001(17) 0.69739(18) 0.43734(16) 0.0237 1.0000 Uani . . . . . .
C2 C 0.3612(2) 0.7077(2) 0.33315(18) 0.0287 1.0000 Uani . . . . . .
C3 C 0.30874(18) 0.7519(2) 0.4422(2) 0.0293 1.0000 Uani . . . . . .
C11 C 0.2003(2) 0.6765(2) 0.33928(19) 0.0310 1.0000 Uani . . . . . .
C12 C 0.1507(2) 0.6358(2) 0.3222(2) 0.0388 1.0000 Uani . . . . . .
C13 C 0.1640(2) 0.5784(2) 0.3484(2) 0.0339 1.0000 Uani . . . . . .
C14 C 0.2078(3) 0.7442(2) 0.3230(3) 0.0460 1.0000 Uani . . . . . .
C15 C 0.1278(3) 0.5173(3) 0.3441(3) 0.0491 1.0000 Uani . . . . . .
C21 C 0.4131(2) 0.5460(2) 0.3504(2) 0.0326 1.0000 Uani . . . . . .
C22 C 0.4039(2) 0.4811(2) 0.3442(2) 0.0389 1.0000 Uani . . . . . .
C23 C 0.3458(2) 0.4677(2) 0.3694(2) 0.0370 1.0000 Uani . . . . . .
C24 C 0.4687(2) 0.5840(3) 0.3302(2) 0.0432 1.0000 Uani . . . . . .
C25 C 0.3127(3) 0.4051(2) 0.3757(3) 0.0553 1.0000 Uani . . . . . .
C31 C 0.3043(2) 0.6254(2) 0.55127(18) 0.0306 1.0000 Uani . . . . . .
C32 C 0.2680(2) 0.5801(2) 0.5809(2) 0.0369 1.0000 Uani . . . . . .
C33 C 0.2437(2) 0.5410(2) 0.5366(2) 0.0324 1.0000 Uani . . . . . .
C34 C 0.3415(2) 0.6788(3) 0.5781(2) 0.0405 1.0000 Uani . . . . . .
C35 C 0.2034(2) 0.4828(2) 0.5429(2) 0.0424 1.0000 Uani . . . . . .
C41 C 0.4852(2) 0.7573(2) 0.53463(18) 0.0332 1.0000 Uani . . . . . .
C42 C 0.5202(3) 0.7339(3) 0.5831(2) 0.0437 1.0000 Uani . . . . . .
C43 C 0.5086(3) 0.7566(4) 0.6415(2) 0.0591 1.0000 Uani . . . . . .
C44 C 0.4636(4) 0.8024(4) 0.6512(2) 0.0638 1.0000 Uani . . . . . .
C45 C 0.4287(3) 0.8267(3) 0.6029(3) 0.0604 1.0000 Uani . . . . . .
C46 C 0.4399(3) 0.8045(3) 0.5448(2) 0.0424 1.0000 Uani . . . . . .
C51 C 0.5435(2) 0.6577(2) 0.4616(2) 0.0310 1.0000 Uani . . . . . .
C52 C 0.5257(2) 0.6093(2) 0.5013(2) 0.0408 1.0000 Uani . . . . . .
C53 C 0.5601(3) 0.5531(3) 0.5023(3) 0.0549 1.0000 Uani . . . . . .
C54 C 0.6105(3) 0.5439(3) 0.4633(4) 0.0634 1.0000 Uani . . . . . .
C55 C 0.6278(3) 0.5912(3) 0.4232(3) 0.0585 1.0000 Uani . . . . . .
C56 C 0.5943(2) 0.6483(3) 0.4226(2) 0.0413 1.0000 Uani . . . . . .
C61 C 0.5780(2) 0.9086(2) 0.3935(2) 0.0368 1.0000 Uani . . . . . .
C62 C 0.6121(2) 0.8702(2) 0.3535(2) 0.0344 1.0000 Uani . . . . . .
C63 C 0.64107(19) 0.8190(2) 0.3880(2) 0.0313 1.0000 Uani . . . . . .
C64 C 0.6249(2) 0.8285(2) 0.44979(19) 0.0334 1.0000 Uani . . . . . .
C65 C 0.5830(2) 0.8820(2) 0.4537(2) 0.0352 1.0000 Uani . . . . . .
C66 C 0.5413(3) 0.9675(3) 0.3782(3) 0.0594 1.0000 Uani . . . . . .
C67 C 0.6195(3) 0.8787(3) 0.2866(2) 0.0543 1.0000 Uani . . . . . .
C68 C 0.6866(2) 0.7724(3) 0.3614(3) 0.0459 1.0000 Uani . . . . . .
C69 C 0.6527(2) 0.7931(3) 0.5021(2) 0.0444 1.0000 Uani . . . . . .
C70 C 0.5576(3) 0.9118(3) 0.5103(3) 0.0571 1.0000 Uani . . . . . .
C71 C 0.5989(3) 0.3590(3) 0.2636(3) 0.0525 1.0000 Uani . . . . . .
C72 C 0.2026(4) 0.0843(4) 0.2346(3) 0.0737 1.0000 Uani . . . . . .
B1 B 0.2551(2) 0.5348(2) 0.4189(2) 0.0307 1.0000 Uani . . . . . .
H121 H 0.1151 0.6453 0.2981 0.0472 1.0000 Uiso R . . . . .
H143 H 0.1695 0.7602 0.3053 0.0687 1.0000 Uiso R . . . . .
H142 H 0.2172 0.7691 0.3580 0.0693 1.0000 Uiso R . . . . .
H141 H 0.2419 0.7496 0.2943 0.0691 1.0000 Uiso R . . . . .
H153 H 0.0886 0.5240 0.3230 0.0741 1.0000 Uiso R . . . . .
H152 H 0.1189 0.5011 0.3833 0.0739 1.0000 Uiso R . . . . .
H151 H 0.1526 0.4868 0.3226 0.0737 1.0000 Uiso R . . . . .
H221 H 0.4313 0.4522 0.3270 0.0470 1.0000 Uiso R . . . . .
H242 H 0.4980 0.5584 0.3082 0.0652 1.0000 Uiso R . . . . .
H241 H 0.4904 0.6008 0.3641 0.0654 1.0000 Uiso R . . . . .
H243 H 0.4546 0.6182 0.3053 0.0653 1.0000 Uiso R . . . . .
H252 H 0.3411 0.3726 0.3620 0.0831 1.0000 Uiso R . . . . .
H251 H 0.3026 0.3981 0.4175 0.0830 1.0000 Uiso R . . . . .
H253 H 0.2741 0.4039 0.3525 0.0830 1.0000 Uiso R . . . . .
H321 H 0.2616 0.5767 0.6221 0.0444 1.0000 Uiso R . . . . .
H341 H 0.3325 0.6811 0.6210 0.0611 1.0000 Uiso R . . . . .
H343 H 0.3287 0.7180 0.5598 0.0612 1.0000 Uiso R . . . . .
H342 H 0.3864 0.6724 0.5715 0.0612 1.0000 Uiso R . . . . .
H351 H 0.1907 0.4778 0.5845 0.0641 1.0000 Uiso R . . . . .
H353 H 0.1660 0.4867 0.5178 0.0638 1.0000 Uiso R . . . . .
H352 H 0.2284 0.4469 0.5306 0.0643 1.0000 Uiso R . . . . .
H421 H 0.5511 0.7035 0.5767 0.0521 1.0000 Uiso R . . . . .
H431 H 0.5312 0.7405 0.6740 0.0710 1.0000 Uiso R . . . . .
H441 H 0.4565 0.8176 0.6903 0.0772 1.0000 Uiso R . . . . .
H451 H 0.3983 0.8578 0.6091 0.0721 1.0000 Uiso R . . . . .
H461 H 0.4168 0.8207 0.5126 0.0508 1.0000 Uiso R . . . . .
H521 H 0.4904 0.6148 0.5268 0.0490 1.0000 Uiso R . . . . .
H531 H 0.5492 0.5215 0.5300 0.0661 1.0000 Uiso R . . . . .
H541 H 0.6331 0.5060 0.4640 0.0761 1.0000 Uiso R . . . . .
H551 H 0.6618 0.5849 0.3970 0.0702 1.0000 Uiso R . . . . .
H561 H 0.6056 0.6798 0.3956 0.0497 1.0000 Uiso R . . . . .
H661 H 0.4988 0.9636 0.3934 0.0892 1.0000 Uiso R . . . . .
H663 H 0.5611 1.0034 0.3966 0.0890 1.0000 Uiso R . . . . .
H662 H 0.5400 0.9736 0.3354 0.0892 1.0000 Uiso R . . . . .
H671 H 0.6045 0.8418 0.2661 0.0809 1.0000 Uiso R . . . . .
H673 H 0.6634 0.8849 0.2774 0.0811 1.0000 Uiso R . . . . .
H672 H 0.5954 0.9146 0.2740 0.0810 1.0000 Uiso R . . . . .
H681 H 0.7001 0.7425 0.3917 0.0690 1.0000 Uiso R . . . . .
H683 H 0.7236 0.7946 0.3470 0.0691 1.0000 Uiso R . . . . .
H682 H 0.6670 0.7504 0.3280 0.0689 1.0000 Uiso R . . . . .
H691 H 0.6244 0.7949 0.5362 0.0668 1.0000 Uiso R . . . . .
H693 H 0.6929 0.8114 0.5141 0.0669 1.0000 Uiso R . . . . .
H692 H 0.6596 0.7498 0.4911 0.0672 1.0000 Uiso R . . . . .
H701 H 0.5545 0.8804 0.5416 0.0859 1.0000 Uiso R . . . . .
H703 H 0.5858 0.9445 0.5234 0.0861 1.0000 Uiso R . . . . .
H702 H 0.5161 0.9293 0.5029 0.0860 1.0000 Uiso R . . . . .
H711 H 0.5905 0.3200 0.2856 0.0631 1.0000 Uiso R . . . . .
H712 H 0.5787 0.3568 0.2242 0.0632 1.0000 Uiso R . . . . .
H722 H 0.2062 0.0986 0.2763 0.0880 1.0000 Uiso R . . . . .
H721 H 0.1570 0.0718 0.2216 0.0871 1.0000 Uiso R . . . . .
H11 H 0.2295 0.4900 0.4228 0.0349 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.11955(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . N11 . 2.318(3) yes
W1 . N21 . 2.219(3) yes
W1 . N31 . 2.217(3) yes
W1 . C1 . 1.824(4) yes
W1 . C2 . 2.003(4) yes
W1 . C3 . 2.010(4) yes
Rh1 . P1 . 2.3198(10) yes
Rh1 . Cl1 . 2.4017(11) yes
Rh1 . Cl2 . 2.3973(11) yes
Rh1 . C61 . 2.224(4) yes
Rh1 . C62 . 2.214(4) yes
Rh1 . C63 . 2.171(4) yes
Rh1 . C64 . 2.184(4) yes
Rh1 . C65 . 2.161(4) yes
P1 . C1 . 1.798(4) yes
P1 . C41 . 1.835(4) yes
P1 . C51 . 1.828(4) yes
Cl3 . C71 . 1.764(6) yes
Cl4 . C71 . 1.758(6) yes
Cl5 . C72 . 1.718(8) yes
Cl6 . C72 . 1.762(8) yes
O2 . C2 . 1.143(5) yes
O3 . C3 . 1.147(5) yes
N11 . N12 . 1.382(5) yes
N11 . C11 . 1.347(5) yes
N12 . C13 . 1.352(5) yes
N12 . B1 . 1.549(6) yes
N21 . N22 . 1.380(5) yes
N21 . C21 . 1.348(5) yes
N22 . C23 . 1.349(6) yes
N22 . B1 . 1.537(6) yes
N31 . N32 . 1.378(5) yes
N31 . C31 . 1.348(5) yes
N32 . C33 . 1.353(5) yes
N32 . B1 . 1.537(6) yes
C11 . C12 . 1.402(6) yes
C11 . C14 . 1.482(6) yes
C12 . C13 . 1.373(7) yes
C12 . H121 . 0.939 no
C13 . C15 . 1.501(7) yes
C14 . H143 . 0.955 no
C14 . H142 . 0.956 no
C14 . H141 . 0.962 no
C15 . H153 . 0.956 no
C15 . H152 . 0.950 no
C15 . H151 . 0.954 no
C21 . C22 . 1.392(6) yes
C21 . C24 . 1.484(6) yes
C22 . C23 . 1.368(7) yes
C22 . H221 . 0.921 no
C23 . C25 . 1.500(7) yes
C24 . H242 . 0.954 no
C24 . H241 . 0.946 no
C24 . H243 . 0.955 no
C25 . H252 . 0.957 no
C25 . H251 . 0.961 no
C25 . H253 . 0.959 no
C31 . C32 . 1.387(6) yes
C31 . C34 . 1.495(7) yes
C32 . C33 . 1.380(7) yes
C32 . H321 . 0.925 no
C33 . C35 . 1.498(6) yes
C34 . H341 . 0.970 no
C34 . H343 . 0.959 no
C34 . H342 . 0.960 no
C35 . H351 . 0.965 no
C35 . H353 . 0.964 no
C35 . H352 . 0.960 no
C41 . C42 . 1.391(6) yes
C41 . C46 . 1.394(7) yes
C42 . C43 . 1.399(7) yes
C42 . H421 . 0.922 no
C43 . C44 . 1.370(10) yes
C43 . H431 . 0.927 no
C44 . C45 . 1.391(11) yes
C44 . H441 . 0.936 no
C45 . C46 . 1.390(7) yes
C45 . H451 . 0.925 no
C46 . H461 . 0.927 no
C51 . C52 . 1.399(6) yes
C51 . C56 . 1.385(6) yes
C52 . C53 . 1.389(8) yes
C52 . H521 . 0.937 no
C53 . C54 . 1.378(10) yes
C53 . H531 . 0.934 no
C54 . C55 . 1.385(9) yes
C54 . H541 . 0.931 no
C55 . C56 . 1.396(7) yes
C55 . H551 . 0.928 no
C56 . H561 . 0.925 no
C61 . C62 . 1.398(7) yes
C61 . C65 . 1.449(7) yes
C61 . C66 . 1.501(7) yes
C62 . C63 . 1.455(6) yes
C62 . C67 . 1.500(7) yes
C63 . C64 . 1.423(6) yes
C63 . C68 . 1.492(7) yes
C64 . C65 . 1.435(7) yes
C64 . C69 . 1.497(6) yes
C65 . C70 . 1.499(7) yes
C66 . H661 . 0.956 no
C66 . H663 . 0.954 no
C66 . H662 . 0.956 no
C67 . H671 . 0.955 no
C67 . H673 . 0.951 no
C67 . H672 . 0.954 no
C68 . H681 . 0.963 no
C68 . H683 . 0.960 no
C68 . H682 . 0.965 no
C69 . H691 . 0.959 no
C69 . H693 . 0.965 no
C69 . H692 . 0.958 no
C70 . H701 . 0.962 no
C70 . H703 . 0.955 no
C70 . H702 . 0.959 no
C71 . H711 . 0.972 no
C71 . H712 . 0.970 no
C72 . H722 . 0.974 no
C72 . H721 . 1.030 no
B1 . H11 . 1.091 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 . W1 . N21 . 81.66(12) yes
N11 . W1 . N31 . 81.33(12) yes
N21 . W1 . N31 . 82.21(13) yes
N11 . W1 . C1 . 171.14(15) yes
N21 . W1 . C1 . 103.74(15) yes
N31 . W1 . C1 . 106.19(15) yes
N11 . W1 . C2 . 86.32(14) yes
N21 . W1 . C2 . 92.85(15) yes
N31 . W1 . C2 . 167.24(15) yes
C1 . W1 . C2 . 86.39(16) yes
N11 . W1 . C3 . 89.47(14) yes
N21 . W1 . C3 . 170.81(14) yes
N31 . W1 . C3 . 94.13(15) yes
C1 . W1 . C3 . 85.36(16) yes
C2 . W1 . C3 . 88.96(18) yes
P1 . Rh1 . Cl1 . 90.29(4) yes
P1 . Rh1 . Cl2 . 86.95(4) yes
Cl1 . Rh1 . Cl2 . 93.04(4) yes
P1 . Rh1 . C61 . 147.69(14) yes
Cl1 . Rh1 . C61 . 122.01(14) yes
Cl2 . Rh1 . C61 . 90.42(13) yes
P1 . Rh1 . C62 . 157.81(13) yes
Cl1 . Rh1 . C62 . 92.15(12) yes
Cl2 . Rh1 . C62 . 114.92(13) yes
C61 . Rh1 . C62 . 36.71(18) yes
P1 . Rh1 . C63 . 119.06(12) yes
Cl1 . Rh1 . C63 . 94.64(12) yes
Cl2 . Rh1 . C63 . 152.76(12) yes
C61 . Rh1 . C63 . 63.45(17) yes
C62 . Rh1 . C63 . 38.75(17) yes
P1 . Rh1 . C64 . 98.00(12) yes
Cl1 . Rh1 . C64 . 128.83(13) yes
Cl2 . Rh1 . C64 . 137.57(13) yes
C61 . Rh1 . C64 . 63.52(18) yes
C62 . Rh1 . C64 . 63.71(16) yes
P1 . Rh1 . C65 . 110.50(13) yes
Cl1 . Rh1 . C65 . 155.68(12) yes
Cl2 . Rh1 . C65 . 100.31(13) yes
C61 . Rh1 . C65 . 38.56(18) yes
C62 . Rh1 . C65 . 63.81(17) yes
C63 . Rh1 . C64 . 38.15(16) yes
C63 . Rh1 . C65 . 64.65(17) yes
C64 . Rh1 . C65 . 38.56(18) yes
Rh1 . P1 . C1 . 119.23(13) yes
Rh1 . P1 . C41 . 110.53(15) yes
C1 . P1 . C41 . 103.18(18) yes
Rh1 . P1 . C51 . 116.68(15) yes
C1 . P1 . C51 . 99.73(18) yes
C41 . P1 . C51 . 105.8(2) yes
W1 . N11 . N12 . 118.7(2) yes
W1 . N11 . C11 . 134.5(3) yes
N12 . N11 . C11 . 106.5(3) yes
N11 . N12 . C13 . 109.6(4) yes
N11 . N12 . B1 . 120.4(3) yes
C13 . N12 . B1 . 130.0(4) yes
W1 . N21 . N22 . 120.7(3) yes
W1 . N21 . C21 . 132.7(3) yes
N22 . N21 . C21 . 106.5(3) yes
N21 . N22 . C23 . 109.6(4) yes
N21 . N22 . B1 . 120.7(3) yes
C23 . N22 . B1 . 129.5(4) yes
W1 . N31 . N32 . 121.0(3) yes
W1 . N31 . C31 . 132.2(3) yes
N32 . N31 . C31 . 106.6(3) yes
N31 . N32 . C33 . 109.5(4) yes
N31 . N32 . B1 . 120.6(3) yes
C33 . N32 . B1 . 129.8(4) yes
P1 . C1 . W1 . 175.8(2) yes
W1 . C2 . O2 . 176.7(4) yes
W1 . C3 . O3 . 179.5(4) yes
N11 . C11 . C12 . 109.5(4) yes
N11 . C11 . C14 . 123.2(4) yes
C12 . C11 . C14 . 127.3(4) yes
C11 . C12 . C13 . 106.1(4) yes
C11 . C12 . H121 . 127.6 no
C13 . C12 . H121 . 126.3 no
C12 . C13 . N12 . 108.3(4) yes
C12 . C13 . C15 . 129.0(4) yes
N12 . C13 . C15 . 122.6(5) yes
C11 . C14 . H143 . 110.6 no
C11 . C14 . H142 . 110.9 no
H143 . C14 . H142 . 108.0 no
C11 . C14 . H141 . 110.8 no
H143 . C14 . H141 . 108.0 no
H142 . C14 . H141 . 108.4 no
C13 . C15 . H153 . 109.7 no
C13 . C15 . H152 . 110.5 no
H153 . C15 . H152 . 109.3 no
C13 . C15 . H151 . 109.6 no
H153 . C15 . H151 . 108.9 no
H152 . C15 . H151 . 108.7 no
N21 . C21 . C22 . 109.3(4) yes
N21 . C21 . C24 . 123.0(4) yes
C22 . C21 . C24 . 127.8(4) yes
C21 . C22 . C23 . 106.6(4) yes
C21 . C22 . H221 . 127.5 no
C23 . C22 . H221 . 125.9 no
C22 . C23 . N22 . 108.0(4) yes
C22 . C23 . C25 . 129.1(4) yes
N22 . C23 . C25 . 122.8(4) yes
C21 . C24 . H242 . 110.6 no
C21 . C24 . H241 . 110.1 no
H242 . C24 . H241 . 107.9 no
C21 . C24 . H243 . 110.0 no
H242 . C24 . H243 . 109.4 no
H241 . C24 . H243 . 108.8 no
C23 . C25 . H252 . 108.4 no
C23 . C25 . H251 . 109.1 no
H252 . C25 . H251 . 109.3 no
C23 . C25 . H253 . 111.3 no
H252 . C25 . H253 . 109.7 no
H251 . C25 . H253 . 109.0 no
N31 . C31 . C32 . 109.7(4) yes
N31 . C31 . C34 . 121.9(4) yes
C32 . C31 . C34 . 128.3(4) yes
C31 . C32 . C33 . 106.3(4) yes
C31 . C32 . H321 . 126.9 no
C33 . C32 . H321 . 126.7 no
C32 . C33 . N32 . 107.9(4) yes
C32 . C33 . C35 . 129.4(4) yes
N32 . C33 . C35 . 122.7(4) yes
C31 . C34 . H341 . 108.9 no
C31 . C34 . H343 . 109.8 no
H341 . C34 . H343 . 108.3 no
C31 . C34 . H342 . 110.1 no
H341 . C34 . H342 . 110.3 no
H343 . C34 . H342 . 109.4 no
C33 . C35 . H351 . 109.4 no
C33 . C35 . H353 . 109.5 no
H351 . C35 . H353 . 109.5 no
C33 . C35 . H352 . 108.3 no
H351 . C35 . H352 . 109.6 no
H353 . C35 . H352 . 110.4 no
P1 . C41 . C42 . 123.2(4) yes
P1 . C41 . C46 . 117.5(4) yes
C42 . C41 . C46 . 119.3(4) yes
C41 . C42 . C43 . 119.8(6) yes
C41 . C42 . H421 . 120.0 no
C43 . C42 . H421 . 120.2 no
C42 . C43 . C44 . 120.5(6) yes
C42 . C43 . H431 . 120.2 no
C44 . C43 . H431 . 119.4 no
C43 . C44 . C45 . 120.2(5) yes
C43 . C44 . H441 . 119.8 no
C45 . C44 . H441 . 120.1 no
C44 . C45 . C46 . 119.8(7) yes
C44 . C45 . H451 . 120.7 no
C46 . C45 . H451 . 119.6 no
C41 . C46 . C45 . 120.4(6) yes
C41 . C46 . H461 . 119.8 no
C45 . C46 . H461 . 119.8 no
P1 . C51 . C52 . 120.6(4) yes
P1 . C51 . C56 . 119.8(3) yes
C52 . C51 . C56 . 119.4(4) yes
C51 . C52 . C53 . 119.9(5) yes
C51 . C52 . H521 . 119.8 no
C53 . C52 . H521 . 120.3 no
C52 . C53 . C54 . 120.4(5) yes
C52 . C53 . H531 . 119.7 no
C54 . C53 . H531 . 119.9 no
C53 . C54 . C55 . 120.1(5) yes
C53 . C54 . H541 . 120.1 no
C55 . C54 . H541 . 119.8 no
C54 . C55 . C56 . 119.8(6) yes
C54 . C55 . H551 . 119.9 no
C56 . C55 . H551 . 120.3 no
C55 . C56 . C51 . 120.4(5) yes
C55 . C56 . H561 . 119.9 no
C51 . C56 . H561 . 119.7 no
Rh1 . C61 . C62 . 71.2(3) yes
Rh1 . C61 . C65 . 68.3(2) yes
C62 . C61 . C65 . 108.6(4) yes
Rh1 . C61 . C66 . 125.8(3) yes
C62 . C61 . C66 . 127.0(5) yes
C65 . C61 . C66 . 124.4(5) yes
Rh1 . C62 . C61 . 72.0(3) yes
Rh1 . C62 . C63 . 69.0(2) yes
C61 . C62 . C63 . 108.2(4) yes
Rh1 . C62 . C67 . 125.1(3) yes
C61 . C62 . C67 . 127.5(5) yes
C63 . C62 . C67 . 124.3(5) yes
C62 . C63 . Rh1 . 72.2(2) yes
C62 . C63 . C64 . 107.5(4) yes
Rh1 . C63 . C64 . 71.4(2) yes
C62 . C63 . C68 . 123.4(4) yes
Rh1 . C63 . C68 . 128.5(3) yes
C64 . C63 . C68 . 128.5(4) yes
C63 . C64 . Rh1 . 70.4(2) yes
C63 . C64 . C65 . 108.3(4) yes
Rh1 . C64 . C65 . 69.8(2) yes
C63 . C64 . C69 . 125.5(5) yes
Rh1 . C64 . C69 . 130.5(3) yes
C65 . C64 . C69 . 125.9(4) yes
C61 . C65 . C64 . 107.2(4) yes
C61 . C65 . Rh1 . 73.1(2) yes
C64 . C65 . Rh1 . 71.6(2) yes
C61 . C65 . C70 . 125.4(5) yes
C64 . C65 . C70 . 126.7(5) yes
Rh1 . C65 . C70 . 128.1(3) yes
C61 . C66 . H661 . 109.1 no
C61 . C66 . H663 . 109.9 no
H661 . C66 . H663 . 108.9 no
C61 . C66 . H662 . 110.4 no
H661 . C66 . H662 . 109.4 no
H663 . C66 . H662 . 109.1 no
C62 . C67 . H671 . 109.6 no
C62 . C67 . H673 . 109.1 no
H671 . C67 . H673 . 109.3 no
C62 . C67 . H672 . 109.1 no
H671 . C67 . H672 . 109.7 no
H673 . C67 . H672 . 109.9 no
C63 . C68 . H681 . 110.3 no
C63 . C68 . H683 . 108.9 no
H681 . C68 . H683 . 108.4 no
C63 . C68 . H682 . 110.3 no
H681 . C68 . H682 . 110.0 no
H683 . C68 . H682 . 108.9 no
C64 . C69 . H691 . 110.3 no
C64 . C69 . H693 . 110.5 no
H691 . C69 . H693 . 107.9 no
C64 . C69 . H692 . 109.9 no
H691 . C69 . H692 . 109.4 no
H693 . C69 . H692 . 108.7 no
C65 . C70 . H701 . 109.8 no
C65 . C70 . H703 . 109.8 no
H701 . C70 . H703 . 108.6 no
C65 . C70 . H702 . 110.1 no
H701 . C70 . H702 . 109.1 no
H703 . C70 . H702 . 109.5 no
Cl3 . C71 . Cl4 . 110.5(4) yes
Cl3 . C71 . H711 . 109.8 no
Cl4 . C71 . H711 . 108.7 no
Cl3 . C71 . H712 . 109.5 no
Cl4 . C71 . H712 . 109.0 no
H711 . C71 . H712 . 109.4 no
Cl6 . C72 . Cl5 . 112.6(4) yes
Cl6 . C72 . H722 . 111.9 no
Cl5 . C72 . H722 . 111.2 no
Cl6 . C72 . H721 . 104.0 no
Cl5 . C72 . H721 . 102.0 no
H722 . C72 . H721 . 114.5 no
N12 . B1 . N32 . 108.8(3) yes
N12 . B1 . N22 . 109.1(3) yes
N32 . B1 . N22 . 108.5(4) yes
N12 . B1 . H11 . 112.8 no
N32 . B1 . H11 . 108.7 no
N22 . B1 . H11 . 108.9 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 04/04/12 at 15:38:54
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 153,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 251,X'S) H   ( 253,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 343,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 353,X'S) H   ( 352,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 663,X'S) H   ( 662,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) H   ( 673,X'S) H   ( 672,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 683,X'S) H   ( 682,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) H   ( 693,X'S) H   ( 692,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 703,X'S) H   ( 702,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE C   (  72,X'S) H   ( 722,X'S) H   ( 721,X'S) 
RIDE B   (   1,X'S) H   (  11,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 04/04/12 at 15:38:54
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
2 2 0 x .



####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 995724'
_audit_update_record             
;
2014-04-07 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   10.31720(10)
_cell_length_b                   13.5659(2)
_cell_length_c                   25.2039(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.3693(5)
_cell_angle_gamma                90
_cell_volume                     3490.02(7)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956
12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C30 H32 Au1 B1 Cl1 N6 O2 P1 W1 
# Dc =      1.84 Fooo =   1840.00 Mu =     76.49 M =    966.68
# Found Formula = C30 H32 Au1 B1 Cl1 N6 O2 P1 W1 
# Dc =      1.84 FOOO =   1840.00 Mu =     76.49 M =    966.68

_chemical_formula_sum            'C30 H32 Au1 B1 Cl1 N6 O2 P1 W1'
_chemical_formula_moiety         'C30 H32 Au1 B1 Cl1 N6 O2 P1 W1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         966.68


_cell_measurement_reflns_used    95459
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      30.03
_cell_measurement_temperature    200

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_max          0.380

_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1840
_exptl_absorpt_coefficient_mu    7.649

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.200
0 1 0 0.180
0 -1 0 0.200
0 0 1 0.020
0 0 -1 0.030
-4 -4 0 0.157
3 3 0 0.120
8 2 0 0.143


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            83785
_reflns_number_total             10247
_diffrn_reflns_av_R_equivalents  0.071
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 10247 
# Theoretical number of reflections is about 20568 


_diffrn_reflns_theta_min         2.716
_diffrn_reflns_theta_max         30.112
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        30.112
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              35

_oxford_diffrn_Wilson_B_factor   2.39
_oxford_diffrn_Wilson_scale      50.77

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.07
_refine_diff_density_max         1.44


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         10245
_refine_ls_number_restraints     0
_refine_ls_number_parameters     388
_oxford_refine_ls_R_factor_ref   0.0467
_refine_ls_wR_factor_ref         0.0668
_refine_ls_goodness_of_fit_ref   0.9827
_refine_ls_shift/su_max          0.0014644
_refine_ls_shift/su_mean         0.0000387


# The values computed from all data 
_oxford_reflns_number_all        10245
_refine_ls_R_factor_all          0.0467
_refine_ls_wR_factor_all         0.0668

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8112
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_gt          0.0616

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 8.82P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.092327(13) 0.587923(11) 0.318876(6) 0.0253 1.0000 Uani . . . . . .
Au1 Au 0.071407(15) 0.645015(14) 0.132251(7) 0.0419 1.0000 Uani . . . . . .
Cl1 Cl 0.19511(14) 0.72744(17) 0.07919(7) 0.0983 1.0000 Uani . . . . . .
P1 P -0.05788(9) 0.56917(7) 0.18263(4) 0.0283 1.0000 Uani . . . . . .
O2 O 0.1385(3) 0.3624(2) 0.29778(15) 0.0527 1.0000 Uani . . . . . .
O3 O 0.3187(3) 0.6203(3) 0.24973(15) 0.0594 1.0000 Uani . . . . . .
N11 N 0.0730(3) 0.7442(2) 0.34080(13) 0.0314 1.0000 Uani . . . . . .
N12 N 0.0661(3) 0.7712(3) 0.39277(14) 0.0370 1.0000 Uani . . . . . .
N21 N 0.2421(3) 0.5844(2) 0.39543(13) 0.0307 1.0000 Uani . . . . . .
N22 N 0.2189(3) 0.6430(2) 0.43748(13) 0.0312 1.0000 Uani . . . . . .
N31 N -0.0462(3) 0.5668(2) 0.37647(12) 0.0285 1.0000 Uani . . . . . .
N32 N -0.0253(3) 0.6150(3) 0.42536(13) 0.0337 1.0000 Uani . . . . . .
C1 C -0.0035(3) 0.5819(3) 0.25232(15) 0.0289 1.0000 Uani . . . . . .
C2 C 0.1217(4) 0.4426(3) 0.30761(17) 0.0339 1.0000 Uani . . . . . .
C3 C 0.2385(4) 0.6116(3) 0.27622(17) 0.0361 1.0000 Uani . . . . . .
C11 C 0.0647(4) 0.8284(3) 0.31173(17) 0.0376 1.0000 Uani . . . . . .
C12 C 0.0540(5) 0.9073(3) 0.3452(2) 0.0513 1.0000 Uani . . . . . .
C13 C 0.0561(5) 0.8703(3) 0.3960(2) 0.0514 1.0000 Uani . . . . . .
C14 C 0.0634(6) 0.8288(4) 0.25276(19) 0.0533 1.0000 Uani . . . . . .
C15 C 0.0445(9) 0.9226(4) 0.4472(2) 0.0960 1.0000 Uani . . . . . .
C21 C 0.3667(4) 0.5520(3) 0.40776(17) 0.0341 1.0000 Uani . . . . . .
C22 C 0.4228(4) 0.5912(3) 0.45619(18) 0.0397 1.0000 Uani . . . . . .
C23 C 0.3272(4) 0.6491(3) 0.47428(16) 0.0368 1.0000 Uani . . . . . .
C24 C 0.4269(4) 0.4832(4) 0.3723(2) 0.0484 1.0000 Uani . . . . . .
C25 C 0.3348(5) 0.7110(4) 0.52359(18) 0.0513 1.0000 Uani . . . . . .
C31 C -0.1504(4) 0.5071(3) 0.37750(17) 0.0336 1.0000 Uani . . . . . .
C32 C -0.1945(4) 0.5177(3) 0.42683(18) 0.0397 1.0000 Uani . . . . . .
C33 C -0.1154(4) 0.5847(3) 0.45595(17) 0.0389 1.0000 Uani . . . . . .
C34 C -0.2018(4) 0.4424(4) 0.33140(19) 0.0447 1.0000 Uani . . . . . .
C35 C -0.1190(5) 0.6212(4) 0.51161(19) 0.0548 1.0000 Uani . . . . . .
C41 C -0.2234(4) 0.6183(3) 0.17204(16) 0.0310 1.0000 Uani . . . . . .
C42 C -0.2853(4) 0.6483(3) 0.21455(17) 0.0358 1.0000 Uani . . . . . .
C43 C -0.4122(4) 0.6854(4) 0.2045(2) 0.0457 1.0000 Uani . . . . . .
C44 C -0.4766(4) 0.6915(3) 0.1530(2) 0.0474 1.0000 Uani . . . . . .
C45 C -0.4152(4) 0.6630(3) 0.1108(2) 0.0463 1.0000 Uani . . . . . .
C46 C -0.2880(4) 0.6267(3) 0.11997(18) 0.0404 1.0000 Uani . . . . . .
C51 C -0.0736(4) 0.4375(3) 0.16839(16) 0.0339 1.0000 Uani . . . . . .
C52 C 0.0356(5) 0.3863(4) 0.1576(2) 0.0518 1.0000 Uani . . . . . .
C53 C 0.0254(6) 0.2868(4) 0.1449(2) 0.0647 1.0000 Uani . . . . . .
C54 C -0.0932(6) 0.2387(4) 0.1429(2) 0.0656 1.0000 Uani . . . . . .
C55 C -0.2021(5) 0.2889(4) 0.1550(2) 0.0569 1.0000 Uani . . . . . .
C56 C -0.1918(4) 0.3886(3) 0.1684(2) 0.0454 1.0000 Uani . . . . . .
B1 B 0.0835(4) 0.6931(4) 0.43737(18) 0.0343 1.0000 Uani . . . . . .
H121 H 0.0467 0.9726 0.3352 0.0621 1.0000 Uiso R . . . . .
H142 H 0.0582 0.8954 0.2401 0.0801 1.0000 Uiso R . . . . .
H143 H 0.1410 0.7979 0.2443 0.0801 1.0000 Uiso R . . . . .
H141 H -0.0122 0.7927 0.2359 0.0801 1.0000 Uiso R . . . . .
H153 H 0.0471 0.9923 0.4414 0.1438 1.0000 Uiso R . . . . .
H151 H 0.1157 0.9028 0.4736 0.1439 1.0000 Uiso R . . . . .
H152 H -0.0374 0.9043 0.4584 0.1440 1.0000 Uiso R . . . . .
H221 H 0.5075 0.5797 0.4730 0.0477 1.0000 Uiso R . . . . .
H243 H 0.5141 0.4680 0.3880 0.0732 1.0000 Uiso R . . . . .
H241 H 0.4266 0.5142 0.3383 0.0732 1.0000 Uiso R . . . . .
H242 H 0.3761 0.4247 0.3678 0.0732 1.0000 Uiso R . . . . .
H251 H 0.4186 0.7030 0.5441 0.0772 1.0000 Uiso R . . . . .
H253 H 0.3216 0.7788 0.5139 0.0770 1.0000 Uiso R . . . . .
H252 H 0.2695 0.6917 0.5446 0.0769 1.0000 Uiso R . . . . .
H321 H -0.2640 0.4855 0.4386 0.0478 1.0000 Uiso R . . . . .
H341 H -0.2661 0.3981 0.3409 0.0674 1.0000 Uiso R . . . . .
H343 H -0.2411 0.4809 0.3016 0.0675 1.0000 Uiso R . . . . .
H342 H -0.1328 0.4048 0.3203 0.0682 1.0000 Uiso R . . . . .
H352 H -0.1805 0.5854 0.5277 0.0819 1.0000 Uiso R . . . . .
H351 H -0.1422 0.6892 0.5108 0.0816 1.0000 Uiso R . . . . .
H353 H -0.0350 0.6135 0.5326 0.0821 1.0000 Uiso R . . . . .
H421 H -0.2424 0.6429 0.2490 0.0427 1.0000 Uiso R . . . . .
H431 H -0.4521 0.7051 0.2331 0.0548 1.0000 Uiso R . . . . .
H441 H -0.5618 0.7167 0.1470 0.0571 1.0000 Uiso R . . . . .
H451 H -0.4580 0.6691 0.0759 0.0559 1.0000 Uiso R . . . . .
H461 H -0.2478 0.6083 0.0911 0.0487 1.0000 Uiso R . . . . .
H521 H 0.1151 0.4183 0.1588 0.0620 1.0000 Uiso R . . . . .
H531 H 0.1000 0.2525 0.1371 0.0784 1.0000 Uiso R . . . . .
H541 H -0.1000 0.1718 0.1332 0.0791 1.0000 Uiso R . . . . .
H551 H -0.2815 0.2561 0.1542 0.0682 1.0000 Uiso R . . . . .
H561 H -0.2642 0.4224 0.1773 0.0540 1.0000 Uiso R . . . . .
H11 H 0.0788 0.7263 0.4778 0.0225 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.15565(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . N11 . 2.207(3) yes
W1 . N21 . 2.290(3) yes
W1 . N31 . 2.199(3) yes
W1 . C1 . 1.821(4) yes
W1 . C2 . 2.021(4) yes
W1 . C3 . 2.002(4) yes
Au1 . Cl1 . 2.2724(13) yes
Au1 . P1 . 2.2234(10) yes
P1 . C1 . 1.773(4) yes
P1 . C41 . 1.816(4) yes
P1 . C51 . 1.825(4) yes
O2 . C2 . 1.135(5) yes
O3 . C3 . 1.142(5) yes
N11 . N12 . 1.372(4) yes
N11 . C11 . 1.353(5) yes
N12 . C13 . 1.351(5) yes
N12 . B1 . 1.536(6) yes
N21 . N22 . 1.374(4) yes
N21 . C21 . 1.351(5) yes
N22 . C23 . 1.347(5) yes
N22 . B1 . 1.553(5) yes
N31 . N32 . 1.383(4) yes
N31 . C31 . 1.349(5) yes
N32 . C33 . 1.354(5) yes
N32 . B1 . 1.542(6) yes
C11 . C12 . 1.378(6) yes
C11 . C14 . 1.484(6) yes
C12 . C13 . 1.373(7) yes
C12 . H121 . 0.921 no
C13 . C15 . 1.494(7) yes
C14 . H142 . 0.957 no
C14 . H143 . 0.955 no
C14 . H141 . 0.966 no
C15 . H153 . 0.958 no
C15 . H151 . 0.955 no
C15 . H152 . 0.960 no
C21 . C22 . 1.379(6) yes
C21 . C24 . 1.489(6) yes
C22 . C23 . 1.389(6) yes
C22 . H221 . 0.927 no
C23 . C25 . 1.493(6) yes
C24 . H243 . 0.952 no
C24 . H241 . 0.955 no
C24 . H242 . 0.948 no
C25 . H251 . 0.947 no
C25 . H253 . 0.956 no
C25 . H252 . 0.953 no
C31 . C32 . 1.392(6) yes
C31 . C34 . 1.491(6) yes
C32 . C33 . 1.363(6) yes
C32 . H321 . 0.924 no
C33 . C35 . 1.494(6) yes
C34 . H341 . 0.951 no
C34 . H343 . 0.956 no
C34 . H342 . 0.950 no
C35 . H352 . 0.937 no
C35 . H351 . 0.952 no
C35 . H353 . 0.953 no
C41 . C42 . 1.386(6) yes
C41 . C46 . 1.387(6) yes
C42 . C43 . 1.391(6) yes
C42 . H421 . 0.919 no
C43 . C44 . 1.371(7) yes
C43 . H431 . 0.921 no
C44 . C45 . 1.371(7) yes
C44 . H441 . 0.935 no
C45 . C46 . 1.390(6) yes
C45 . H451 . 0.929 no
C46 . H461 . 0.922 no
C51 . C52 . 1.384(6) yes
C51 . C56 . 1.388(6) yes
C52 . C53 . 1.387(7) yes
C52 . H521 . 0.924 no
C53 . C54 . 1.381(8) yes
C53 . H531 . 0.945 no
C54 . C55 . 1.386(8) yes
C54 . H541 . 0.939 no
C55 . C56 . 1.393(7) yes
C55 . H551 . 0.930 no
C56 . H561 . 0.932 no
B1 . H11 . 1.122 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 . W1 . N21 . 83.32(11) yes
N11 . W1 . N31 . 82.45(12) yes
N21 . W1 . N31 . 82.23(11) yes
N11 . W1 . C1 . 102.53(14) yes
N21 . W1 . C1 . 169.92(13) yes
N31 . W1 . C1 . 106.52(14) yes
N11 . W1 . C2 . 173.22(14) yes
N21 . W1 . C2 . 90.07(14) yes
N31 . W1 . C2 . 95.22(14) yes
C1 . W1 . C2 . 84.22(17) yes
N11 . W1 . C3 . 94.75(15) yes
N21 . W1 . C3 . 89.27(14) yes
N31 . W1 . C3 . 171.29(14) yes
C1 . W1 . C3 . 82.12(16) yes
C2 . W1 . C3 . 86.63(17) yes
Cl1 . Au1 . P1 . 177.17(5) yes
Au1 . P1 . C1 . 113.02(12) yes
Au1 . P1 . C41 . 112.07(13) yes
C1 . P1 . C41 . 105.37(18) yes
Au1 . P1 . C51 . 112.61(14) yes
C1 . P1 . C51 . 107.26(18) yes
C41 . P1 . C51 . 105.97(18) yes
W1 . N11 . N12 . 121.0(2) yes
W1 . N11 . C11 . 132.6(3) yes
N12 . N11 . C11 . 106.4(3) yes
N11 . N12 . C13 . 109.8(4) yes
N11 . N12 . B1 . 119.8(3) yes
C13 . N12 . B1 . 130.1(4) yes
W1 . N21 . N22 . 117.8(2) yes
W1 . N21 . C21 . 134.7(3) yes
N22 . N21 . C21 . 106.1(3) yes
N21 . N22 . C23 . 110.2(3) yes
N21 . N22 . B1 . 120.6(3) yes
C23 . N22 . B1 . 129.1(3) yes
W1 . N31 . N32 . 119.6(2) yes
W1 . N31 . C31 . 133.4(3) yes
N32 . N31 . C31 . 106.7(3) yes
N31 . N32 . C33 . 109.4(3) yes
N31 . N32 . B1 . 120.9(3) yes
C33 . N32 . B1 . 129.6(4) yes
P1 . C1 . W1 . 165.5(2) yes
W1 . C2 . O2 . 175.4(4) yes
W1 . C3 . O3 . 175.6(4) yes
N11 . C11 . C12 . 109.2(4) yes
N11 . C11 . C14 . 122.4(4) yes
C12 . C11 . C14 . 128.3(4) yes
C11 . C12 . C13 . 107.2(4) yes
C11 . C12 . H121 . 126.2 no
C13 . C12 . H121 . 126.6 no
C12 . C13 . N12 . 107.4(4) yes
C12 . C13 . C15 . 129.8(5) yes
N12 . C13 . C15 . 122.8(5) yes
C11 . C14 . H142 . 109.2 no
C11 . C14 . H143 . 109.6 no
H142 . C14 . H143 . 110.3 no
C11 . C14 . H141 . 109.1 no
H142 . C14 . H141 . 109.3 no
H143 . C14 . H141 . 109.2 no
C13 . C15 . H153 . 109.2 no
C13 . C15 . H151 . 108.5 no
H153 . C15 . H151 . 110.4 no
C13 . C15 . H152 . 108.3 no
H153 . C15 . H152 . 110.2 no
H151 . C15 . H152 . 110.2 no
N21 . C21 . C22 . 109.9(4) yes
N21 . C21 . C24 . 122.1(4) yes
C22 . C21 . C24 . 127.9(4) yes
C21 . C22 . C23 . 106.4(3) yes
C21 . C22 . H221 . 125.9 no
C23 . C22 . H221 . 127.7 no
C22 . C23 . N22 . 107.3(4) yes
C22 . C23 . C25 . 129.6(4) yes
N22 . C23 . C25 . 123.0(4) yes
C21 . C24 . H243 . 109.8 no
C21 . C24 . H241 . 108.4 no
H243 . C24 . H241 . 110.3 no
C21 . C24 . H242 . 108.9 no
H243 . C24 . H242 . 109.9 no
H241 . C24 . H242 . 109.4 no
C23 . C25 . H251 . 108.9 no
C23 . C25 . H253 . 109.9 no
H251 . C25 . H253 . 109.6 no
C23 . C25 . H252 . 110.6 no
H251 . C25 . H252 . 109.1 no
H253 . C25 . H252 . 108.7 no
N31 . C31 . C32 . 108.7(4) yes
N31 . C31 . C34 . 122.2(3) yes
C32 . C31 . C34 . 129.1(4) yes
C31 . C32 . C33 . 107.5(4) yes
C31 . C32 . H321 . 127.4 no
C33 . C32 . H321 . 125.1 no
C32 . C33 . N32 . 107.6(4) yes
C32 . C33 . C35 . 129.2(4) yes
N32 . C33 . C35 . 123.1(4) yes
C31 . C34 . H341 . 111.0 no
C31 . C34 . H343 . 110.7 no
H341 . C34 . H343 . 108.1 no
C31 . C34 . H342 . 110.4 no
H341 . C34 . H342 . 108.3 no
H343 . C34 . H342 . 108.2 no
C33 . C35 . H352 . 110.2 no
C33 . C35 . H351 . 110.0 no
H352 . C35 . H351 . 109.2 no
C33 . C35 . H353 . 109.9 no
H352 . C35 . H353 . 108.6 no
H351 . C35 . H353 . 108.9 no
P1 . C41 . C42 . 121.5(3) yes
P1 . C41 . C46 . 118.8(3) yes
C42 . C41 . C46 . 119.7(4) yes
C41 . C42 . C43 . 119.5(4) yes
C41 . C42 . H421 . 119.7 no
C43 . C42 . H421 . 120.8 no
C42 . C43 . C44 . 120.5(4) yes
C42 . C43 . H431 . 118.6 no
C44 . C43 . H431 . 120.9 no
C43 . C44 . C45 . 120.2(4) yes
C43 . C44 . H441 . 119.4 no
C45 . C44 . H441 . 120.4 no
C44 . C45 . C46 . 120.1(4) yes
C44 . C45 . H451 . 120.1 no
C46 . C45 . H451 . 119.7 no
C45 . C46 . C41 . 119.9(4) yes
C45 . C46 . H461 . 119.1 no
C41 . C46 . H461 . 120.9 no
P1 . C51 . C52 . 118.6(3) yes
P1 . C51 . C56 . 121.4(3) yes
C52 . C51 . C56 . 120.0(4) yes
C51 . C52 . C53 . 119.8(5) yes
C51 . C52 . H521 . 120.1 no
C53 . C52 . H521 . 120.1 no
C52 . C53 . C54 . 120.4(5) yes
C52 . C53 . H531 . 119.3 no
C54 . C53 . H531 . 120.3 no
C53 . C54 . C55 . 120.1(5) yes
C53 . C54 . H541 . 119.9 no
C55 . C54 . H541 . 120.0 no
C54 . C55 . C56 . 119.6(5) yes
C54 . C55 . H551 . 120.0 no
C56 . C55 . H551 . 120.3 no
C55 . C56 . C51 . 120.0(4) yes
C55 . C56 . H561 . 120.0 no
C51 . C56 . H561 . 120.0 no
N22 . B1 . N32 . 109.2(3) yes
N22 . B1 . N12 . 108.2(3) yes
N32 . B1 . N12 . 109.1(3) yes
N22 . B1 . H11 . 109.4 no
N32 . B1 . H11 . 109.1 no
N12 . B1 . H11 . 111.8 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 22/02/12 at 16:56:59
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 143,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 153,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 243,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 253,X'S) H   ( 252,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 343,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) H   ( 353,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE B   (   1,X'S) H   (  11,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 22/02/12 at 16:56:59
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 0 4 x .
0 2 0 x .

# SQUEEZE RESULTS (APPEND TO CIF)

# Note: Data are Listed for all Voids in the P1 Unit Cell

# i.e. Centre of Gravity, Solvent Accessible Volume,

# Recovered number of Electrons in the Void and

# Details about the Squeezed Material

loop_

_platon_squeeze_void_nr

_platon_squeeze_void_average_x

_platon_squeeze_void_average_y

_platon_squeeze_void_average_z

_platon_squeeze_void_volume

_platon_squeeze_void_count_electrons

_platon_squeeze_void_content


1 0.000 0.500 0.000 126 30 ' '
2 0.500 0.000 0.500 126 30 ' '

_platon_squeeze_details          
;

;










####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 995725'
_audit_update_record             
;
2014-04-07 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   16.5513(2)
_cell_length_b                   12.9890(2)
_cell_length_c                   17.7921(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.5027(7)
_cell_angle_gamma                90
_cell_volume                     3507.71(8)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956
12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C30 H32 Au2 B1 Cl2 N6 O2 P1 W1 
# Dc =      2.27 Fooo =   2224.00 Mu =    118.50 M =   1199.10
# Found Formula = C30 H32 Au2 B1 Cl2 N6 O2 P1 W1 
# Dc =      2.27 FOOO =   2224.00 Mu =    118.50 M =   1199.10

_chemical_formula_sum            'C30 H32 Au2 B1 Cl2 N6 O2 P1 W1'
_chemical_formula_moiety         'C30 H32 Au2 B1 Cl2 N6 O2 P1 W1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         1199.10


_cell_measurement_reflns_used    54304
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      30.03
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.260
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_max          0.360

_exptl_crystal_density_diffrn    2.270
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2224
_exptl_absorpt_coefficient_mu    11.850

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.150
-1 0 0 0.140
0 1 0 0.140
0 -1 0 0.220
0 0 1 0.140
0 0 -1 0.150
1 0 -1 0.145
-4 0 4 0.205
1 0 1 0.120
-1 0 -1 0.139
1 -1 -1 0.152
-1 1 1 0.175
1 1 -1 0.096
-3 -2 3 0.241
-3 -2 -1 0.167


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_T_max  0.136
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            91567
_reflns_number_total             10263
_diffrn_reflns_av_R_equivalents  0.093
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 10263 
# Theoretical number of reflections is about 20547 


_diffrn_reflns_theta_min         2.675
_diffrn_reflns_theta_max         30.045
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        30.045
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -23
_reflns_limit_h_max              21
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   1.96
_oxford_diffrn_Wilson_scale      153.92

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.61
_refine_diff_density_max         1.80


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         10262
_refine_ls_number_restraints     0
_refine_ls_number_parameters     406
_oxford_refine_ls_R_factor_ref   0.0525
_refine_ls_wR_factor_ref         0.0804
_refine_ls_goodness_of_fit_ref   1.0116
_refine_ls_shift/su_max          0.0020233
_refine_ls_shift/su_mean         0.0000295


# The values computed from all data 
_oxford_reflns_number_all        10262
_refine_ls_R_factor_all          0.0525
_refine_ls_wR_factor_all         0.0804

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8079
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_gt          0.0734

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 2.09P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.562501(12) 0.101772(14) 0.322129(11) 0.0230 1.0000 Uani . . . . . .
Au1 Au 0.712669(12) -0.140807(16) 0.476152(11) 0.0296 1.0000 Uani . . . . . .
Au2 Au 0.430562(12) -0.028305(15) 0.217511(11) 0.0303 1.0000 Uani . . . . . .
P1 P 0.58617(8) -0.16377(9) 0.36797(7) 0.0231 1.0000 Uani . . . . . .
Cl1 Cl 0.84281(10) -0.10626(15) 0.58174(10) 0.0576 1.0000 Uani . . . . . .
Cl2 Cl 0.30385(11) -0.05097(15) 0.10396(10) 0.0623 1.0000 Uani . . . . . .
O2 O 0.5826(3) 0.0709(3) 0.5041(2) 0.0443 1.0000 Uani . . . . . .
O3 O 0.7477(2) 0.0131(3) 0.3438(3) 0.0424 1.0000 Uani . . . . . .
N11 N 0.5532(3) 0.1679(3) 0.2046(2) 0.0298 1.0000 Uani . . . . . .
N12 N 0.5399(3) 0.2720(3) 0.1919(2) 0.0297 1.0000 Uani . . . . . .
N21 N 0.4511(3) 0.2044(3) 0.3031(2) 0.0295 1.0000 Uani . . . . . .
N22 N 0.4542(3) 0.3040(3) 0.2787(3) 0.0325 1.0000 Uani . . . . . .
N31 N 0.6434(3) 0.2386(3) 0.3774(2) 0.0280 1.0000 Uani . . . . . .
N32 N 0.6176(3) 0.3322(3) 0.3377(3) 0.0295 1.0000 Uani . . . . . .
C1 C 0.5412(3) -0.0418(3) 0.3220(3) 0.0231 1.0000 Uani . . . . . .
C2 C 0.5777(3) 0.0809(4) 0.4388(3) 0.0288 1.0000 Uani . . . . . .
C3 C 0.6810(3) 0.0444(4) 0.3383(3) 0.0298 1.0000 Uani . . . . . .
C11 C 0.5666(4) 0.1294(4) 0.1399(3) 0.0345 1.0000 Uani . . . . . .
C12 C 0.5614(4) 0.2095(4) 0.0865(3) 0.0391 1.0000 Uani . . . . . .
C13 C 0.5449(4) 0.2977(4) 0.1203(3) 0.0333 1.0000 Uani . . . . . .
C14 C 0.5838(5) 0.0175(4) 0.1307(4) 0.0466 1.0000 Uani . . . . . .
C15 C 0.5351(5) 0.4056(5) 0.0892(4) 0.0481 1.0000 Uani . . . . . .
C21 C 0.3806(3) 0.1971(4) 0.3236(3) 0.0323 1.0000 Uani . . . . . .
C22 C 0.3398(3) 0.2921(5) 0.3120(3) 0.0382 1.0000 Uani . . . . . .
C23 C 0.3865(4) 0.3577(4) 0.2849(3) 0.0387 1.0000 Uani . . . . . .
C24 C 0.3561(4) 0.0999(5) 0.3529(4) 0.0474 1.0000 Uani . . . . . .
C25 C 0.3723(5) 0.4701(5) 0.2651(5) 0.0589 1.0000 Uani . . . . . .
C31 C 0.7191(3) 0.2577(4) 0.4442(3) 0.0311 1.0000 Uani . . . . . .
C32 C 0.7397(4) 0.3607(4) 0.4454(3) 0.0385 1.0000 Uani . . . . . .
C33 C 0.6756(4) 0.4056(4) 0.3788(3) 0.0363 1.0000 Uani . . . . . .
C34 C 0.7667(4) 0.1788(4) 0.5080(3) 0.0373 1.0000 Uani . . . . . .
C35 C 0.6661(5) 0.5162(4) 0.3512(4) 0.0525 1.0000 Uani . . . . . .
C41 C 0.5055(3) -0.2361(4) 0.3914(3) 0.0274 1.0000 Uani . . . . . .
C42 C 0.5369(4) -0.2968(4) 0.4615(3) 0.0381 1.0000 Uani . . . . . .
C43 C 0.4791(5) -0.3550(5) 0.4830(4) 0.0479 1.0000 Uani . . . . . .
C44 C 0.3905(4) -0.3537(5) 0.4354(4) 0.0447 1.0000 Uani . . . . . .
C45 C 0.3582(4) -0.2937(5) 0.3656(4) 0.0412 1.0000 Uani . . . . . .
C46 C 0.4151(3) -0.2342(4) 0.3433(3) 0.0331 1.0000 Uani . . . . . .
C51 C 0.6028(3) -0.2248(4) 0.2837(3) 0.0250 1.0000 Uani . . . . . .
C52 C 0.5336(3) -0.2614(4) 0.2151(3) 0.0305 1.0000 Uani . . . . . .
C53 C 0.5478(4) -0.2948(5) 0.1473(3) 0.0407 1.0000 Uani . . . . . .
C54 C 0.6327(4) -0.2924(5) 0.1490(4) 0.0438 1.0000 Uani . . . . . .
C55 C 0.7029(4) -0.2588(5) 0.2184(4) 0.0413 1.0000 Uani . . . . . .
C56 C 0.6890(3) -0.2253(4) 0.2860(3) 0.0312 1.0000 Uani . . . . . .
B1 B 0.5317(4) 0.3417(4) 0.2588(4) 0.0324 1.0000 Uani . . . . . .
H121 H 0.5669 0.2039 0.0374 0.0471 1.0000 Uiso R . . . . .
H141 H 0.5961 0.0069 0.0828 0.0690 1.0000 Uiso R . . . . .
H142 H 0.6331 -0.0051 0.1781 0.0692 1.0000 Uiso R . . . . .
H143 H 0.5329 -0.0223 0.1245 0.0692 1.0000 Uiso R . . . . .
H151 H 0.5448 0.4077 0.0402 0.0720 1.0000 Uiso R . . . . .
H152 H 0.5759 0.4508 0.1286 0.0719 1.0000 Uiso R . . . . .
H153 H 0.4777 0.4295 0.0781 0.0721 1.0000 Uiso R . . . . .
H221 H 0.2898 0.3084 0.3211 0.0464 1.0000 Uiso R . . . . .
H241 H 0.3005 0.1080 0.3561 0.0711 1.0000 Uiso R . . . . .
H242 H 0.4000 0.0814 0.4054 0.0710 1.0000 Uiso R . . . . .
H243 H 0.3508 0.0459 0.3155 0.0710 1.0000 Uiso R . . . . .
H251 H 0.3249 0.4935 0.2784 0.0888 1.0000 Uiso R . . . . .
H252 H 0.4243 0.5086 0.2958 0.0890 1.0000 Uiso R . . . . .
H253 H 0.3569 0.4800 0.2074 0.0888 1.0000 Uiso R . . . . .
H321 H 0.7882 0.3934 0.4843 0.0462 1.0000 Uiso R . . . . .
H341 H 0.8248 0.2026 0.5381 0.0561 1.0000 Uiso R . . . . .
H342 H 0.7692 0.1135 0.4834 0.0560 1.0000 Uiso R . . . . .
H343 H 0.7375 0.1695 0.5447 0.0559 1.0000 Uiso R . . . . .
H351 H 0.7080 0.5581 0.3912 0.0790 1.0000 Uiso R . . . . .
H352 H 0.6754 0.5219 0.3022 0.0790 1.0000 Uiso R . . . . .
H353 H 0.6089 0.5407 0.3418 0.0789 1.0000 Uiso R . . . . .
H421 H 0.5964 -0.2987 0.4942 0.0459 1.0000 Uiso R . . . . .
H431 H 0.5003 -0.3956 0.5293 0.0570 1.0000 Uiso R . . . . .
H441 H 0.3531 -0.3936 0.4508 0.0532 1.0000 Uiso R . . . . .
H451 H 0.2976 -0.2935 0.3327 0.0490 1.0000 Uiso R . . . . .
H461 H 0.3930 -0.1938 0.2965 0.0404 1.0000 Uiso R . . . . .
H521 H 0.4775 -0.2641 0.2149 0.0369 1.0000 Uiso R . . . . .
H531 H 0.5008 -0.3188 0.1009 0.0488 1.0000 Uiso R . . . . .
H541 H 0.6419 -0.3126 0.1030 0.0520 1.0000 Uiso R . . . . .
H551 H 0.7596 -0.2582 0.2196 0.0501 1.0000 Uiso R . . . . .
H561 H 0.7364 -0.2029 0.3339 0.0370 1.0000 Uiso R . . . . .
H11 H 0.5210 0.4139 0.2359 0.0254 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.22813(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . Au2 . 2.8011(3) yes
W1 . N11 . 2.208(4) yes
W1 . N21 . 2.189(4) yes
W1 . N31 . 2.207(4) yes
W1 . C1 . 1.897(4) yes
W1 . C2 . 2.007(5) yes
W1 . C3 . 2.009(5) yes
Au1 . P1 . 2.2278(12) yes
Au1 . Cl1 . 2.2677(14) yes
Au2 . Cl2 . 2.2775(15) yes
Au2 . C1 . 2.031(4) yes
P1 . C1 . 1.802(4) yes
P1 . C41 . 1.812(5) yes
P1 . C51 . 1.811(5) yes
O2 . C2 . 1.140(6) yes
O3 . C3 . 1.143(6) yes
N11 . N12 . 1.375(6) yes
N11 . C11 . 1.353(6) yes
N12 . C13 . 1.351(6) yes
N12 . B1 . 1.543(7) yes
N21 . N22 . 1.372(6) yes
N21 . C21 . 1.358(6) yes
N22 . C23 . 1.362(7) yes
N22 . B1 . 1.541(7) yes
N31 . N32 . 1.385(6) yes
N31 . C31 . 1.363(6) yes
N32 . C33 . 1.343(7) yes
N32 . B1 . 1.554(8) yes
C11 . C12 . 1.388(7) yes
C11 . C14 . 1.503(8) yes
C12 . C13 . 1.371(7) yes
C12 . H121 . 0.917 no
C13 . C15 . 1.492(7) yes
C14 . H141 . 0.961 no
C14 . H142 . 0.956 no
C14 . H143 . 0.957 no
C15 . H151 . 0.947 no
C15 . H152 . 0.956 no
C15 . H153 . 0.944 no
C21 . C22 . 1.382(7) yes
C21 . C24 . 1.483(8) yes
C22 . C23 . 1.361(8) yes
C22 . H221 . 0.930 no
C23 . C25 . 1.498(8) yes
C24 . H241 . 0.950 no
C24 . H242 . 0.957 no
C24 . H243 . 0.947 no
C25 . H251 . 0.955 no
C25 . H252 . 0.956 no
C25 . H253 . 0.962 no
C31 . C32 . 1.378(7) yes
C31 . C34 . 1.499(7) yes
C32 . C33 . 1.366(8) yes
C32 . H321 . 0.928 no
C33 . C35 . 1.506(8) yes
C34 . H341 . 0.946 no
C34 . H342 . 0.962 no
C34 . H343 . 0.962 no
C35 . H351 . 0.943 no
C35 . H352 . 0.947 no
C35 . H353 . 0.948 no
C41 . C42 . 1.390(7) yes
C41 . C46 . 1.396(7) yes
C42 . C43 . 1.387(8) yes
C42 . H421 . 0.923 no
C43 . C44 . 1.370(9) yes
C43 . H431 . 0.922 no
C44 . C45 . 1.381(8) yes
C44 . H441 . 0.928 no
C45 . C46 . 1.393(7) yes
C45 . H451 . 0.938 no
C46 . H461 . 0.926 no
C51 . C52 . 1.383(7) yes
C51 . C56 . 1.410(6) yes
C52 . C53 . 1.389(7) yes
C52 . H521 . 0.927 no
C53 . C54 . 1.392(8) yes
C53 . H531 . 0.933 no
C54 . C55 . 1.386(8) yes
C54 . H541 . 0.929 no
C55 . C56 . 1.382(7) yes
C55 . H551 . 0.931 no
C56 . H561 . 0.945 no
B1 . H11 . 1.009 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Au2 . W1 . N11 . 82.18(11) yes
Au2 . W1 . N21 . 83.06(11) yes
N11 . W1 . N21 . 83.12(15) yes
Au2 . W1 . N31 . 162.89(10) yes
N11 . W1 . N31 . 84.81(15) yes
N21 . W1 . N31 . 84.39(15) yes
Au2 . W1 . C1 . 46.47(13) yes
N11 . W1 . C1 . 115.98(17) yes
N21 . W1 . C1 . 116.99(17) yes
N31 . W1 . C1 . 150.64(16) yes
Au2 . W1 . C2 . 110.41(14) yes
N11 . W1 . C2 . 164.65(17) yes
N21 . W1 . C2 . 89.57(17) yes
N31 . W1 . C2 . 81.04(17) yes
C1 . W1 . C2 . 79.37(19) yes
Au2 . W1 . C3 . 109.23(14) yes
N11 . W1 . C3 . 88.56(17) yes
N21 . W1 . C3 . 164.13(17) yes
N31 . W1 . C3 . 81.41(18) yes
C1 . W1 . C3 . 78.81(19) yes
C2 . W1 . C3 . 95.2(2) yes
P1 . Au1 . Cl1 . 175.66(6) yes
W1 . Au2 . Cl2 . 149.94(5) yes
W1 . Au2 . C1 . 42.64(13) yes
Cl2 . Au2 . C1 . 167.42(14) yes
Au1 . P1 . C1 . 110.50(15) yes
Au1 . P1 . C41 . 113.31(16) yes
C1 . P1 . C41 . 110.6(2) yes
Au1 . P1 . C51 . 111.90(16) yes
C1 . P1 . C51 . 100.4(2) yes
C41 . P1 . C51 . 109.4(2) yes
W1 . N11 . N12 . 119.0(3) yes
W1 . N11 . C11 . 133.6(3) yes
N12 . N11 . C11 . 107.1(4) yes
N11 . N12 . C13 . 109.3(4) yes
N11 . N12 . B1 . 120.5(4) yes
C13 . N12 . B1 . 129.8(4) yes
W1 . N21 . N22 . 119.2(3) yes
W1 . N21 . C21 . 132.6(3) yes
N22 . N21 . C21 . 107.1(4) yes
N21 . N22 . C23 . 108.8(4) yes
N21 . N22 . B1 . 120.8(4) yes
C23 . N22 . B1 . 130.1(5) yes
W1 . N31 . N32 . 118.1(3) yes
W1 . N31 . C31 . 135.9(3) yes
N32 . N31 . C31 . 105.9(4) yes
N31 . N32 . C33 . 109.7(4) yes
N31 . N32 . B1 . 121.0(4) yes
C33 . N32 . B1 . 129.3(4) yes
P1 . C1 . Au2 . 123.3(2) yes
P1 . C1 . W1 . 145.1(3) yes
Au2 . C1 . W1 . 90.90(18) yes
W1 . C2 . O2 . 177.0(5) yes
W1 . C3 . O3 . 176.8(4) yes
N11 . C11 . C12 . 108.6(5) yes
N11 . C11 . C14 . 123.6(5) yes
C12 . C11 . C14 . 127.8(5) yes
C11 . C12 . C13 . 107.1(5) yes
C11 . C12 . H121 . 126.2 no
C13 . C12 . H121 . 126.7 no
C12 . C13 . N12 . 107.8(4) yes
C12 . C13 . C15 . 129.3(5) yes
N12 . C13 . C15 . 122.9(5) yes
C11 . C14 . H141 . 110.6 no
C11 . C14 . H142 . 109.4 no
H141 . C14 . H142 . 109.2 no
C11 . C14 . H143 . 109.7 no
H141 . C14 . H143 . 108.1 no
H142 . C14 . H143 . 109.8 no
C13 . C15 . H151 . 109.6 no
C13 . C15 . H152 . 111.4 no
H151 . C15 . H152 . 109.1 no
C13 . C15 . H153 . 109.7 no
H151 . C15 . H153 . 108.8 no
H152 . C15 . H153 . 108.1 no
N21 . C21 . C22 . 108.6(5) yes
N21 . C21 . C24 . 122.6(5) yes
C22 . C21 . C24 . 128.8(5) yes
C21 . C22 . C23 . 107.4(5) yes
C21 . C22 . H221 . 126.4 no
C23 . C22 . H221 . 126.2 no
N22 . C23 . C22 . 108.0(5) yes
N22 . C23 . C25 . 122.5(6) yes
C22 . C23 . C25 . 129.5(5) yes
C21 . C24 . H241 . 109.5 no
C21 . C24 . H242 . 110.5 no
H241 . C24 . H242 . 110.2 no
C21 . C24 . H243 . 110.2 no
H241 . C24 . H243 . 107.6 no
H242 . C24 . H243 . 108.8 no
C23 . C25 . H251 . 108.5 no
C23 . C25 . H252 . 110.7 no
H251 . C25 . H252 . 109.5 no
C23 . C25 . H253 . 109.4 no
H251 . C25 . H253 . 109.1 no
H252 . C25 . H253 . 109.6 no
N31 . C31 . C32 . 109.0(5) yes
N31 . C31 . C34 . 124.0(5) yes
C32 . C31 . C34 . 126.9(5) yes
C31 . C32 . C33 . 107.5(5) yes
C31 . C32 . H321 . 126.2 no
C33 . C32 . H321 . 126.3 no
C32 . C33 . N32 . 107.9(5) yes
C32 . C33 . C35 . 129.4(5) yes
N32 . C33 . C35 . 122.7(5) yes
C31 . C34 . H341 . 108.2 no
C31 . C34 . H342 . 111.2 no
H341 . C34 . H342 . 109.1 no
C31 . C34 . H343 . 110.2 no
H341 . C34 . H343 . 109.2 no
H342 . C34 . H343 . 108.8 no
C33 . C35 . H351 . 110.8 no
C33 . C35 . H352 . 109.9 no
H351 . C35 . H352 . 107.9 no
C33 . C35 . H353 . 110.2 no
H351 . C35 . H353 . 108.8 no
H352 . C35 . H353 . 109.2 no
P1 . C41 . C42 . 117.0(4) yes
P1 . C41 . C46 . 123.9(4) yes
C42 . C41 . C46 . 119.1(5) yes
C41 . C42 . C43 . 120.3(5) yes
C41 . C42 . H421 . 120.3 no
C43 . C42 . H421 . 119.4 no
C42 . C43 . C44 . 120.6(5) yes
C42 . C43 . H431 . 119.9 no
C44 . C43 . H431 . 119.5 no
C43 . C44 . C45 . 119.9(5) yes
C43 . C44 . H441 . 119.0 no
C45 . C44 . H441 . 121.1 no
C44 . C45 . C46 . 120.4(5) yes
C44 . C45 . H451 . 119.7 no
C46 . C45 . H451 . 119.9 no
C41 . C46 . C45 . 119.8(5) yes
C41 . C46 . H461 . 120.3 no
C45 . C46 . H461 . 120.0 no
P1 . C51 . C52 . 122.3(4) yes
P1 . C51 . C56 . 117.6(4) yes
C52 . C51 . C56 . 119.8(4) yes
C51 . C52 . C53 . 120.4(5) yes
C51 . C52 . H521 . 119.5 no
C53 . C52 . H521 . 120.1 no
C52 . C53 . C54 . 119.5(5) yes
C52 . C53 . H531 . 120.1 no
C54 . C53 . H531 . 120.4 no
C53 . C54 . C55 . 120.5(5) yes
C53 . C54 . H541 . 119.5 no
C55 . C54 . H541 . 120.0 no
C54 . C55 . C56 . 120.2(5) yes
C54 . C55 . H551 . 120.1 no
C56 . C55 . H551 . 119.7 no
C51 . C56 . C55 . 119.6(5) yes
C51 . C56 . H561 . 119.5 no
C55 . C56 . H561 . 120.9 no
N32 . B1 . N12 . 108.7(4) yes
N32 . B1 . N22 . 108.2(4) yes
N12 . B1 . N22 . 109.1(4) yes
N32 . B1 . H11 . 112.9 no
N12 . B1 . H11 . 106.8 no
N22 . B1 . H11 . 111.0 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C24 . H242 . O2 2_656 132.55(18) 0.957 2.493 3.219(8) yes
C34 . H342 . C3 . 131.00 0.962 2.568 3.280(8) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 28/02/12 at 13:03:19
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE B   (   1,X'S) H   (  11,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 28/02/12 at 13:03:19
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-2 0 2 x .







####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 995726'
_audit_update_record             
;
2014-04-07 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   16.6239(3)
_cell_length_b                   12.8664(3)
_cell_length_c                   17.4284(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.7247(10)
_cell_angle_gamma                90
_cell_volume                     3329.55(12)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956
12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C30 H32 Au1 B1 Cl1 N6 O2 P1 S1 W1 
# Dc =      1.99 Fooo =   1904.00 Mu =     80.82 M =    998.74
# Found Formula = C30 H32 Au1 B1 Cl1 N6 O2 P1 S1 W1 
# Dc =      1.99 FOOO =   1904.00 Mu =     80.82 M =    998.74

_chemical_formula_sum            'C30 H32 Au1 B1 Cl1 N6 O2 P1 S1 W1'
_chemical_formula_moiety         'C30 H32 Au1 B1 Cl1 N6 O2 P1 S1 W1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         998.74


_cell_measurement_reflns_used    40706
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_max          0.100

_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    8.082
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.030
-1 0 0 0.050
0 1 0 0.030
0 -1 0 0.060
0 0 1 0.030
0 0 -1 0.070
1 -2 0 0.040


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            77719
_reflns_number_total             7648
_diffrn_reflns_av_R_equivalents  0.105
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7648 
# Theoretical number of reflections is about 15274 


_diffrn_reflns_theta_min         2.617
_diffrn_reflns_theta_max         27.485
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.485
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              -21
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   2.70
_oxford_diffrn_Wilson_scale      337.63

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.53
_refine_diff_density_max         2.11


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7645
_refine_ls_number_restraints     0
_refine_ls_number_parameters     397
_oxford_refine_ls_R_factor_ref   0.0688
_refine_ls_wR_factor_ref         0.1180
_refine_ls_goodness_of_fit_ref   0.9435
_refine_ls_shift/su_max          0.0012418
_refine_ls_shift/su_mean         0.0000242


# The values computed from all data 
_oxford_reflns_number_all        7645
_refine_ls_R_factor_all          0.0688
_refine_ls_wR_factor_all         0.1180

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5693
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_gt          0.0954

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 10.7 15.3 7.87 2.19 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.73899(2) 0.39099(2) 0.66441(2) 0.0305 1.0000 Uani . . . . . .
Au1 Au 0.69695(2) 0.51994(3) 0.77030(2) 0.0386 1.0000 Uani . . . . . .
P1 P 0.72310(16) 0.66069(17) 0.62006(16) 0.0392 1.0000 Uani . . . . . .
S1 S 0.7483(3) 0.6512(3) 0.5188(2) 0.0738 1.0000 Uani . . . . . .
Cl1 Cl 0.6643(2) 0.5404(3) 0.88295(19) 0.0661 1.0000 Uani . . . . . .
O2 O 0.8972(6) 0.4763(6) 0.6312(6) 0.0645 1.0000 Uani . . . . . .
O3 O 0.5858(5) 0.4310(6) 0.4772(5) 0.0630 1.0000 Uani . . . . . .
N11 N 0.7705(5) 0.2541(5) 0.6071(4) 0.0338 1.0000 Uani . . . . . .
N12 N 0.7905(5) 0.1626(5) 0.6520(4) 0.0316 1.0000 Uani . . . . . .
N21 N 0.6556(4) 0.2792(5) 0.6923(4) 0.0320 1.0000 Uani . . . . . .
N22 N 0.6904(5) 0.1831(5) 0.7239(5) 0.0356 1.0000 Uani . . . . . .
N31 N 0.8462(5) 0.3330(6) 0.7877(4) 0.0354 1.0000 Uani . . . . . .
N32 N 0.8546(4) 0.2285(5) 0.8035(4) 0.0296 1.0000 Uani . . . . . .
C1 C 0.7191(6) 0.5369(8) 0.6648(6) 0.0401 1.0000 Uani . . . . . .
C2 C 0.8374(7) 0.4496(7) 0.6406(7) 0.0470 1.0000 Uani . . . . . .
C3 C 0.6417(6) 0.4165(7) 0.5441(6) 0.0414 1.0000 Uani . . . . . .
C11 C 0.7801(6) 0.2377(7) 0.5351(5) 0.0356 1.0000 Uani . . . . . .
C12 C 0.8050(7) 0.1339(8) 0.5338(6) 0.0436 1.0000 Uani . . . . . .
C13 C 0.8103(6) 0.0877(7) 0.6071(6) 0.0379 1.0000 Uani . . . . . .
C14 C 0.7607(8) 0.3139(9) 0.4647(6) 0.0535 1.0000 Uani . . . . . .
C15 C 0.8321(10) -0.0211(8) 0.6376(8) 0.0634 1.0000 Uani . . . . . .
C21 C 0.5707(6) 0.2792(7) 0.6825(6) 0.0422 1.0000 Uani . . . . . .
C22 C 0.5511(7) 0.1845(8) 0.7074(7) 0.0496 1.0000 Uani . . . . . .
C23 C 0.6263(7) 0.1237(7) 0.7328(6) 0.0416 1.0000 Uani . . . . . .
C24 C 0.5088(7) 0.3712(9) 0.6467(8) 0.0593 1.0000 Uani . . . . . .
C25 C 0.6431(9) 0.0150(8) 0.7633(8) 0.0602 1.0000 Uani . . . . . .
C31 C 0.9171(6) 0.3784(7) 0.8537(6) 0.0385 1.0000 Uani . . . . . .
C32 C 0.9690(6) 0.3018(8) 0.9103(6) 0.0436 1.0000 Uani . . . . . .
C33 C 0.9302(6) 0.2088(6) 0.8772(5) 0.0341 1.0000 Uani . . . . . .
C34 C 0.9317(7) 0.4933(8) 0.8606(7) 0.0528 1.0000 Uani . . . . . .
C35 C 0.9573(7) 0.1005(8) 0.9107(6) 0.0484 1.0000 Uani . . . . . .
C41 C 0.6217(6) 0.7354(7) 0.5967(6) 0.0407 1.0000 Uani . . . . . .
C42 C 0.5718(7) 0.7282(8) 0.6429(7) 0.0478 1.0000 Uani . . . . . .
C43 C 0.4964(7) 0.7886(8) 0.6221(7) 0.0533 1.0000 Uani . . . . . .
C44 C 0.4687(8) 0.8566(9) 0.5538(7) 0.0566 1.0000 Uani . . . . . .
C45 C 0.5161(9) 0.8633(9) 0.5070(7) 0.0643 1.0000 Uani . . . . . .
C46 C 0.5934(7) 0.8041(8) 0.5290(6) 0.0482 1.0000 Uani . . . . . .
C51 C 0.8146(6) 0.7228(6) 0.7116(6) 0.0391 1.0000 Uani . . . . . .
C52 C 0.8040(7) 0.7595(8) 0.7811(6) 0.0501 1.0000 Uani . . . . . .
C53 C 0.8775(7) 0.7966(9) 0.8536(7) 0.0543 1.0000 Uani . . . . . .
C54 C 0.9621(7) 0.7955(9) 0.8557(7) 0.0592 1.0000 Uani . . . . . .
C55 C 0.9726(8) 0.7596(9) 0.7865(8) 0.0578 1.0000 Uani . . . . . .
C56 C 0.8991(6) 0.7235(7) 0.7151(7) 0.0438 1.0000 Uani . . . . . .
B1 B 0.7853(7) 0.1522(8) 0.7373(6) 0.0354 1.0000 Uani . . . . . .
H121 H 0.8158 0.1026 0.4912 0.0521 1.0000 Uiso R . . . . .
H142 H 0.7874 0.2907 0.4292 0.0799 1.0000 Uiso R . . . . .
H143 H 0.7848 0.3808 0.4882 0.0800 1.0000 Uiso R . . . . .
H141 H 0.6966 0.3196 0.4302 0.0800 1.0000 Uiso R . . . . .
H153 H 0.8392 -0.0615 0.5948 0.0950 1.0000 Uiso R . . . . .
H151 H 0.8872 -0.0232 0.6903 0.0951 1.0000 Uiso R . . . . .
H152 H 0.7842 -0.0496 0.6472 0.0951 1.0000 Uiso R . . . . .
H221 H 0.4971 0.1652 0.7069 0.0590 1.0000 Uiso R . . . . .
H243 H 0.4482 0.3507 0.6323 0.0889 1.0000 Uiso R . . . . .
H241 H 0.5269 0.4260 0.6887 0.0891 1.0000 Uiso R . . . . .
H242 H 0.5115 0.3959 0.5961 0.0891 1.0000 Uiso R . . . . .
H251 H 0.5906 -0.0124 0.7657 0.0901 1.0000 Uiso R . . . . .
H253 H 0.6932 0.0119 0.8195 0.0901 1.0000 Uiso R . . . . .
H252 H 0.6562 -0.0266 0.7244 0.0901 1.0000 Uiso R . . . . .
H321 H 1.0209 0.3121 0.9615 0.0519 1.0000 Uiso R . . . . .
H341 H 0.9930 0.5081 0.9007 0.0790 1.0000 Uiso R . . . . .
H343 H 0.9191 0.5220 0.8054 0.0790 1.0000 Uiso R . . . . .
H342 H 0.8922 0.5242 0.8807 0.0791 1.0000 Uiso R . . . . .
H352 H 1.0186 0.1008 0.9549 0.0730 1.0000 Uiso R . . . . .
H351 H 0.9530 0.0556 0.8647 0.0730 1.0000 Uiso R . . . . .
H353 H 0.9183 0.0750 0.9339 0.0730 1.0000 Uiso R . . . . .
H421 H 0.5897 0.6823 0.6884 0.0570 1.0000 Uiso R . . . . .
H431 H 0.4641 0.7834 0.6538 0.0640 1.0000 Uiso R . . . . .
H441 H 0.4178 0.8975 0.5393 0.0680 1.0000 Uiso R . . . . .
H451 H 0.4968 0.9084 0.4603 0.0770 1.0000 Uiso R . . . . .
H461 H 0.6264 0.8108 0.4982 0.0580 1.0000 Uiso R . . . . .
H521 H 0.7473 0.7590 0.7792 0.0599 1.0000 Uiso R . . . . .
H531 H 0.8701 0.8221 0.9000 0.0650 1.0000 Uiso R . . . . .
H541 H 1.0120 0.8194 0.9042 0.0710 1.0000 Uiso R . . . . .
H551 H 1.0292 0.7598 0.7879 0.0690 1.0000 Uiso R . . . . .
H561 H 0.9062 0.6988 0.6684 0.0520 1.0000 Uiso R . . . . .
H11 H 0.8040 0.0712 0.7611 0.0393 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.075103(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . Au1 . 2.7940(5) yes
W1 . N11 . 2.201(7) yes
W1 . N21 . 2.198(7) yes
W1 . N31 . 2.215(7) yes
W1 . C1 . 1.907(10) yes
W1 . C2 . 2.007(11) yes
W1 . C3 . 2.018(9) yes
Au1 . Cl1 . 2.275(3) yes
Au1 . C1 . 2.043(10) yes
P1 . S1 . 1.992(5) yes
P1 . C1 . 1.788(10) yes
P1 . C41 . 1.821(10) yes
P1 . C51 . 1.820(9) yes
O2 . C2 . 1.131(12) yes
O3 . C3 . 1.133(11) yes
N11 . N12 . 1.370(9) yes
N11 . C11 . 1.349(11) yes
N12 . C13 . 1.371(10) yes
N12 . B1 . 1.534(11) yes
N21 . N22 . 1.371(10) yes
N21 . C21 . 1.343(11) yes
N22 . C23 . 1.375(11) yes
N22 . B1 . 1.539(12) yes
N31 . N32 . 1.367(9) yes
N31 . C31 . 1.354(11) yes
N32 . C33 . 1.356(10) yes
N32 . B1 . 1.557(11) yes
C11 . C12 . 1.401(13) yes
C11 . C14 . 1.489(13) yes
C12 . C13 . 1.377(13) yes
C12 . H121 . 0.930 no
C13 . C15 . 1.483(13) yes
C14 . H142 . 0.957 no
C14 . H143 . 0.960 no
C14 . H141 . 0.962 no
C15 . H153 . 0.958 no
C15 . H151 . 0.962 no
C15 . H152 . 0.957 no
C21 . C22 . 1.380(14) yes
C21 . C24 . 1.508(14) yes
C22 . C23 . 1.368(15) yes
C22 . H221 . 0.929 no
C23 . C25 . 1.477(14) yes
C24 . H243 . 0.959 no
C24 . H241 . 0.962 no
C24 . H242 . 0.957 no
C25 . H251 . 0.959 no
C25 . H253 . 0.960 no
C25 . H252 . 0.962 no
C31 . C32 . 1.387(12) yes
C31 . C34 . 1.494(13) yes
C32 . C33 . 1.359(13) yes
C32 . H321 . 0.931 no
C33 . C35 . 1.500(11) yes
C34 . H341 . 0.961 no
C34 . H343 . 0.962 no
C34 . H342 . 0.959 no
C35 . H352 . 0.962 no
C35 . H351 . 0.964 no
C35 . H353 . 0.963 no
C41 . C42 . 1.395(14) yes
C41 . C46 . 1.377(12) yes
C42 . C43 . 1.376(14) yes
C42 . H421 . 0.924 no
C43 . C44 . 1.379(15) yes
C43 . H431 . 0.931 no
C44 . C45 . 1.367(17) yes
C44 . H441 . 0.931 no
C45 . C46 . 1.391(15) yes
C45 . H451 . 0.931 no
C46 . H461 . 0.928 no
C51 . C52 . 1.384(14) yes
C51 . C56 . 1.378(13) yes
C52 . C53 . 1.389(14) yes
C52 . H521 . 0.927 no
C53 . C54 . 1.390(16) yes
C53 . H531 . 0.930 no
C54 . C55 . 1.375(17) yes
C54 . H541 . 0.930 no
C55 . C56 . 1.375(14) yes
C55 . H551 . 0.929 no
C56 . H561 . 0.931 no
B1 . H11 . 1.113 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Au1 . W1 . N11 . 162.99(18) yes
Au1 . W1 . N21 . 82.70(18) yes
N11 . W1 . N21 . 83.1(3) yes
Au1 . W1 . N31 . 83.70(19) yes
N11 . W1 . N31 . 85.4(3) yes
N21 . W1 . N31 . 82.9(3) yes
Au1 . W1 . C1 . 47.0(3) yes
N11 . W1 . C1 . 150.0(3) yes
N21 . W1 . C1 . 121.1(3) yes
N31 . W1 . C1 . 113.2(3) yes
Au1 . W1 . C2 . 112.5(3) yes
N11 . W1 . C2 . 79.9(3) yes
N21 . W1 . C2 . 160.9(3) yes
N31 . W1 . C2 . 87.3(3) yes
C1 . W1 . C2 . 77.9(4) yes
Au1 . W1 . C3 . 105.6(3) yes
N11 . W1 . C3 . 84.3(3) yes
N21 . W1 . C3 . 92.6(3) yes
N31 . W1 . C3 . 169.2(3) yes
C1 . W1 . C3 . 77.5(4) yes
C2 . W1 . C3 . 94.0(4) yes
W1 . Au1 . Cl1 . 150.04(8) yes
W1 . Au1 . C1 . 43.0(3) yes
Cl1 . Au1 . C1 . 166.8(3) yes
S1 . P1 . C1 . 113.3(3) yes
S1 . P1 . C41 . 112.1(3) yes
C1 . P1 . C41 . 110.8(4) yes
S1 . P1 . C51 . 112.2(4) yes
C1 . P1 . C51 . 100.9(4) yes
C41 . P1 . C51 . 106.8(4) yes
W1 . N11 . N12 . 118.3(5) yes
W1 . N11 . C11 . 134.3(6) yes
N12 . N11 . C11 . 107.2(7) yes
N11 . N12 . C13 . 109.7(7) yes
N11 . N12 . B1 . 121.6(7) yes
C13 . N12 . B1 . 128.7(7) yes
W1 . N21 . N22 . 119.0(5) yes
W1 . N21 . C21 . 134.6(6) yes
N22 . N21 . C21 . 106.3(7) yes
N21 . N22 . C23 . 109.8(7) yes
N21 . N22 . B1 . 120.8(7) yes
C23 . N22 . B1 . 129.2(8) yes
W1 . N31 . N32 . 119.4(5) yes
W1 . N31 . C31 . 133.8(6) yes
N32 . N31 . C31 . 106.4(7) yes
N31 . N32 . C33 . 110.0(7) yes
N31 . N32 . B1 . 119.8(7) yes
C33 . N32 . B1 . 130.2(7) yes
P1 . C1 . Au1 . 123.0(5) yes
P1 . C1 . W1 . 146.6(6) yes
Au1 . C1 . W1 . 90.0(4) yes
W1 . C2 . O2 . 174.4(9) yes
W1 . C3 . O3 . 178.5(10) yes
N11 . C11 . C12 . 109.0(8) yes
N11 . C11 . C14 . 126.2(8) yes
C12 . C11 . C14 . 124.7(8) yes
C11 . C12 . C13 . 107.0(8) yes
C11 . C12 . H121 . 126.3 no
C13 . C12 . H121 . 126.8 no
C12 . C13 . N12 . 107.1(8) yes
C12 . C13 . C15 . 130.1(9) yes
N12 . C13 . C15 . 122.8(8) yes
C11 . C14 . H142 . 109.7 no
C11 . C14 . H143 . 110.1 no
H142 . C14 . H143 . 109.2 no
C11 . C14 . H141 . 109.6 no
H142 . C14 . H141 . 109.0 no
H143 . C14 . H141 . 109.3 no
C13 . C15 . H153 . 109.2 no
C13 . C15 . H151 . 110.1 no
H153 . C15 . H151 . 109.4 no
C13 . C15 . H152 . 109.6 no
H153 . C15 . H152 . 109.3 no
H151 . C15 . H152 . 109.3 no
N21 . C21 . C22 . 110.0(8) yes
N21 . C21 . C24 . 122.4(9) yes
C22 . C21 . C24 . 127.6(9) yes
C21 . C22 . C23 . 107.2(8) yes
C21 . C22 . H221 . 126.7 no
C23 . C22 . H221 . 126.1 no
N22 . C23 . C22 . 106.7(8) yes
N22 . C23 . C25 . 122.4(9) yes
C22 . C23 . C25 . 131.0(9) yes
C21 . C24 . H243 . 109.5 no
C21 . C24 . H241 . 109.8 no
H243 . C24 . H241 . 109.4 no
C21 . C24 . H242 . 109.6 no
H243 . C24 . H242 . 109.2 no
H241 . C24 . H242 . 109.3 no
C23 . C25 . H251 . 109.6 no
C23 . C25 . H253 . 110.1 no
H251 . C25 . H253 . 109.1 no
C23 . C25 . H252 . 109.8 no
H251 . C25 . H252 . 109.0 no
H253 . C25 . H252 . 109.3 no
N31 . C31 . C32 . 108.8(8) yes
N31 . C31 . C34 . 122.9(8) yes
C32 . C31 . C34 . 128.3(8) yes
C31 . C32 . C33 . 107.4(8) yes
C31 . C32 . H321 . 126.3 no
C33 . C32 . H321 . 126.3 no
C32 . C33 . N32 . 107.4(7) yes
C32 . C33 . C35 . 130.6(8) yes
N32 . C33 . C35 . 122.0(8) yes
C31 . C34 . H341 . 109.6 no
C31 . C34 . H343 . 110.2 no
H341 . C34 . H343 . 109.5 no
C31 . C34 . H342 . 109.1 no
H341 . C34 . H342 . 109.2 no
H343 . C34 . H342 . 109.3 no
C33 . C35 . H352 . 109.5 no
C33 . C35 . H351 . 109.7 no
H352 . C35 . H351 . 108.9 no
C33 . C35 . H353 . 109.8 no
H352 . C35 . H353 . 109.5 no
H351 . C35 . H353 . 109.4 no
P1 . C41 . C42 . 124.6(7) yes
P1 . C41 . C46 . 117.1(8) yes
C42 . C41 . C46 . 118.3(9) yes
C41 . C42 . C43 . 121.1(9) yes
C41 . C42 . H421 . 119.4 no
C43 . C42 . H421 . 119.4 no
C42 . C43 . C44 . 119.8(11) yes
C42 . C43 . H431 . 120.1 no
C44 . C43 . H431 . 120.1 no
C43 . C44 . C45 . 119.8(10) yes
C43 . C44 . H441 . 120.2 no
C45 . C44 . H441 . 120.0 no
C44 . C45 . C46 . 120.6(10) yes
C44 . C45 . H451 . 119.8 no
C46 . C45 . H451 . 119.6 no
C45 . C46 . C41 . 120.3(10) yes
C45 . C46 . H461 . 120.2 no
C41 . C46 . H461 . 119.5 no
P1 . C51 . C52 . 122.1(8) yes
P1 . C51 . C56 . 118.4(7) yes
C52 . C51 . C56 . 119.2(9) yes
C51 . C52 . C53 . 120.5(11) yes
C51 . C52 . H521 . 119.5 no
C53 . C52 . H521 . 120.0 no
C52 . C53 . C54 . 119.2(11) yes
C52 . C53 . H531 . 120.3 no
C54 . C53 . H531 . 120.5 no
C53 . C54 . C55 . 120.4(10) yes
C53 . C54 . H541 . 120.0 no
C55 . C54 . H541 . 119.6 no
C54 . C55 . C56 . 119.7(11) yes
C54 . C55 . H551 . 120.2 no
C56 . C55 . H551 . 120.2 no
C51 . C56 . C55 . 121.1(10) yes
C51 . C56 . H561 . 119.2 no
C55 . C56 . H561 . 119.7 no
N32 . B1 . N22 . 108.5(7) yes
N32 . B1 . N12 . 108.5(7) yes
N22 . B1 . N12 . 109.3(7) yes
N32 . B1 . H11 . 109.0 no
N22 . B1 . H11 . 113.1 no
N12 . B1 . H11 . 108.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C14 . H143 . C2 . 129.6(3) 0.960 2.552 3.249(16) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 06/11/12 at 15:26:46
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 143,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 153,X'S) H   ( 152,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 243,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 253,X'S) H   ( 252,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE B   (   1,X'S) H   (  11,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 06/11/12 at 15:26:46
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 1 1 x .
2 0 0 x .
0 0 2 x .




####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1518122'
_audit_update_record             
;
2016-11-20 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   23.7948(4)
_cell_length_b                   10.6312(2)
_cell_length_c                   24.9238(5)
_cell_angle_alpha                90
_cell_angle_beta                 116.0601(9)
_cell_angle_gamma                90
_cell_volume                     5663.91(19)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956
12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C43 H51 Au3 B2 Cl5 N12 O4 P1 W2 
# Dc =      2.33 Fooo =   3680.00 Mu =    121.05 M =   1988.42
# Found Formula = C43 H51 Au3 B2 Cl5 N12 O4 P1 W2 
# Dc =      2.33 FOOO =   3680.00 Mu =    121.05 M =   1988.42

_chemical_formula_sum            'C43 H51 Au3 B2 Cl5 N12 O4 P1 W2'
_chemical_formula_moiety         'C42 H49 Au3 B2 Cl3 N12 O4 P1 W2, C H2 Cl2'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         1988.42


_cell_measurement_reflns_used    101682
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25.03
_cell_measurement_temperature    200

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.030
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_max          0.170

_exptl_crystal_density_diffrn    2.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3680
_exptl_absorpt_coefficient_mu    12.105

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.030
-1 0 0 0.000
0 1 0 0.070
0 -1 0 0.100
0 0 1 0.020
0 0 -1 0.020


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            68238
_reflns_number_total             9980
_diffrn_reflns_av_R_equivalents  0.136
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9980 
# Theoretical number of reflections is about 20009 


_diffrn_reflns_theta_min         2.570
_diffrn_reflns_theta_max         25.025
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        25.025
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_reflns_limit_h_min              -28
_reflns_limit_h_max              25
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              29

_oxford_diffrn_Wilson_B_factor   3.06
_oxford_diffrn_Wilson_scale      418.75

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -3.28
_refine_diff_density_max         4.16


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         9972
_refine_ls_number_restraints     14
_refine_ls_number_parameters     649
_oxford_refine_ls_R_factor_ref   0.0865
_refine_ls_wR_factor_ref         0.1602
_refine_ls_goodness_of_fit_ref   0.9445
_refine_ls_shift/su_max          0.0009430
_refine_ls_shift/su_mean         0.0000359


# The values computed from all data 
_oxford_reflns_number_all        9972
_refine_ls_R_factor_all          0.0865
_refine_ls_wR_factor_all         0.1602

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7173
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_gt          0.1340

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 21.0 31.3 16.1 4.32 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.67194(3) 0.55122(6) 0.76573(3) 0.0385 1.0000 Uani . . . . . .
W2 W 0.80438(3) 0.31597(6) 0.60466(3) 0.0371 1.0000 Uani . . . . . .
Au1 Au 0.71706(3) 0.30681(6) 0.76222(3) 0.0404 1.0000 Uani . . . . . .
Au2 Au 0.81976(3) 0.30976(6) 0.72140(3) 0.0396 1.0000 Uani . . . . . .
Au3 Au 0.66637(3) 0.64823(6) 0.59633(3) 0.0445 1.0000 Uani . . . . . .
P1 P 0.68475(19) 0.4548(4) 0.63557(18) 0.0394 1.0000 Uani . . . . . .
Cl1 Cl 0.7367(2) 0.1048(4) 0.7967(2) 0.0598 1.0000 Uani . . . . . .
Cl2 Cl 0.8909(2) 0.2370(5) 0.81260(19) 0.0564 1.0000 Uani . . . . . .
Cl3 Cl 0.6435(2) 0.8480(4) 0.5616(2) 0.0615 1.0000 Uani . . . . . .
Cl101 Cl 0.7690(4) -0.1221(8) 0.9079(4) 0.1175 1.0000 Uani . . . . . .
Cl102 Cl 0.8937(5) -0.0931(12) 1.0044(7) 0.1969 1.0000 Uani . . . . . .
N11 N 0.8242(6) 0.2808(14) 0.5280(6) 0.0464 1.0000 Uani . . . . . .
N12 N 0.8848(7) 0.2532(14) 0.5400(6) 0.0503 1.0000 Uani . . . . . .
N21 N 0.8954(7) 0.4096(13) 0.6443(6) 0.0485 1.0000 Uani . . . . . .
N22 N 0.9452(6) 0.3566(16) 0.6403(6) 0.0528 1.0000 Uani . . . . . .
N31 N 0.8593(6) 0.1423(13) 0.6380(5) 0.0420 1.0000 Uani . . . . . .
N32 N 0.9148(6) 0.1305(15) 0.6338(7) 0.0508 1.0000 Uani . . . . . .
N41 N 0.6358(7) 0.7185(13) 0.7937(6) 0.0458 1.0000 Uani . . . . . .
N42 N 0.6334(6) 0.7135(14) 0.8477(6) 0.0456 1.0000 Uani . . . . . .
N51 N 0.7417(6) 0.5480(13) 0.8588(6) 0.0418 1.0000 Uani . . . . . .
N52 N 0.7230(6) 0.5652(12) 0.9037(6) 0.0416 1.0000 Uani . . . . . .
N61 N 0.6146(7) 0.4422(13) 0.7984(6) 0.0448 1.0000 Uani . . . . . .
N62 N 0.6137(6) 0.4816(13) 0.8512(6) 0.0429 1.0000 Uani . . . . . .
O2 O 0.7545(6) 0.7513(14) 0.7397(6) 0.0654 1.0000 Uani . . . . . .
O3 O 0.5493(6) 0.5967(14) 0.6473(6) 0.0637 1.0000 Uani . . . . . .
O5 O 0.7468(8) 0.5621(16) 0.5294(7) 0.0809 1.0000 Uani . . . . . .
O6 O 0.6834(6) 0.1525(16) 0.5314(6) 0.0750 1.0000 Uani . . . . . .
C1 C 0.6898(7) 0.4635(15) 0.7099(7) 0.0417 1.0000 Uani . . . . . .
C2 C 0.7252(10) 0.6793(19) 0.7488(8) 0.0587 1.0000 Uani . . . . . .
C3 C 0.5948(8) 0.5783(16) 0.6907(8) 0.0478 1.0000 Uani . . . . . .
C4 C 0.7552(7) 0.3734(15) 0.6417(6) 0.0358 1.0000 Uani . . . . . .
C5 C 0.7683(10) 0.4723(19) 0.5574(9) 0.0576 1.0000 Uani . . . . . .
C6 C 0.7255(9) 0.2109(18) 0.5576(8) 0.0519 1.0000 Uani . . . . . .
C11 C 0.7218(8) 0.305(2) 0.4350(8) 0.0581 1.0000 Uani . . . . . .
C12 C 0.7919(9) 0.2876(16) 0.4673(7) 0.0483 1.0000 Uani . . . . . .
C13 C 0.8321(9) 0.265(2) 0.4435(8) 0.0612 1.0000 Uani . . . . . .
C14 C 0.8894(9) 0.2455(19) 0.4873(8) 0.0575 1.0000 Uani . . . . . .
C15 C 0.9507(9) 0.220(3) 0.4837(10) 0.0847 1.0000 Uani . . . . . .
C21 C 0.8721(14) 0.606(2) 0.6863(13) 0.0925 1.0000 Uani . . . . . .
C22 C 0.9130(10) 0.523(2) 0.6700(12) 0.0734 1.0000 Uani . . . . . .
C23 C 0.9762(11) 0.539(3) 0.6840(11) 0.0818 1.0000 Uani . . . . . .
C24 C 0.9966(10) 0.435(3) 0.6640(11) 0.0838 1.0000 Uani . . . . . .
C25 C 1.0583(11) 0.403(3) 0.6634(14) 0.1156 1.0000 Uani . . . . . .
C31 C 0.7938(9) 0.0108(19) 0.6708(9) 0.0604 1.0000 Uani . . . . . .
C32 C 0.8506(9) 0.0378(17) 0.6613(8) 0.0524 1.0000 Uani . . . . . .
C33 C 0.9006(11) -0.041(2) 0.6717(11) 0.0759 1.0000 Uani . . . . . .
C34 C 0.9394(10) 0.019(2) 0.6555(12) 0.0769 1.0000 Uani . . . . . .
C35 C 0.9985(12) -0.030(3) 0.6536(15) 0.1218 1.0000 Uani . . . . . .
C41 C 0.6162(9) 0.8849(18) 0.7153(8) 0.0531 1.0000 Uani . . . . . .
C42 C 0.6193(7) 0.8335(16) 0.7734(6) 0.0398 1.0000 Uani . . . . . .
C43 C 0.6039(9) 0.9014(18) 0.8117(10) 0.0648 1.0000 Uani . . . . . .
C44 C 0.6117(8) 0.8231(18) 0.8580(7) 0.0491 1.0000 Uani . . . . . .
C45 C 0.6030(10) 0.850(2) 0.9116(10) 0.0731 1.0000 Uani . . . . . .
C51 C 0.8450(9) 0.539(2) 0.8527(10) 0.0730 1.0000 Uani . . . . . .
C52 C 0.8051(8) 0.5502(16) 0.8859(8) 0.0484 1.0000 Uani . . . . . .
C53 C 0.8268(8) 0.5611(16) 0.9473(7) 0.0471 1.0000 Uani . . . . . .
C54 C 0.7750(8) 0.5755(16) 0.9585(8) 0.0522 1.0000 Uani . . . . . .
C55 C 0.7703(9) 0.599(2) 1.0148(7) 0.0596 1.0000 Uani . . . . . .
C61 C 0.5626(8) 0.2791(19) 0.7213(10) 0.0612 1.0000 Uani . . . . . .
C62 C 0.5744(7) 0.3440(16) 0.7773(8) 0.0485 1.0000 Uani . . . . . .
C63 C 0.5476(8) 0.3218(19) 0.8158(8) 0.0538 1.0000 Uani . . . . . .
C64 C 0.5723(7) 0.4071(19) 0.8620(8) 0.0514 1.0000 Uani . . . . . .
C65 C 0.5570(9) 0.428(2) 0.9131(8) 0.0606 1.0000 Uani . . . . . .
C71 C 0.6215(7) 0.3493(13) 0.5959(6) 0.0443 1.0000 Uani D U . . . .
C72 C 0.5700(8) 0.3861(18) 0.5438(8) 0.0564 1.0000 Uani . . . . . .
C73 C 0.5209(8) 0.2991(17) 0.5152(9) 0.0622 1.0000 Uani . . . . . .
C74 C 0.5250(9) 0.1757(19) 0.5354(8) 0.0575 1.0000 Uani . . . . . .
C75 C 0.5764(6) 0.1371(16) 0.5845(7) 0.0471 1.0000 Uani D U . . . .
C76 C 0.6205(6) 0.2292(12) 0.6121(6) 0.0388 1.0000 Uani D U . . . .
C100 C 0.8475(14) -0.102(4) 0.9233(16) 0.1259 1.0000 Uani . . . . . .
B2 B 0.9383(8) 0.235(2) 0.6049(8) 0.0457 1.0000 Uani . . . . . .
B1 B 0.6519(9) 0.5913(19) 0.8868(9) 0.0460 1.0000 Uani . . . . . .
H11 H 0.9816 0.2087 0.6039 0.0544 1.0000 Uiso R . . . . .
H21 H 0.6456 0.6048 0.9270 0.0552 1.0000 Uiso R . . . . .
H111 H 0.7112 0.3421 0.3966 0.0859 1.0000 Uiso R . . . . .
H112 H 0.7080 0.3592 0.4577 0.0859 1.0000 Uiso R . . . . .
H113 H 0.7016 0.2250 0.4301 0.0860 1.0000 Uiso R . . . . .
H131 H 0.8218 0.2639 0.4030 0.0739 1.0000 Uiso R . . . . .
H151 H 0.9443 0.2271 0.4431 0.1270 1.0000 Uiso R . . . . .
H152 H 0.9814 0.2805 0.5078 0.1270 1.0000 Uiso R . . . . .
H153 H 0.9651 0.1373 0.4982 0.1270 1.0000 Uiso R . . . . .
H211 H 0.8978 0.6554 0.7208 0.1400 1.0000 Uiso R . . . . .
H212 H 0.8433 0.5569 0.6951 0.1400 1.0000 Uiso R . . . . .
H213 H 0.8489 0.6619 0.6536 0.1400 1.0000 Uiso R . . . . .
H231 H 1.0005 0.6086 0.7035 0.1000 1.0000 Uiso R . . . . .
H251 H 1.0872 0.4794 0.6802 0.1759 1.0000 Uiso R . . . . .
H252 H 1.0761 0.3247 0.6900 0.1760 1.0000 Uiso R . . . . .
H253 H 1.0494 0.3851 0.6199 0.1760 1.0000 Uiso R . . . . .
H311 H 0.7753 -0.0669 0.6517 0.0900 1.0000 Uiso R . . . . .
H312 H 0.8056 0.0042 0.7127 0.0900 1.0000 Uiso R . . . . .
H313 H 0.7641 0.0777 0.6542 0.0900 1.0000 Uiso R . . . . .
H331 H 0.9060 -0.1226 0.6869 0.0911 1.0000 Uiso R . . . . .
H351 H 1.0030 -0.1182 0.6632 0.1850 1.0000 Uiso R . . . . .
H352 H 1.0339 0.0148 0.6822 0.1850 1.0000 Uiso R . . . . .
H353 H 0.9957 -0.0182 0.6145 0.1850 1.0000 Uiso R . . . . .
H411 H 0.5888 0.9561 0.7028 0.0781 1.0000 Uiso R . . . . .
H412 H 0.6572 0.9100 0.7212 0.0780 1.0000 Uiso R . . . . .
H413 H 0.6007 0.8212 0.6849 0.0780 1.0000 Uiso R . . . . .
H431 H 0.5907 0.9850 0.8073 0.0780 1.0000 Uiso R . . . . .
H451 H 0.5873 0.9341 0.9093 0.1090 1.0000 Uiso R . . . . .
H452 H 0.6426 0.8428 0.9463 0.1090 1.0000 Uiso R . . . . .
H453 H 0.5739 0.7913 0.9147 0.1090 1.0000 Uiso R . . . . .
H511 H 0.8852 0.5054 0.8788 0.1080 1.0000 Uiso R . . . . .
H512 H 0.8504 0.6208 0.8392 0.1080 1.0000 Uiso R . . . . .
H513 H 0.8251 0.4845 0.8190 0.1080 1.0000 Uiso R . . . . .
H531 H 0.8685 0.5594 0.9756 0.0570 1.0000 Uiso R . . . . .
H551 H 0.8046 0.5591 1.0472 0.0890 1.0000 Uiso R . . . . .
H552 H 0.7718 0.6876 1.0222 0.0890 1.0000 Uiso R . . . . .
H553 H 0.7316 0.5657 1.0120 0.0890 1.0000 Uiso R . . . . .
H611 H 0.5261 0.2273 0.7094 0.0921 1.0000 Uiso R . . . . .
H612 H 0.5979 0.2268 0.7273 0.0919 1.0000 Uiso R . . . . .
H613 H 0.5563 0.3393 0.6905 0.0920 1.0000 Uiso R . . . . .
H631 H 0.5181 0.2602 0.8112 0.0650 1.0000 Uiso R . . . . .
H651 H 0.5325 0.3594 0.9162 0.0900 1.0000 Uiso R . . . . .
H652 H 0.5949 0.4356 0.9494 0.0900 1.0000 Uiso R . . . . .
H653 H 0.5335 0.5048 0.9067 0.0900 1.0000 Uiso R . . . . .
H721 H 0.5680 0.4664 0.5283 0.0671 1.0000 Uiso R . . . . .
H731 H 0.4852 0.3250 0.4818 0.0749 1.0000 Uiso R . . . . .
H741 H 0.4922 0.1204 0.5153 0.0690 1.0000 Uiso R . . . . .
H751 H 0.5813 0.0546 0.5984 0.0651 1.0000 Uiso R . . . . .
H761 H 0.6544 0.2047 0.6465 0.0379 1.0000 Uiso R . . . . .
H1001 H 0.8611 -0.1734 0.9077 0.1500 1.0000 Uiso R . . . . .
H1002 H 0.8526 -0.0254 0.9047 0.1500 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.050516(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . Au1 . 2.8275(9) yes
W1 . N41 . 2.217(13) yes
W1 . N51 . 2.180(13) yes
W1 . N61 . 2.201(13) yes
W1 . C1 . 1.874(15) yes
W1 . C2 . 2.03(2) yes
W1 . C3 . 1.983(19) yes
W2 . Au2 . 2.7691(9) yes
W2 . N11 . 2.192(13) yes
W2 . N21 . 2.186(14) yes
W2 . N31 . 2.203(14) yes
W2 . C4 . 1.884(14) yes
W2 . C5 . 2.00(2) yes
W2 . C6 . 2.05(2) yes
Au1 . Au2 . 3.0318(8) yes
Au1 . P1 . 3.301(4) yes
Au1 . Cl1 . 2.283(4) yes
Au1 . C1 . 2.038(17) yes
Au2 . Cl2 . 2.291(4) yes
Au2 . C4 . 2.020(15) yes
Au3 . P1 . 2.237(4) yes
Au3 . Cl3 . 2.268(4) yes
P1 . C1 . 1.804(16) yes
P1 . C4 . 1.831(15) yes
P1 . C71 . 1.786(14) yes
Cl101 . C100 . 1.75(3) yes
Cl102 . C100 . 1.83(4) yes
N11 . N12 . 1.37(2) yes
N11 . C12 . 1.36(2) yes
N12 . C14 . 1.37(2) yes
N12 . B2 . 1.57(2) yes
N21 . N22 . 1.35(2) yes
N21 . C22 . 1.34(2) yes
N22 . C24 . 1.38(2) yes
N22 . B2 . 1.53(3) yes
N31 . N32 . 1.375(18) yes
N31 . C32 . 1.31(2) yes
N32 . C34 . 1.33(2) yes
N32 . B2 . 1.56(3) yes
N41 . N42 . 1.374(19) yes
N41 . C42 . 1.32(2) yes
N42 . C44 . 1.34(2) yes
N42 . B1 . 1.57(2) yes
N51 . N52 . 1.386(19) yes
N51 . C52 . 1.36(2) yes
N52 . C54 . 1.39(2) yes
N52 . B1 . 1.58(2) yes
N61 . N62 . 1.390(18) yes
N61 . C62 . 1.36(2) yes
N62 . C64 . 1.38(2) yes
N62 . B1 . 1.50(2) yes
O2 . C2 . 1.12(2) yes
O3 . C3 . 1.16(2) yes
O5 . C5 . 1.16(2) yes
O6 . C6 . 1.11(2) yes
C11 . C12 . 1.51(2) yes
C11 . H111 . 0.959 no
C11 . H112 . 0.960 no
C11 . H113 . 0.961 no
C12 . C13 . 1.35(3) yes
C13 . C14 . 1.34(3) yes
C13 . H131 . 0.929 no
C14 . C15 . 1.52(2) yes
C15 . H151 . 0.960 no
C15 . H152 . 0.959 no
C15 . H153 . 0.958 no
C21 . C22 . 1.50(3) yes
C21 . H211 . 0.962 no
C21 . H212 . 0.961 no
C21 . H213 . 0.960 no
C22 . C23 . 1.40(3) yes
C23 . C24 . 1.39(3) yes
C23 . H231 . 0.931 no
C24 . C25 . 1.51(3) yes
C25 . H251 . 1.030 no
C25 . H252 . 1.031 no
C25 . H253 . 1.028 no
C31 . C32 . 1.50(3) yes
C31 . H311 . 0.959 no
C31 . H312 . 0.959 no
C31 . H313 . 0.960 no
C32 . C33 . 1.39(3) yes
C33 . C34 . 1.32(3) yes
C33 . H331 . 0.929 no
C34 . C35 . 1.52(3) yes
C35 . H351 . 0.959 no
C35 . H352 . 0.960 no
C35 . H353 . 0.958 no
C41 . C42 . 1.52(2) yes
C41 . H411 . 0.958 no
C41 . H412 . 0.959 no
C41 . H413 . 0.960 no
C42 . C43 . 1.37(3) yes
C43 . C44 . 1.37(3) yes
C43 . H431 . 0.932 no
C44 . C45 . 1.47(3) yes
C45 . H451 . 0.962 no
C45 . H452 . 0.962 no
C45 . H453 . 0.959 no
C51 . C52 . 1.51(3) yes
C51 . H511 . 0.959 no
C51 . H512 . 0.962 no
C51 . H513 . 0.958 no
C52 . C53 . 1.39(2) yes
C53 . C54 . 1.39(3) yes
C53 . H531 . 0.930 no
C54 . C55 . 1.48(3) yes
C55 . H551 . 0.958 no
C55 . H552 . 0.958 no
C55 . H553 . 0.960 no
C61 . C62 . 1.47(3) yes
C61 . H611 . 0.960 no
C61 . H612 . 0.961 no
C61 . H613 . 0.959 no
C62 . C63 . 1.39(3) yes
C63 . C64 . 1.38(3) yes
C63 . H631 . 0.929 no
C64 . C65 . 1.49(2) yes
C65 . H651 . 0.960 no
C65 . H652 . 0.960 no
C65 . H653 . 0.959 no
C71 . C72 . 1.39(2) yes
C71 . C76 . 1.342(9) yes
C72 . C73 . 1.41(3) yes
C72 . H721 . 0.930 no
C73 . C74 . 1.39(3) yes
C73 . H731 . 0.932 no
C74 . C75 . 1.36(2) yes
C74 . H741 . 0.927 no
C75 . C76 . 1.378(9) yes
C75 . H751 . 0.931 no
C76 . H761 . 0.920 no
C100 . H1001 . 0.971 no
C100 . H1002 . 0.969 no
B2 . H11 . 1.080 no
B1 . H21 . 1.087 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Au1 . W1 . N41 . 162.2(4) yes
Au1 . W1 . N51 . 84.1(4) yes
N41 . W1 . N51 . 84.1(5) yes
Au1 . W1 . N61 . 80.4(4) yes
N41 . W1 . N61 . 85.2(5) yes
N51 . W1 . N61 . 84.5(5) yes
Au1 . W1 . C1 . 46.1(5) yes
N41 . W1 . C1 . 151.5(6) yes
N51 . W1 . C1 . 117.9(6) yes
N61 . W1 . C1 . 113.1(6) yes
Au1 . W1 . C2 . 109.3(6) yes
N41 . W1 . C2 . 83.7(7) yes
N51 . W1 . C2 . 88.8(6) yes
N61 . W1 . C2 . 167.6(7) yes
C1 . W1 . C2 . 79.2(8) yes
Au1 . W1 . C3 . 108.1(5) yes
N41 . W1 . C3 . 81.6(6) yes
N51 . W1 . C3 . 164.2(6) yes
N61 . W1 . C3 . 87.6(6) yes
C1 . W1 . C3 . 77.9(6) yes
C2 . W1 . C3 . 96.4(7) yes
Au2 . W2 . N11 . 158.8(3) yes
Au2 . W2 . N21 . 83.6(4) yes
N11 . W2 . N21 . 85.5(5) yes
Au2 . W2 . N31 . 78.5(3) yes
N11 . W2 . N31 . 82.3(5) yes
N21 . W2 . N31 . 84.6(5) yes
Au2 . W2 . C4 . 46.8(5) yes
N11 . W2 . C4 . 154.3(6) yes
N21 . W2 . C4 . 109.7(6) yes
N31 . W2 . C4 . 118.7(6) yes
Au2 . W2 . C5 . 117.6(5) yes
N11 . W2 . C5 . 80.2(6) yes
N21 . W2 . C5 . 88.4(7) yes
N31 . W2 . C5 . 161.6(6) yes
C4 . W2 . C5 . 79.7(7) yes
Au2 . W2 . C6 . 104.6(5) yes
N11 . W2 . C6 . 84.4(6) yes
N21 . W2 . C6 . 169.1(6) yes
N31 . W2 . C6 . 90.1(6) yes
C4 . W2 . C6 . 81.2(7) yes
C5 . W2 . C6 . 93.9(8) yes
W1 . Au1 . Au2 . 111.95(3) yes
W1 . Au1 . P1 . 70.10(7) yes
Au2 . Au1 . P1 . 63.75(7) yes
W1 . Au1 . Cl1 . 150.50(14) yes
Au2 . Au1 . Cl1 . 94.24(14) yes
P1 . Au1 . Cl1 . 136.97(15) yes
W1 . Au1 . C1 . 41.5(4) yes
Au2 . Au1 . C1 . 81.5(4) yes
P1 . Au1 . C1 . 28.7(4) yes
Cl1 . Au1 . C1 . 164.6(4) yes
Au1 . Au2 . W2 . 126.79(3) yes
Au1 . Au2 . Cl2 . 90.96(12) yes
W2 . Au2 . Cl2 . 138.53(13) yes
Au1 . Au2 . C4 . 87.5(4) yes
W2 . Au2 . C4 . 42.9(4) yes
Cl2 . Au2 . C4 . 178.4(4) yes
P1 . Au3 . Cl3 . 175.03(18) yes
Au3 . P1 . Au1 . 140.81(17) yes
Au3 . P1 . C1 . 108.3(6) yes
Au3 . P1 . C4 . 117.8(5) yes
Au1 . P1 . C4 . 82.8(5) yes
C1 . P1 . C4 . 107.0(7) yes
Au3 . P1 . C71 . 112.3(5) yes
Au1 . P1 . C71 . 90.9(5) yes
C1 . P1 . C71 . 105.1(7) yes
C4 . P1 . C71 . 105.5(7) yes
W2 . N11 . N12 . 117.1(10) yes
W2 . N11 . C12 . 136.4(11) yes
N12 . N11 . C12 . 106.2(13) yes
N11 . N12 . C14 . 109.0(14) yes
N11 . N12 . B2 . 123.4(13) yes
C14 . N12 . B2 . 127.7(15) yes
W2 . N21 . N22 . 120.1(10) yes
W2 . N21 . C22 . 131.6(13) yes
N22 . N21 . C22 . 108.1(15) yes
N21 . N22 . C24 . 110.9(17) yes
N21 . N22 . B2 . 121.2(13) yes
C24 . N22 . B2 . 127.3(16) yes
W2 . N31 . N32 . 118.6(11) yes
W2 . N31 . C32 . 133.9(12) yes
N32 . N31 . C32 . 107.5(14) yes
N31 . N32 . C34 . 108.4(16) yes
N31 . N32 . B2 . 121.5(14) yes
C34 . N32 . B2 . 130.0(16) yes
W1 . N41 . N42 . 117.8(10) yes
W1 . N41 . C42 . 135.8(11) yes
N42 . N41 . C42 . 106.2(13) yes
N41 . N42 . C44 . 109.8(14) yes
N41 . N42 . B1 . 121.3(13) yes
C44 . N42 . B1 . 128.9(14) yes
W1 . N51 . N52 . 119.5(10) yes
W1 . N51 . C52 . 133.7(11) yes
N52 . N51 . C52 . 106.1(13) yes
N51 . N52 . C54 . 110.0(14) yes
N51 . N52 . B1 . 119.6(13) yes
C54 . N52 . B1 . 129.5(15) yes
W1 . N61 . N62 . 117.5(10) yes
W1 . N61 . C62 . 135.1(12) yes
N62 . N61 . C62 . 107.3(13) yes
N61 . N62 . C64 . 108.7(13) yes
N61 . N62 . B1 . 122.3(13) yes
C64 . N62 . B1 . 128.9(15) yes
P1 . C1 . Au1 . 118.3(8) yes
P1 . C1 . W1 . 148.6(10) yes
Au1 . C1 . W1 . 92.5(7) yes
W1 . C2 . O2 . 179.3(19) yes
W1 . C3 . O3 . 178.4(14) yes
P1 . C4 . Au2 . 120.9(7) yes
P1 . C4 . W2 . 148.8(9) yes
Au2 . C4 . W2 . 90.3(6) yes
W2 . C5 . O5 . 179.1(19) yes
W2 . C6 . O6 . 178.3(16) yes
C12 . C11 . H111 . 109.2 no
C12 . C11 . H112 . 110.0 no
H111 . C11 . H112 . 109.6 no
C12 . C11 . H113 . 109.4 no
H111 . C11 . H113 . 109.7 no
H112 . C11 . H113 . 108.9 no
C11 . C12 . N11 . 123.4(16) yes
C11 . C12 . C13 . 128.0(16) yes
N11 . C12 . C13 . 108.4(16) yes
C12 . C13 . C14 . 109.5(17) yes
C12 . C13 . H131 . 125.6 no
C14 . C13 . H131 . 125.0 no
N12 . C14 . C13 . 107.0(17) yes
N12 . C14 . C15 . 123.4(18) yes
C13 . C14 . C15 . 129.7(19) yes
C14 . C15 . H151 . 109.8 no
C14 . C15 . H152 . 109.4 no
H151 . C15 . H152 . 109.4 no
C14 . C15 . H153 . 109.5 no
H151 . C15 . H153 . 109.4 no
H152 . C15 . H153 . 109.4 no
C22 . C21 . H211 . 109.3 no
C22 . C21 . H212 . 110.5 no
H211 . C21 . H212 . 109.2 no
C22 . C21 . H213 . 109.6 no
H211 . C21 . H213 . 109.0 no
H212 . C21 . H213 . 109.2 no
C21 . C22 . N21 . 124.0(18) yes
C21 . C22 . C23 . 127.8(20) yes
N21 . C22 . C23 . 107.9(20) yes
C22 . C23 . C24 . 108.5(19) yes
C22 . C23 . H231 . 125.7 no
C24 . C23 . H231 . 125.8 no
C23 . C24 . N22 . 104.6(19) yes
C23 . C24 . C25 . 133(2) yes
N22 . C24 . C25 . 123(2) yes
C24 . C25 . H251 . 107.3 no
C24 . C25 . H252 . 107.7 no
H251 . C25 . H252 . 111.3 no
C24 . C25 . H253 . 107.5 no
H251 . C25 . H253 . 111.3 no
H252 . C25 . H253 . 111.6 no
C32 . C31 . H311 . 109.7 no
C32 . C31 . H312 . 109.5 no
H311 . C31 . H312 . 109.2 no
C32 . C31 . H313 . 109.6 no
H311 . C31 . H313 . 109.5 no
H312 . C31 . H313 . 109.3 no
C31 . C32 . N31 . 124.2(16) yes
C31 . C32 . C33 . 127.9(18) yes
N31 . C32 . C33 . 107.9(18) yes
C32 . C33 . C34 . 107.7(18) yes
C32 . C33 . H331 . 126.3 no
C34 . C33 . H331 . 126.0 no
N32 . C34 . C33 . 108.4(18) yes
N32 . C34 . C35 . 123(2) yes
C33 . C34 . C35 . 128(2) yes
C34 . C35 . H351 . 109.4 no
C34 . C35 . H352 . 109.2 no
H351 . C35 . H352 . 109.6 no
C34 . C35 . H353 . 109.6 no
H351 . C35 . H353 . 109.5 no
H352 . C35 . H353 . 109.5 no
C42 . C41 . H411 . 109.5 no
C42 . C41 . H412 . 109.4 no
H411 . C41 . H412 . 109.3 no
C42 . C41 . H413 . 109.8 no
H411 . C41 . H413 . 109.4 no
H412 . C41 . H413 . 109.3 no
C41 . C42 . N41 . 125.5(15) yes
C41 . C42 . C43 . 124.0(16) yes
N41 . C42 . C43 . 110.4(15) yes
C42 . C43 . C44 . 106.8(16) yes
C42 . C43 . H431 . 126.9 no
C44 . C43 . H431 . 126.3 no
C43 . C44 . N42 . 106.7(15) yes
C43 . C44 . C45 . 129.0(18) yes
N42 . C44 . C45 . 124.2(18) yes
C44 . C45 . H451 . 109.3 no
C44 . C45 . H452 . 109.3 no
H451 . C45 . H452 . 109.3 no
C44 . C45 . H453 . 109.9 no
H451 . C45 . H453 . 109.6 no
H452 . C45 . H453 . 109.5 no
C52 . C51 . H511 . 109.7 no
C52 . C51 . H512 . 109.4 no
H511 . C51 . H512 . 109.2 no
C52 . C51 . H513 . 109.8 no
H511 . C51 . H513 . 109.4 no
H512 . C51 . H513 . 109.3 no
C51 . C52 . N51 . 123.6(16) yes
C51 . C52 . C53 . 126.1(16) yes
N51 . C52 . C53 . 110.2(15) yes
C52 . C53 . C54 . 107.2(15) yes
C52 . C53 . H531 . 126.3 no
C54 . C53 . H531 . 126.5 no
C53 . C54 . N52 . 106.3(15) yes
C53 . C54 . C55 . 130.8(16) yes
N52 . C54 . C55 . 122.9(16) yes
C54 . C55 . H551 . 109.5 no
C54 . C55 . H552 . 109.6 no
H551 . C55 . H552 . 109.2 no
C54 . C55 . H553 . 109.8 no
H551 . C55 . H553 . 109.6 no
H552 . C55 . H553 . 109.2 no
C62 . C61 . H611 . 109.3 no
C62 . C61 . H612 . 109.5 no
H611 . C61 . H612 . 109.1 no
C62 . C61 . H613 . 110.1 no
H611 . C61 . H613 . 109.5 no
H612 . C61 . H613 . 109.3 no
C61 . C62 . N61 . 122.5(16) yes
C61 . C62 . C63 . 128.6(16) yes
N61 . C62 . C63 . 108.8(16) yes
C62 . C63 . C64 . 108.1(16) yes
C62 . C63 . H631 . 125.9 no
C64 . C63 . H631 . 126.0 no
N62 . C64 . C63 . 107.1(15) yes
N62 . C64 . C65 . 123.0(17) yes
C63 . C64 . C65 . 129.9(17) yes
C64 . C65 . H651 . 109.6 no
C64 . C65 . H652 . 109.6 no
H651 . C65 . H652 . 109.8 no
C64 . C65 . H653 . 109.3 no
H651 . C65 . H653 . 109.3 no
H652 . C65 . H653 . 109.2 no
P1 . C71 . C72 . 121.4(12) yes
P1 . C71 . C76 . 123.6(11) yes
C72 . C71 . C76 . 115.0(15) yes
C71 . C72 . C73 . 118.7(17) yes
C71 . C72 . H721 . 120.6 no
C73 . C72 . H721 . 120.7 no
C72 . C73 . C74 . 121.6(17) yes
C72 . C73 . H731 . 119.0 no
C74 . C73 . H731 . 119.5 no
C73 . C74 . C75 . 120.1(17) yes
C73 . C74 . H741 . 119.6 no
C75 . C74 . H741 . 120.3 no
C74 . C75 . C76 . 114.9(17) yes
C74 . C75 . H751 . 122.3 no
C76 . C75 . H751 . 122.7 no
C75 . C76 . C71 . 129.5(15) yes
C75 . C76 . H761 . 115.3 no
C71 . C76 . H761 . 115.2 no
Cl102 . C100 . Cl101 . 108.3(19) yes
Cl102 . C100 . H1001 . 109.7 no
Cl101 . C100 . H1001 . 109.1 no
Cl102 . C100 . H1002 . 110.2 no
Cl101 . C100 . H1002 . 110.1 no
H1001 . C100 . H1002 . 109.4 no
N12 . B2 . N32 . 105.7(13) yes
N12 . B2 . N22 . 108.9(14) yes
N32 . B2 . N22 . 107.8(14) yes
N12 . B2 . H11 . 111.0 no
N32 . B2 . H11 . 111.4 no
N22 . B2 . H11 . 111.8 no
N52 . B1 . N42 . 106.7(13) yes
N52 . B1 . N62 . 108.7(14) yes
N42 . B1 . N62 . 110.2(14) yes
N52 . B1 . H21 . 110.1 no
N42 . B1 . H21 . 110.4 no
N62 . B1 . H21 . 110.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C11 . H112 . C5 . 132.0 0.960 2.558 3.27(3) yes
C31 . H313 . C6 . 134.0 0.960 2.588 3.33(3) yes
C41 . H413 . C3 . 132.0 0.960 2.594 3.31(3) yes
C65 . H652 . O6 4_555 152.0 0.960 2.388 3.27(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/02/14 at 16:11:54
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) H   ( 453,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) H   ( 513,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) H   ( 553,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) H   ( 612,X'S) H   ( 613,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) H   ( 653,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) H   (1002,X'S) 
RIDE B   (  1,X'S)  H   ( 11,X'S) 
RIDE B   (  2,X'S)  H   ( 21,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 17/02/14 at 16:11:54
#
#LIST     16                                                                    
NO 
DIST 1.37 , 0.01 = C(71) TO C(76) 
DIST 1.37 , 0.01 = C(75) TO C(76) 
REM 
U(IJ) 0.0 , 0.005 = C(71) TO C(76) 
U(IJ) 0.0 , 0.005 = C(75) TO C(76) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
2 7 2 x .
-6 0 6 x .
2 1 0 x .
-5 0 8 x .
2 0 2 x .
-9 3 8 x .
0 7 4 x .
-3 0 2 x .

# start Validation Reply Form
_vrf_PLAT342_1                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0303 Ang.  
RESPONSE: The crystals which were obtained of this compound 
were all of poor quality.
Data were collected on the best of the sampled crystals,
even though it was known to diffract only weakly.
The precision is therefore lower than we would like,
but the identity of the compound is clearly established
and there do not appear to be any major refinement anomalies.
;
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1518123'
_audit_update_record             
;
2016-11-20 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   12.5001(13)
_cell_length_b                   14.7647(14)
_cell_length_c                   17.4599(10)
_cell_angle_alpha                66.723(7)
_cell_angle_beta                 69.805(7)
_cell_angle_gamma                73.373(9)
_cell_volume                     2735.9(5)

_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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956
12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C46 H59 Au1 B2 Cl1 N12 O5 P1 W2 
# Dc =      1.84 Fooo =   1456.00 Mu =     70.01 M =   1512.77
# Found Formula = C46 H59 Au1 B2 Cl1 N12 O5 P1 W2 
# Dc =      1.84 FOOO =   1456.00 Mu =     70.01 M =   1512.77

_chemical_formula_sum            'C46 H59 Au1 B2 Cl1 N12 O5 P1 W2'
_chemical_formula_moiety         'C42 H49 Au1 B2 Cl1 N12 O4 P1 W2, C4 H10 O'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         1512.77


_cell_measurement_reflns_used    3130
_cell_measurement_theta_min      2
_cell_measurement_theta_max      26
_cell_measurement_temperature    150

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.072
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_max          0.185

_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1456
_exptl_absorpt_coefficient_mu    7.001

# Sheldrick geometric approximatio 0.56 0.60 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Agilent Technologies, 2013)'
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_T_max  0.60
_diffrn_measurement_device_type  'Agilent Technologies Xcalibur'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Agilent Technologies, 2013)'
_computing_cell_refinement       'CrysAlis, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis, (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            20633
_reflns_number_total             11228
_diffrn_reflns_av_R_equivalents  0.081
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 11228 
# Theoretical number of reflections is about 27850 


_diffrn_reflns_theta_min         1.763
_diffrn_reflns_theta_max         28.540
_diffrn_measured_fraction_theta_max 0.806

_diffrn_reflns_theta_full        25.115
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -14
_reflns_limit_h_max              16
_reflns_limit_k_min              -16
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      0.16

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -6.38
_refine_diff_density_max         11.22


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         9625
_refine_ls_number_restraints     44
_refine_ls_number_parameters     631
_oxford_refine_ls_R_factor_ref   0.1542
_refine_ls_wR_factor_ref         0.1747
_refine_ls_goodness_of_fit_ref   0.9965
_refine_ls_shift/su_max          0.0019174
_refine_ls_shift/su_mean         0.0000917


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9625
_refine_ls_R_factor_all          0.1542
_refine_ls_wR_factor_all         0.1747

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5382
_refine_ls_R_factor_gt           0.0806
_refine_ls_wR_factor_gt          0.1292

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.474E+04 0.404E+04 0.217E+04 0.110E+04 -321. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.79879(8) 0.46267(8) 0.32100(6) 0.0361 1.0000 Uani . . . . . .
W2 W 1.17783(9) 0.16605(8) 0.18374(7) 0.0398 1.0000 Uani . . . . . .
Au1 Au 1.19451(8) 0.49790(8) 0.18473(6) 0.0370 1.0000 Uani . . . . . .
P1 P 1.1032(5) 0.3684(5) 0.2697(4) 0.0345 1.0000 Uani . U . . . .
Cl1 Cl 1.2849(5) 0.6326(5) 0.1007(4) 0.0420 1.0000 Uani . . . . . .
N11 N 0.6095(15) 0.5358(14) 0.3577(12) 0.0340 1.0000 Uani . . . . . .
N12 N 0.5318(14) 0.5239(14) 0.3258(11) 0.0306 1.0000 Uani . . . . . .
N21 N 0.7109(15) 0.3357(13) 0.3651(11) 0.0274 1.0000 Uani . . . . . .
N22 N 0.6124(17) 0.3421(17) 0.3423(13) 0.0445 1.0000 Uani . . . . . .
N31 N 0.7556(15) 0.4974(16) 0.2001(12) 0.0370 1.0000 Uani . U . . . .
N32 N 0.6641(16) 0.4727(16) 0.1963(12) 0.0414 1.0000 Uani . U . . . .
N41 N 1.2338(16) 0.0205(15) 0.1554(13) 0.0391 1.0000 Uani . . . . . .
N42 N 1.2445(16) 0.0211(16) 0.0728(12) 0.0390 1.0000 Uani . . . . . .
N51 N 1.2960(17) 0.2199(15) 0.0540(12) 0.0375 1.0000 Uani . . . . . .
N52 N 1.2908(16) 0.1941(16) -0.0126(12) 0.0408 1.0000 Uani . . . . . .
N61 N 1.0551(15) 0.1942(14) 0.1102(11) 0.0339 1.0000 Uani . . . . . .
N62 N 1.0860(17) 0.1683(15) 0.0365(12) 0.0388 1.0000 Uani . . . . . .
O2 O 0.8875(17) 0.6608(14) 0.2728(12) 0.0574 1.0000 Uani . U . . . .
O3 O 0.8460(15) 0.4131(16) 0.4996(12) 0.0617 1.0000 Uani . . . . . .
O5 O 1.0215(16) 0.0510(14) 0.3603(12) 0.0580 1.0000 Uani . U . . . .
O6 O 1.3754(19) 0.0951(18) 0.2782(14) 0.0794 1.0000 Uani . . . . . .
O7 O 0.7577(18) 0.9416(17) 0.3004(13) 0.0829 1.0000 Uani . . . . . .
C1 C 0.9530(18) 0.4064(17) 0.2921(14) 0.0287 1.0000 Uani . U . . . .
C2 C 0.856(2) 0.5879(19) 0.2892(16) 0.0394 1.0000 Uani . U . . . .
C3 C 0.8232(17) 0.4304(19) 0.4370(13) 0.0333 1.0000 Uani . . . . . .
C4 C 1.1366(18) 0.2767(18) 0.2227(15) 0.0358 1.0000 Uani . . . . . .
C5 C 1.077(2) 0.0954(19) 0.2923(17) 0.0451 1.0000 Uani . U . . . .
C6 C 1.302(2) 0.1228(18) 0.2421(16) 0.0487 1.0000 Uani . . . . . .
C11 C 0.608(2) 0.632(2) 0.4475(15) 0.0482 1.0000 Uani . . . . . .
C12 C 0.5519(18) 0.6038(16) 0.4022(14) 0.0278 1.0000 Uani . . . . . .
C13 C 0.442(2) 0.6309(19) 0.3946(14) 0.0394 1.0000 Uani . . . . . .
C14 C 0.429(2) 0.5811(18) 0.3467(13) 0.0357 1.0000 Uani . . . . . .
C15 C 0.329(2) 0.580(2) 0.3198(17) 0.0486 1.0000 Uani . . . . . .
C21 C 0.828(2) 0.2002(18) 0.4573(17) 0.0471 1.0000 Uani . . . . . .
C22 C 0.7292(18) 0.242(2) 0.4155(15) 0.0407 1.0000 Uani . . . . . .
C23 C 0.649(2) 0.1885(19) 0.4247(16) 0.0460 1.0000 Uani . . . . . .
C24 C 0.577(2) 0.255(2) 0.3783(17) 0.0481 1.0000 Uani . . . . . .
C25 C 0.469(2) 0.244(2) 0.3652(17) 0.0539 1.0000 Uani . . . . . .
C31 C 0.937(2) 0.561(2) 0.0902(15) 0.0452 1.0000 Uani . . . . . .
C32 C 0.823(2) 0.5248(18) 0.1161(14) 0.0352 1.0000 Uani . . . . . .
C33 C 0.7719(18) 0.5123(19) 0.0638(14) 0.0372 1.0000 Uani . . . . . .
C34 C 0.6666(19) 0.4811(19) 0.1174(15) 0.0390 1.0000 Uani . U . . . .
C35 C 0.5826(18) 0.4481(19) 0.0960(15) 0.0352 1.0000 Uani . U . . . .
C41 C 1.261(3) -0.113(2) 0.2909(19) 0.0676 1.0000 Uani . . . . . .
C42 C 1.261(2) -0.0788(18) 0.1956(15) 0.0458 1.0000 Uani . U . . . .
C43 C 1.288(2) -0.1353(17) 0.1459(16) 0.0480 1.0000 Uani . U . . . .
C44 C 1.279(2) -0.071(2) 0.0671(17) 0.0480 1.0000 Uani . . . . . .
C45 C 1.303(2) -0.092(2) -0.0137(19) 0.0611 1.0000 Uani . . . . . .
C51 C 1.419(2) 0.305(2) 0.0781(19) 0.0573 1.0000 Uani . . . . . .
C52 C 1.385(2) 0.2678(18) 0.0210(18) 0.0470 1.0000 Uani . . . . . .
C53 C 1.436(2) 0.2783(19) -0.0637(16) 0.0434 1.0000 Uani . . . . . .
C54 C 1.377(2) 0.2298(19) -0.0829(16) 0.0394 1.0000 Uani . . . . . .
C55 C 1.396(2) 0.220(2) -0.1693(17) 0.0543 1.0000 Uani . . . . . .
C61 C 0.870(2) 0.255(2) 0.2067(16) 0.0457 1.0000 Uani . . . . . .
C62 C 0.939(2) 0.227(2) 0.1257(16) 0.0451 1.0000 Uani . . . . . .
C63 C 0.900(2) 0.230(2) 0.0603(16) 0.0479 1.0000 Uani . . . . . .
C64 C 0.993(2) 0.1885(16) 0.0056(15) 0.0364 1.0000 Uani . . . . . .
C65 C 0.998(2) 0.173(2) -0.0730(18) 0.0536 1.0000 Uani . . . . . .
C71 C 1.1314(17) 0.3134(16) 0.3786(14) 0.0308 1.0000 Uani . U . . . .
C72 C 1.123(2) 0.3825(19) 0.4161(16) 0.0411 1.0000 Uani . U . . . .
C73 C 1.136(2) 0.347(3) 0.5003(18) 0.0578 1.0000 Uani . U . . . .
C74 C 1.154(3) 0.242(3) 0.5435(18) 0.0645 1.0000 Uani . U . . . .
C75 C 1.159(3) 0.179(2) 0.5043(17) 0.0579 1.0000 Uani . U . . . .
C76 C 1.146(2) 0.213(2) 0.4218(15) 0.0429 1.0000 Uani . U . . . .
C81 C 0.954(3) 0.941(4) 0.233(2) 0.1034 1.0000 Uani . . . . . .
C82 C 0.836(4) 0.983(3) 0.227(2) 0.0955 1.0000 Uani . . . . . .
C83 C 0.641(3) 0.984(3) 0.299(2) 0.0880 1.0000 Uani . . . . . .
C84 C 0.566(4) 0.936(4) 0.389(3) 0.1346 1.0000 Uani . . . . . .
B1 B 0.562(2) 0.444(2) 0.2807(18) 0.0381 1.0000 Uani . . . . . .
B2 B 1.212(3) 0.120(2) 0.0029(19) 0.0435 1.0000 Uani . . . . . .
H111 H 0.5615 0.6912 0.4630 0.0710 1.0000 Uiso . . . . . .
H113 H 0.6831 0.6496 0.4117 0.0710 1.0000 Uiso . . . . . .
H112 H 0.6183 0.5794 0.4999 0.0710 1.0000 Uiso . . . . . .
H131 H 0.3827 0.6769 0.4188 0.0460 1.0000 Uiso . . . . . .
H153 H 0.2608 0.6252 0.3387 0.0710 1.0000 Uiso . . . . . .
H152 H 0.3472 0.6014 0.2566 0.0710 1.0000 Uiso . . . . . .
H151 H 0.3104 0.5136 0.3423 0.0710 1.0000 Uiso . . . . . .
H211 H 0.8313 0.1295 0.4882 0.0640 1.0000 Uiso . . . . . .
H213 H 0.8200 0.2340 0.4965 0.0640 1.0000 Uiso . . . . . .
H212 H 0.9007 0.2099 0.4130 0.0641 1.0000 Uiso . . . . . .
H231 H 0.6446 0.1193 0.4570 0.0561 1.0000 Uiso . . . . . .
H253 H 0.4584 0.1749 0.3864 0.0770 1.0000 Uiso . . . . . .
H252 H 0.3992 0.2810 0.3944 0.0770 1.0000 Uiso . . . . . .
H251 H 0.4700 0.2703 0.3038 0.0770 1.0000 Uiso . . . . . .
H311 H 0.9461 0.6124 0.0343 0.0629 1.0000 Uiso . . . . . .
H313 H 0.9406 0.5860 0.1316 0.0630 1.0000 Uiso . . . . . .
H312 H 1.0017 0.5057 0.0853 0.0630 1.0000 Uiso . . . . . .
H331 H 0.8006 0.5246 0.0038 0.0440 1.0000 Uiso . . . . . .
H353 H 0.6206 0.4277 0.0451 0.0690 1.0000 Uiso . . . . . .
H352 H 0.5195 0.5016 0.0845 0.0690 1.0000 Uiso . . . . . .
H351 H 0.5532 0.3913 0.1431 0.0689 1.0000 Uiso . . . . . .
H411 H 1.2953 -0.1825 0.3109 0.0980 1.0000 Uiso . . . . . .
H413 H 1.3051 -0.0739 0.2987 0.0980 1.0000 Uiso . . . . . .
H412 H 1.1830 -0.1036 0.3270 0.0980 1.0000 Uiso . . . . . .
H431 H 1.3081 -0.2055 0.1628 0.0660 1.0000 Uiso . . . . . .
H453 H 1.3173 -0.1640 -0.0033 0.0900 1.0000 Uiso . . . . . .
H452 H 1.3702 -0.0660 -0.0566 0.0900 1.0000 Uiso . . . . . .
H451 H 1.2378 -0.0627 -0.0392 0.0900 1.0000 Uiso . . . . . .
H511 H 1.4918 0.3291 0.0491 0.0820 1.0000 Uiso . . . . . .
H513 H 1.4273 0.2518 0.1316 0.0820 1.0000 Uiso . . . . . .
H512 H 1.3609 0.3594 0.0928 0.0820 1.0000 Uiso . . . . . .
H531 H 1.4980 0.3129 -0.1019 0.0520 1.0000 Uiso . . . . . .
H553 H 1.4548 0.2560 -0.2137 0.0790 1.0000 Uiso . . . . . .
H552 H 1.4199 0.1498 -0.1663 0.0790 1.0000 Uiso . . . . . .
H551 H 1.3250 0.2448 -0.1881 0.0790 1.0000 Uiso . . . . . .
H611 H 0.7888 0.2637 0.2133 0.0740 1.0000 Uiso . . . . . .
H613 H 0.8877 0.3171 0.2016 0.0740 1.0000 Uiso . . . . . .
H612 H 0.8902 0.2034 0.2567 0.0740 1.0000 Uiso . . . . . .
H631 H 0.8236 0.2556 0.0541 0.0550 1.0000 Uiso . . . . . .
H653 H 0.9229 0.1937 -0.0846 0.0780 1.0000 Uiso . . . . . .
H652 H 1.0516 0.2107 -0.1224 0.0780 1.0000 Uiso . . . . . .
H651 H 1.0239 0.1029 -0.0675 0.0780 1.0000 Uiso . . . . . .
H721 H 1.1085 0.4531 0.3849 0.0520 1.0000 Uiso . . . . . .
H731 H 1.1373 0.3914 0.5270 0.0760 1.0000 Uiso . . . . . .
H741 H 1.1638 0.2163 0.5998 0.0720 1.0000 Uiso . . . . . .
H751 H 1.1706 0.1069 0.5345 0.0690 1.0000 Uiso . . . . . .
H761 H 1.1473 0.1683 0.3939 0.0530 1.0000 Uiso . . . . . .
H812 H 1.0117 0.9585 0.1785 0.1430 1.0000 Uiso . . . . . .
H811 H 0.9721 0.9602 0.2736 0.1430 1.0000 Uiso . . . . . .
H813 H 0.9628 0.8673 0.2552 0.1430 1.0000 Uiso . . . . . .
H822 H 0.8261 1.0575 0.2139 0.1030 1.0000 Uiso . . . . . .
H821 H 0.8277 0.9759 0.1755 0.1030 1.0000 Uiso . . . . . .
H831 H 0.6272 1.0573 0.2847 0.1050 1.0000 Uiso . . . . . .
H832 H 0.6209 0.9714 0.2543 0.1050 1.0000 Uiso . . . . . .
H842 H 0.4830 0.9590 0.3921 0.1790 1.0000 Uiso . . . . . .
H841 H 0.5816 0.9506 0.4322 0.1790 1.0000 Uiso . . . . . .
H843 H 0.5797 0.8634 0.4031 0.1790 1.0000 Uiso . . . . . .
H21 H 1.2212 0.1097 -0.0582 0.0487 1.0000 Uiso . . . . . .
H11 H 0.4867 0.4377 0.2665 0.0413 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.154(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . N11 . 2.284(18) yes
W1 . N21 . 2.184(17) yes
W1 . N31 . 2.186(17) yes
W1 . C1 . 1.84(2) yes
W1 . C2 . 1.97(3) yes
W1 . C3 . 2.00(2) yes
W2 . N41 . 2.26(2) yes
W2 . N51 . 2.210(19) yes
W2 . N61 . 2.179(18) yes
W2 . C4 . 1.89(2) yes
W2 . C5 . 1.95(3) yes
W2 . C6 . 1.97(3) yes
Au1 . P1 . 2.235(7) yes
Au1 . Cl1 . 2.284(6) yes
P1 . C1 . 1.75(2) yes
P1 . C4 . 1.73(2) yes
P1 . C71 . 1.87(2) yes
N11 . N12 . 1.35(2) yes
N11 . C12 . 1.39(3) yes
N12 . C14 . 1.34(3) yes
N12 . B1 . 1.56(3) yes
N21 . N22 . 1.39(2) yes
N21 . C22 . 1.32(3) yes
N22 . C24 . 1.32(3) yes
N22 . B1 . 1.57(3) yes
N31 . N32 . 1.33(2) yes
N31 . C32 . 1.38(3) yes
N32 . C34 . 1.32(3) yes
N32 . B1 . 1.58(3) yes
N41 . N42 . 1.40(3) yes
N41 . C42 . 1.35(3) yes
N42 . C44 . 1.34(3) yes
N42 . B2 . 1.55(4) yes
N51 . N52 . 1.39(2) yes
N51 . C52 . 1.33(3) yes
N52 . C54 . 1.36(3) yes
N52 . B2 . 1.56(3) yes
N61 . N62 . 1.38(2) yes
N61 . C62 . 1.36(3) yes
N62 . C64 . 1.36(3) yes
N62 . B2 . 1.54(3) yes
O2 . C2 . 1.15(3) yes
O3 . C3 . 1.14(2) yes
O5 . C5 . 1.18(3) yes
O6 . C6 . 1.17(3) yes
O7 . C82 . 1.36(4) yes
O7 . C83 . 1.41(4) yes
C11 . C12 . 1.45(3) yes
C11 . H111 . 0.981 no
C11 . H113 . 0.971 no
C11 . H112 . 0.958 no
C12 . C13 . 1.36(3) yes
C13 . C14 . 1.38(3) yes
C13 . H131 . 0.952 no
C14 . C15 . 1.48(3) yes
C15 . H153 . 0.963 no
C15 . H152 . 0.981 no
C15 . H151 . 0.968 no
C21 . C22 . 1.50(3) yes
C21 . H211 . 0.962 no
C21 . H213 . 0.962 no
C21 . H212 . 0.977 no
C22 . C23 . 1.38(3) yes
C23 . C24 . 1.34(4) yes
C23 . H231 . 0.958 no
C24 . C25 . 1.51(4) yes
C25 . H253 . 0.969 no
C25 . H252 . 0.977 no
C25 . H251 . 0.982 no
C31 . C32 . 1.52(3) yes
C31 . H311 . 0.966 no
C31 . H313 . 0.954 no
C31 . H312 . 0.975 no
C32 . C33 . 1.37(3) yes
C33 . C34 . 1.41(3) yes
C33 . H331 . 0.941 no
C34 . C35 . 1.48(3) yes
C35 . H353 . 0.972 no
C35 . H352 . 0.956 no
C35 . H351 . 0.968 no
C41 . C42 . 1.54(4) yes
C41 . H411 . 0.965 no
C41 . H413 . 0.974 no
C41 . H412 . 0.965 no
C42 . C43 . 1.33(3) yes
C43 . C44 . 1.35(3) yes
C43 . H431 . 0.940 no
C44 . C45 . 1.47(4) yes
C45 . H453 . 0.984 no
C45 . H452 . 0.970 no
C45 . H451 . 0.967 no
C51 . C52 . 1.53(4) yes
C51 . H511 . 0.964 no
C51 . H513 . 0.973 no
C51 . H512 . 0.963 no
C52 . C53 . 1.36(3) yes
C53 . C54 . 1.36(3) yes
C53 . H531 . 0.948 no
C54 . C55 . 1.51(3) yes
C55 . H553 . 0.967 no
C55 . H552 . 0.978 no
C55 . H551 . 0.970 no
C61 . C62 . 1.52(3) yes
C61 . H611 . 0.963 no
C61 . H613 . 0.968 no
C61 . H612 . 0.956 no
C62 . C63 . 1.37(3) yes
C63 . C64 . 1.38(3) yes
C63 . H631 . 0.950 no
C64 . C65 . 1.45(3) yes
C65 . H653 . 0.971 no
C65 . H652 . 0.965 no
C65 . H651 . 0.969 no
C71 . C72 . 1.38(3) yes
C71 . C76 . 1.37(3) yes
C72 . C73 . 1.40(3) yes
C72 . H721 . 0.963 no
C73 . C74 . 1.42(4) yes
C73 . H731 . 0.946 no
C74 . C75 . 1.33(4) yes
C74 . H741 . 0.941 no
C75 . C76 . 1.38(3) yes
C75 . H751 . 0.978 no
C76 . H761 . 0.951 no
C81 . C82 . 1.45(5) yes
C81 . H812 . 0.966 no
C81 . H811 . 0.964 no
C81 . H813 . 0.991 no
C82 . H822 . 1.008 no
C82 . H821 . 0.981 no
C83 . C84 . 1.53(5) yes
C83 . H831 . 0.982 no
C83 . H832 . 0.998 no
C84 . H842 . 0.979 no
C84 . H841 . 0.953 no
C84 . H843 . 0.981 no
B1 . H11 . 1.095 no
B2 . H21 . 1.099 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 . W1 . N21 . 78.7(7) yes
N11 . W1 . N31 . 80.8(7) yes
N21 . W1 . N31 . 83.8(7) yes
N11 . W1 . C1 . 178.3(8) yes
N21 . W1 . C1 . 102.9(8) yes
N31 . W1 . C1 . 100.1(8) yes
N11 . W1 . C2 . 92.9(9) yes
N21 . W1 . C2 . 171.4(8) yes
N31 . W1 . C2 . 96.9(8) yes
C1 . W1 . C2 . 85.5(10) yes
N11 . W1 . C3 . 94.6(8) yes
N21 . W1 . C3 . 93.0(8) yes
N31 . W1 . C3 . 174.8(8) yes
C1 . W1 . C3 . 84.6(9) yes
C2 . W1 . C3 . 85.7(10) yes
N41 . W2 . N51 . 82.3(7) yes
N41 . W2 . N61 . 82.3(7) yes
N51 . W2 . N61 . 83.2(6) yes
N41 . W2 . C4 . 171.7(9) yes
N51 . W2 . C4 . 102.9(8) yes
N61 . W2 . C4 . 104.6(9) yes
N41 . W2 . C5 . 86.7(9) yes
N51 . W2 . C5 . 168.8(9) yes
N61 . W2 . C5 . 93.1(9) yes
C4 . W2 . C5 . 88.3(10) yes
N41 . W2 . C6 . 88.6(9) yes
N51 . W2 . C6 . 93.1(8) yes
N61 . W2 . C6 . 170.6(9) yes
C4 . W2 . C6 . 84.7(10) yes
C5 . W2 . C6 . 88.8(10) yes
P1 . Au1 . Cl1 . 178.4(2) yes
Au1 . P1 . C1 . 111.2(8) yes
Au1 . P1 . C4 . 112.3(8) yes
C1 . P1 . C4 . 106.8(10) yes
Au1 . P1 . C71 . 112.0(7) yes
C1 . P1 . C71 . 103.7(10) yes
C4 . P1 . C71 . 110.4(11) yes
W1 . N11 . N12 . 119.6(13) yes
W1 . N11 . C12 . 133.1(14) yes
N12 . N11 . C12 . 106.9(17) yes
N11 . N12 . C14 . 110.7(18) yes
N11 . N12 . B1 . 121.0(17) yes
C14 . N12 . B1 . 127.9(19) yes
W1 . N21 . N22 . 122.9(14) yes
W1 . N21 . C22 . 133.6(16) yes
N22 . N21 . C22 . 103.5(18) yes
N21 . N22 . C24 . 110(2) yes
N21 . N22 . B1 . 119.0(19) yes
C24 . N22 . B1 . 131(2) yes
W1 . N31 . N32 . 123.5(14) yes
W1 . N31 . C32 . 129.8(14) yes
N32 . N31 . C32 . 105.1(17) yes
N31 . N32 . C34 . 113.7(19) yes
N31 . N32 . B1 . 119.3(18) yes
C34 . N32 . B1 . 126.8(20) yes
W2 . N41 . N42 . 119.6(15) yes
W2 . N41 . C42 . 140.1(17) yes
N42 . N41 . C42 . 100.2(19) yes
N41 . N42 . C44 . 112(2) yes
N41 . N42 . B2 . 120.0(20) yes
C44 . N42 . B2 . 128(2) yes
W2 . N51 . N52 . 119.1(14) yes
W2 . N51 . C52 . 135.4(18) yes
N52 . N51 . C52 . 105.1(20) yes
N51 . N52 . C54 . 107.4(19) yes
N51 . N52 . B2 . 122.0(18) yes
C54 . N52 . B2 . 130(2) yes
W2 . N61 . N62 . 122.2(14) yes
W2 . N61 . C62 . 132.4(15) yes
N62 . N61 . C62 . 105.0(18) yes
N61 . N62 . C64 . 110.7(18) yes
N61 . N62 . B2 . 119.8(19) yes
C64 . N62 . B2 . 129(2) yes
C82 . O7 . C83 . 114(3) yes
P1 . C1 . W1 . 170.3(13) yes
W1 . C2 . O2 . 178(2) yes
W1 . C3 . O3 . 174.5(18) yes
P1 . C4 . W2 . 173.2(16) yes
W2 . C5 . O5 . 176(2) yes
W2 . C6 . O6 . 179(2) yes
C12 . C11 . H111 . 110.5 no
C12 . C11 . H113 . 111.6 no
H111 . C11 . H113 . 106.6 no
C12 . C11 . H112 . 111.7 no
H111 . C11 . H112 . 107.5 no
H113 . C11 . H112 . 108.8 no
C11 . C12 . N11 . 122.1(20) yes
C11 . C12 . C13 . 131(2) yes
N11 . C12 . C13 . 106.7(19) yes
C12 . C13 . C14 . 109(2) yes
C12 . C13 . H131 . 125.0 no
C14 . C13 . H131 . 125.6 no
C13 . C14 . N12 . 106(2) yes
C13 . C14 . C15 . 133(2) yes
N12 . C14 . C15 . 121(2) yes
C14 . C15 . H153 . 112.0 no
C14 . C15 . H152 . 110.1 no
H153 . C15 . H152 . 107.5 no
C14 . C15 . H151 . 111.1 no
H153 . C15 . H151 . 108.7 no
H152 . C15 . H151 . 107.2 no
C22 . C21 . H211 . 111.6 no
C22 . C21 . H213 . 110.7 no
H211 . C21 . H213 . 109.2 no
C22 . C21 . H212 . 109.6 no
H211 . C21 . H212 . 107.8 no
H213 . C21 . H212 . 107.8 no
C21 . C22 . N21 . 123(2) yes
C21 . C22 . C23 . 125(2) yes
N21 . C22 . C23 . 112(2) yes
C22 . C23 . C24 . 104(2) yes
C22 . C23 . H231 . 127.9 no
C24 . C23 . H231 . 127.6 no
C23 . C24 . N22 . 109(2) yes
C23 . C24 . C25 . 130(3) yes
N22 . C24 . C25 . 120(3) yes
C24 . C25 . H253 . 112.7 no
C24 . C25 . H252 . 111.7 no
H253 . C25 . H252 . 107.4 no
C24 . C25 . H251 . 111.4 no
H253 . C25 . H251 . 106.8 no
H252 . C25 . H251 . 106.4 no
C32 . C31 . H311 . 109.8 no
C32 . C31 . H313 . 111.3 no
H311 . C31 . H313 . 109.3 no
C32 . C31 . H312 . 110.2 no
H311 . C31 . H312 . 107.5 no
H313 . C31 . H312 . 108.5 no
C31 . C32 . N31 . 123.1(19) yes
C31 . C32 . C33 . 128(2) yes
N31 . C32 . C33 . 109.1(20) yes
C32 . C33 . C34 . 106.1(20) yes
C32 . C33 . H331 . 126.5 no
C34 . C33 . H331 . 127.4 no
C33 . C34 . N32 . 105.9(20) yes
C33 . C34 . C35 . 129(2) yes
N32 . C34 . C35 . 125(2) yes
C34 . C35 . H353 . 109.5 no
C34 . C35 . H352 . 110.2 no
H353 . C35 . H352 . 109.0 no
C34 . C35 . H351 . 110.7 no
H353 . C35 . H351 . 108.0 no
H352 . C35 . H351 . 109.4 no
C42 . C41 . H411 . 111.1 no
C42 . C41 . H413 . 110.4 no
H411 . C41 . H413 . 107.9 no
C42 . C41 . H412 . 110.9 no
H411 . C41 . H412 . 108.5 no
H413 . C41 . H412 . 107.9 no
C41 . C42 . N41 . 117(2) yes
C41 . C42 . C43 . 128(2) yes
N41 . C42 . C43 . 115(2) yes
C42 . C43 . C44 . 106(2) yes
C42 . C43 . H431 . 126.9 no
C44 . C43 . H431 . 127.5 no
C43 . C44 . N42 . 107(2) yes
C43 . C44 . C45 . 129(3) yes
N42 . C44 . C45 . 123(3) yes
C44 . C45 . H453 . 111.1 no
C44 . C45 . H452 . 112.2 no
H453 . C45 . H452 . 106.7 no
C44 . C45 . H451 . 111.9 no
H453 . C45 . H451 . 106.8 no
H452 . C45 . H451 . 107.9 no
C52 . C51 . H511 . 110.8 no
C52 . C51 . H513 . 110.4 no
H511 . C51 . H513 . 107.9 no
C52 . C51 . H512 . 111.1 no
H511 . C51 . H512 . 108.5 no
H513 . C51 . H512 . 108.0 no
C51 . C52 . N51 . 120(2) yes
C51 . C52 . C53 . 127(2) yes
N51 . C52 . C53 . 113(2) yes
C52 . C53 . C54 . 104(2) yes
C52 . C53 . H531 . 128.8 no
C54 . C53 . H531 . 127.1 no
N52 . C54 . C53 . 110(2) yes
N52 . C54 . C55 . 123(2) yes
C53 . C54 . C55 . 127(2) yes
C54 . C55 . H553 . 112.1 no
C54 . C55 . H552 . 110.7 no
H553 . C55 . H552 . 107.3 no
C54 . C55 . H551 . 111.4 no
H553 . C55 . H551 . 107.9 no
H552 . C55 . H551 . 107.1 no
C62 . C61 . H611 . 109.9 no
C62 . C61 . H613 . 109.8 no
H611 . C61 . H613 . 108.2 no
C62 . C61 . H612 . 110.3 no
H611 . C61 . H612 . 109.5 no
H613 . C61 . H612 . 109.1 no
C61 . C62 . N61 . 121(2) yes
C61 . C62 . C63 . 129(2) yes
N61 . C62 . C63 . 110(2) yes
C62 . C63 . C64 . 107(2) yes
C62 . C63 . H631 . 125.8 no
C64 . C63 . H631 . 126.9 no
C63 . C64 . N62 . 106.4(20) yes
C63 . C64 . C65 . 130(2) yes
N62 . C64 . C65 . 124(2) yes
C64 . C65 . H653 . 111.0 no
C64 . C65 . H652 . 111.4 no
H653 . C65 . H652 . 108.1 no
C64 . C65 . H651 . 110.3 no
H653 . C65 . H651 . 107.8 no
H652 . C65 . H651 . 108.1 no
P1 . C71 . C72 . 114.7(17) yes
P1 . C71 . C76 . 122.5(17) yes
C72 . C71 . C76 . 122(2) yes
C71 . C72 . C73 . 118(2) yes
C71 . C72 . H721 . 120.2 no
C73 . C72 . H721 . 121.5 no
C72 . C73 . C74 . 118(3) yes
C72 . C73 . H731 . 121.3 no
C74 . C73 . H731 . 120.1 no
C73 . C74 . C75 . 120(3) yes
C73 . C74 . H741 . 120.0 no
C75 . C74 . H741 . 119.7 no
C74 . C75 . C76 . 122(3) yes
C74 . C75 . H751 . 119.9 no
C76 . C75 . H751 . 118.1 no
C75 . C76 . C71 . 118(3) yes
C75 . C76 . H761 . 122.6 no
C71 . C76 . H761 . 119.0 no
C82 . C81 . H812 . 113.7 no
C82 . C81 . H811 . 112.2 no
H812 . C81 . H811 . 108.6 no
C82 . C81 . H813 . 108.6 no
H812 . C81 . H813 . 106.6 no
H811 . C81 . H813 . 106.7 no
C81 . C82 . O7 . 112(3) yes
C81 . C82 . H822 . 106.3 no
O7 . C82 . H822 . 111.2 no
C81 . C82 . H821 . 108.7 no
O7 . C82 . H821 . 113.0 no
H822 . C82 . H821 . 105.7 no
O7 . C83 . C84 . 107(3) yes
O7 . C83 . H831 . 111.9 no
C84 . C83 . H831 . 110.3 no
O7 . C83 . H832 . 110.9 no
C84 . C83 . H832 . 110.3 no
H831 . C83 . H832 . 106.4 no
C83 . C84 . H842 . 111.9 no
C83 . C84 . H841 . 111.4 no
H842 . C84 . H841 . 108.6 no
C83 . C84 . H843 . 110.2 no
H842 . C84 . H843 . 106.3 no
H841 . C84 . H843 . 108.4 no
N32 . B1 . N22 . 106.2(18) yes
N32 . B1 . N12 . 109(2) yes
N22 . B1 . N12 . 107.5(19) yes
N32 . B1 . H11 . 111.7 no
N22 . B1 . H11 . 111.2 no
N12 . B1 . H11 . 111.4 no
N52 . B2 . N42 . 108(2) yes
N52 . B2 . N62 . 107.1(20) yes
N42 . B2 . N62 . 110(2) yes
N52 . B2 . H21 . 110.0 no
N42 . B2 . H21 . 112.4 no
N62 . B2 . H21 . 109.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C15 . H153 . O3 2_666 121.0 0.963 2.576 3.18(4) yes
C31 . H313 . C2 . 145.0 0.954 2.595 3.42(4) yes
C51 . H513 . C6 . 133.0 0.973 2.552 3.30(4) yes
C61 . H612 . C5 . 135.0 0.956 2.545 3.29(4) yes
C65 . H652 . O2 2_765 156.0 0.965 2.566 3.47(4) yes
C74 . H741 . O7 2_766 139.0 0.941 2.469 3.24(4) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 02/10/14 at 16:51:20
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
REM CONT EXTPARAM 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 02/10/14 at 16:51:20
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.01 = C(35) TO C(34) 
U(IJ) 0.0, 0.01 = C(1) TO P(1) 
U(IJ) 0.0, 0.01 = C(2) TO O(2) 
U(IJ) 0.0, 0.01 = C(5) TO O(5) 
U(IJ) 0.0, 0.01 = C(43) TO C(42) 
U(IJ) 0.0, 0.01 = N(31) TO N(32) 
VIBR 0.0, 0.01 = C(71) TO C(72), C(72) TO C(73) 
VIBR 0.0, 0.01 = C(72) TO C(73), C(73) TO C(74) 
VIBR 0.0, 0.01 = C(73) TO C(74), C(74) TO C(75) 
VIBR 0.0, 0.01 = C(74) TO C(75), C(75) TO C(76) 
VIBR 0.0, 0.01 = C(75) TO C(76), C(76) TO C(77) 
VIBR 0.0, 0.01 = C(76) TO C(71), C(71) TO C(78) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
7 6 14 x .

# start Validation Reply Form
_vrf_DIFMX01_1                   
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: The difference electron density map revealed three large peaks
in interstitial space, isolated from the principal molecule. 
These do not appear to correspond to any solvent 
or from an image of the heavy atoms from a small twin component.
The crystals obtained were of poor quality which led to the
anomolous electron density.
;
_vrf_PLAT097_1                   
;
PROBLEM: Large Reported Max.  (Positive) Residual Density      11.22 eA-3  
RESPONSE: The difference electron density map revealed three large peaks
in interstitial space, isolated from the principal molecule. 
These do not appear to correspond to any solvent 
or from an image of the heavy atoms from a small twin component.
The crystals obtained were of poor quality which led to the
anomolous electron density.
;
_vrf_PLAT342_1                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0425 Ang.  
RESPONSE: The crystals which were obtained of this compound 
were all of poor quality. Data were collected on the best of the 
sampled crystals, even though it was known to diffract only weakly.
The precision is therefore lower than we would like,
but the identity of the compound is clearly established
and there do not appear to be any major refinement anomalies.

;
