# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1423314'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2016-12-22 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          Twin
#--------------------------------------------------------------- 
# _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                   22.1833(6)
_cell_length_b                   10.5501(3)
_cell_length_c                   23.1940(4)
_cell_angle_alpha                90
_cell_angle_beta                 114.4551(14)
_cell_angle_gamma                90
_cell_volume                     4941.2(2)

_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'
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'
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'
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'
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 = C38 H48 B2 Cl5 N12 O4 P1 W2 
# Dc =      1.79 Fooo =   2600.00 Mu =     50.06 M =   1334.44
# Found Formula = C38 H48 B2 Cl5 N12 O4 P1 W2 
# Dc =      1.79 FOOO =   2600.00 Mu =     50.06 M =   1334.44

_chemical_formula_sum            'C38 H48 B2 Cl5 N12 O4 P1 W2'
_chemical_formula_moiety         'C36 H44 B2 Cl1 N12 O4 P1 W2, 2(C1 H2 Cl2)'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         1334.44


_cell_measurement_reflns_used    9219
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_min          0.040
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_max          0.090

_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2600
_exptl_absorpt_coefficient_mu    5.006

# Sheldrick geometric approximatio 0.74 0.82 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.82

# 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 (Farrugia, 1997)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            8702
_reflns_number_total             8702
_diffrn_reflns_av_R_equivalents  0.000
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8702 
# Theoretical number of reflections is about 17404 


_diffrn_reflns_theta_min         2.618
_diffrn_reflns_theta_max         24.999
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -26
_reflns_limit_h_max              24
_reflns_limit_k_min              -12
_reflns_limit_k_max              12
_reflns_limit_l_min              -27
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   3.01
_oxford_diffrn_Wilson_scale      354.66

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

_refine_diff_density_min         -3.78
_refine_diff_density_max         2.75


# 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         8662
_refine_ls_number_restraints     170
_refine_ls_number_parameters     576
_oxford_refine_ls_R_factor_ref   0.1150
_refine_ls_wR_factor_ref         0.2416
_refine_ls_goodness_of_fit_ref   1.0583
_refine_ls_shift/su_max          0.0049398
_refine_ls_shift/su_mean         0.0004225


# The values computed from all data 
_oxford_reflns_number_all        8662
_refine_ls_R_factor_all          0.1150
_refine_ls_wR_factor_all         0.2416

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6928
_refine_ls_R_factor_gt           0.0964
_refine_ls_wR_factor_gt          0.2367

# 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: 
 9.45 12.4 5.95 1.52 
;

# 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
B1 B 0.8485(12) 0.592(2) 0.5057(12) 0.0399 1.0000 Uani . U . . . .
B2 B 0.5416(14) 0.596(3) 0.6451(13) 0.0412 1.0000 Uani . . . . . .
Cl1 Cl 0.7783(5) 1.1538(7) 0.6430(5) 0.0945 1.0000 Uani . . . . . .
Cl2 Cl 0.7456(5) 0.3271(9) 0.8314(5) 0.0969 1.0000 Uani D . . . . .
Cl3 Cl 0.6161(5) 0.2390(10) 0.7431(5) 0.0907 1.0000 Uani D . . . . .
Cl4 Cl 0.0349(4) 0.7862(11) 0.0972(5) 0.1024 1.0000 Uani D . . . . .
Cl5 Cl 0.1039(7) 0.6621(15) 0.2149(8) 0.1608 1.0000 Uani D . . . . .
N11 N 0.8697(10) 0.831(2) 0.5027(10) 0.0496 1.0000 Uani . . . . . .
N12 N 0.8740(10) 0.712(2) 0.4825(10) 0.0491 1.0000 Uani . U . . . .
N21 N 0.7551(8) 0.7282(17) 0.5133(9) 0.0373 1.0000 Uani . U . . . .
N22 N 0.7744(9) 0.6249(17) 0.4907(8) 0.0381 1.0000 Uani . U . . . .
N31 N 0.8881(8) 0.6852(19) 0.6162(9) 0.0418 1.0000 Uani . . . . . .
N32 N 0.8844(9) 0.5887(19) 0.5782(10) 0.0454 1.0000 Uani . U . . . .
N41 N 0.6380(10) 0.6459(17) 0.7480(9) 0.0404 1.0000 Uani . . . . . .
N42 N 0.5730(10) 0.590(2) 0.7159(9) 0.0445 1.0000 Uani . . . . . .
N51 N 0.6495(9) 0.5649(17) 0.6330(8) 0.0353 1.0000 Uani . U . . . .
N52 N 0.5837(9) 0.5244(17) 0.6165(8) 0.0354 1.0000 Uani . U . . . .
N61 N 0.5884(11) 0.8103(18) 0.6330(10) 0.0468 1.0000 Uani . . . . . .
N62 N 0.5324(9) 0.7359(18) 0.6219(8) 0.0393 1.0000 Uani . . . . . .
O3 O 0.9616(10) 1.0308(19) 0.6371(10) 0.0722 1.0000 Uani . . . . . .
O4 O 0.7528(11) 1.097(2) 0.4931(11) 0.0798 1.0000 Uani . . . . . .
O5 O 0.7392(11) 0.977(2) 0.7748(11) 0.0817 1.0000 Uani . . . . . .
O6 O 0.8251(9) 0.622(2) 0.7816(9) 0.0739 1.0000 Uani . . . . . .
P1 P 0.8384(4) 0.9854(7) 0.6720(4) 0.0621 1.0000 Uani . . . . . .
W1 W 0.83329(4) 0.86497(8) 0.57643(5) 0.0368 1.0000 Uani . . . . . .
W2 W 0.68797(5) 0.73648(8) 0.69041(5) 0.0391 1.0000 Uani . . . . . .
C1 C 0.7859(10) 0.861(2) 0.6313(9) 0.0294 1.0000 Uani . . . . . .
C2 C 0.7376(11) 0.8049(19) 0.6524(10) 0.0352 1.0000 Uani . . . . . .
C3 C 0.9144(12) 0.973(2) 0.6171(13) 0.0535 1.0000 Uani . . . . . .
C4 C 0.7826(13) 1.013(3) 0.5252(13) 0.0526 1.0000 Uani . . . . . .
C5 C 0.7167(13) 0.887(2) 0.7428(14) 0.0557 1.0000 Uani . . . . . .
C6 C 0.7733(15) 0.658(3) 0.7460(12) 0.0535 1.0000 Uani . . . . . .
C11 C 0.8952(6) 0.908(3) 0.4697(9) 0.0618 1.0000 Uani D . . . . .
C12 C 0.9124(5) 0.838(3) 0.4306(8) 0.0784 1.0000 Uani D . . . . .
C13 C 0.8993(6) 0.716(3) 0.4386(8) 0.0689 1.0000 Uani D U . . . .
C14 C 0.9028(12) 1.049(3) 0.4778(14) 0.0871 1.0000 Uani D . . . . .
C15 C 0.9058(14) 0.600(3) 0.4050(14) 0.0919 1.0000 Uani D U . . . .
C21 C 0.6882(8) 0.7256(17) 0.4873(7) 0.0382 1.0000 Uani D U . . . .
C22 C 0.6653(10) 0.6223(17) 0.4501(6) 0.0431 1.0000 Uani D U . . . .
C23 C 0.7209(9) 0.557(2) 0.4523(7) 0.0461 1.0000 Uani D . . . . .
C24 C 0.6481(9) 0.829(2) 0.4995(11) 0.0454 1.0000 Uani D . . . . .
C25 C 0.7225(11) 0.439(2) 0.4186(12) 0.0569 1.0000 Uani D . . . . .
C31 C 0.9222(6) 0.655(3) 0.6767(10) 0.0553 1.0000 Uani D . . . . .
C32 C 0.9404(7) 0.527(2) 0.6764(13) 0.0682 1.0000 Uani D U . . . .
C33 C 0.9169(7) 0.487(2) 0.6139(13) 0.0622 1.0000 Uani D U . . . .
C34 C 0.9414(12) 0.738(2) 0.7318(11) 0.0632 1.0000 Uani D . . . . .
C35 C 0.9200(12) 0.361(3) 0.5876(14) 0.0855 1.0000 Uani D . . . . .
C41 C 0.6543(11) 0.6306(14) 0.8096(8) 0.0447 1.0000 Uani D . . . . .
C42 C 0.6050(10) 0.5658(12) 0.8187(10) 0.0521 1.0000 Uani D . . . . .
C43 C 0.5549(12) 0.5429(14) 0.7596(11) 0.0539 1.0000 Uani D . . . . .
C44 C 0.7218(15) 0.671(2) 0.8595(11) 0.0783 1.0000 Uani D . . . . .
C45 C 0.4894(12) 0.467(3) 0.7411(12) 0.0803 1.0000 Uani D . . . . .
C51 C 0.6770(11) 0.4820(16) 0.6100(6) 0.0386 1.0000 Uani D U . . . .
C52 C 0.6320(11) 0.3857(17) 0.5779(6) 0.0438 1.0000 Uani D U . . . .
C53 C 0.5735(10) 0.4180(16) 0.5827(6) 0.0353 1.0000 Uani D . . . . .
C54 C 0.7497(10) 0.489(2) 0.6182(11) 0.0499 1.0000 Uani D . . . . .
C55 C 0.5090(10) 0.347(2) 0.5575(11) 0.0475 1.0000 Uani D . . . . .
C61 C 0.5669(12) 0.9231(18) 0.6068(6) 0.0444 1.0000 Uani D . . . . .
C62 C 0.4953(12) 0.922(2) 0.5806(6) 0.0520 1.0000 Uani D . . . . .
C63 C 0.4758(11) 0.806(2) 0.5923(6) 0.0462 1.0000 Uani D . . . . .
C64 C 0.6097(11) 1.030(2) 0.6095(10) 0.0475 1.0000 Uani D . . . . .
C65 C 0.4129(15) 0.761(3) 0.5798(12) 0.0804 1.0000 Uani D . . . . .
C101 C 0.693(2) 0.311(3) 0.7520(15) 0.0990 1.0000 Uani D . . . . .
C201 C 0.0921(16) 0.795(4) 0.1748(18) 0.1236 1.0000 Uani D . . . . .
H1 H 0.8540 0.5035 0.4832 0.0481 1.0000 Uiso R . . . . .
H2 H 0.4926 0.5515 0.6281 0.0502 1.0000 Uiso R . . . . .
H121 H 0.9299 0.8686 0.4030 0.0960 1.0000 Uiso DR . . . . .
H141 H 0.8887 1.0885 0.4371 0.1290 1.0000 Uiso DR . . . . .
H142 H 0.9484 1.0691 0.5031 0.1290 1.0000 Uiso DR . . . . .
H143 H 0.8761 1.0786 0.4986 0.1290 1.0000 Uiso DR . . . . .
H221 H 0.6213 0.5998 0.4276 0.0510 1.0000 Uiso DR . . . . .
H241 H 0.6073 0.7940 0.4975 0.0680 1.0000 Uiso DR . . . . .
H242 H 0.6727 0.8649 0.5408 0.0680 1.0000 Uiso DR . . . . .
H243 H 0.6385 0.8940 0.4680 0.0680 1.0000 Uiso DR . . . . .
H251 H 0.6817 0.4302 0.3817 0.0830 1.0000 Uiso DR . . . . .
H252 H 0.7280 0.3677 0.4460 0.0830 1.0000 Uiso DR . . . . .
H253 H 0.7588 0.4424 0.4061 0.0830 1.0000 Uiso DR . . . . .
H321 H 0.9642 0.4779 0.7118 0.0901 1.0000 Uiso DR . . . . .
H351 H 0.9407 0.3016 0.6215 0.1250 1.0000 Uiso DR . . . . .
H352 H 0.9454 0.3663 0.5627 0.1250 1.0000 Uiso DR . . . . .
H353 H 0.8760 0.3321 0.5614 0.1250 1.0000 Uiso DR . . . . .
H421 H 0.6054 0.5418 0.8574 0.0630 1.0000 Uiso DR . . . . .
H441 H 0.7164 0.7080 0.8948 0.1179 1.0000 Uiso DR . . . . .
H442 H 0.7414 0.7314 0.8416 0.1180 1.0000 Uiso DR . . . . .
H443 H 0.7501 0.5978 0.8735 0.1180 1.0000 Uiso DR . . . . .
H451 H 0.4787 0.4621 0.7771 0.1230 1.0000 Uiso DR . . . . .
H452 H 0.4544 0.5092 0.7070 0.1230 1.0000 Uiso DR . . . . .
H453 H 0.4952 0.3834 0.7282 0.1229 1.0000 Uiso DR . . . . .
H521 H 0.6396 0.3154 0.5577 0.0580 1.0000 Uiso DR . . . . .
H541 H 0.7542 0.4467 0.5835 0.0720 1.0000 Uiso DR . . . . .
H542 H 0.7780 0.4488 0.6571 0.0720 1.0000 Uiso DR . . . . .
H543 H 0.7628 0.5762 0.6190 0.0720 1.0000 Uiso DR . . . . .
H551 H 0.5107 0.2785 0.5311 0.0719 1.0000 Uiso DR . . . . .
H552 H 0.5007 0.3144 0.5921 0.0720 1.0000 Uiso DR . . . . .
H553 H 0.4738 0.4039 0.5331 0.0720 1.0000 Uiso DR . . . . .
H621 H 0.4676 0.9879 0.5592 0.0630 1.0000 Uiso DR . . . . .
H641 H 0.5836 1.1000 0.5873 0.0578 1.0000 Uiso DR . . . . .
H642 H 0.6348 1.0524 0.6525 0.0578 1.0000 Uiso DR . . . . .
H643 H 0.6388 1.0060 0.5907 0.0578 1.0000 Uiso DR . . . . .
H651 H 0.3803 0.8176 0.5514 0.1190 1.0000 Uiso DR . . . . .
H652 H 0.4075 0.7545 0.6188 0.1190 1.0000 Uiso DR . . . . .
H653 H 0.4074 0.6782 0.5606 0.1190 1.0000 Uiso DR . . . . .
H1011 H 0.7147 0.2582 0.7316 0.1210 1.0000 Uiso DR . . . . .
H1012 H 0.6846 0.3944 0.7322 0.1210 1.0000 Uiso DR . . . . .
H2011 H 0.0772 0.8592 0.1960 0.1430 1.0000 Uiso DR . . . . .
H2012 H 0.1341 0.8212 0.1749 0.1430 1.0000 Uiso DR . . . . .
H151 H 0.9246 0.6216 0.3762 0.1536 1.0000 Uiso DR . . . . .
H152 H 0.9338 0.5413 0.4353 0.1536 1.0000 Uiso DR . . . . .
H153 H 0.8634 0.5631 0.3825 0.1536 1.0000 Uiso DR . . . . .
H341 H 0.9655 0.6909 0.7691 0.0750 1.0000 Uiso DR . . . . .
H342 H 0.9684 0.8051 0.7282 0.0750 1.0000 Uiso DR . . . . .
H343 H 0.9028 0.7727 0.7339 0.0750 1.0000 Uiso DR . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06064(2)

loop_
_oxford_twin_element_scale_factors
0.590(2)
0.410(2)
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
B1 . N12 . 1.57(3) yes
B1 . N22 . 1.57(3) yes
B1 . N32 . 1.53(3) yes
B1 . H1 . 1.100 no
B2 . N42 . 1.49(3) yes
B2 . N52 . 1.55(3) yes
B2 . N62 . 1.55(3) yes
B2 . H2 . 1.100 no
Cl1 . P1 . 2.155(12) yes
Cl2 . C101 . 1.73(4) yes
Cl3 . C101 . 1.81(4) yes
Cl4 . C201 . 1.72(4) yes
Cl5 . C201 . 1.65(4) yes
N11 . N12 . 1.36(3) yes
N11 . W1 . 2.20(2) yes
N11 . C11 . 1.38(3) yes
N12 . C13 . 1.35(3) yes
N21 . N22 . 1.35(3) yes
N21 . W1 . 2.266(17) yes
N21 . C21 . 1.35(2) yes
N22 . C23 . 1.36(3) yes
N31 . N32 . 1.33(3) yes
N31 . W1 . 2.236(19) yes
N31 . C31 . 1.33(3) yes
N32 . C33 . 1.36(3) yes
N41 . N42 . 1.45(3) yes
N41 . W2 . 2.270(19) yes
N41 . C41 . 1.33(2) yes
N42 . C43 . 1.33(3) yes
N51 . N52 . 1.41(2) yes
N51 . W2 . 2.199(18) yes
N51 . C51 . 1.30(2) yes
N52 . C53 . 1.33(3) yes
N61 . N62 . 1.40(3) yes
N61 . W2 . 2.20(2) yes
N61 . C61 . 1.33(3) yes
N62 . C63 . 1.37(3) yes
O3 . C3 . 1.13(3) yes
O4 . C4 . 1.17(3) yes
O5 . C5 . 1.18(3) yes
O6 . C6 . 1.17(3) yes
P1 . W1 . 2.517(7) yes
P1 . C1 . 1.75(2) yes
W1 . C1 . 1.958(19) yes
W1 . C3 . 2.00(3) yes
W1 . C4 . 2.00(3) yes
W2 . C2 . 1.82(2) yes
W2 . C5 . 1.94(3) yes
W2 . C6 . 1.98(3) yes
C1 . C2 . 1.47(3) yes
C11 . C12 . 1.34(4) yes
C11 . C14 . 1.50(4) yes
C12 . C13 . 1.36(4) yes
C12 . H121 . 0.931 no
C13 . C15 . 1.49(4) yes
C14 . H141 . 0.960 no
C14 . H142 . 0.960 no
C14 . H143 . 0.959 no
C15 . H151 . 0.950 no
C15 . H152 . 0.950 no
C15 . H153 . 0.950 no
C21 . C22 . 1.35(3) yes
C21 . C24 . 1.51(3) yes
C22 . C23 . 1.40(3) yes
C22 . H221 . 0.928 no
C23 . C25 . 1.47(3) yes
C24 . H241 . 0.959 no
C24 . H242 . 0.961 no
C24 . H243 . 0.960 no
C25 . H251 . 0.959 no
C25 . H252 . 0.960 no
C25 . H253 . 0.963 no
C31 . C32 . 1.41(4) yes
C31 . C34 . 1.46(4) yes
C32 . C33 . 1.39(4) yes
C32 . H321 . 0.931 no
C33 . C35 . 1.48(4) yes
C34 . H341 . 0.950 no
C34 . H342 . 0.950 no
C34 . H343 . 0.950 no
C35 . H351 . 0.957 no
C35 . H352 . 0.960 no
C35 . H353 . 0.960 no
C41 . C42 . 1.38(3) yes
C41 . C44 . 1.52(4) yes
C42 . C43 . 1.38(3) yes
C42 . H421 . 0.930 no
C43 . C45 . 1.55(4) yes
C44 . H441 . 0.960 no
C44 . H442 . 0.961 no
C44 . H443 . 0.960 no
C45 . H451 . 0.960 no
C45 . H452 . 0.958 no
C45 . H453 . 0.959 no
C51 . C52 . 1.40(3) yes
C51 . C54 . 1.55(3) yes
C52 . C53 . 1.39(3) yes
C52 . H521 . 0.929 no
C53 . C55 . 1.50(3) yes
C54 . H541 . 0.960 no
C54 . H542 . 0.960 no
C54 . H543 . 0.962 no
C55 . H551 . 0.960 no
C55 . H552 . 0.960 no
C55 . H553 . 0.960 no
C61 . C62 . 1.45(3) yes
C61 . C64 . 1.46(3) yes
C62 . C63 . 1.36(3) yes
C62 . H621 . 0.928 no
C63 . C65 . 1.39(4) yes
C64 . H641 . 0.950 no
C64 . H642 . 0.950 no
C64 . H643 . 0.950 no
C65 . H651 . 0.963 no
C65 . H652 . 0.962 no
C65 . H653 . 0.961 no
C101 . H1011 . 0.971 no
C101 . H1012 . 0.970 no
C201 . H2011 . 0.969 no
C201 . H2012 . 0.971 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
N12 . B1 . N22 . 103.7(17) yes
N12 . B1 . N32 . 107.2(20) yes
N22 . B1 . N32 . 105.5(19) yes
N12 . B1 . H1 . 113.1 no
N22 . B1 . H1 . 113.3 no
N32 . B1 . H1 . 113.2 no
N42 . B2 . N52 . 111(2) yes
N42 . B2 . N62 . 111(2) yes
N52 . B2 . N62 . 109.5(18) yes
N42 . B2 . H2 . 108.5 no
N52 . B2 . H2 . 108.4 no
N62 . B2 . H2 . 108.4 no
N12 . N11 . W1 . 121.1(16) yes
N12 . N11 . C11 . 104(2) yes
W1 . N11 . C11 . 134.5(19) yes
B1 . N12 . N11 . 123(2) yes
B1 . N12 . C13 . 127(2) yes
N11 . N12 . C13 . 110(2) yes
N22 . N21 . W1 . 118.8(12) yes
N22 . N21 . C21 . 106.0(16) yes
W1 . N21 . C21 . 135.0(14) yes
B1 . N22 . N21 . 124.3(18) yes
B1 . N22 . C23 . 125.2(19) yes
N21 . N22 . C23 . 110.5(18) yes
N32 . N31 . W1 . 120.2(14) yes
N32 . N31 . C31 . 112(2) yes
W1 . N31 . C31 . 127.8(18) yes
B1 . N32 . N31 . 125.0(19) yes
B1 . N32 . C33 . 126(2) yes
N31 . N32 . C33 . 109(2) yes
N42 . N41 . W2 . 119.5(13) yes
N42 . N41 . C41 . 105.9(19) yes
W2 . N41 . C41 . 134.5(17) yes
N41 . N42 . B2 . 117.4(17) yes
N41 . N42 . C43 . 108.1(19) yes
B2 . N42 . C43 . 135(2) yes
N52 . N51 . W2 . 120.7(13) yes
N52 . N51 . C51 . 107.1(18) yes
W2 . N51 . C51 . 132.2(15) yes
N51 . N52 . B2 . 118.3(18) yes
N51 . N52 . C53 . 108.6(17) yes
B2 . N52 . C53 . 132.7(19) yes
N62 . N61 . W2 . 120.4(14) yes
N62 . N61 . C61 . 107.1(20) yes
W2 . N61 . C61 . 132.4(17) yes
N61 . N62 . B2 . 119.3(18) yes
N61 . N62 . C63 . 110.4(19) yes
B2 . N62 . C63 . 130(2) yes
Cl1 . P1 . W1 . 110.2(4) yes
Cl1 . P1 . C1 . 105.2(8) yes
W1 . P1 . C1 . 50.8(7) yes
N31 . W1 . N11 . 82.6(8) yes
N31 . W1 . N21 . 82.3(7) yes
N11 . W1 . N21 . 79.9(7) yes
N31 . W1 . P1 . 104.3(6) yes
N11 . W1 . P1 . 150.3(6) yes
N21 . W1 . P1 . 129.3(5) yes
N31 . W1 . C1 . 93.5(8) yes
N11 . W1 . C1 . 165.9(8) yes
N21 . W1 . C1 . 86.1(8) yes
P1 . W1 . C1 . 43.8(6) yes
N31 . W1 . C3 . 93.3(8) yes
N11 . W1 . C3 . 84.9(10) yes
N21 . W1 . C3 . 164.6(10) yes
P1 . W1 . C3 . 66.1(9) yes
C1 . W1 . C3 . 109.0(11) yes
N31 . W1 . C4 . 169.3(10) yes
N11 . W1 . C4 . 87.8(10) yes
N21 . W1 . C4 . 91.3(9) yes
P1 . W1 . C4 . 86.4(8) yes
C1 . W1 . C4 . 94.6(10) yes
C3 . W1 . C4 . 90.6(10) yes
N51 . W2 . N61 . 83.3(7) yes
N51 . W2 . N41 . 81.3(6) yes
N61 . W2 . N41 . 83.8(7) yes
N51 . W2 . C2 . 101.2(8) yes
N61 . W2 . C2 . 102.9(9) yes
N41 . W2 . C2 . 173.0(8) yes
N51 . W2 . C5 . 176.0(10) yes
N61 . W2 . C5 . 94.4(9) yes
N41 . W2 . C5 . 95.2(10) yes
C2 . W2 . C5 . 82.6(11) yes
N51 . W2 . C6 . 94.5(10) yes
N61 . W2 . C6 . 174.2(10) yes
N41 . W2 . C6 . 90.5(9) yes
C2 . W2 . C6 . 82.8(10) yes
C5 . W2 . C6 . 87.5(11) yes
P1 . C1 . W1 . 85.3(9) yes
P1 . C1 . C2 . 122.4(15) yes
W1 . C1 . C2 . 152.1(16) yes
C1 . C2 . W2 . 171.3(17) yes
W1 . C3 . O3 . 175(3) yes
W1 . C4 . O4 . 177(3) yes
W2 . C5 . O5 . 175(3) yes
W2 . C6 . O6 . 174(3) yes
N11 . C11 . C12 . 111(2) yes
N11 . C11 . C14 . 124(2) yes
C12 . C11 . C14 . 125.4(19) yes
C11 . C12 . C13 . 107.0(18) yes
C11 . C12 . H121 . 126.4 no
C13 . C12 . H121 . 126.6 no
C12 . C13 . N12 . 108(2) yes
C12 . C13 . C15 . 129.6(19) yes
N12 . C13 . C15 . 122(2) yes
C11 . C14 . H141 . 109.6 no
C11 . C14 . H142 . 109.5 no
H141 . C14 . H142 . 109.6 no
C11 . C14 . H143 . 109.2 no
H141 . C14 . H143 . 109.4 no
H142 . C14 . H143 . 109.5 no
C13 . C15 . H151 . 109.9 no
C13 . C15 . H152 . 108.9 no
H151 . C15 . H152 . 109.5 no
C13 . C15 . H153 . 109.6 no
H151 . C15 . H153 . 109.5 no
H152 . C15 . H153 . 109.5 no
N21 . C21 . C22 . 110.7(17) yes
N21 . C21 . C24 . 121.7(16) yes
C22 . C21 . C24 . 127.5(15) yes
C21 . C22 . C23 . 106.5(16) yes
C21 . C22 . H221 . 126.5 no
C23 . C22 . H221 . 126.9 no
C22 . C23 . N22 . 106.2(19) yes
C22 . C23 . C25 . 127.8(15) yes
N22 . C23 . C25 . 126.0(18) yes
C21 . C24 . H241 . 109.2 no
C21 . C24 . H242 . 109.6 no
H241 . C24 . H242 . 109.6 no
C21 . C24 . H243 . 109.5 no
H241 . C24 . H243 . 109.4 no
H242 . C24 . H243 . 109.5 no
C23 . C25 . H251 . 109.6 no
C23 . C25 . H252 . 109.6 no
H251 . C25 . H252 . 109.2 no
C23 . C25 . H253 . 109.7 no
H251 . C25 . H253 . 109.3 no
H252 . C25 . H253 . 109.5 no
N31 . C31 . C32 . 105(2) yes
N31 . C31 . C34 . 128(2) yes
C32 . C31 . C34 . 126.8(18) yes
C31 . C32 . C33 . 108.3(18) yes
C31 . C32 . H321 . 126.1 no
C33 . C32 . H321 . 125.6 no
C32 . C33 . N32 . 106(2) yes
C32 . C33 . C35 . 130.0(18) yes
N32 . C33 . C35 . 124(2) yes
C31 . C34 . H341 . 109.4 no
C31 . C34 . H342 . 109.6 no
H341 . C34 . H342 . 109.5 no
C31 . C34 . H343 . 109.3 no
H341 . C34 . H343 . 109.5 no
H342 . C34 . H343 . 109.5 no
C33 . C35 . H351 . 109.7 no
C33 . C35 . H352 . 109.3 no
H351 . C35 . H352 . 109.4 no
C33 . C35 . H353 . 109.7 no
H351 . C35 . H353 . 109.3 no
H352 . C35 . H353 . 109.4 no
N41 . C41 . C42 . 110.1(20) yes
N41 . C41 . C44 . 121.8(20) yes
C42 . C41 . C44 . 127.9(16) yes
C41 . C42 . C43 . 107.4(17) yes
C41 . C42 . H421 . 126.4 no
C43 . C42 . H421 . 126.2 no
C42 . C43 . N42 . 108(2) yes
C42 . C43 . C45 . 129.8(17) yes
N42 . C43 . C45 . 121.6(20) yes
C41 . C44 . H441 . 109.4 no
C41 . C44 . H442 . 109.7 no
H441 . C44 . H442 . 109.4 no
C41 . C44 . H443 . 109.5 no
H441 . C44 . H443 . 109.5 no
H442 . C44 . H443 . 109.3 no
C43 . C45 . H451 . 109.2 no
C43 . C45 . H452 . 109.6 no
H451 . C45 . H452 . 109.5 no
C43 . C45 . H453 . 109.2 no
H451 . C45 . H453 . 109.6 no
H452 . C45 . H453 . 109.7 no
N51 . C51 . C52 . 110.6(18) yes
N51 . C51 . C54 . 124.1(18) yes
C52 . C51 . C54 . 125.3(15) yes
C51 . C52 . C53 . 105.3(16) yes
C51 . C52 . H521 . 127.4 no
C53 . C52 . H521 . 127.3 no
C52 . C53 . N52 . 108.4(18) yes
C52 . C53 . C55 . 128.2(16) yes
N52 . C53 . C55 . 123.4(17) yes
C51 . C54 . H541 . 109.8 no
C51 . C54 . H542 . 109.7 no
H541 . C54 . H542 . 109.3 no
C51 . C54 . H543 . 109.8 no
H541 . C54 . H543 . 109.1 no
H542 . C54 . H543 . 109.2 no
C53 . C55 . H551 . 109.9 no
C53 . C55 . H552 . 109.6 no
H551 . C55 . H552 . 109.4 no
C53 . C55 . H553 . 109.5 no
H551 . C55 . H553 . 109.3 no
H552 . C55 . H553 . 109.1 no
N61 . C61 . C62 . 107.8(20) yes
N61 . C61 . C64 . 124.5(20) yes
C62 . C61 . C64 . 127.6(16) yes
C61 . C62 . C63 . 108.1(17) yes
C61 . C62 . H621 . 125.9 no
C63 . C62 . H621 . 126.0 no
N62 . C63 . C62 . 106.4(20) yes
N62 . C63 . C65 . 124(2) yes
C62 . C63 . C65 . 130.0(18) yes
C61 . C64 . H641 . 109.9 no
C61 . C64 . H642 . 109.2 no
H641 . C64 . H642 . 109.5 no
C61 . C64 . H643 . 109.3 no
H641 . C64 . H643 . 109.5 no
H642 . C64 . H643 . 109.5 no
C63 . C65 . H651 . 109.5 no
C63 . C65 . H652 . 109.4 no
H651 . C65 . H652 . 109.6 no
C63 . C65 . H653 . 109.5 no
H651 . C65 . H653 . 109.4 no
H652 . C65 . H653 . 109.5 no
Cl3 . C101 . Cl2 . 110.2(16) yes
Cl3 . C101 . H1011 . 109.2 no
Cl2 . C101 . H1011 . 109.2 no
Cl3 . C101 . H1012 . 109.2 no
Cl2 . C101 . H1012 . 109.3 no
H1011 . C101 . H1012 . 109.7 no
Cl4 . C201 . Cl5 . 115(2) yes
Cl4 . C201 . H2011 . 108.1 no
Cl5 . C201 . H2011 . 108.3 no
Cl4 . C201 . H2012 . 108.0 no
Cl5 . C201 . H2012 . 108.1 no
H2011 . C201 . H2012 . 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
C14 . H143 . C4 . 142.00 0.959 2.494 3.30(3) yes
C24 . H242 . C1 . 141.00 0.961 2.520 3.33(3) yes
C24 . H242 . C2 . 142.00 0.961 2.467 3.28(3) yes
C44 . H441 . C21 4_565 169.7(7) 0.960 2.570 3.52(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 04/04/13 at 11:18:28
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE B   (   1,X'S) H   (   1,X'S) 
RIDE B   (   2,X'S) H   (   2,X'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   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) H   ( 443,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) H   ( 453,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) H   ( 543,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) H   ( 553,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) H   ( 642,X'S) H   ( 643,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) H   ( 653,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) H   (1012,X'S) 
RIDE C   ( 201,X'S) H   (2011,X'S) H   (2012,X'S) 
REM 
FIX C(21,U[23]) 
FIX C(21,U[12]) 
REM FIX C(21,U[22]) 
REM FIX C(21,U[11]) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 04/04/13 at 11:18:28
#
#LIST     16                                                                    
REM 
U(IJ) 0.0, 0.02 = B(1) TO N(12) 
U(IJ) 0.0, 0.02 = B(1) TO N(22) 
U(IJ) 0.0, 0.02 = B(1) TO N(32) 
U(IJ) 0.0, 0.01 = C(21) TO N(21) 
U(IJ) 0.0, 0.01 = C(21) TO C(22) 
U(IJ) 0.0, 0.02 = C(15) TO C(13) 
U(IJ) 0.0, 0.02 = C(32) TO C(33) 
U(IJ) 0.0, 0.001 = N(51) TO N(52) 
U(IJ) 0.0, 0.01 = C(51) TO C(52) 
REM 
REM NO H   NO #H U MULT DIST 
REM C-H 
REM >4           1.5    .96 DISORDER 
REM 1      1     1.2    .93 C C-H (ACETYLENE) 
REM 1      2     1.2    .93 C-C(H)-C 
REM 1      3     1.2    .98 (C)3-C-H 
REM 2      1     1.2    .93 C=C-H(2) 
REM 2      2     1.2    .97 (C)2-C-(H)2 
REM 3      1     1.5    .96 C-C-(H)3 
REM N-H 
REM >4           1.5    .89 DISORDER 
REM 1      1     1.2    .86 N-N/H 
REM 1      2     1.2    .86 (C)2-N-H 
REM 1      3     1.2    .89 (C)3-N-H 
REM 2      1     1.2    .86 C-N-(H)2 
REM 2      2     1.2    .89 (C)2-N-(H)2 
REM 3      1     1.2    .89 C-H-(H)3 
REM O-H 
REM 1      1     1.5    .82 O-H 
REM 
REM DIST      ESD = 0.02 
REM VIB       ESD = 0.002 
REM ANGLE     ESD = 2.0 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 12) TO H(121) 
REST 0.096, 0.002 = H(121,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(121) TO C ( 12) TO C(11) 
CONT H(121) TO C ( 12) TO C(13) 
PLANAR C ( 12) C(11) C(13) H(121) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 14) TO H(141) 
CONT C ( 14) TO H(142) 
CONT C ( 14) TO H(143) 
REST 0.129, 0.002 = H(141,U[ISO]) 
REST 0.129, 0.002 = H(142,U[ISO]) 
REST 0.129, 0.002 = H(143,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(11) TO C ( 14) TO H(141) 
CONT C(11) TO C ( 14) TO H(142) 
CONT C(11) TO C ( 14) TO H(143) 
ANGLE 0.0, 2.0 = MEAN H(141) TO C ( 14) TO H(142) 
CONT H(141) TO C ( 14) TO H(143) 
CONT H(142) TO C ( 14) TO H(143) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 15) TO H(151) 
CONT C ( 15) TO H(152) 
CONT C ( 15) TO H(153) 
REST 0.207, 0.002 = H(151,U[ISO]) 
REST 0.207, 0.002 = H(152,U[ISO]) 
REST 0.207, 0.002 = H(153,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(13) TO C ( 15) TO H(151) 
CONT C(13) TO C ( 15) TO H(152) 
CONT C(13) TO C ( 15) TO H(153) 
ANGLE 0.0, 2.0 = MEAN H(151) TO C ( 15) TO H(152) 
CONT H(151) TO C ( 15) TO H(153) 
CONT H(152) TO C ( 15) TO H(153) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 22) TO H(221) 
REST 0.051, 0.002 = H(221,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(221) TO C ( 22) TO C(21) 
CONT H(221) TO C ( 22) TO C(23) 
PLANAR C ( 22) C(21) C(23) H(221) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 24) TO H(241) 
CONT C ( 24) TO H(242) 
CONT C ( 24) TO H(243) 
REST 0.068, 0.002 = H(241,U[ISO]) 
REST 0.068, 0.002 = H(242,U[ISO]) 
REST 0.068, 0.002 = H(243,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(21) TO C ( 24) TO H(241) 
CONT C(21) TO C ( 24) TO H(242) 
CONT C(21) TO C ( 24) TO H(243) 
ANGLE 0.0, 2.0 = MEAN H(241) TO C ( 24) TO H(242) 
CONT H(241) TO C ( 24) TO H(243) 
CONT H(242) TO C ( 24) TO H(243) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 25) TO H(251) 
CONT C ( 25) TO H(252) 
CONT C ( 25) TO H(253) 
REST 0.083, 0.002 = H(251,U[ISO]) 
REST 0.083, 0.002 = H(252,U[ISO]) 
REST 0.083, 0.002 = H(253,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(23) TO C ( 25) TO H(251) 
CONT C(23) TO C ( 25) TO H(252) 
CONT C(23) TO C ( 25) TO H(253) 
ANGLE 0.0, 2.0 = MEAN H(251) TO C ( 25) TO H(252) 
CONT H(251) TO C ( 25) TO H(253) 
CONT H(252) TO C ( 25) TO H(253) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 32) TO H(321) 
REST 0.090, 0.002 = H(321,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(321) TO C ( 32) TO C(31) 
CONT H(321) TO C ( 32) TO C(33) 
PLANAR C ( 32) C(31) C(33) H(321) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 34) TO H(341) 
CONT C ( 34) TO H(342) 
CONT C ( 34) TO H(343) 
REST 0.096, 0.002 = H(341,U[ISO]) 
REST 0.096, 0.002 = H(342,U[ISO]) 
REST 0.096, 0.002 = H(343,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(31) TO C ( 34) TO H(341) 
CONT C(31) TO C ( 34) TO H(342) 
CONT C(31) TO C ( 34) TO H(343) 
ANGLE 0.0, 2.0 = MEAN H(341) TO C ( 34) TO H(342) 
CONT H(341) TO C ( 34) TO H(343) 
CONT H(342) TO C ( 34) TO H(343) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 35) TO H(351) 
CONT C ( 35) TO H(352) 
CONT C ( 35) TO H(353) 
REST 0.125, 0.002 = H(351,U[ISO]) 
REST 0.125, 0.002 = H(352,U[ISO]) 
REST 0.125, 0.002 = H(353,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(33) TO C ( 35) TO H(351) 
CONT C(33) TO C ( 35) TO H(352) 
CONT C(33) TO C ( 35) TO H(353) 
ANGLE 0.0, 2.0 = MEAN H(351) TO C ( 35) TO H(352) 
CONT H(351) TO C ( 35) TO H(353) 
CONT H(352) TO C ( 35) TO H(353) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 42) TO H(421) 
REST 0.063, 0.002 = H(421,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(421) TO C ( 42) TO C(41) 
CONT H(421) TO C ( 42) TO C(43) 
PLANAR C ( 42) C(41) C(43) H(421) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 44) TO H(441) 
CONT C ( 44) TO H(442) 
CONT C ( 44) TO H(443) 
REST 0.118, 0.002 = H(441,U[ISO]) 
REST 0.118, 0.002 = H(442,U[ISO]) 
REST 0.118, 0.002 = H(443,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(41) TO C ( 44) TO H(441) 
CONT C(41) TO C ( 44) TO H(442) 
CONT C(41) TO C ( 44) TO H(443) 
ANGLE 0.0, 2.0 = MEAN H(441) TO C ( 44) TO H(442) 
CONT H(441) TO C ( 44) TO H(443) 
CONT H(442) TO C ( 44) TO H(443) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 45) TO H(451) 
CONT C ( 45) TO H(452) 
CONT C ( 45) TO H(453) 
REST 0.123, 0.002 = H(451,U[ISO]) 
REST 0.123, 0.002 = H(452,U[ISO]) 
REST 0.123, 0.002 = H(453,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(43) TO C ( 45) TO H(451) 
CONT C(43) TO C ( 45) TO H(452) 
CONT C(43) TO C ( 45) TO H(453) 
ANGLE 0.0, 2.0 = MEAN H(451) TO C ( 45) TO H(452) 
CONT H(451) TO C ( 45) TO H(453) 
CONT H(452) TO C ( 45) TO H(453) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 52) TO H(521) 
REST 0.058, 0.002 = H(521,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(521) TO C ( 52) TO C(51) 
CONT H(521) TO C ( 52) TO C(53) 
PLANAR C ( 52) C(51) C(53) H(521) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 54) TO H(541) 
CONT C ( 54) TO H(542) 
CONT C ( 54) TO H(543) 
REST 0.072, 0.002 = H(541,U[ISO]) 
REST 0.072, 0.002 = H(542,U[ISO]) 
REST 0.072, 0.002 = H(543,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(51) TO C ( 54) TO H(541) 
CONT C(51) TO C ( 54) TO H(542) 
CONT C(51) TO C ( 54) TO H(543) 
ANGLE 0.0, 2.0 = MEAN H(541) TO C ( 54) TO H(542) 
CONT H(541) TO C ( 54) TO H(543) 
CONT H(542) TO C ( 54) TO H(543) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 55) TO H(551) 
CONT C ( 55) TO H(552) 
CONT C ( 55) TO H(553) 
REST 0.072, 0.002 = H(551,U[ISO]) 
REST 0.072, 0.002 = H(552,U[ISO]) 
REST 0.072, 0.002 = H(553,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(53) TO C ( 55) TO H(551) 
CONT C(53) TO C ( 55) TO H(552) 
CONT C(53) TO C ( 55) TO H(553) 
ANGLE 0.0, 2.0 = MEAN H(551) TO C ( 55) TO H(552) 
CONT H(551) TO C ( 55) TO H(553) 
CONT H(552) TO C ( 55) TO H(553) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 62) TO H(621) 
REST 0.063, 0.002 = H(621,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(621) TO C ( 62) TO C(61) 
CONT H(621) TO C ( 62) TO C(63) 
PLANAR C ( 62) C(61) C(63) H(621) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 64) TO H(641) 
CONT C ( 64) TO H(642) 
CONT C ( 64) TO H(643) 
REST 0.072, 0.002 = H(641,U[ISO]) 
REST 0.072, 0.002 = H(642,U[ISO]) 
REST 0.072, 0.002 = H(643,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(61) TO C ( 64) TO H(641) 
CONT C(61) TO C ( 64) TO H(642) 
CONT C(61) TO C ( 64) TO H(643) 
ANGLE 0.0, 2.0 = MEAN H(641) TO C ( 64) TO H(642) 
CONT H(641) TO C ( 64) TO H(643) 
CONT H(642) TO C ( 64) TO H(643) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 65) TO H(651) 
CONT C ( 65) TO H(652) 
CONT C ( 65) TO H(653) 
REST 0.119, 0.002 = H(651,U[ISO]) 
REST 0.119, 0.002 = H(652,U[ISO]) 
REST 0.119, 0.002 = H(653,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(63) TO C ( 65) TO H(651) 
CONT C(63) TO C ( 65) TO H(652) 
CONT C(63) TO C ( 65) TO H(653) 
ANGLE 0.0, 2.0 = MEAN H(651) TO C ( 65) TO H(652) 
CONT H(651) TO C ( 65) TO H(653) 
CONT H(652) TO C ( 65) TO H(653) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 101) TO H(1011) 
CONT C ( 101) TO H(1012) 
REST 0.121, 0.002 = H(1011,U[ISO]) 
REST 0.121, 0.002 = H(1012,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(1011) TO C ( 101) TO CL(3) 
CONT H(1011) TO C ( 101) TO CL(2) 
CONT H(1012) TO C ( 101) TO CL(3) 
CONT H(1012) TO C ( 101) TO CL(2) 
ANGLE 109.54, 2.0 = 
CONT H(1011) TO C ( 101) TO H(1012) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 201) TO H(2011) 
CONT C ( 201) TO H(2012) 
REST 0.143, 0.002 = H(2011,U[ISO]) 
REST 0.143, 0.002 = H(2012,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(2011) TO C ( 201) TO CL(4) 
CONT H(2011) TO C ( 201) TO CL(5) 
CONT H(2012) TO C ( 201) TO CL(4) 
CONT H(2012) TO C ( 201) TO CL(5) 
ANGLE 109.54, 2.0 = 
CONT H(2011) TO C ( 201) TO H(2012) 
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 1 4 x .
3 5 4 x .
-2 4 4 x .
-2 4 4 x .
-1 5 4 x .
-3 5 4 x .
-10 0 6 x .
-10 4 4 x .
-8 1 4 x .
5 5 4 x .
-6 5 6 x .
4 4 4 x .
-7 2 4 x .
7 0 4 x .
2 0 8 x .
1 0 4 x .
-7 0 4 x .
-7 0 6 x .
2 0 6 x .
-12 0 4 x .
9 0 4 x .
-9 2 6 x .
-6 1 4 x .
7 4 6 x .
-8 4 4 x .
-16 1 6 x .
1 4 6 x .
-13 1 4 x .
-2 6 4 x .
2 4 4 x .
2 4 4 x .
6 2 4 x .
-1 7 1 x .
-9 1 6 x .
-9 5 4 x .
-9 5 4 x .
-1 7 1 x .
-12 1 4 x .
-9 3 4 x .
-14 0 4 x .
-3 7 6 x .
-8 0 4 x .
0 9 4 x .
-10 5 4 x .


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/pentane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_ALC715F3a_scale_sq
_database_code_depnum_ccdc_archive 'CCDC 1519746'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_audit_creation_date             2016-11-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H49 B2 N12 O4 P W2'
_chemical_formula_sum            'C42 H49 B2 N12 O4 P W2'
_chemical_formula_weight         1206.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5139(4)
_cell_length_b                   21.4625(9)
_cell_length_c                   24.2130(9)
_cell_angle_alpha                66.375(4)
_cell_angle_beta                 88.740(3)
_cell_angle_gamma                84.806(3)
_cell_volume                     4984.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12680
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.9490
_cell_measurement_theta_min      1.8370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.696
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2359
_exptl_crystal_size_max          0.2357
_exptl_crystal_size_mid          0.1219
_exptl_crystal_size_min          0.0669
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41274
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.907
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.8182
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -18.00   98.00   1.0000   82.6350
omega____ theta____ kappa____ phi______ frames
    -       13.9272   77.0000 -120.0000 116

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   95.00   1.0000   82.6350
omega____ theta____ kappa____ phi______ frames
    -       13.9272   77.0000    0.0000 115

#__ type_ start__ end____ width___ exp.time_
  3 omega  -15.00   96.00   1.0000   82.6350
omega____ theta____ kappa____ phi______ frames
    -       13.9272   77.0000  120.0000 111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_orient_matrix_UB_11      -0.0409291000
_diffrn_orient_matrix_UB_12      0.0238280000
_diffrn_orient_matrix_UB_13      -0.0232177000
_diffrn_orient_matrix_UB_21      0.0414338000
_diffrn_orient_matrix_UB_22      0.0257536000
_diffrn_orient_matrix_UB_23      -0.0040619000
_diffrn_orient_matrix_UB_31      0.0346132000
_diffrn_orient_matrix_UB_32      -0.0089772000
_diffrn_orient_matrix_UB_33      -0.0216109000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14950
_reflns_number_total             20313
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.298
_refine_diff_density_min         -1.725
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1159
_refine_ls_number_reflns         20313
_refine_ls_number_restraints     429
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0228P)²+49.3460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1275
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N111, N112, C112, C113, C114, C115, C111
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N131, N132, C132, C133, C134, C135, C131
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C121, C122, N121, N122, C124, C123, C125
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N51, N52, C52, C53, C54, C51, C55
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N11, N12, C12, C13, C14, C11, C15
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N31, N32, C32, C33, C34, C31, C35
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C171, C172, C173, C174, C175, C176
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
N31 \\sim C32 \\sim N32 \\sim C34 \\sim C33 \\sim C31 \\sim C35: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
N11 \\sim N12 \\sim C12 \\sim C13 \\sim C14 \\sim C11 \\sim C15: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
N52 \\sim C52 \\sim C53 \\sim N51 \\sim C54 \\sim C51 \\sim C55: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
N131 \\sim N132 \\sim C132 \\sim C133 \\sim C134 \\sim C135 \\sim C131: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
N111 \\sim N112 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C111: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C153 \\sim C154 \\sim N152 \\sim N151 \\sim C152 \\sim C155 \\sim C151: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C171 \\sim C172 \\sim C173 \\sim C174 \\sim C175 \\sim C176: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C3) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
4. Rigid body (RIGU) restrains
 O3, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N162, N142, N152, B4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C23(H23), C33(H33), C43(H43), C53(H53), C63(H63), C72(H72),
 C73(H73), C74(H74), C75(H75), C76(H76), C113(H113), C123(H123), C133(H133),
 C143(H143), C153(H153), C163(H163), C172(H172), C173(H173), C174(H174),
 C175(H175), C176(H176)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C45(H45A,
 H45B,H45C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C61(H61A,H61B,H61C),
 C65(H65A,H65B,H65C), C111(H11D,H11E,H11F), C115(H11G,H11H,H11I), C121(H12A,
 H12B,H12C), C125(H12D,H12E,H12F), C131(H13A,H13B,H13C), C135(H13D,H13E,H13F),
 C141(H14A,H14B,H14C), C145(H14D,H14E,H14F), C151(H15D,H15E,H15F), C155(H15G,
 H15H,H15I), C161(H16A,H16B,H16C), C165(H16D,H16E,H16F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.23981(4) 1.02125(2) 0.36512(2) 0.02180(10) Uani 1 1 d . . . . .
W2 W 0.24710(4) 0.91977(2) 0.17502(2) 0.02080(10) Uani 1 1 d . . . . .
W3 W 0.25161(4) 0.54125(2) 0.11514(2) 0.01983(10) Uani 1 1 d . . . . .
W4 W 0.27918(4) 0.43350(2) 0.37701(2) 0.01947(10) Uani 1 1 d . . . . .
P1 P 0.0461(2) 0.95960(13) 0.28006(12) 0.0210(5) Uani 1 1 d . . . . .
P2 P 0.4669(2) 0.48387(13) 0.24324(11) 0.0207(5) Uani 1 1 d . . . . .
N11 N 0.3527(7) 1.0628(4) 0.4221(3) 0.0219(16) Uani 1 1 d . U . . .
N12 N 0.4500(7) 1.1023(4) 0.3950(4) 0.0216(16) Uani 1 1 d . U . . .
N21 N 0.4365(8) 0.9968(4) 0.3405(4) 0.027(2) Uani 1 1 d . . . . .
N22 N 0.5261(7) 1.0439(4) 0.3277(4) 0.0220(18) Uani 1 1 d . . . . .
N31 N 0.2610(7) 1.1240(4) 0.2969(3) 0.0225(16) Uani 1 1 d . U . . .
N32 N 0.3774(7) 1.1509(4) 0.2867(3) 0.0215(16) Uani 1 1 d . U . . .
N41 N 0.3374(7) 0.9133(4) 0.0902(4) 0.0235(19) Uani 1 1 d . . . . .
N42 N 0.4672(7) 0.8972(4) 0.0898(4) 0.0234(19) Uani 1 1 d . . . . .
N51 N 0.3795(8) 0.8265(4) 0.2212(3) 0.0222(16) Uani 1 1 d . U . . .
N52 N 0.5024(8) 0.8222(4) 0.2003(4) 0.0258(17) Uani 1 1 d . U . . .
N61 N 0.4192(7) 0.9742(4) 0.1685(4) 0.0219(18) Uani 1 1 d . . . . .
N62 N 0.5387(7) 0.9448(4) 0.1627(3) 0.0223(18) Uani 1 1 d . . . . .
N111 N 0.1305(8) 0.5763(4) 0.0272(4) 0.0261(17) Uani 1 1 d . U . . .
N112 N 0.0250(7) 0.6204(4) 0.0210(3) 0.0242(17) Uani 1 1 d . U . . .
N121 N 0.0599(7) 0.5265(4) 0.1530(3) 0.0212(16) Uani 1 1 d . U . . .
N122 N -0.0410(7) 0.5755(4) 0.1285(4) 0.0213(16) Uani 1 1 d . U . . .
N131 N 0.2027(7) 0.6472(4) 0.1053(3) 0.0188(16) Uani 1 1 d . U . . .
N132 N 0.0813(7) 0.6795(4) 0.0862(3) 0.0191(16) Uani 1 1 d . U . . .
N141 N 0.1910(8) 0.4169(4) 0.4682(3) 0.0236(19) Uani 1 1 d . . . . .
N142 N 0.0604(7) 0.4105(4) 0.4753(4) 0.0231(16) Uani 1 1 d . U . . .
N151 N 0.0972(7) 0.4955(4) 0.3446(3) 0.0181(17) Uani 1 1 d . U . . .
N152 N -0.0181(7) 0.4710(4) 0.3676(4) 0.0229(16) Uani 1 1 d . U . . .
N161 N 0.1622(7) 0.3488(4) 0.3863(4) 0.0217(18) Uani 1 1 d . . . . .
N162 N 0.0428(7) 0.3457(4) 0.4099(3) 0.0226(16) Uani 1 1 d . U . . .
O2 O -0.0174(8) 1.0697(5) 0.4099(4) 0.056(2) Uani 1 1 d . . . . .
O3 O 0.2235(10) 0.8770(5) 0.4702(4) 0.078(4) Uani 1 1 d . U . . .
O5 O 0.0723(8) 1.0506(4) 0.0954(4) 0.048(2) Uani 1 1 d . . . . .
O6 O 0.0115(7) 0.8415(4) 0.1711(4) 0.046(2) Uani 1 1 d . . . . .
O102 O 0.5012(7) 0.5751(4) 0.0368(4) 0.046(2) Uani 1 1 d . . . . .
O103 O 0.3022(8) 0.3922(4) 0.1212(4) 0.047(2) Uani 1 1 d . . . . .
O105 O 0.5245(8) 0.3384(5) 0.4415(4) 0.054(2) Uani 1 1 d . . . . .
O106 O 0.4259(8) 0.5552(4) 0.3761(4) 0.047(2) Uani 1 1 d . . . . .
C1 C 0.1464(9) 0.9863(5) 0.3231(4) 0.020(2) Uani 1 1 d . . . . .
C2 C 0.0773(11) 1.0527(6) 0.3933(5) 0.034(3) Uani 1 1 d . . . . .
C3 C 0.2365(11) 0.9299(5) 0.4311(5) 0.039(3) Uani 1 1 d . U . . .
C4 C 0.1603(9) 0.9308(5) 0.2366(5) 0.024(2) Uani 1 1 d . . . . .
C5 C 0.1385(10) 1.0039(6) 0.1231(5) 0.029(2) Uani 1 1 d . . . . .
C6 C 0.1001(10) 0.8689(6) 0.1714(5) 0.028(2) Uani 1 1 d . . . . .
C11 C 0.2489(11) 1.0239(6) 0.5211(5) 0.043(3) Uani 1 1 d . U . . .
H11A H 0.1644 1.0443 0.5069 0.065 Uiso 1 1 calc GR . . . .
H11B H 0.2642 1.0253 0.5596 0.065 Uiso 1 1 calc GR . . . .
H11C H 0.2566 0.9774 0.5252 0.065 Uiso 1 1 calc GR . . . .
C12 C 0.3428(10) 1.0618(5) 0.4779(4) 0.026(2) Uani 1 1 d . U . . .
C13 C 0.4323(10) 1.1013(5) 0.4857(5) 0.032(2) Uani 1 1 d . U . . .
H13 H 0.4456 1.1094 0.5200 0.039 Uiso 1 1 calc R . . . .
C14 C 0.4966(9) 1.1259(5) 0.4332(4) 0.0238(19) Uani 1 1 d . U . . .
C15 C 0.6019(10) 1.1729(5) 0.4159(5) 0.032(2) Uani 1 1 d . U . . .
H15A H 0.6807 1.1480 0.4132 0.048 Uiso 1 1 calc GR . . . .
H15B H 0.6107 1.1910 0.4459 0.048 Uiso 1 1 calc GR . . . .
H15C H 0.5817 1.2097 0.3776 0.048 Uiso 1 1 calc GR . . . .
C21 C 0.4313(11) 0.8778(6) 0.3484(6) 0.045(3) Uani 1 1 d . . . . .
H21A H 0.4185 0.8536 0.3908 0.067 Uiso 1 1 calc GR . . . .
H21B H 0.4822 0.8488 0.3333 0.067 Uiso 1 1 calc GR . . . .
H21C H 0.3501 0.8912 0.3277 0.067 Uiso 1 1 calc GR . . . .
C22 C 0.4988(10) 0.9403(5) 0.3379(4) 0.027(2) Uani 1 1 d . . . . .
C23 C 0.6241(10) 0.9510(6) 0.3244(5) 0.033(3) Uani 1 1 d . . . . .
H23 H 0.6869 0.9199 0.3201 0.040 Uiso 1 1 calc R . . . .
C24 C 0.6400(9) 1.0163(6) 0.3183(5) 0.031(3) Uani 1 1 d . . . . .
C25 C 0.7540(10) 1.0559(6) 0.3007(5) 0.045(3) Uani 1 1 d . . . . .
H25A H 0.7327 1.0979 0.2665 0.067 Uiso 1 1 calc GR . . . .
H25B H 0.8221 1.0297 0.2905 0.067 Uiso 1 1 calc GR . . . .
H25C H 0.7807 1.0658 0.3338 0.067 Uiso 1 1 calc GR . . . .
C31 C 0.0399(10) 1.1614(6) 0.2520(5) 0.041(3) Uani 1 1 d . U . . .
H31A H 0.0332 1.1205 0.2456 0.061 Uiso 1 1 calc GR . . . .
H31B H -0.0006 1.1997 0.2190 0.061 Uiso 1 1 calc GR . . . .
H31C H -0.0013 1.1575 0.2889 0.061 Uiso 1 1 calc GR . . . .
C32 C 0.1791(9) 1.1717(5) 0.2560(4) 0.0241(19) Uani 1 1 d . U . . .
C33 C 0.2428(10) 1.2271(5) 0.2205(4) 0.0266(19) Uani 1 1 d . U . . .
H33 H 0.2081 1.2664 0.1890 0.032 Uiso 1 1 calc R . . . .
C34 C 0.3676(10) 1.2130(5) 0.2406(4) 0.0247(19) Uani 1 1 d . U . . .
C35 C 0.4798(10) 1.2548(5) 0.2191(5) 0.035(3) Uani 1 1 d . U . . .
H35A H 0.5067 1.2682 0.2501 0.052 Uiso 1 1 calc GR . . . .
H35B H 0.4556 1.2948 0.1836 0.052 Uiso 1 1 calc GR . . . .
H35C H 0.5488 1.2281 0.2100 0.052 Uiso 1 1 calc GR . . . .
C41 C 0.1578(10) 0.9474(6) 0.0157(5) 0.037(3) Uani 1 1 d . . . . .
H41A H 0.1059 0.9308 0.0509 0.055 Uiso 1 1 calc GR . . . .
H41B H 0.1357 0.9278 -0.0117 0.055 Uiso 1 1 calc GR . . . .
H41C H 0.1432 0.9962 -0.0035 0.055 Uiso 1 1 calc GR . . . .
C42 C 0.2953(10) 0.9278(5) 0.0337(4) 0.025(2) Uani 1 1 d . . . . .
C43 C 0.3972(10) 0.9211(5) -0.0023(5) 0.032(3) Uani 1 1 d . . . . .
H43 H 0.3934 0.9274 -0.0426 0.039 Uiso 1 1 calc R . . . .
C44 C 0.5037(10) 0.9034(5) 0.0342(5) 0.028(2) Uani 1 1 d . . . . .
C45 C 0.6391(10) 0.8903(6) 0.0184(5) 0.042(3) Uani 1 1 d . . . . .
H45A H 0.6928 0.9171 0.0298 0.063 Uiso 1 1 calc GR . . . .
H45B H 0.6446 0.9025 -0.0243 0.063 Uiso 1 1 calc GR . . . .
H45C H 0.6667 0.8427 0.0395 0.063 Uiso 1 1 calc GR . . . .
C51 C 0.2437(11) 0.7547(5) 0.3021(5) 0.039(3) Uani 1 1 d . U . . .
H51A H 0.2238 0.7893 0.3174 0.059 Uiso 1 1 calc GR . . . .
H51B H 0.2527 0.7107 0.3351 0.059 Uiso 1 1 calc GR . . . .
H51C H 0.1760 0.7560 0.2756 0.059 Uiso 1 1 calc GR . . . .
C52 C 0.3644(11) 0.7672(5) 0.2687(5) 0.034(2) Uani 1 1 d . U . . .
C53 C 0.4764(11) 0.7260(5) 0.2784(5) 0.039(3) Uani 1 1 d . U . . .
H53 H 0.4920 0.6824 0.3086 0.047 Uiso 1 1 calc R . . . .
C54 C 0.5613(11) 0.7604(5) 0.2356(5) 0.036(2) Uani 1 1 d . U . . .
C55 C 0.6977(12) 0.7397(7) 0.2251(6) 0.061(4) Uani 1 1 d . U . . .
H55A H 0.7031 0.7360 0.1868 0.092 Uiso 1 1 calc GR . . . .
H55B H 0.7253 0.6964 0.2566 0.092 Uiso 1 1 calc GR . . . .
H55C H 0.7515 0.7735 0.2252 0.092 Uiso 1 1 calc GR . . . .
C61 C 0.3285(10) 1.0794(6) 0.1800(5) 0.036(3) Uani 1 1 d . . . . .
H61A H 0.2803 1.1005 0.1429 0.053 Uiso 1 1 calc GR . . . .
H61B H 0.3616 1.1140 0.1898 0.053 Uiso 1 1 calc GR . . . .
H61C H 0.2739 1.0535 0.2117 0.053 Uiso 1 1 calc GR . . . .
C62 C 0.4366(10) 1.0328(5) 0.1733(4) 0.028(2) Uani 1 1 d . . . . .
C63 C 0.5664(10) 1.0421(5) 0.1701(4) 0.030(2) Uani 1 1 d . . . . .
H63 H 0.6041 1.0787 0.1721 0.036 Uiso 1 1 calc R . . . .
C64 C 0.6268(10) 0.9868(6) 0.1635(4) 0.029(2) Uani 1 1 d . . . . .
C65 C 0.7666(10) 0.9693(7) 0.1596(6) 0.046(3) Uani 1 1 d . . . . .
H65A H 0.7941 0.9291 0.1945 0.069 Uiso 1 1 calc GR . . . .
H65B H 0.8127 1.0066 0.1580 0.069 Uiso 1 1 calc GR . . . .
H65C H 0.7828 0.9608 0.1240 0.069 Uiso 1 1 calc GR . . . .
C71 C -0.0221(8) 0.8836(5) 0.3361(4) 0.021(2) Uani 1 1 d . . . . .
C72 C -0.0494(10) 0.8800(5) 0.3937(4) 0.030(2) Uani 1 1 d . . . . .
H72 H -0.0258 0.9138 0.4053 0.036 Uiso 1 1 calc R . . . .
C73 C -0.1115(10) 0.8264(6) 0.4338(5) 0.037(3) Uani 1 1 d . . . . .
H73 H -0.1309 0.8246 0.4721 0.044 Uiso 1 1 calc R . . . .
C74 C -0.1451(11) 0.7751(6) 0.4174(6) 0.045(3) Uani 1 1 d . . . . .
H74 H -0.1830 0.7379 0.4451 0.053 Uiso 1 1 calc R . . . .
C75 C -0.1220(11) 0.7796(6) 0.3598(6) 0.041(3) Uani 1 1 d . . . . .
H75 H -0.1480 0.7462 0.3483 0.050 Uiso 1 1 calc R . . . .
C76 C -0.0605(10) 0.8333(5) 0.3187(5) 0.034(3) Uani 1 1 d . . . . .
H76 H -0.0449 0.8359 0.2799 0.040 Uiso 1 1 calc R . . . .
C101 C 0.3552(10) 0.5089(4) 0.1818(4) 0.022(2) Uani 1 1 d . . . . .
C102 C 0.4093(10) 0.5647(5) 0.0647(5) 0.028(2) Uani 1 1 d . . . . .
C103 C 0.2812(9) 0.4481(6) 0.1182(5) 0.033(3) Uani 1 1 d . . . . .
C104 C 0.3669(8) 0.4494(5) 0.3071(4) 0.020(2) Uani 1 1 d . . . . .
C105 C 0.4339(10) 0.3723(5) 0.4182(5) 0.030(2) Uani 1 1 d . . . . .
C106 C 0.3701(10) 0.5109(5) 0.3765(4) 0.027(2) Uani 1 1 d . . . . .
C111 C 0.2388(12) 0.5135(6) -0.0297(5) 0.043(3) Uani 1 1 d . U . . .
H11D H 0.3208 0.5304 -0.0310 0.065 Uiso 1 1 calc GR . . . .
H11E H 0.2236 0.5086 -0.0667 0.065 Uiso 1 1 calc GR . . . .
H11F H 0.2374 0.4699 0.0035 0.065 Uiso 1 1 calc GR . . . .
C112 C 0.1382(11) 0.5621(5) -0.0220(5) 0.032(2) Uani 1 1 d . U . . .
C113 C 0.0346(11) 0.5993(6) -0.0608(5) 0.039(2) Uani 1 1 d . U . . .
H113 H 0.0161 0.5995 -0.0982 0.047 Uiso 1 1 calc R . . . .
C114 C -0.0330(10) 0.6350(6) -0.0323(5) 0.034(2) Uani 1 1 d . U . . .
C115 C -0.1529(13) 0.6825(7) -0.0529(6) 0.063(4) Uani 1 1 d . U . . .
H11G H -0.2153 0.6690 -0.0217 0.095 Uiso 1 1 calc GR . . . .
H11H H -0.1862 0.6803 -0.0886 0.095 Uiso 1 1 calc GR . . . .
H11I H -0.1339 0.7283 -0.0614 0.095 Uiso 1 1 calc GR . . . .
C121 C 0.0889(10) 0.4094(5) 0.2354(5) 0.033(2) Uani 1 1 d . U . . .
H12A H 0.1135 0.3834 0.2119 0.049 Uiso 1 1 calc GR . . . .
H12B H 0.0394 0.3828 0.2690 0.049 Uiso 1 1 calc GR . . . .
H12C H 0.1639 0.4208 0.2499 0.049 Uiso 1 1 calc GR . . . .
C122 C 0.0110(9) 0.4731(5) 0.1972(4) 0.024(2) Uani 1 1 d . U . . .
C123 C -0.1207(10) 0.4888(6) 0.1997(5) 0.029(2) Uani 1 1 d . U . . .
H123 H -0.1777 0.4608 0.2258 0.035 Uiso 1 1 calc R . . . .
C124 C -0.1494(9) 0.5524(5) 0.1569(5) 0.027(2) Uani 1 1 d . U . . .
C125 C -0.2737(9) 0.5941(6) 0.1402(5) 0.039(3) Uani 1 1 d . U . . .
H12D H -0.2645 0.6389 0.1386 0.058 Uiso 1 1 calc GR . . . .
H12E H -0.3360 0.5728 0.1698 0.058 Uiso 1 1 calc GR . . . .
H12F H -0.3012 0.5977 0.1014 0.058 Uiso 1 1 calc GR . . . .
C131 C 0.4063(9) 0.6800(5) 0.1327(5) 0.032(2) Uani 1 1 d . U . . .
H13A H 0.4128 0.6453 0.1730 0.048 Uiso 1 1 calc GR . . . .
H13B H 0.4379 0.7208 0.1321 0.048 Uiso 1 1 calc GR . . . .
H13C H 0.4559 0.6644 0.1062 0.048 Uiso 1 1 calc GR . . . .
C132 C 0.2700(9) 0.6947(5) 0.1123(4) 0.0229(19) Uani 1 1 d . U . . .
C133 C 0.1927(9) 0.7539(5) 0.1002(5) 0.027(2) Uani 1 1 d . U . . .
H133 H 0.2157 0.7934 0.1030 0.032 Uiso 1 1 calc R . . . .
C134 C 0.0739(9) 0.7437(5) 0.0830(5) 0.024(2) Uani 1 1 d . U . . .
C135 C -0.0454(10) 0.7905(5) 0.0643(5) 0.036(3) Uani 1 1 d . U . . .
H13D H -0.0739 0.7940 0.0257 0.054 Uiso 1 1 calc GR . . . .
H13E H -0.0288 0.8349 0.0616 0.054 Uiso 1 1 calc GR . . . .
H13F H -0.1103 0.7729 0.0936 0.054 Uiso 1 1 calc GR . . . .
C141 C 0.3707(11) 0.4200(7) 0.5305(6) 0.047(3) Uani 1 1 d . . . . .
H14A H 0.4211 0.3844 0.5233 0.071 Uiso 1 1 calc GR . . . .
H14B H 0.3843 0.4147 0.5712 0.071 Uiso 1 1 calc GR . . . .
H14C H 0.3956 0.4636 0.5032 0.071 Uiso 1 1 calc GR . . . .
C142 C 0.2322(10) 0.4157(5) 0.5205(5) 0.029(2) Uani 1 1 d . . . . .
C143 C 0.1335(11) 0.4090(5) 0.5604(5) 0.036(3) Uani 1 1 d . . . . .
H143 H 0.1385 0.4072 0.5993 0.043 Uiso 1 1 calc R . . . .
C144 C 0.0268(10) 0.4055(5) 0.5308(4) 0.029(2) Uani 1 1 d . . . . .
C145 C -0.1082(12) 0.3989(6) 0.5517(5) 0.048(3) Uani 1 1 d . . . . .
H14D H -0.1621 0.4372 0.5249 0.072 Uiso 1 1 calc GR . . . .
H14E H -0.1131 0.3978 0.5917 0.072 Uiso 1 1 calc GR . . . .
H14F H -0.1361 0.3574 0.5519 0.072 Uiso 1 1 calc GR . . . .
C151 C 0.1674(10) 0.6003(5) 0.2611(4) 0.029(2) Uani 1 1 d . U . . .
H15D H 0.2163 0.6148 0.2861 0.044 Uiso 1 1 calc GR . . . .
H15E H 0.1268 0.6395 0.2290 0.044 Uiso 1 1 calc GR . . . .
H15F H 0.2230 0.5744 0.2445 0.044 Uiso 1 1 calc GR . . . .
C152 C 0.0686(9) 0.5570(5) 0.2978(4) 0.022(2) Uani 1 1 d . U . . .
C153 C -0.0628(9) 0.5703(5) 0.2912(4) 0.027(2) Uani 1 1 d . U . . .
H153 H -0.1073 0.6085 0.2624 0.033 Uiso 1 1 calc R . . . .
C154 C -0.1144(9) 0.5161(6) 0.3352(5) 0.029(2) Uani 1 1 d . U . . .
C155 C -0.2531(10) 0.5032(7) 0.3468(6) 0.048(3) Uani 1 1 d . U . . .
H15G H -0.2698 0.4641 0.3392 0.071 Uiso 1 1 calc GR . . . .
H15H H -0.3058 0.5424 0.3206 0.071 Uiso 1 1 calc GR . . . .
H15I H -0.2719 0.4949 0.3880 0.071 Uiso 1 1 calc GR . . . .
C161 C 0.3116(11) 0.2780(6) 0.3494(6) 0.044(3) Uani 1 1 d . . . . .
H16A H 0.3185 0.3120 0.3092 0.066 Uiso 1 1 calc GR . . . .
H16B H 0.3134 0.2337 0.3484 0.066 Uiso 1 1 calc GR . . . .
H16C H 0.3818 0.2789 0.3737 0.066 Uiso 1 1 calc GR . . . .
C162 C 0.1893(10) 0.2928(5) 0.3758(5) 0.028(2) Uani 1 1 d . . . . .
C163 C 0.0849(11) 0.2531(5) 0.3927(5) 0.036(3) Uani 1 1 d . . . . .
H163 H 0.0779 0.2117 0.3896 0.043 Uiso 1 1 calc R . . . .
C164 C -0.0045(10) 0.2874(5) 0.4146(4) 0.028(2) Uani 1 1 d . . . . .
C165 C -0.1320(11) 0.2676(6) 0.4414(5) 0.044(3) Uani 1 1 d . . . . .
H16D H -0.1301 0.2596 0.4834 0.067 Uiso 1 1 calc GR . . . .
H16E H -0.1510 0.2267 0.4374 0.067 Uiso 1 1 calc GR . . . .
H16F H -0.1965 0.3038 0.4208 0.067 Uiso 1 1 calc GR . . . .
C171 C 0.5728(9) 0.4133(5) 0.2390(4) 0.0195(18) Uani 1 1 d . U . . .
C172 C 0.6054(9) 0.4123(5) 0.1822(4) 0.0229(19) Uani 1 1 d . U . . .
H172 H 0.5630 0.4434 0.1475 0.028 Uiso 1 1 calc R . . . .
C173 C 0.7011(9) 0.3647(5) 0.1782(5) 0.029(2) Uani 1 1 d . U . . .
H173 H 0.7219 0.3633 0.1412 0.035 Uiso 1 1 calc R . . . .
C174 C 0.7632(10) 0.3203(5) 0.2296(5) 0.032(2) Uani 1 1 d . U . . .
H174 H 0.8281 0.2894 0.2268 0.039 Uiso 1 1 calc R . . . .
C175 C 0.7338(10) 0.3196(5) 0.2855(5) 0.032(2) Uani 1 1 d . U . . .
H175 H 0.7774 0.2883 0.3198 0.038 Uiso 1 1 calc R . . . .
C176 C 0.6373(10) 0.3665(5) 0.2901(5) 0.030(2) Uani 1 1 d . U . . .
H176 H 0.6164 0.3662 0.3277 0.036 Uiso 1 1 calc R . . . .
B1 B 0.4906(11) 1.1131(6) 0.3298(5) 0.022(2) Uani 1 1 d . . . . .
H1 H 0.5641 1.1404 0.3184 0.026 Uiso 1 1 calc R . . . .
B2 B 0.5508(11) 0.8820(6) 0.1471(5) 0.026(3) Uani 1 1 d . . . . .
H2 H 0.6403 0.8710 0.1396 0.031 Uiso 1 1 calc R . . . .
B3 B -0.0193(11) 0.6402(6) 0.0728(5) 0.021(2) Uani 1 1 d . . . . .
H3 H -0.0997 0.6694 0.0611 0.026 Uiso 1 1 calc R . . . .
B4 B -0.0201(11) 0.4049(6) 0.4254(5) 0.0233(16) Uani 1 1 d . U . . .
H4 H -0.1080 0.3966 0.4387 0.028 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 N11 2.314(8) . ?
W1 N21 2.216(8) . ?
W1 N31 2.189(8) . ?
W1 C1 1.830(9) . ?
W1 C2 1.987(12) . ?
W1 C3 1.974(10) . ?
W2 N41 2.293(8) . ?
W2 N51 2.228(8) . ?
W2 N61 2.212(8) . ?
W2 C4 1.816(10) . ?
W2 C5 2.003(11) . ?
W2 C6 1.993(11) . ?
W3 N111 2.320(8) . ?
W3 N121 2.192(8) . ?
W3 N131 2.204(7) . ?
W3 C101 1.821(10) . ?
W3 C102 2.016(11) . ?
W3 C103 1.967(12) . ?
W4 N141 2.282(7) . ?
W4 N151 2.194(8) . ?
W4 N161 2.222(8) . ?
W4 C104 1.832(10) . ?
W4 C105 2.000(11) . ?
W4 C106 1.986(11) . ?
P1 C1 1.779(10) . ?
P1 C4 1.805(11) . ?
P1 C71 1.847(10) . ?
P2 C101 1.789(10) . ?
P2 C104 1.788(10) . ?
P2 C171 1.832(10) . ?
N11 N12 1.371(10) . ?
N11 C12 1.346(12) . ?
N12 C14 1.338(11) . ?
N12 B1 1.557(13) . ?
N21 N22 1.384(11) . ?
N21 C22 1.348(12) . ?
N22 C24 1.343(12) . ?
N22 B1 1.519(13) . ?
N31 N32 1.376(10) . ?
N31 C32 1.355(12) . ?
N32 C34 1.349(12) . ?
N32 B1 1.537(13) . ?
N41 N42 1.379(11) . ?
N41 C42 1.351(12) . ?
N42 C44 1.350(12) . ?
N42 B2 1.563(14) . ?
N51 N52 1.386(11) . ?
N51 C52 1.350(12) . ?
N52 C54 1.358(12) . ?
N52 B2 1.525(14) . ?
N61 N62 1.384(11) . ?
N61 C62 1.336(12) . ?
N62 C64 1.355(12) . ?
N62 B2 1.535(14) . ?
N111 N112 1.361(11) . ?
N111 C112 1.343(12) . ?
N112 C114 1.346(12) . ?
N112 B3 1.529(13) . ?
N121 N122 1.381(10) . ?
N121 C122 1.351(12) . ?
N122 C124 1.346(12) . ?
N122 B3 1.531(13) . ?
N131 N132 1.390(10) . ?
N131 C132 1.355(11) . ?
N132 C134 1.346(12) . ?
N132 B3 1.526(13) . ?
N141 N142 1.393(11) . ?
N141 C142 1.336(12) . ?
N142 C144 1.348(12) . ?
N142 B4 1.537(13) . ?
N151 N152 1.381(10) . ?
N151 C152 1.364(11) . ?
N152 C154 1.352(12) . ?
N152 B4 1.544(14) . ?
N161 N162 1.363(10) . ?
N161 C162 1.330(12) . ?
N162 C164 1.351(12) . ?
N162 B4 1.554(13) . ?
O2 C2 1.149(13) . ?
O3 C3 1.168(12) . ?
O5 C5 1.139(12) . ?
O6 C6 1.148(12) . ?
O102 C102 1.152(12) . ?
O103 C103 1.172(12) . ?
O105 C105 1.151(12) . ?
O106 C106 1.158(12) . ?
C11 C12 1.466(14) . ?
C12 C13 1.385(14) . ?
C13 C14 1.356(14) . ?
C14 C15 1.505(13) . ?
C21 C22 1.503(14) . ?
C22 C23 1.368(15) . ?
C23 C24 1.374(15) . ?
C24 C25 1.488(15) . ?
C31 C32 1.510(14) . ?
C32 C33 1.379(13) . ?
C33 C34 1.375(14) . ?
C34 C35 1.504(14) . ?
C41 C42 1.493(14) . ?
C42 C43 1.400(14) . ?
C43 C44 1.370(14) . ?
C44 C45 1.498(14) . ?
C51 C52 1.477(15) . ?
C52 C53 1.372(15) . ?
C53 C54 1.371(15) . ?
C54 C55 1.510(16) . ?
C61 C62 1.494(15) . ?
C62 C63 1.393(14) . ?
C63 C64 1.359(15) . ?
C64 C65 1.494(15) . ?
C71 C72 1.391(13) . ?
C71 C76 1.399(13) . ?
C72 C73 1.380(14) . ?
C73 C74 1.386(16) . ?
C74 C75 1.377(16) . ?
C75 C76 1.388(15) . ?
C111 C112 1.480(15) . ?
C112 C113 1.411(15) . ?
C113 C114 1.368(14) . ?
C114 C115 1.505(15) . ?
C121 C122 1.488(14) . ?
C122 C123 1.401(14) . ?
C123 C124 1.353(14) . ?
C124 C125 1.481(14) . ?
C131 C132 1.491(13) . ?
C132 C133 1.375(13) . ?
C133 C134 1.388(13) . ?
C134 C135 1.489(13) . ?
C141 C142 1.499(14) . ?
C142 C143 1.378(14) . ?
C143 C144 1.366(15) . ?
C144 C145 1.496(15) . ?
C151 C152 1.485(13) . ?
C152 C153 1.384(13) . ?
C153 C154 1.371(14) . ?
C154 C155 1.508(15) . ?
C161 C162 1.487(15) . ?
C162 C163 1.403(15) . ?
C163 C164 1.369(15) . ?
C164 C165 1.497(15) . ?
C171 C172 1.419(13) . ?
C171 C176 1.384(13) . ?
C172 C173 1.398(14) . ?
C173 C174 1.361(14) . ?
C174 C175 1.376(15) . ?
C175 C176 1.398(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N21 W1 N11 80.8(3) . . ?
N31 W1 N11 80.9(3) . . ?
N31 W1 N21 84.9(3) . . ?
C1 W1 N11 177.4(3) . . ?
C1 W1 N21 100.8(4) . . ?
C1 W1 N31 101.2(3) . . ?
C1 W1 C2 88.8(4) . . ?
C1 W1 C3 84.6(4) . . ?
C2 W1 N11 89.6(3) . . ?
C2 W1 N21 170.2(4) . . ?
C2 W1 N31 91.7(4) . . ?
C3 W1 N11 93.4(4) . . ?
C3 W1 N21 92.0(4) . . ?
C3 W1 N31 173.9(3) . . ?
C3 W1 C2 90.6(5) . . ?
N51 W2 N41 82.6(3) . . ?
N61 W2 N41 79.6(3) . . ?
N61 W2 N51 84.0(3) . . ?
C4 W2 N41 173.4(4) . . ?
C4 W2 N51 103.6(4) . . ?
C4 W2 N61 103.2(3) . . ?
C4 W2 C5 84.2(4) . . ?
C4 W2 C6 84.2(4) . . ?
C5 W2 N41 89.7(4) . . ?
C5 W2 N51 172.2(4) . . ?
C5 W2 N61 94.3(4) . . ?
C6 W2 N41 93.0(3) . . ?
C6 W2 N51 94.9(4) . . ?
C6 W2 N61 172.6(3) . . ?
C6 W2 C5 85.7(4) . . ?
N121 W3 N111 79.9(3) . . ?
N121 W3 N131 83.3(3) . . ?
N131 W3 N111 83.3(3) . . ?
C101 W3 N111 175.1(3) . . ?
C101 W3 N121 103.2(4) . . ?
C101 W3 N131 100.8(3) . . ?
C101 W3 C102 88.1(4) . . ?
C101 W3 C103 84.7(4) . . ?
C102 W3 N111 89.0(4) . . ?
C102 W3 N121 168.6(3) . . ?
C102 W3 N131 93.3(3) . . ?
C103 W3 N111 91.2(4) . . ?
C103 W3 N121 94.1(4) . . ?
C103 W3 N131 174.3(3) . . ?
C103 W3 C102 88.3(4) . . ?
N151 W4 N141 81.6(3) . . ?
N151 W4 N161 82.6(3) . . ?
N161 W4 N141 81.3(3) . . ?
C104 W4 N141 173.2(3) . . ?
C104 W4 N151 102.7(3) . . ?
C104 W4 N161 104.4(3) . . ?
C104 W4 C105 85.5(4) . . ?
C104 W4 C106 82.5(4) . . ?
C105 W4 N141 90.3(4) . . ?
C105 W4 N151 171.8(4) . . ?
C105 W4 N161 94.8(4) . . ?
C106 W4 N141 91.9(3) . . ?
C106 W4 N151 94.3(3) . . ?
C106 W4 N161 172.8(4) . . ?
C106 W4 C105 87.4(4) . . ?
C1 P1 C4 102.2(4) . . ?
C1 P1 C71 104.5(4) . . ?
C4 P1 C71 107.7(4) . . ?
C101 P2 C171 106.1(4) . . ?
C104 P2 C101 102.1(4) . . ?
C104 P2 C171 107.9(4) . . ?
N12 N11 W1 118.0(5) . . ?
C12 N11 W1 135.4(7) . . ?
C12 N11 N12 106.4(8) . . ?
N11 N12 B1 120.4(7) . . ?
C14 N12 N11 109.3(8) . . ?
C14 N12 B1 130.3(8) . . ?
N22 N21 W1 120.2(6) . . ?
C22 N21 W1 133.7(7) . . ?
C22 N21 N22 106.0(8) . . ?
N21 N22 B1 120.5(8) . . ?
C24 N22 N21 109.7(8) . . ?
C24 N22 B1 129.7(9) . . ?
N32 N31 W1 121.3(6) . . ?
C32 N31 W1 133.0(6) . . ?
C32 N31 N32 105.6(8) . . ?
N31 N32 B1 119.7(8) . . ?
C34 N32 N31 110.2(8) . . ?
C34 N32 B1 129.8(8) . . ?
N42 N41 W2 119.1(6) . . ?
C42 N41 W2 135.0(7) . . ?
C42 N41 N42 105.5(8) . . ?
N41 N42 B2 120.2(8) . . ?
C44 N42 N41 110.1(8) . . ?
C44 N42 B2 129.5(9) . . ?
N52 N51 W2 120.2(6) . . ?
C52 N51 W2 132.2(7) . . ?
C52 N51 N52 107.6(8) . . ?
N51 N52 B2 120.8(7) . . ?
C54 N52 N51 108.1(8) . . ?
C54 N52 B2 131.1(9) . . ?
N62 N61 W2 120.4(6) . . ?
C62 N61 W2 132.2(7) . . ?
C62 N61 N62 107.1(8) . . ?
N61 N62 B2 120.1(7) . . ?
C64 N62 N61 108.2(8) . . ?
C64 N62 B2 130.9(9) . . ?
N112 N111 W3 117.6(6) . . ?
C112 N111 W3 134.3(7) . . ?
C112 N111 N112 108.0(8) . . ?
N111 N112 B3 120.9(8) . . ?
C114 N112 N111 109.4(8) . . ?
C114 N112 B3 129.3(8) . . ?
N122 N121 W3 121.2(6) . . ?
C122 N121 W3 132.2(7) . . ?
C122 N121 N122 106.4(8) . . ?
N121 N122 B3 119.3(8) . . ?
C124 N122 N121 109.7(8) . . ?
C124 N122 B3 130.7(8) . . ?
N132 N131 W3 120.8(5) . . ?
C132 N131 W3 133.6(6) . . ?
C132 N131 N132 105.5(7) . . ?
N131 N132 B3 119.2(7) . . ?
C134 N132 N131 110.3(7) . . ?
C134 N132 B3 130.4(8) . . ?
N142 N141 W4 118.9(6) . . ?
C142 N141 W4 135.8(7) . . ?
C142 N141 N142 105.1(8) . . ?
N141 N142 B4 120.6(8) . . ?
C144 N142 N141 109.4(8) . . ?
C144 N142 B4 129.9(9) . . ?
N152 N151 W4 121.6(6) . . ?
C152 N151 W4 131.7(6) . . ?
C152 N151 N152 106.4(7) . . ?
N151 N152 B4 119.8(8) . . ?
C154 N152 N151 109.2(8) . . ?
C154 N152 B4 130.8(9) . . ?
N162 N161 W4 121.0(6) . . ?
C162 N161 W4 131.3(7) . . ?
C162 N161 N162 107.6(8) . . ?
N161 N162 B4 120.8(8) . . ?
C164 N162 N161 109.6(8) . . ?
C164 N162 B4 129.6(9) . . ?
P1 C1 W1 174.6(6) . . ?
O2 C2 W1 178.8(9) . . ?
O3 C3 W1 174.2(11) . . ?
P1 C4 W2 163.4(6) . . ?
O5 C5 W2 176.9(10) . . ?
O6 C6 W2 176.1(9) . . ?
N11 C12 C11 122.6(9) . . ?
N11 C12 C13 109.2(9) . . ?
C13 C12 C11 128.2(10) . . ?
C14 C13 C12 106.3(9) . . ?
N12 C14 C13 108.8(9) . . ?
N12 C14 C15 122.0(9) . . ?
C13 C14 C15 129.2(9) . . ?
N21 C22 C21 121.5(10) . . ?
N21 C22 C23 109.7(9) . . ?
C23 C22 C21 128.8(10) . . ?
C22 C23 C24 107.3(9) . . ?
N22 C24 C23 107.4(9) . . ?
N22 C24 C25 122.1(10) . . ?
C23 C24 C25 130.4(10) . . ?
N31 C32 C31 122.2(9) . . ?
N31 C32 C33 110.0(9) . . ?
C33 C32 C31 127.7(9) . . ?
C34 C33 C32 106.5(9) . . ?
N32 C34 C33 107.6(8) . . ?
N32 C34 C35 122.2(9) . . ?
C33 C34 C35 130.2(9) . . ?
N41 C42 C41 122.0(9) . . ?
N41 C42 C43 110.3(9) . . ?
C43 C42 C41 127.6(10) . . ?
C44 C43 C42 105.5(9) . . ?
N42 C44 C43 108.5(9) . . ?
N42 C44 C45 123.5(10) . . ?
C43 C44 C45 128.0(10) . . ?
N51 C52 C51 121.9(9) . . ?
N51 C52 C53 108.5(10) . . ?
C53 C52 C51 129.6(10) . . ?
C54 C53 C52 107.8(10) . . ?
N52 C54 C53 107.9(10) . . ?
N52 C54 C55 121.4(10) . . ?
C53 C54 C55 130.6(10) . . ?
N61 C62 C61 122.7(9) . . ?
N61 C62 C63 109.5(9) . . ?
C63 C62 C61 127.8(9) . . ?
C64 C63 C62 106.2(9) . . ?
N62 C64 C63 109.0(9) . . ?
N62 C64 C65 122.0(10) . . ?
C63 C64 C65 129.0(10) . . ?
C72 C71 P1 120.2(8) . . ?
C72 C71 C76 119.5(9) . . ?
C76 C71 P1 119.9(8) . . ?
C73 C72 C71 120.3(10) . . ?
C72 C73 C74 120.3(11) . . ?
C75 C74 C73 119.7(11) . . ?
C74 C75 C76 120.8(11) . . ?
C75 C76 C71 119.4(10) . . ?
P2 C101 W3 174.3(6) . . ?
O102 C102 W3 176.9(9) . . ?
O103 C103 W3 177.9(9) . . ?
P2 C104 W4 164.1(6) . . ?
O105 C105 W4 178.5(11) . . ?
O106 C106 W4 178.3(9) . . ?
N111 C112 C111 123.0(10) . . ?
N111 C112 C113 108.0(9) . . ?
C113 C112 C111 129.0(10) . . ?
C114 C113 C112 106.3(9) . . ?
N112 C114 C113 108.3(10) . . ?
N112 C114 C115 122.6(10) . . ?
C113 C114 C115 129.1(10) . . ?
N121 C122 C121 123.7(9) . . ?
N121 C122 C123 108.5(9) . . ?
C123 C122 C121 127.8(9) . . ?
C124 C123 C122 107.2(9) . . ?
N122 C124 C123 108.2(9) . . ?
N122 C124 C125 121.8(9) . . ?
C123 C124 C125 130.0(9) . . ?
N131 C132 C131 122.4(9) . . ?
N131 C132 C133 110.0(8) . . ?
C133 C132 C131 127.6(9) . . ?
C132 C133 C134 107.1(9) . . ?
N132 C134 C133 107.0(8) . . ?
N132 C134 C135 122.5(9) . . ?
C133 C134 C135 130.5(9) . . ?
N141 C142 C141 120.6(10) . . ?
N141 C142 C143 111.3(9) . . ?
C143 C142 C141 128.0(10) . . ?
C144 C143 C142 105.7(9) . . ?
N142 C144 C143 108.4(9) . . ?
N142 C144 C145 122.0(10) . . ?
C143 C144 C145 129.5(10) . . ?
N151 C152 C151 123.1(8) . . ?
N151 C152 C153 109.2(9) . . ?
C153 C152 C151 127.6(9) . . ?
C154 C153 C152 106.7(9) . . ?
N152 C154 C153 108.5(9) . . ?
N152 C154 C155 122.7(10) . . ?
C153 C154 C155 128.7(10) . . ?
N161 C162 C161 123.4(9) . . ?
N161 C162 C163 108.8(10) . . ?
C163 C162 C161 127.7(10) . . ?
C164 C163 C162 106.3(9) . . ?
N162 C164 C163 107.7(10) . . ?
N162 C164 C165 122.6(10) . . ?
C163 C164 C165 129.7(10) . . ?
C172 C171 P2 120.2(7) . . ?
C176 C171 P2 120.3(8) . . ?
C176 C171 C172 118.7(9) . . ?
C173 C172 C171 120.3(9) . . ?
C174 C173 C172 118.8(10) . . ?
C173 C174 C175 122.6(10) . . ?
C174 C175 C176 119.1(10) . . ?
C171 C176 C175 120.5(10) . . ?
N22 B1 N12 108.9(8) . . ?
N22 B1 N32 110.3(8) . . ?
N32 B1 N12 108.4(8) . . ?
N52 B2 N42 109.6(9) . . ?
N52 B2 N62 108.2(8) . . ?
N62 B2 N42 109.2(8) . . ?
N112 B3 N122 109.2(8) . . ?
N132 B3 N112 109.7(8) . . ?
N132 B3 N122 110.5(8) . . ?
N142 B4 N152 109.7(8) . . ?
N142 B4 N162 108.5(8) . . ?
N152 B4 N162 106.9(8) . . ?


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
15 -3 2 0.0850 15.0001 -3.0000 2.0001 -0.7319 0.5361 0.5029
0 -3 30 0.0451 0.0000 -3.0001 29.9990 -0.7680 -0.1991 -0.6214
0 23 -9 0.0370 -0.0000 22.9995 -8.9998 0.7570 0.6289 -0.0120
0 5 -29 0.0215 -0.0000 5.0000 -28.9991 0.7924 0.2466 0.5818
0 -23 9 0.0370 0.0000 -22.9995 8.9998 -0.7570 -0.6289 0.0120
0 -17 -33 0.0350 0.1000 -16.9994 -33.0988 0.3593 -0.2992 0.8714
-2 17 33 0.0474 -2.0000 16.9995 32.9988 -0.2792 0.2209 -0.9350
-15 3 -2 0.1150 -15.0001 3.0000 -2.0001 0.7319 -0.5361 -0.5029


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_ALC734
_database_code_depnum_ccdc_archive 'CCDC 1519747'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_audit_creation_date             13-12-04
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 'ALC734 At 9:58 on 28/11'
_chemical_name_systematic        ?
_chemical_melting_point          ?

# Hand-made tables can be put in the cif. The number of columns 
# is set in the loop header. 
# The contants of each column can either be a piece of text 
# without any spaces (eg a number) or other text enclosed in " " 
# Remove the leading # in the following example 

#geom_extra_table_head_A 
#; 
#Table 2. 
#Molecular parameters deviating most from MOGUL averages 
#; 
# 
#loop_ 
#_geom_extra_tableA_col_1 
#_geom_extra_tableA_col_2 
#_geom_extra_tableA_col_3 
#_geom_extra_tableA_col_4 
# 
#Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" 
#N5-C6-C4 129 124 "7 (\%)" 
#C3-O10-C2 105 109 "2 (\%)" 
#C6-O7 1.25 1.22 ".02 (\%A)" 
#  

_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                   24.2055(3)
_cell_length_b                   10.40920(10)
_cell_length_c                   25.5107(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.9841(6)
_cell_angle_gamma                90
_cell_volume                     6179.17(12)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_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'
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'
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 = C48 H61 B2 N12 O4 P1 W2 
# Dc =      1.39 Fooo =   2552.00 Mu =     37.92 M =   1290.39
# Found Formula = C48 H61 B2 N12 O4 P1 W2 
# Dc =      1.39 FOOO =   2552.00 Mu =     37.92 M =   1290.39

_chemical_formula_sum            'C48 H61 B2 N12 O4 P1 W2'
_chemical_formula_moiety         'C42 H55 B2 N12 O4 P1 W2, C6 H6'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         1290.39


_cell_measurement_reflns_used    172784
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.090
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_max          0.190

_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2552
_exptl_absorpt_coefficient_mu    3.792

# 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 0.050
-1 0 0 0.040
0 1 0 0.120
0 -1 0 0.070
0 0 1 0.100
0 0 -1 0.080


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;
_diffrn_reflns_av_R_equivalents  0.042


# 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 0.500 -0.013 0.250 573 80 ' '
2 0.500 -0.025 0.750 573 80 ' '
3 0.181 0.186 0.194 19 2 ' '
4 0.181 0.314 0.694 19 2 ' '
5 0.818 0.686 0.306 19 2 ' '
6 0.818 0.814 0.806 19 1 ' '
_platon_squeeze_details          
;
;

# 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    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            14148
_reflns_number_total             14148
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 14148 
# Theoretical number of reflections is about 28316 


_diffrn_reflns_theta_min         2.560
_diffrn_reflns_theta_max         27.474
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.474
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       33
_reflns_limit_h_min              -31
_reflns_limit_h_max              30
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              33

_oxford_diffrn_Wilson_B_factor   2.25
_oxford_diffrn_Wilson_scale      127.75

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

_refine_diff_density_min         -2.19
_refine_diff_density_max         1.74


# 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         14144
_refine_ls_number_restraints     0
_refine_ls_number_parameters     622
_oxford_refine_ls_R_factor_ref   0.0584
_refine_ls_wR_factor_ref         0.0999
_refine_ls_goodness_of_fit_ref   0.9504
_refine_ls_shift/su_max          0.0030543
_refine_ls_shift/su_mean         0.0001635


# The values computed from all data 
_oxford_reflns_number_all        14144
_refine_ls_R_factor_all          0.0584
_refine_ls_wR_factor_all         0.0999

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10493
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_gt          0.0827

# 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: 
 18.3 26.9 13.7 3.67 
;

# 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 0.667007(8) 0.253008(18) 0.561609(8) 0.0295 1.0000 Uani . . . . . .
W2 W 0.864996(8) 0.239408(17) 0.475324(7) 0.0278 1.0000 Uani . . . . . .
P1 P 0.77905(6) 0.44781(12) 0.53453(5) 0.0292 1.0000 Uani . . . . . .
O2 O 0.6569(2) 0.4910(5) 0.6337(2) 0.0635 1.0000 Uani . . . . . .
O3 O 0.6005(2) 0.4242(5) 0.4631(2) 0.0651 1.0000 Uani . . . . . .
O5 O 0.9486(2) 0.2656(5) 0.59342(18) 0.0610 1.0000 Uani . . . . . .
O6 O 0.9194(2) 0.4987(4) 0.4509(2) 0.0552 1.0000 Uani . . . . . .
N11 N 0.58300(19) 0.1683(4) 0.5717(2) 0.0387 1.0000 Uani . . . . . .
N12 N 0.5788(2) 0.0369(4) 0.5775(2) 0.0410 1.0000 Uani . . . . . .
N21 N 0.66270(19) 0.0771(4) 0.51212(19) 0.0359 1.0000 Uani . . . . . .
N22 N 0.6516(2) -0.0410(4) 0.5314(2) 0.0386 1.0000 Uani . . . . . .
N31 N 0.70379(18) 0.1201(4) 0.63056(18) 0.0322 1.0000 Uani . . . . . .
N32 N 0.6814(2) -0.0015(4) 0.6320(2) 0.0388 1.0000 Uani . . . . . .
N41 N 0.92802(18) 0.1206(4) 0.44202(17) 0.0315 1.0000 Uani . . . . . .
N42 N 0.90582(19) 0.0246(4) 0.40540(18) 0.0340 1.0000 Uani . . . . . .
N51 N 0.80896(17) 0.2140(4) 0.39108(16) 0.0283 1.0000 Uani . . . . . .
N52 N 0.80375(19) 0.0955(4) 0.36608(16) 0.0307 1.0000 Uani . . . . . .
N61 N 0.83563(18) 0.0438(4) 0.48746(17) 0.0311 1.0000 Uani . . . . . .
N62 N 0.8292(2) -0.0478(4) 0.44738(18) 0.0343 1.0000 Uani . . . . . .
C1 C 0.7298(2) 0.3389(5) 0.5521(2) 0.0310 1.0000 Uani . . . . . .
C2 C 0.6607(2) 0.4036(5) 0.6087(2) 0.0392 1.0000 Uani . . . . . .
C3 C 0.6240(3) 0.3600(6) 0.4986(3) 0.0429 1.0000 Uani . . . . . .
C4 C 0.8187(2) 0.3394(5) 0.5046(2) 0.0297 1.0000 Uani . . . . . .
C5 C 0.9188(2) 0.2506(5) 0.5496(2) 0.0389 1.0000 Uani . . . . . .
C6 C 0.8997(2) 0.4044(5) 0.4586(2) 0.0370 1.0000 Uani . . . . . .
C11 C 0.5178(3) 0.3573(7) 0.5620(4) 0.0639 1.0000 Uani . . . . . .
C12 C 0.5307(2) 0.2172(7) 0.5686(3) 0.0473 1.0000 Uani . . . . . .
C13 C 0.4934(3) 0.1176(7) 0.5723(3) 0.0565 1.0000 Uani . . . . . .
C14 C 0.5247(3) 0.0059(7) 0.5775(3) 0.0491 1.0000 Uani . . . . . .
C15 C 0.5051(3) -0.1284(8) 0.5825(3) 0.0708 1.0000 Uani . . . . . .
C21 C 0.6856(3) 0.1607(7) 0.4292(3) 0.0525 1.0000 Uani . . . . . .
C22 C 0.6722(2) 0.0563(6) 0.4632(2) 0.0408 1.0000 Uani . . . . . .
C23 C 0.6682(3) -0.0746(6) 0.4520(3) 0.0473 1.0000 Uani . . . . . .
C24 C 0.6558(3) -0.1338(6) 0.4955(3) 0.0484 1.0000 Uani . . . . . .
C25 C 0.6483(3) -0.2739(6) 0.5059(3) 0.0652 1.0000 Uani . . . . . .
C31 C 0.7829(3) 0.2502(5) 0.6883(2) 0.0439 1.0000 Uani . . . . . .
C32 C 0.7472(2) 0.1322(5) 0.6759(2) 0.0356 1.0000 Uani . . . . . .
C33 C 0.7527(3) 0.0200(6) 0.7064(2) 0.0423 1.0000 Uani . . . . . .
C34 C 0.7112(3) -0.0623(6) 0.6777(2) 0.0439 1.0000 Uani . . . . . .
C35 C 0.6977(3) -0.1963(7) 0.6912(3) 0.0651 1.0000 Uani . . . . . .
C41 C 1.0240(2) 0.2195(6) 0.4828(3) 0.0451 1.0000 Uani . . . . . .
C42 C 0.9848(2) 0.1285(5) 0.4454(2) 0.0360 1.0000 Uani . . . . . .
C43 C 0.9981(3) 0.0381(6) 0.4106(2) 0.0427 1.0000 Uani . . . . . .
C44 C 0.9476(2) -0.0255(6) 0.3851(2) 0.0391 1.0000 Uani . . . . . .
C45 C 0.9367(3) -0.1317(7) 0.3444(3) 0.0574 1.0000 Uani . . . . . .
C51 C 0.7661(3) 0.4299(5) 0.3703(2) 0.0440 1.0000 Uani . . . . . .
C52 C 0.7728(2) 0.2925(5) 0.3572(2) 0.0331 1.0000 Uani . . . . . .
C53 C 0.7424(2) 0.2251(5) 0.3101(2) 0.0371 1.0000 Uani . . . . . .
C54 C 0.7634(2) 0.1022(5) 0.3170(2) 0.0380 1.0000 Uani . . . . . .
C55 C 0.7467(3) -0.0124(6) 0.2802(3) 0.0525 1.0000 Uani . . . . . .
C61 C 0.8235(3) 0.0572(6) 0.5812(2) 0.0474 1.0000 Uani . . . . . .
C62 C 0.8218(2) -0.0124(5) 0.5297(2) 0.0356 1.0000 Uani . . . . . .
C63 C 0.8060(2) -0.1390(5) 0.5163(3) 0.0422 1.0000 Uani . . . . . .
C64 C 0.8110(2) -0.1596(5) 0.4648(2) 0.0382 1.0000 Uani . . . . . .
C65 C 0.8000(3) -0.2777(6) 0.4304(3) 0.0595 1.0000 Uani . . . . . .
C71 C 0.8323(2) 0.4937(5) 0.5990(2) 0.0319 1.0000 Uani . . . . . .
C72 C 0.8044(2) 0.5772(5) 0.6340(2) 0.0369 1.0000 Uani . . . . . .
C73 C 0.8480(3) 0.6197(7) 0.6864(3) 0.0528 1.0000 Uani . . . . . .
C74 C 0.8990(3) 0.6891(7) 0.6747(3) 0.0598 1.0000 Uani . . . . . .
C75 C 0.9269(3) 0.6062(6) 0.6398(3) 0.0489 1.0000 Uani . . . . . .
C76 C 0.8834(2) 0.5641(5) 0.5874(2) 0.0359 1.0000 Uani . . . . . .
C81 C 0.0673(3) 0.7328(9) 0.2236(4) 0.0773 1.0000 Uani . . . . . .
C82 C 0.0567(4) 0.7959(12) 0.2677(4) 0.0828 1.0000 Uani . . . . . .
C83 C 0.0641(4) 0.9261(12) 0.2726(4) 0.0892 1.0000 Uani . . . . . .
C84 C 0.0811(4) 0.9954(11) 0.2336(4) 0.0874 1.0000 Uani . . . . . .
C85 C 0.0918(4) 0.9298(12) 0.1904(4) 0.0883 1.0000 Uani . . . . . .
C86 C 0.0844(3) 0.8012(12) 0.1853(3) 0.0832 1.0000 Uani . . . . . .
B1 B 0.6319(3) -0.0491(6) 0.5841(3) 0.0408 1.0000 Uani . . . . . .
B2 B 0.8422(2) -0.0162(5) 0.3936(2) 0.0305 1.0000 Uani . . . . . .
H111 H 0.4801 0.3735 0.5652 0.0960 1.0000 Uiso R . . . . .
H113 H 0.5441 0.4062 0.5894 0.0961 1.0000 Uiso R . . . . .
H112 H 0.5197 0.3867 0.5270 0.0962 1.0000 Uiso R . . . . .
H131 H 0.4546 0.1253 0.5712 0.0678 1.0000 Uiso R . . . . .
H153 H 0.4641 -0.1307 0.5742 0.1059 1.0000 Uiso R . . . . .
H152 H 0.5210 -0.1583 0.6189 0.1059 1.0000 Uiso R . . . . .
H151 H 0.5175 -0.1838 0.5581 0.1060 1.0000 Uiso R . . . . .
H211 H 0.6921 0.1248 0.3966 0.0789 1.0000 Uiso R . . . . .
H213 H 0.7191 0.2068 0.4486 0.0789 1.0000 Uiso R . . . . .
H212 H 0.6539 0.2189 0.4192 0.0790 1.0000 Uiso R . . . . .
H231 H 0.6732 -0.1146 0.4209 0.0571 1.0000 Uiso R . . . . .
H253 H 0.6477 -0.3221 0.4739 0.0981 1.0000 Uiso R . . . . .
H252 H 0.6793 -0.3043 0.5354 0.0979 1.0000 Uiso R . . . . .
H251 H 0.6128 -0.2878 0.5148 0.0980 1.0000 Uiso R . . . . .
H311 H 0.8095 0.2441 0.7240 0.0661 1.0000 Uiso R . . . . .
H312 H 0.8042 0.2626 0.6623 0.0658 1.0000 Uiso R . . . . .
H313 H 0.7584 0.3233 0.6874 0.0659 1.0000 Uiso R . . . . .
H331 H 0.7795 0.0048 0.7396 0.0510 1.0000 Uiso R . . . . .
H351 H 0.7186 -0.2158 0.7278 0.0978 1.0000 Uiso R . . . . .
H353 H 0.7086 -0.2552 0.6672 0.0981 1.0000 Uiso R . . . . .
H352 H 0.6577 -0.2052 0.6873 0.0980 1.0000 Uiso R . . . . .
H411 H 1.0624 0.2112 0.4801 0.0679 1.0000 Uiso R . . . . .
H412 H 1.0246 0.2012 0.5194 0.0681 1.0000 Uiso R . . . . .
H413 H 1.0117 0.3061 0.4752 0.0681 1.0000 Uiso R . . . . .
H431 H 1.0340 0.0234 0.4056 0.0507 1.0000 Uiso R . . . . .
H451 H 0.9706 -0.1466 0.3329 0.0860 1.0000 Uiso R . . . . .
H453 H 0.9271 -0.2089 0.3607 0.0859 1.0000 Uiso R . . . . .
H452 H 0.9058 -0.1092 0.3132 0.0860 1.0000 Uiso R . . . . .
H511 H 0.7384 0.4699 0.3407 0.0660 1.0000 Uiso R . . . . .
H512 H 0.8019 0.4735 0.3766 0.0661 1.0000 Uiso R . . . . .
H513 H 0.7528 0.4356 0.4023 0.0660 1.0000 Uiso R . . . . .
H531 H 0.7139 0.2575 0.2806 0.0449 1.0000 Uiso R . . . . .
H552 H 0.7170 0.0114 0.2481 0.0790 1.0000 Uiso R . . . . .
H551 H 0.7793 -0.0434 0.2692 0.0789 1.0000 Uiso R . . . . .
H553 H 0.7328 -0.0804 0.2984 0.0789 1.0000 Uiso R . . . . .
H612 H 0.8093 0.0028 0.6050 0.0710 1.0000 Uiso R . . . . .
H611 H 0.8621 0.0824 0.5993 0.0713 1.0000 Uiso R . . . . .
H613 H 0.8003 0.1328 0.5730 0.0709 1.0000 Uiso R . . . . .
H631 H 0.7942 -0.1984 0.5376 0.0508 1.0000 Uiso R . . . . .
H652 H 0.7888 -0.3456 0.4504 0.0890 1.0000 Uiso R . . . . .
H651 H 0.8343 -0.3004 0.4205 0.0890 1.0000 Uiso R . . . . .
H653 H 0.7697 -0.2602 0.3982 0.0889 1.0000 Uiso R . . . . .
H711 H 0.8466 0.4153 0.6190 0.0380 1.0000 Uiso R . . . . .
H721 H 0.7884 0.6536 0.6139 0.0441 1.0000 Uiso R . . . . .
H722 H 0.7738 0.5311 0.6434 0.0439 1.0000 Uiso R . . . . .
H731 H 0.8620 0.5449 0.7087 0.0631 1.0000 Uiso R . . . . .
H732 H 0.8289 0.6760 0.7062 0.0629 1.0000 Uiso R . . . . .
H742 H 0.9276 0.7086 0.7088 0.0720 1.0000 Uiso R . . . . .
H741 H 0.8860 0.7684 0.6552 0.0718 1.0000 Uiso R . . . . .
H752 H 0.9574 0.6545 0.6312 0.0590 1.0000 Uiso R . . . . .
H751 H 0.9432 0.5310 0.6604 0.0588 1.0000 Uiso R . . . . .
H761 H 0.9019 0.5092 0.5668 0.0431 1.0000 Uiso R . . . . .
H762 H 0.8687 0.6403 0.5656 0.0429 1.0000 Uiso R . . . . .
H811 H 0.0630 0.6442 0.2203 0.0930 1.0000 Uiso R . . . . .
H821 H 0.0448 0.7499 0.2938 0.0990 1.0000 Uiso R . . . . .
H831 H 0.0574 0.9681 0.3024 0.1070 1.0000 Uiso R . . . . .
H841 H 0.0850 1.0846 0.2361 0.1051 1.0000 Uiso R . . . . .
H851 H 0.1041 0.9755 0.1643 0.1060 1.0000 Uiso R . . . . .
H861 H 0.0912 0.7592 0.1554 0.0999 1.0000 Uiso R . . . . .
H21 H 0.8340 -0.0993 0.3690 0.0467 1.0000 Uiso R . . . . .
H11 H 0.6201 -0.1498 0.5917 0.0483 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.11172(2)
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 . 2.295(4) yes
W1 . N21 . 2.210(4) yes
W1 . N31 . 2.222(4) yes
W1 . C1 . 1.837(5) yes
W1 . C2 . 2.006(6) yes
W1 . C3 . 1.997(6) yes
W2 . N41 . 2.300(4) yes
W2 . N51 . 2.219(4) yes
W2 . N61 . 2.207(4) yes
W2 . C4 . 1.832(5) yes
W2 . C5 . 1.985(5) yes
W2 . C6 . 2.008(5) yes
P1 . C1 . 1.788(5) yes
P1 . C4 . 1.784(5) yes
P1 . C71 . 1.852(5) yes
O2 . C2 . 1.129(7) yes
O3 . C3 . 1.142(7) yes
O5 . C5 . 1.162(7) yes
O6 . C6 . 1.132(7) yes
N11 . N12 . 1.383(6) yes
N11 . C12 . 1.346(7) yes
N12 . C14 . 1.349(7) yes
N12 . B1 . 1.538(8) yes
N21 . N22 . 1.378(6) yes
N21 . C22 . 1.347(7) yes
N22 . C24 . 1.353(7) yes
N22 . B1 . 1.547(8) yes
N31 . N32 . 1.381(6) yes
N31 . C32 . 1.338(7) yes
N32 . C34 . 1.348(7) yes
N32 . B1 . 1.538(8) yes
N41 . N42 . 1.372(6) yes
N41 . C42 . 1.356(7) yes
N42 . C44 . 1.361(7) yes
N42 . B2 . 1.546(7) yes
N51 . N52 . 1.379(5) yes
N51 . C52 . 1.328(7) yes
N52 . C54 . 1.362(7) yes
N52 . B2 . 1.533(7) yes
N61 . N62 . 1.375(6) yes
N61 . C62 . 1.348(7) yes
N62 . C64 . 1.361(6) yes
N62 . B2 . 1.525(7) yes
C11 . C12 . 1.491(9) yes
C11 . H111 . 0.953 no
C11 . H113 . 0.953 no
C11 . H112 . 0.957 no
C12 . C13 . 1.394(9) yes
C13 . C14 . 1.373(10) yes
C13 . H131 . 0.935 no
C14 . C15 . 1.493(9) yes
C15 . H153 . 0.957 no
C15 . H152 . 0.954 no
C15 . H151 . 0.955 no
C21 . C22 . 1.483(9) yes
C21 . H211 . 0.961 no
C21 . H213 . 0.956 no
C21 . H212 . 0.955 no
C22 . C23 . 1.390(8) yes
C23 . C24 . 1.374(10) yes
C23 . H231 . 0.932 no
C24 . C25 . 1.502(9) yes
C25 . H253 . 0.955 no
C25 . H252 . 0.959 no
C25 . H251 . 0.957 no
C31 . C32 . 1.484(7) yes
C31 . H311 . 0.962 no
C31 . H312 . 0.956 no
C31 . H313 . 0.961 no
C32 . C33 . 1.389(8) yes
C33 . C34 . 1.369(8) yes
C33 . H331 . 0.928 no
C34 . C35 . 1.495(8) yes
C35 . H351 . 0.952 no
C35 . H353 . 0.954 no
C35 . H352 . 0.950 no
C41 . C42 . 1.486(8) yes
C41 . H411 . 0.955 no
C41 . H412 . 0.950 no
C41 . H413 . 0.952 no
C42 . C43 . 1.391(8) yes
C43 . C44 . 1.385(8) yes
C43 . H431 . 0.924 no
C44 . C45 . 1.489(8) yes
C45 . H451 . 0.957 no
C45 . H453 . 0.961 no
C45 . H452 . 0.960 no
C51 . C52 . 1.488(7) yes
C51 . H511 . 0.955 no
C51 . H512 . 0.953 no
C51 . H513 . 0.958 no
C52 . C53 . 1.409(7) yes
C53 . C54 . 1.370(8) yes
C53 . H531 . 0.934 no
C54 . C55 . 1.502(7) yes
C55 . H552 . 0.961 no
C55 . H551 . 0.964 no
C55 . H553 . 0.957 no
C61 . C62 . 1.491(8) yes
C61 . H612 . 0.959 no
C61 . H611 . 0.958 no
C61 . H613 . 0.957 no
C62 . C63 . 1.388(8) yes
C63 . C64 . 1.370(8) yes
C63 . H631 . 0.920 no
C64 . C65 . 1.491(8) yes
C65 . H652 . 0.954 no
C65 . H651 . 0.960 no
C65 . H653 . 0.956 no
C71 . C72 . 1.530(7) yes
C71 . C76 . 1.535(7) yes
C71 . H711 . 0.974 no
C72 . C73 . 1.524(8) yes
C72 . H721 . 0.968 no
C72 . H722 . 0.967 no
C73 . C74 . 1.529(9) yes
C73 . H731 . 0.969 no
C73 . H732 . 0.970 no
C74 . C75 . 1.523(9) yes
C74 . H742 . 0.973 no
C74 . H741 . 0.970 no
C75 . C76 . 1.521(7) yes
C75 . H752 . 0.968 no
C75 . H751 . 0.965 no
C76 . H761 . 0.965 no
C76 . H762 . 0.978 no
C81 . C82 . 1.385(12) yes
C81 . C86 . 1.364(13) yes
C81 . H811 . 0.929 no
C82 . C83 . 1.368(14) yes
C82 . H821 . 0.929 no
C83 . C84 . 1.381(14) yes
C83 . H831 . 0.927 no
C84 . C85 . 1.380(12) yes
C84 . H841 . 0.934 no
C85 . C86 . 1.353(14) yes
C85 . H851 . 0.931 no
C86 . H861 . 0.931 no
B1 . H11 . 1.118 no
B2 . H21 . 1.055 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 . 80.92(17) yes
N11 . W1 . N31 . 81.16(16) yes
N21 . W1 . N31 . 83.22(16) yes
N11 . W1 . C1 . 173.28(19) yes
N21 . W1 . C1 . 103.79(19) yes
N31 . W1 . C1 . 104.00(19) yes
N11 . W1 . C2 . 90.9(2) yes
N21 . W1 . C2 . 171.85(19) yes
N31 . W1 . C2 . 95.3(2) yes
C1 . W1 . C2 . 84.3(2) yes
N11 . W1 . C3 . 91.3(2) yes
N21 . W1 . C3 . 94.0(2) yes
N31 . W1 . C3 . 172.3(2) yes
C1 . W1 . C3 . 83.6(2) yes
C2 . W1 . C3 . 86.4(2) yes
N41 . W2 . N51 . 82.47(15) yes
N41 . W2 . N61 . 80.08(15) yes
N51 . W2 . N61 . 83.76(15) yes
N41 . W2 . C4 . 176.43(18) yes
N51 . W2 . C4 . 100.52(19) yes
N61 . W2 . C4 . 102.11(19) yes
N41 . W2 . C5 . 93.23(19) yes
N51 . W2 . C5 . 175.48(19) yes
N61 . W2 . C5 . 94.2(2) yes
C4 . W2 . C5 . 83.8(2) yes
N41 . W2 . C6 . 91.30(18) yes
N51 . W2 . C6 . 94.37(19) yes
N61 . W2 . C6 . 171.34(19) yes
C4 . W2 . C6 . 86.5(2) yes
C5 . W2 . C6 . 87.1(2) yes
C1 . P1 . C4 . 100.4(2) yes
C1 . P1 . C71 . 106.9(2) yes
C4 . P1 . C71 . 102.6(2) yes
W1 . N11 . N12 . 119.0(3) yes
W1 . N11 . C12 . 134.1(4) yes
N12 . N11 . C12 . 106.5(5) yes
N11 . N12 . C14 . 109.7(5) yes
N11 . N12 . B1 . 120.3(4) yes
C14 . N12 . B1 . 130.1(5) yes
W1 . N21 . N22 . 121.2(3) yes
W1 . N21 . C22 . 132.0(4) yes
N22 . N21 . C22 . 106.7(4) yes
N21 . N22 . C24 . 109.7(5) yes
N21 . N22 . B1 . 119.7(4) yes
C24 . N22 . B1 . 130.3(5) yes
W1 . N31 . N32 . 121.1(3) yes
W1 . N31 . C32 . 132.4(4) yes
N32 . N31 . C32 . 106.5(4) yes
N31 . N32 . C34 . 109.4(5) yes
N31 . N32 . B1 . 120.0(4) yes
C34 . N32 . B1 . 130.5(5) yes
W2 . N41 . N42 . 117.9(3) yes
W2 . N41 . C42 . 135.1(3) yes
N42 . N41 . C42 . 106.7(4) yes
N41 . N42 . C44 . 110.2(4) yes
N41 . N42 . B2 . 121.0(4) yes
C44 . N42 . B2 . 128.7(4) yes
W2 . N51 . N52 . 120.6(3) yes
W2 . N51 . C52 . 132.4(3) yes
N52 . N51 . C52 . 106.8(4) yes
N51 . N52 . C54 . 109.3(4) yes
N51 . N52 . B2 . 120.0(4) yes
C54 . N52 . B2 . 130.6(4) yes
W2 . N61 . N62 . 120.7(3) yes
W2 . N61 . C62 . 132.3(4) yes
N62 . N61 . C62 . 107.0(4) yes
N61 . N62 . C64 . 109.3(4) yes
N61 . N62 . B2 . 120.7(4) yes
C64 . N62 . B2 . 130.0(4) yes
P1 . C1 . W1 . 167.0(3) yes
W1 . C2 . O2 . 177.6(6) yes
W1 . C3 . O3 . 178.0(5) yes
P1 . C4 . W2 . 174.5(3) yes
W2 . C5 . O5 . 175.1(5) yes
W2 . C6 . O6 . 177.7(5) yes
C12 . C11 . H111 . 109.8 no
C12 . C11 . H113 . 111.3 no
H111 . C11 . H113 . 107.9 no
C12 . C11 . H112 . 110.8 no
H111 . C11 . H112 . 108.3 no
H113 . C11 . H112 . 108.6 no
C11 . C12 . N11 . 122.7(6) yes
C11 . C12 . C13 . 128.0(6) yes
N11 . C12 . C13 . 109.3(6) yes
C12 . C13 . C14 . 106.7(5) yes
C12 . C13 . H131 . 126.7 no
C14 . C13 . H131 . 126.7 no
C13 . C14 . N12 . 107.9(6) yes
C13 . C14 . C15 . 128.5(6) yes
N12 . C14 . C15 . 123.7(6) yes
C14 . C15 . H153 . 109.8 no
C14 . C15 . H152 . 109.7 no
H153 . C15 . H152 . 108.8 no
C14 . C15 . H151 . 110.2 no
H153 . C15 . H151 . 109.5 no
H152 . C15 . H151 . 108.9 no
C22 . C21 . H211 . 109.6 no
C22 . C21 . H213 . 110.8 no
H211 . C21 . H213 . 109.0 no
C22 . C21 . H212 . 109.4 no
H211 . C21 . H212 . 109.0 no
H213 . C21 . H212 . 109.0 no
C21 . C22 . N21 . 123.1(5) yes
C21 . C22 . C23 . 127.7(6) yes
N21 . C22 . C23 . 109.2(6) yes
C22 . C23 . C24 . 106.9(6) yes
C22 . C23 . H231 . 126.6 no
C24 . C23 . H231 . 126.6 no
C23 . C24 . N22 . 107.5(5) yes
C23 . C24 . C25 . 129.9(6) yes
N22 . C24 . C25 . 122.5(7) yes
C24 . C25 . H253 . 109.5 no
C24 . C25 . H252 . 110.7 no
H253 . C25 . H252 . 108.8 no
C24 . C25 . H251 . 110.4 no
H253 . C25 . H251 . 108.6 no
H252 . C25 . H251 . 108.8 no
C32 . C31 . H311 . 110.3 no
C32 . C31 . H312 . 110.9 no
H311 . C31 . H312 . 108.6 no
C32 . C31 . H313 . 109.4 no
H311 . C31 . H313 . 108.9 no
H312 . C31 . H313 . 108.8 no
C31 . C32 . N31 . 122.4(5) yes
C31 . C32 . C33 . 128.0(5) yes
N31 . C32 . C33 . 109.6(5) yes
C32 . C33 . C34 . 106.5(5) yes
C32 . C33 . H331 . 126.1 no
C34 . C33 . H331 . 127.4 no
C33 . C34 . N32 . 107.9(5) yes
C33 . C34 . C35 . 129.5(6) yes
N32 . C34 . C35 . 122.6(6) yes
C34 . C35 . H351 . 109.5 no
C34 . C35 . H353 . 109.4 no
H351 . C35 . H353 . 109.0 no
C34 . C35 . H352 . 110.4 no
H351 . C35 . H352 . 109.6 no
H353 . C35 . H352 . 108.9 no
C42 . C41 . H411 . 111.0 no
C42 . C41 . H412 . 109.7 no
H411 . C41 . H412 . 107.6 no
C42 . C41 . H413 . 111.4 no
H411 . C41 . H413 . 109.2 no
H412 . C41 . H413 . 107.9 no
C41 . C42 . N41 . 122.5(5) yes
C41 . C42 . C43 . 128.4(5) yes
N41 . C42 . C43 . 109.1(5) yes
C42 . C43 . C44 . 107.1(5) yes
C42 . C43 . H431 . 126.2 no
C44 . C43 . H431 . 126.7 no
C43 . C44 . N42 . 106.9(5) yes
C43 . C44 . C45 . 130.3(5) yes
N42 . C44 . C45 . 122.8(5) yes
C44 . C45 . H451 . 109.4 no
C44 . C45 . H453 . 109.8 no
H451 . C45 . H453 . 109.0 no
C44 . C45 . H452 . 110.2 no
H451 . C45 . H452 . 108.7 no
H453 . C45 . H452 . 109.7 no
C52 . C51 . H511 . 109.8 no
C52 . C51 . H512 . 110.2 no
H511 . C51 . H512 . 109.4 no
C52 . C51 . H513 . 109.5 no
H511 . C51 . H513 . 108.7 no
H512 . C51 . H513 . 109.2 no
C51 . C52 . N51 . 122.6(5) yes
C51 . C52 . C53 . 127.3(5) yes
N51 . C52 . C53 . 110.1(4) yes
C52 . C53 . C54 . 105.6(4) yes
C52 . C53 . H531 . 127.2 no
C54 . C53 . H531 . 127.3 no
C53 . C54 . N52 . 108.1(4) yes
C53 . C54 . C55 . 129.5(5) yes
N52 . C54 . C55 . 122.4(5) yes
C54 . C55 . H552 . 109.7 no
C54 . C55 . H551 . 110.2 no
H552 . C55 . H551 . 108.4 no
C54 . C55 . H553 . 110.8 no
H552 . C55 . H553 . 108.9 no
H551 . C55 . H553 . 108.7 no
C62 . C61 . H612 . 109.9 no
C62 . C61 . H611 . 110.2 no
H612 . C61 . H611 . 109.2 no
C62 . C61 . H613 . 109.6 no
H612 . C61 . H613 . 109.5 no
H611 . C61 . H613 . 108.5 no
C61 . C62 . N61 . 122.7(5) yes
C61 . C62 . C63 . 128.2(5) yes
N61 . C62 . C63 . 109.1(5) yes
C62 . C63 . C64 . 107.1(5) yes
C62 . C63 . H631 . 127.0 no
C64 . C63 . H631 . 125.8 no
C63 . C64 . N62 . 107.6(5) yes
C63 . C64 . C65 . 130.1(5) yes
N62 . C64 . C65 . 122.3(5) yes
C64 . C65 . H652 . 109.2 no
C64 . C65 . H651 . 109.3 no
H652 . C65 . H651 . 110.6 no
C64 . C65 . H653 . 108.6 no
H652 . C65 . H653 . 109.6 no
H651 . C65 . H653 . 109.4 no
P1 . C71 . C72 . 110.7(4) yes
P1 . C71 . C76 . 110.6(4) yes
C72 . C71 . C76 . 110.5(4) yes
P1 . C71 . H711 . 108.0 no
C72 . C71 . H711 . 108.6 no
C76 . C71 . H711 . 108.3 no
C71 . C72 . C73 . 111.5(5) yes
C71 . C72 . H721 . 109.5 no
C73 . C72 . H721 . 107.8 no
C71 . C72 . H722 . 110.8 no
C73 . C72 . H722 . 108.7 no
H721 . C72 . H722 . 108.4 no
C72 . C73 . C74 . 111.5(5) yes
C72 . C73 . H731 . 109.1 no
C74 . C73 . H731 . 108.9 no
C72 . C73 . H732 . 108.5 no
C74 . C73 . H732 . 110.1 no
H731 . C73 . H732 . 108.7 no
C73 . C74 . C75 . 111.0(5) yes
C73 . C74 . H742 . 109.7 no
C75 . C74 . H742 . 108.7 no
C73 . C74 . H741 . 109.6 no
C75 . C74 . H741 . 108.5 no
H742 . C74 . H741 . 109.3 no
C74 . C75 . C76 . 111.5(5) yes
C74 . C75 . H752 . 109.1 no
C76 . C75 . H752 . 109.7 no
C74 . C75 . H751 . 108.7 no
C76 . C75 . H751 . 109.0 no
H752 . C75 . H751 . 108.7 no
C71 . C76 . C75 . 111.5(5) yes
C71 . C76 . H761 . 110.0 no
C75 . C76 . H761 . 109.7 no
C71 . C76 . H762 . 108.1 no
C75 . C76 . H762 . 108.7 no
H761 . C76 . H762 . 108.7 no
C82 . C81 . C86 . 119.7(10) yes
C82 . C81 . H811 . 120.2 no
C86 . C81 . H811 . 120.1 no
C81 . C82 . C83 . 119.7(10) yes
C81 . C82 . H821 . 120.1 no
C83 . C82 . H821 . 120.2 no
C82 . C83 . C84 . 120.5(8) yes
C82 . C83 . H831 . 119.7 no
C84 . C83 . H831 . 119.8 no
C83 . C84 . C85 . 118.4(10) yes
C83 . C84 . H841 . 121.0 no
C85 . C84 . H841 . 120.6 no
C84 . C85 . C86 . 121.2(10) yes
C84 . C85 . H851 . 119.1 no
C86 . C85 . H851 . 119.7 no
C81 . C86 . C85 . 120.4(8) yes
C81 . C86 . H861 . 119.9 no
C85 . C86 . H861 . 119.7 no
N22 . B1 . N32 . 108.3(5) yes
N22 . B1 . N12 . 108.8(5) yes
N32 . B1 . N12 . 110.1(5) yes
N22 . B1 . H11 . 111.0 no
N32 . B1 . H11 . 110.1 no
N12 . B1 . H11 . 108.5 no
N42 . B2 . N52 . 109.1(4) yes
N42 . B2 . N62 . 109.0(4) yes
N52 . B2 . N62 . 109.0(4) yes
N42 . B2 . H21 . 110.8 no
N52 . B2 . H21 . 111.0 no
N62 . B2 . H21 . 107.9 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 04/12/13 at 15:33:14
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 113,X'S) H   ( 112,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 153,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 213,X'S) H   ( 212,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 252,X'S) H   ( 251,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   ( 353,X'S) H   ( 352,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   ( 453,X'S) H   ( 452,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   ( 552,X'S) H   ( 551,X'S) H   ( 553,X'S) 
RIDE C   (  61,X'S) H   ( 612,X'S) H   ( 611,X'S) H   ( 613,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  65,X'S) H   ( 652,X'S) H   ( 651,X'S) H   ( 653,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) 
RIDE C   (  74,X'S) H   ( 742,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 752,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,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 04/12/13 at 15:33:15
#
#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
6 0 0 x .
-4 0 2 x .
-6 0 2 x .
5 0 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 1520168'
_audit_update_record             
;
2016-12-01 deposited with the CCDC.
2016-12-22 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                   24.8643(5)
_cell_length_b                   10.7400(2)
_cell_length_c                   19.2900(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5151.25(18)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P c a 21 '
_symmetry_space_group_name_Hall  'P 2c -2ac'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x+1/2,y,z+1/2
x+1/2,-y,z
-x,-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'
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 = C48 H55 B2 N12 O4 P1 W2 
# Dc =      1.66 Fooo =   2528.00 Mu =     45.48 M =   1284.34
# Found Formula = C48 H55 B2 N12 O4 P1 W2 
# Dc =      1.66 FOOO =   2528.00 Mu =     45.48 M =   1284.34

_chemical_formula_sum            'C48 H55 B2 N12 O4 P1 W2'
_chemical_formula_moiety         'C42 H49 B2 N12 O4 P1 W2, C6 H6'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         1284.34


_cell_measurement_reflns_used    28631
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25.03
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            'dark purple'
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_max          0.100

_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    4.548

# 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 0.020
-1 0 0 0.050
0 1 0 0.025
0 -1 0 0.035
0 0 1 0.050
0 0 -1 0.050


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_T_max  0.777
_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            34628
_reflns_number_total             8997
_diffrn_reflns_av_R_equivalents  0.074
# Number of reflections without Friedels Law is 8997 
# Number of reflections with Friedels Law is 4690 
# Theoretical number of reflections is about 4544 


_diffrn_reflns_theta_min         2.673
_diffrn_reflns_theta_max         25.014
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        25.014
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              0
_reflns_limit_h_max              29
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              -22
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   2.64
_oxford_diffrn_Wilson_scale      198.19

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

_refine_diff_density_min         -1.90
_refine_diff_density_max         1.48


# 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         8963
_refine_ls_number_restraints     37
_refine_ls_number_parameters     623
_oxford_refine_ls_R_factor_ref   0.0678
_refine_ls_wR_factor_ref         0.0894
_refine_ls_goodness_of_fit_ref   0.9560
_refine_ls_shift/su_max          0.0047711
_refine_ls_shift/su_mean         0.0001111


# The values computed from all data 
_oxford_reflns_number_all        8963
_refine_ls_R_factor_all          0.0678
_refine_ls_wR_factor_all         0.0894

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6669
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_gt          0.0735

_refine_ls_abs_structure_Flack   -0.008(13)
_refine_ls_abs_structure_details 'Flack (1983), 4307 Friedel-pairs'
# 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 ad


_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: 
 7.18 8.87 4.14 0.919 
;

# 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 0.401573(14) 0.36635(4) 0.66558(8) 0.0327 1.0000 Uani . . . . . .
W2 W 0.603130(14) 0.27727(3) 0.66786(8) 0.0337 1.0000 Uani . . . . . .
P1 P 0.45679(12) 0.3674(3) 0.55207(17) 0.0363 1.0000 Uani . . . . . .
N11 N 0.3266(4) 0.4137(10) 0.7253(5) 0.0385 1.0000 Uani . . . . . .
N12 N 0.3302(5) 0.4749(13) 0.7865(6) 0.0355 1.0000 Uani . . . . . .
N21 N 0.4250(3) 0.3020(9) 0.7726(5) 0.0337 1.0000 Uani . . . . . .
N22 N 0.4153(4) 0.3775(9) 0.8297(5) 0.0339 1.0000 Uani . . . . . .
N31 N 0.4246(4) 0.5532(9) 0.7020(5) 0.0365 1.0000 Uani . . . . . .
N32 N 0.4181(4) 0.5842(9) 0.7720(5) 0.0345 1.0000 Uani . . . . . .
N41 N 0.6944(3) 0.2757(8) 0.6725(8) 0.0379 1.0000 Uani . . . . . .
N42 N 0.7200(4) 0.2161(11) 0.7256(5) 0.0405 1.0000 Uani . . . . . .
N51 N 0.6132(4) 0.3047(10) 0.7810(6) 0.0361 1.0000 Uani . . . . . .
N52 N 0.6485(4) 0.2362(10) 0.8187(5) 0.0391 1.0000 Uani . . . . . .
N61 N 0.6177(4) 0.0800(9) 0.6925(5) 0.0385 1.0000 Uani . . . . . .
N62 N 0.6550(4) 0.0446(10) 0.7432(5) 0.0427 1.0000 Uani . . . . . .
O2 O 0.3407(5) 0.4699(13) 0.5337(6) 0.0549 1.0000 Uani . . . . . .
O3 O 0.3531(4) 0.1012(9) 0.6393(5) 0.0607 1.0000 Uani . . . . . .
O5 O 0.5950(5) 0.2456(13) 0.5074(5) 0.0774 1.0000 Uani . . . . . .
O6 O 0.6030(5) 0.5610(9) 0.6298(5) 0.0693 1.0000 Uani . . . . . .
C1 C 0.4767(5) 0.3183(11) 0.6370(6) 0.0380 1.0000 Uani . . . . . .
C2 C 0.3642(5) 0.4326(13) 0.5810(7) 0.0443 1.0000 Uani . . . . . .
C3 C 0.3711(5) 0.1998(13) 0.6467(6) 0.0495 1.0000 Uani . . . . . .
C4 C 0.5290(4) 0.2934(9) 0.6564(7) 0.0285 1.0000 Uani . . . . . .
C5 C 0.5998(6) 0.2551(15) 0.5682(7) 0.0469 1.0000 Uani . . . . . .
C6 C 0.6036(4) 0.4561(11) 0.6453(5) 0.0342 1.0000 Uani . . . . . .
C11 C 0.2528(5) 0.3308(15) 0.6490(6) 0.0569 1.0000 Uani . . . . . .
C12 C 0.2738(5) 0.4018(12) 0.7103(6) 0.0375 1.0000 Uani . . . . . .
C13 C 0.2442(5) 0.4553(14) 0.7627(7) 0.0496 1.0000 Uani . . . . . .
C14 C 0.2806(5) 0.4996(11) 0.8104(7) 0.0416 1.0000 Uani . . . . . .
C15 C 0.2706(6) 0.5608(15) 0.8795(8) 0.0675 1.0000 Uani . . . . . .
C21 C 0.4644(5) 0.0882(12) 0.7530(7) 0.0474 1.0000 Uani . . . . . .
C22 C 0.4486(5) 0.1988(13) 0.7967(7) 0.0393 1.0000 Uani . . . . . .
C23 C 0.4542(6) 0.2067(13) 0.8673(8) 0.0489 1.0000 Uani . . . . . .
C24 C 0.4330(5) 0.3207(14) 0.8875(6) 0.0413 1.0000 Uani . . . . . .
C25 C 0.4268(7) 0.3783(15) 0.9586(7) 0.0648 1.0000 Uani . . . . . .
C31 C 0.4629(8) 0.6627(16) 0.5985(7) 0.0693 1.0000 Uani . . . . . .
C32 C 0.4496(4) 0.6530(10) 0.6753(10) 0.0403 1.0000 Uani . . . . . .
C33 C 0.4619(5) 0.7426(14) 0.7248(7) 0.0489 1.0000 Uani . . . . . .
C34 C 0.4406(5) 0.6970(12) 0.7843(6) 0.0395 1.0000 Uani . . . . . .
C35 C 0.4406(6) 0.7558(13) 0.8550(7) 0.0520 1.0000 Uani . . . . . .
C41 C 0.7199(6) 0.3796(16) 0.5598(7) 0.0629 1.0000 Uani . . . . . .
C42 C 0.7326(5) 0.3147(15) 0.6258(7) 0.0507 1.0000 Uani . . . . . .
C43 C 0.7821(5) 0.2735(13) 0.6510(7) 0.0526 1.0000 Uani . . . . . .
C44 C 0.7726(5) 0.2170(15) 0.7127(7) 0.0477 1.0000 Uani . . . . . .
C45 C 0.8129(5) 0.1551(17) 0.7598(8) 0.0711 1.0000 Uani . . . . . .
C51 C 0.5457(5) 0.4694(13) 0.8030(7) 0.0502 1.0000 Uani . . . . . .
C52 C 0.5870(4) 0.3807(11) 0.8256(6) 0.0392 1.0000 Uani . . . . . .
C53 C 0.6063(5) 0.3571(12) 0.8925(6) 0.0453 1.0000 Uani . . . . . .
C54 C 0.6441(5) 0.2657(12) 0.8865(5) 0.0403 1.0000 Uani . . . . . .
C55 C 0.6779(5) 0.2017(14) 0.9422(6) 0.0534 1.0000 Uani . . . . . .
C61 C 0.5591(5) -0.0316(14) 0.6083(7) 0.0520 1.0000 Uani . . . . . .
C62 C 0.5995(3) -0.0250(8) 0.6683(11) 0.0303 1.0000 Uani . . . . . .
C63 C 0.6263(5) -0.1273(13) 0.6952(6) 0.0502 1.0000 Uani . . . . . .
C64 C 0.6604(6) -0.0784(13) 0.7432(8) 0.0511 1.0000 Uani . . . . . .
C65 C 0.6998(7) -0.1409(15) 0.7915(8) 0.0725 1.0000 Uani . . . . . .
C71 C 0.4412(5) 0.2285(15) 0.5018(8) 0.0410 1.0000 Uani . . . . . .
C72 C 0.4274(6) 0.2499(18) 0.4326(7) 0.0568 1.0000 Uani . . . . . .
C73 C 0.4205(7) 0.152(2) 0.3875(9) 0.0902 1.0000 Uani . . . . . .
C74 C 0.4267(6) 0.033(2) 0.4088(10) 0.0730 1.0000 Uani . . . . . .
C75 C 0.4415(6) 0.0050(16) 0.4763(9) 0.0663 1.0000 Uani . . . . . .
C76 C 0.4485(5) 0.1061(13) 0.5221(7) 0.0481 1.0000 Uani . . . . . .
C101 C 0.7522(10) -0.044(3) 1.0281(12) 0.1105 1.0000 Uani . U . . . .
C102 C 0.8007(9) -0.005(3) 1.0088(13) 0.1213 1.0000 Uani . U . . . .
C103 C 0.8282(11) -0.058(3) 0.9551(15) 0.1456 1.0000 Uani . U . . . .
C104 C 0.8053(11) -0.172(3) 0.9262(13) 0.1297 1.0000 Uani . U . . . .
C105 C 0.7570(12) -0.211(3) 0.9498(12) 0.1215 1.0000 Uani . U . . . .
C106 C 0.7301(11) -0.146(2) 0.9961(13) 0.1133 1.0000 Uani . U . . . .
B1 B 0.3854(5) 0.5008(14) 0.8203(7) 0.0361 1.0000 Uani . . . . . .
B2 B 0.6871(6) 0.1473(16) 0.7810(7) 0.0453 1.0000 Uani . . . . . .
H111 H 0.2160 0.3520 0.6413 0.0862 1.0000 Uiso R . . . . .
H112 H 0.2559 0.2430 0.6571 0.0860 1.0000 Uiso R . . . . .
H113 H 0.2731 0.3524 0.6085 0.0861 1.0000 Uiso R . . . . .
H131 H 0.2069 0.4609 0.7653 0.0600 1.0000 Uiso R . . . . .
H151 H 0.2326 0.5730 0.8858 0.1020 1.0000 Uiso R . . . . .
H152 H 0.2844 0.5091 0.9160 0.1020 1.0000 Uiso R . . . . .
H153 H 0.2885 0.6402 0.8807 0.1020 1.0000 Uiso R . . . . .
H211 H 0.4875 0.0339 0.7793 0.0721 1.0000 Uiso R . . . . .
H212 H 0.4832 0.1170 0.7128 0.0720 1.0000 Uiso R . . . . .
H213 H 0.4329 0.0437 0.7388 0.0720 1.0000 Uiso R . . . . .
H231 H 0.4694 0.1470 0.8961 0.0580 1.0000 Uiso R . . . . .
H251 H 0.4400 0.3217 0.9932 0.0980 1.0000 Uiso R . . . . .
H252 H 0.4471 0.4545 0.9610 0.0981 1.0000 Uiso R . . . . .
H253 H 0.3893 0.3957 0.9672 0.0980 1.0000 Uiso R . . . . .
H311 H 0.4754 0.7454 0.5882 0.1040 1.0000 Uiso R . . . . .
H312 H 0.4907 0.6036 0.5876 0.1040 1.0000 Uiso R . . . . .
H313 H 0.4314 0.6447 0.5714 0.1040 1.0000 Uiso R . . . . .
H331 H 0.4804 0.8169 0.7185 0.0591 1.0000 Uiso R . . . . .
H351 H 0.4635 0.8278 0.8546 0.0779 1.0000 Uiso R . . . . .
H352 H 0.4539 0.6975 0.8885 0.0780 1.0000 Uiso R . . . . .
H353 H 0.4047 0.7802 0.8669 0.0780 1.0000 Uiso R . . . . .
H411 H 0.7517 0.4192 0.5424 0.0941 1.0000 Uiso R . . . . .
H412 H 0.6929 0.4418 0.5683 0.0940 1.0000 Uiso R . . . . .
H413 H 0.7067 0.3209 0.5263 0.0939 1.0000 Uiso R . . . . .
H431 H 0.8156 0.2834 0.6295 0.0640 1.0000 Uiso R . . . . .
H451 H 0.8489 0.1788 0.7468 0.1060 1.0000 Uiso R . . . . .
H452 H 0.8066 0.1786 0.8070 0.1059 1.0000 Uiso R . . . . .
H453 H 0.8093 0.0662 0.7556 0.1060 1.0000 Uiso R . . . . .
H511 H 0.5269 0.5013 0.8428 0.0749 1.0000 Uiso R . . . . .
H512 H 0.5622 0.5369 0.7786 0.0750 1.0000 Uiso R . . . . .
H513 H 0.5207 0.4280 0.7730 0.0750 1.0000 Uiso R . . . . .
H531 H 0.5956 0.3965 0.9335 0.0540 1.0000 Uiso R . . . . .
H551 H 0.6746 0.2465 0.9851 0.0800 1.0000 Uiso R . . . . .
H552 H 0.7150 0.2000 0.9283 0.0800 1.0000 Uiso R . . . . .
H553 H 0.6655 0.1179 0.9488 0.0801 1.0000 Uiso R . . . . .
H611 H 0.5616 -0.1110 0.5855 0.0780 1.0000 Uiso R . . . . .
H612 H 0.5671 0.0331 0.5754 0.0781 1.0000 Uiso R . . . . .
H613 H 0.5233 -0.0203 0.6251 0.0780 1.0000 Uiso R . . . . .
H631 H 0.6218 -0.2104 0.6831 0.0600 1.0000 Uiso R . . . . .
H651 H 0.7005 -0.2289 0.7826 0.1100 1.0000 Uiso R . . . . .
H652 H 0.7349 -0.1064 0.7842 0.1100 1.0000 Uiso R . . . . .
H653 H 0.6889 -0.1267 0.8384 0.1099 1.0000 Uiso R . . . . .
H721 H 0.4229 0.3308 0.4168 0.0689 1.0000 Uiso R . . . . .
H731 H 0.4113 0.1681 0.3417 0.1090 1.0000 Uiso R . . . . .
H741 H 0.4210 -0.0323 0.3776 0.0880 1.0000 Uiso R . . . . .
H751 H 0.4466 -0.0769 0.4908 0.0790 1.0000 Uiso R . . . . .
H761 H 0.4583 0.0900 0.5674 0.0580 1.0000 Uiso R . . . . .
H1011 H 0.7335 -0.0028 1.0628 0.1320 1.0000 Uiso R . . . . .
H1021 H 0.8161 0.0620 1.0325 0.1449 1.0000 Uiso R . . . . .
H1031 H 0.8599 -0.0243 0.9383 0.1750 1.0000 Uiso R . . . . .
H1041 H 0.8232 -0.2169 0.8920 0.1571 1.0000 Uiso R . . . . .
H1051 H 0.7425 -0.2846 0.9333 0.1460 1.0000 Uiso R . . . . .
H1061 H 0.6953 -0.1698 1.0072 0.1360 1.0000 Uiso R . . . . .
H11 H 0.3799 0.5459 0.8698 0.0431 1.0000 Uiso R . . . . .
H21 H 0.7140 0.1052 0.8182 0.0543 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.071649(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 . P1 . 2.585(3) yes
W1 . N11 . 2.249(9) yes
W1 . N21 . 2.254(10) yes
W1 . N31 . 2.201(10) yes
W1 . C1 . 2.014(12) yes
W1 . C2 . 2.008(15) yes
W1 . C3 . 1.977(14) yes
W2 . N41 . 2.271(8) yes
W2 . N51 . 2.216(11) yes
W2 . N61 . 2.201(10) yes
W2 . C4 . 1.865(10) yes
W2 . C5 . 1.938(14) yes
W2 . C6 . 1.969(11) yes
P1 . C1 . 1.790(12) yes
P1 . C71 . 1.821(15) yes
N11 . N12 . 1.354(16) yes
N11 . C12 . 1.352(14) yes
N12 . C14 . 1.343(16) yes
N12 . B1 . 1.544(17) yes
N21 . N22 . 1.389(12) yes
N21 . C22 . 1.338(16) yes
N22 . C24 . 1.345(15) yes
N22 . B1 . 1.530(17) yes
N31 . N32 . 1.401(12) yes
N31 . C32 . 1.343(15) yes
N32 . C34 . 1.356(15) yes
N32 . B1 . 1.526(15) yes
N41 . N42 . 1.367(16) yes
N41 . C42 . 1.375(17) yes
N42 . C44 . 1.332(15) yes
N42 . B2 . 1.535(19) yes
N51 . N52 . 1.355(13) yes
N51 . C52 . 1.353(15) yes
N52 . C54 . 1.349(14) yes
N52 . B2 . 1.538(17) yes
N61 . N62 . 1.401(13) yes
N61 . C62 . 1.302(14) yes
N62 . C64 . 1.327(17) yes
N62 . B2 . 1.544(18) yes
O2 . C2 . 1.156(17) yes
O3 . C3 . 1.158(15) yes
O5 . C5 . 1.184(16) yes
O6 . C6 . 1.166(13) yes
C1 . C4 . 1.380(14) yes
C11 . C12 . 1.501(17) yes
C11 . H111 . 0.954 no
C11 . H112 . 0.959 no
C11 . H113 . 0.958 no
C12 . C13 . 1.375(17) yes
C13 . C14 . 1.375(18) yes
C13 . H131 . 0.932 no
C14 . C15 . 1.506(17) yes
C15 . H151 . 0.962 no
C15 . H152 . 0.960 no
C15 . H153 . 0.962 no
C21 . C22 . 1.509(18) yes
C21 . H211 . 0.962 no
C21 . H212 . 0.957 no
C21 . H213 . 0.957 no
C22 . C23 . 1.372(19) yes
C23 . C24 . 1.39(2) yes
C23 . H231 . 0.929 no
C24 . C25 . 1.513(18) yes
C25 . H251 . 0.961 no
C25 . H252 . 0.962 no
C25 . H253 . 0.965 no
C31 . C32 . 1.52(2) yes
C31 . H311 . 0.962 no
C31 . H312 . 0.962 no
C31 . H313 . 0.961 no
C32 . C33 . 1.39(2) yes
C33 . C34 . 1.356(18) yes
C33 . H331 . 0.929 no
C34 . C35 . 1.502(17) yes
C35 . H351 . 0.959 no
C35 . H352 . 0.959 no
C35 . H353 . 0.959 no
C41 . C42 . 1.49(2) yes
C41 . H411 . 0.960 no
C41 . H412 . 0.961 no
C41 . H413 . 0.959 no
C42 . C43 . 1.396(19) yes
C43 . C44 . 1.36(2) yes
C43 . H431 . 0.936 no
C44 . C45 . 1.506(19) yes
C45 . H451 . 0.963 no
C45 . H452 . 0.958 no
C45 . H453 . 0.961 no
C51 . C52 . 1.467(17) yes
C51 . H511 . 0.961 no
C51 . H512 . 0.956 no
C51 . H513 . 0.960 no
C52 . C53 . 1.400(17) yes
C53 . C54 . 1.365(17) yes
C53 . H531 . 0.935 no
C54 . C55 . 1.528(16) yes
C55 . H551 . 0.961 no
C55 . H552 . 0.960 no
C55 . H553 . 0.961 no
C61 . C62 . 1.54(2) yes
C61 . H611 . 0.961 no
C61 . H612 . 0.961 no
C61 . H613 . 0.955 no
C62 . C63 . 1.384(17) yes
C63 . C64 . 1.361(18) yes
C63 . H631 . 0.929 no
C64 . C65 . 1.511(19) yes
C65 . H651 . 0.961 no
C65 . H652 . 0.959 no
C65 . H653 . 0.957 no
C71 . C72 . 1.40(2) yes
C71 . C76 . 1.38(2) yes
C72 . C73 . 1.38(2) yes
C72 . H721 . 0.928 no
C73 . C74 . 1.35(3) yes
C73 . H731 . 0.930 no
C74 . C75 . 1.38(2) yes
C74 . H741 . 0.931 no
C75 . C76 . 1.411(19) yes
C75 . H751 . 0.931 no
C76 . H761 . 0.924 no
C101 . C102 . 1.33(3) yes
C101 . C106 . 1.38(3) yes
C101 . H1011 . 0.927 no
C102 . C103 . 1.37(3) yes
C102 . H1021 . 0.931 no
C103 . C104 . 1.46(4) yes
C103 . H1031 . 0.927 no
C104 . C105 . 1.35(3) yes
C104 . H1041 . 0.930 no
C105 . C106 . 1.31(3) yes
C105 . H1051 . 0.930 no
C106 . H1061 . 0.928 no
B1 . H11 . 1.080 no
B2 . H21 . 1.080 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
P1 . W1 . N11 . 150.8(3) yes
P1 . W1 . N21 . 129.8(2) yes
N11 . W1 . N21 . 79.3(3) yes
P1 . W1 . N31 . 97.4(2) yes
N11 . W1 . N31 . 81.1(4) yes
N21 . W1 . N31 . 85.4(3) yes
P1 . W1 . C1 . 43.7(3) yes
N11 . W1 . C1 . 165.1(4) yes
N21 . W1 . C1 . 86.1(4) yes
N31 . W1 . C1 . 94.6(4) yes
P1 . W1 . C2 . 63.6(3) yes
N11 . W1 . C2 . 87.3(4) yes
N21 . W1 . C2 . 166.6(4) yes
N31 . W1 . C2 . 93.2(5) yes
C1 . W1 . C2 . 107.3(5) yes
P1 . W1 . C3 . 93.0(4) yes
N11 . W1 . C3 . 88.9(5) yes
N21 . W1 . C3 . 89.4(4) yes
N31 . W1 . C3 . 169.5(4) yes
C1 . W1 . C3 . 94.2(5) yes
C2 . W1 . C3 . 89.7(5) yes
N41 . W2 . N51 . 81.3(5) yes
N41 . W2 . N61 . 79.6(3) yes
N51 . W2 . N61 . 84.1(4) yes
N41 . W2 . C4 . 173.3(5) yes
N51 . W2 . C4 . 102.5(5) yes
N61 . W2 . C4 . 106.1(4) yes
N41 . W2 . C5 . 94.6(6) yes
N51 . W2 . C5 . 175.9(5) yes
N61 . W2 . C5 . 95.9(5) yes
C4 . W2 . C5 . 81.5(6) yes
N41 . W2 . C6 . 90.6(4) yes
N51 . W2 . C6 . 95.0(4) yes
N61 . W2 . C6 . 170.2(4) yes
C4 . W2 . C6 . 83.6(4) yes
C5 . W2 . C6 . 84.3(5) yes
W1 . P1 . C1 . 51.0(4) yes
W1 . P1 . C71 . 109.6(5) yes
C1 . P1 . C71 . 107.8(7) yes
W1 . N11 . N12 . 120.2(8) yes
W1 . N11 . C12 . 132.4(9) yes
N12 . N11 . C12 . 107.2(10) yes
N11 . N12 . C14 . 109.6(11) yes
N11 . N12 . B1 . 120.9(11) yes
C14 . N12 . B1 . 129.4(12) yes
W1 . N21 . N22 . 120.1(7) yes
W1 . N21 . C22 . 133.3(9) yes
N22 . N21 . C22 . 106.6(10) yes
N21 . N22 . C24 . 109.5(10) yes
N21 . N22 . B1 . 119.7(9) yes
C24 . N22 . B1 . 130.6(10) yes
W1 . N31 . N32 . 119.6(7) yes
W1 . N31 . C32 . 136.6(9) yes
N32 . N31 . C32 . 103.5(11) yes
N31 . N32 . C34 . 109.5(9) yes
N31 . N32 . B1 . 120.7(9) yes
C34 . N32 . B1 . 129.6(10) yes
W2 . N41 . N42 . 119.9(8) yes
W2 . N41 . C42 . 131.5(11) yes
N42 . N41 . C42 . 108.2(9) yes
N41 . N42 . C44 . 108.3(11) yes
N41 . N42 . B2 . 119.9(9) yes
C44 . N42 . B2 . 131.1(11) yes
W2 . N51 . N52 . 122.0(8) yes
W2 . N51 . C52 . 130.7(8) yes
N52 . N51 . C52 . 107.3(10) yes
N51 . N52 . C54 . 109.9(10) yes
N51 . N52 . B2 . 119.1(9) yes
C54 . N52 . B2 . 130.8(10) yes
W2 . N61 . N62 . 121.4(7) yes
W2 . N61 . C62 . 134.4(10) yes
N62 . N61 . C62 . 104.2(11) yes
N61 . N62 . C64 . 109.6(11) yes
N61 . N62 . B2 . 118.5(10) yes
C64 . N62 . B2 . 131.2(12) yes
P1 . C1 . W1 . 85.4(5) yes
P1 . C1 . C4 . 124.5(9) yes
W1 . C1 . C4 . 148.1(9) yes
W1 . C2 . O2 . 177.0(11) yes
W1 . C3 . O3 . 176.5(11) yes
C1 . C4 . W2 . 169.2(10) yes
W2 . C5 . O5 . 176.0(13) yes
W2 . C6 . O6 . 177.7(10) yes
C12 . C11 . H111 . 109.6 no
C12 . C11 . H112 . 110.0 no
H111 . C11 . H112 . 109.6 no
C12 . C11 . H113 . 109.6 no
H111 . C11 . H113 . 108.8 no
H112 . C11 . H113 . 109.2 no
C11 . C12 . N11 . 123.7(11) yes
C11 . C12 . C13 . 127.2(11) yes
N11 . C12 . C13 . 108.8(12) yes
C12 . C13 . C14 . 106.6(11) yes
C12 . C13 . H131 . 126.8 no
C14 . C13 . H131 . 126.6 no
C13 . C14 . N12 . 107.8(11) yes
C13 . C14 . C15 . 129.5(12) yes
N12 . C14 . C15 . 122.7(12) yes
C14 . C15 . H151 . 109.5 no
C14 . C15 . H152 . 109.8 no
H151 . C15 . H152 . 109.6 no
C14 . C15 . H153 . 109.5 no
H151 . C15 . H153 . 109.2 no
H152 . C15 . H153 . 109.3 no
C22 . C21 . H211 . 109.7 no
C22 . C21 . H212 . 109.0 no
H211 . C21 . H212 . 109.5 no
C22 . C21 . H213 . 109.9 no
H211 . C21 . H213 . 109.6 no
H212 . C21 . H213 . 109.2 no
C21 . C22 . N21 . 125.0(12) yes
C21 . C22 . C23 . 125.3(12) yes
N21 . C22 . C23 . 109.7(12) yes
C22 . C23 . C24 . 107.1(13) yes
C22 . C23 . H231 . 126.3 no
C24 . C23 . H231 . 126.6 no
C23 . C24 . N22 . 107.0(12) yes
C23 . C24 . C25 . 130.8(13) yes
N22 . C24 . C25 . 122.2(13) yes
C24 . C25 . H251 . 109.6 no
C24 . C25 . H252 . 109.8 no
H251 . C25 . H252 . 108.9 no
C24 . C25 . H253 . 109.6 no
H251 . C25 . H253 . 109.5 no
H252 . C25 . H253 . 109.5 no
C32 . C31 . H311 . 109.6 no
C32 . C31 . H312 . 108.9 no
H311 . C31 . H312 . 109.4 no
C32 . C31 . H313 . 109.9 no
H311 . C31 . H313 . 109.6 no
H312 . C31 . H313 . 109.5 no
C31 . C32 . N31 . 121.9(13) yes
C31 . C32 . C33 . 125.0(13) yes
N31 . C32 . C33 . 113.0(15) yes
C32 . C33 . C34 . 104.3(13) yes
C32 . C33 . H331 . 127.9 no
C34 . C33 . H331 . 127.8 no
C33 . C34 . N32 . 109.6(11) yes
C33 . C34 . C35 . 128.1(12) yes
N32 . C34 . C35 . 122.3(11) yes
C34 . C35 . H351 . 109.4 no
C34 . C35 . H352 . 109.7 no
H351 . C35 . H352 . 109.1 no
C34 . C35 . H353 . 109.4 no
H351 . C35 . H353 . 109.5 no
H352 . C35 . H353 . 109.8 no
C42 . C41 . H411 . 109.3 no
C42 . C41 . H412 . 109.1 no
H411 . C41 . H412 . 109.2 no
C42 . C41 . H413 . 109.9 no
H411 . C41 . H413 . 109.7 no
H412 . C41 . H413 . 109.6 no
C41 . C42 . N41 . 123.9(12) yes
C41 . C42 . C43 . 129.5(12) yes
N41 . C42 . C43 . 106.5(13) yes
C42 . C43 . C44 . 107.1(12) yes
C42 . C43 . H431 . 126.4 no
C44 . C43 . H431 . 126.5 no
C43 . C44 . N42 . 109.8(13) yes
C43 . C44 . C45 . 127.7(13) yes
N42 . C44 . C45 . 122.5(13) yes
C44 . C45 . H451 . 110.1 no
C44 . C45 . H452 . 110.3 no
H451 . C45 . H452 . 109.2 no
C44 . C45 . H453 . 109.1 no
H451 . C45 . H453 . 109.1 no
H452 . C45 . H453 . 109.0 no
C52 . C51 . H511 . 109.7 no
C52 . C51 . H512 . 109.8 no
H511 . C51 . H512 . 109.4 no
C52 . C51 . H513 . 109.4 no
H511 . C51 . H513 . 109.3 no
H512 . C51 . H513 . 109.4 no
C51 . C52 . N51 . 122.7(11) yes
C51 . C52 . C53 . 129.1(11) yes
N51 . C52 . C53 . 108.2(11) yes
C52 . C53 . C54 . 106.7(10) yes
C52 . C53 . H531 . 126.9 no
C54 . C53 . H531 . 126.4 no
C53 . C54 . N52 . 107.9(10) yes
C53 . C54 . C55 . 130.0(11) yes
N52 . C54 . C55 . 122.1(12) yes
C54 . C55 . H551 . 109.5 no
C54 . C55 . H552 . 109.9 no
H551 . C55 . H552 . 109.4 no
C54 . C55 . H553 . 109.8 no
H551 . C55 . H553 . 109.1 no
H552 . C55 . H553 . 109.1 no
C62 . C61 . H611 . 110.0 no
C62 . C61 . H612 . 109.2 no
H611 . C61 . H612 . 109.1 no
C62 . C61 . H613 . 110.3 no
H611 . C61 . H613 . 109.2 no
H612 . C61 . H613 . 109.0 no
C61 . C62 . N61 . 122.5(12) yes
C61 . C62 . C63 . 124.1(11) yes
N61 . C62 . C63 . 112.8(14) yes
C62 . C63 . C64 . 104.3(12) yes
C62 . C63 . H631 . 127.7 no
C64 . C63 . H631 . 128.0 no
C63 . C64 . N62 . 108.8(13) yes
C63 . C64 . C65 . 130.7(14) yes
N62 . C64 . C65 . 120.5(14) yes
C64 . C65 . H651 . 109.7 no
C64 . C65 . H652 . 109.1 no
H651 . C65 . H652 . 109.8 no
C64 . C65 . H653 . 109.2 no
H651 . C65 . H653 . 109.3 no
H652 . C65 . H653 . 109.6 no
P1 . C71 . C72 . 115.3(13) yes
P1 . C71 . C76 . 126.8(12) yes
C72 . C71 . C76 . 117.3(14) yes
C71 . C72 . C73 . 120.6(18) yes
C71 . C72 . H721 . 119.9 no
C73 . C72 . H721 . 119.6 no
C72 . C73 . C74 . 121.2(18) yes
C72 . C73 . H731 . 119.1 no
C74 . C73 . H731 . 119.7 no
C73 . C74 . C75 . 121.2(17) yes
C73 . C74 . H741 . 119.6 no
C75 . C74 . H741 . 119.2 no
C74 . C75 . C76 . 117.2(17) yes
C74 . C75 . H751 . 121.4 no
C76 . C75 . H751 . 121.4 no
C75 . C76 . C71 . 122.6(14) yes
C75 . C76 . H761 . 118.7 no
C71 . C76 . H761 . 118.7 no
C102 . C101 . C106 . 119(3) yes
C102 . C101 . H1011 . 120.5 no
C106 . C101 . H1011 . 120.2 no
C101 . C102 . C103 . 122(3) yes
C101 . C102 . H1021 . 118.6 no
C103 . C102 . H1021 . 119.3 no
C102 . C103 . C104 . 117(3) yes
C102 . C103 . H1031 . 121.5 no
C104 . C103 . H1031 . 121.9 no
C103 . C104 . C105 . 118(3) yes
C103 . C104 . H1041 . 121.1 no
C105 . C104 . H1041 . 120.6 no
C104 . C105 . C106 . 121(3) yes
C104 . C105 . H1051 . 119.5 no
C106 . C105 . H1051 . 119.0 no
C101 . C106 . C105 . 122(3) yes
C101 . C106 . H1061 . 119.2 no
C105 . C106 . H1061 . 119.3 no
N12 . B1 . N22 . 109.0(11) yes
N12 . B1 . N32 . 108.7(10) yes
N22 . B1 . N32 . 108.8(9) yes
N12 . B1 . H11 . 110.0 no
N22 . B1 . H11 . 110.1 no
N32 . B1 . H11 . 110.1 no
N62 . B2 . N52 . 110.1(10) yes
N62 . B2 . N42 . 107.0(10) yes
N52 . B2 . N42 . 111.3(12) yes
N62 . B2 . H21 . 109.6 no
N52 . B2 . H21 . 109.4 no
N42 . 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
C11 . H113 . O2 . 158.0 0.958 2.549 3.46(2) yes
C11 . H113 . C2 . 138.0 0.958 2.482 3.26(2) yes
C21 . H212 . C4 . 146.0 0.957 2.463 3.30(2) yes
C41 . H411 . O2 3_565 163.0 0.960 2.517 3.45(2) yes
C61 . H612 . C5 . 142.0 0.961 2.523 3.33(2) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/02/14 at 15:41:17
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
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   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,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 15:41:17
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.03 = C(101) TO C(102) 
U(IJ) 0.0, 0.03 = C(102) TO C(103) 
U(IJ) 0.0, 0.03 = C(103) TO C(104) 
U(IJ) 0.0, 0.03 = C(104) TO C(105) 
U(IJ) 0.0, 0.03 = C(105) TO C(106) 
U(IJ) 0.0, 0.03 = C(106) TO C(101) 
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
9 4 -8 x .

# start Validation Reply Form
_vrf_PLAT342_1                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0229 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.
;
