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

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

data_jas167(JSW418)(2)
_database_code_depnum_ccdc_archive 'CCDC 1058393'
_audit_update_record             
;
2015-04-08 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_audit_creation_date             15-02-08
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'C:\Users\Jas\Desktop\jas167(JSW4 At 9:41 on '
_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          SQUEEZE
#--------------------------------------------------------------- 
# _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                   9.51940(10)
_cell_length_b                   15.98130(10)
_cell_length_c                   23.62910(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.1146(4)
_cell_angle_gamma                90
_cell_volume                     3589.44(5)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 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 0.0090 0.0039 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'
Br -0.6763 1.2805 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 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'
Fe -1.1336 3.1974 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 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 0.2955 0.4335 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 0.0492 0.0322 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'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C35 H31 B1 Br5 Cl1 F2 Fe2 N1 O1 P2 S1 
# Dc =      2.17 Fooo =   1844.00 Mu =    154.51 M =   1171.12
# Found Formula = C34 H30 B1 Br4 Fe2 P2 
# Dc =      1.74 FOOO =   1844.00 Mu =    127.13 M =    942.68

_chemical_formula_sum            'C34 H30 B1 Br4 Fe2 P2'
_chemical_formula_moiety         'C34 H30 B1 Fe1 P2, Br4 Fe1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         942.68


_cell_measurement_reflns_used    38517
_cell_measurement_theta_min      3
_cell_measurement_theta_max      72
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_min          0.066
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_max          0.146

_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1844
_exptl_absorpt_coefficient_mu    12.713

# Sheldrick geometric approximatio 0.30 0.43 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_T_max  0.43
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 104 46 ' '
2 0.500 0.500 0.500 104 46 ' '
_platon_squeeze_details          
;
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Agilent Technologies, 2013)'
_computing_cell_refinement       'CrysAlis PRO, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis PRO, (Agilent Technologies, 2013)'
_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      150
_diffrn_reflns_number            70155
_reflns_number_total             7092
_diffrn_reflns_av_R_equivalents  0.029
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7092 
# Theoretical number of reflections is about 14213 


_diffrn_reflns_theta_min         3.340
_diffrn_reflns_theta_max         72.409
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        72.409
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              -16
_reflns_limit_k_max              19
_reflns_limit_l_min              -29
_reflns_limit_l_max              29

_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      0.08

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

_refine_diff_density_min         -1.08
_refine_diff_density_max         0.91


# 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         7091
_refine_ls_number_restraints     0
_refine_ls_number_parameters     388
_oxford_refine_ls_R_factor_ref   0.0327
_refine_ls_wR_factor_ref         0.0869
_refine_ls_goodness_of_fit_ref   0.9969
_refine_ls_shift/su_max          0.0010865
_refine_ls_shift/su_mean         0.0000273


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7091
_refine_ls_R_factor_all          0.0327
_refine_ls_wR_factor_all         0.0869

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6930
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_gt          0.0865

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.242E+04 0.409E+04 0.265E+04 0.124E+04 375. 
;

# 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 0.1191(3) 0.4070(2) 0.23481(13) 0.0172 1.0000 Uani . . . . . .
Br1 Br 0.78324(4) 0.78506(2) 0.046606(15) 0.0328 1.0000 Uani . . . . . .
Br2 Br 0.60284(4) 0.57516(2) 0.067422(17) 0.0338 1.0000 Uani . . . . . .
Br3 Br 0.61852(4) 0.74076(3) 0.184457(15) 0.0359 1.0000 Uani . . . . . .
Br4 Br 0.38557(4) 0.77555(2) 0.050859(17) 0.0360 1.0000 Uani . . . . . .
Fe1 Fe 0.10039(4) 0.59167(3) 0.138245(18) 0.0148 1.0000 Uani . . . . . .
Fe2 Fe 0.59536(5) 0.71875(3) 0.086922(19) 0.0195 1.0000 Uani . . . . . .
P1 P 0.20509(7) 0.50808(4) 0.26414(3) 0.0142 1.0000 Uani . . . . . .
P2 P 0.16449(7) 0.38461(4) 0.15782(3) 0.0140 1.0000 Uani . . . . . .
C1 C 0.1534(3) 0.59758(17) 0.22260(11) 0.0163 1.0000 Uani . . . . . .
C2 C 0.0071(3) 0.61781(19) 0.21179(12) 0.0198 1.0000 Uani . . . . . .
C3 C -0.0011(3) 0.6894(2) 0.17574(13) 0.0238 1.0000 Uani . . . . . .
C4 C 0.1376(4) 0.71343(18) 0.16427(13) 0.0238 1.0000 Uani . . . . . .
C5 C 0.2341(3) 0.65827(17) 0.19312(12) 0.0190 1.0000 Uani . . . . . .
C6 C 0.1237(3) 0.47087(17) 0.11114(11) 0.0158 1.0000 Uani . . . . . .
C7 C -0.0173(3) 0.49959(19) 0.09812(12) 0.0187 1.0000 Uani . . . . . .
C8 C -0.0100(3) 0.57072(19) 0.06206(12) 0.0210 1.0000 Uani . . . . . .
C9 C 0.1346(3) 0.58673(19) 0.05284(12) 0.0217 1.0000 Uani . . . . . .
C10 C 0.2175(3) 0.52620(18) 0.08322(12) 0.0197 1.0000 Uani . . . . . .
C11 C 0.3946(3) 0.49931(17) 0.27123(12) 0.0174 1.0000 Uani . . . . . .
C12 C 0.4543(3) 0.4632(2) 0.32049(13) 0.0241 1.0000 Uani . . . . . .
C13 C 0.5983(4) 0.4460(2) 0.32477(15) 0.0308 1.0000 Uani . . . . . .
C14 C 0.6818(3) 0.4653(2) 0.28083(16) 0.0315 1.0000 Uani . . . . . .
C15 C 0.6227(3) 0.5008(2) 0.23164(14) 0.0258 1.0000 Uani . . . . . .
C16 C 0.4792(3) 0.51749(18) 0.22631(12) 0.0205 1.0000 Uani . . . . . .
C21 C 0.1402(3) 0.52956(18) 0.33317(11) 0.0169 1.0000 Uani . . . . . .
C22 C 0.0496(3) 0.4740(2) 0.35801(12) 0.0241 1.0000 Uani . . . . . .
C23 C -0.0105(4) 0.4961(2) 0.40848(14) 0.0321 1.0000 Uani . . . . . .
C24 C 0.0218(4) 0.5721(2) 0.43383(13) 0.0345 1.0000 Uani . . . . . .
C25 C 0.1142(4) 0.6266(2) 0.40991(13) 0.0319 1.0000 Uani . . . . . .
C26 C 0.1742(4) 0.6060(2) 0.35908(13) 0.0260 1.0000 Uani . . . . . .
C31 C 0.3442(3) 0.35363(17) 0.14844(12) 0.0173 1.0000 Uani . . . . . .
C32 C 0.4230(3) 0.31992(19) 0.19411(13) 0.0219 1.0000 Uani . . . . . .
C33 C 0.5620(4) 0.2974(2) 0.18818(15) 0.0303 1.0000 Uani . . . . . .
C34 C 0.6226(3) 0.3094(2) 0.13619(16) 0.0330 1.0000 Uani . . . . . .
C35 C 0.5432(4) 0.3404(2) 0.09021(15) 0.0297 1.0000 Uani . . . . . .
C36 C 0.4037(3) 0.36184(19) 0.09550(13) 0.0224 1.0000 Uani . . . . . .
C41 C 0.0538(3) 0.29854(17) 0.13289(11) 0.0158 1.0000 Uani . . . . . .
C42 C 0.0188(4) 0.2877(2) 0.07562(13) 0.0251 1.0000 Uani . . . . . .
C43 C -0.0646(4) 0.2202(2) 0.05741(14) 0.0315 1.0000 Uani . . . . . .
C44 C -0.1111(4) 0.1633(2) 0.09635(14) 0.0277 1.0000 Uani . . . . . .
C45 C -0.0753(3) 0.17376(19) 0.15388(14) 0.0250 1.0000 Uani . . . . . .
C46 C 0.0067(3) 0.24133(19) 0.17225(12) 0.0215 1.0000 Uani . . . . . .
H1 H 0.1535 0.3551 0.2600 0.0224 1.0000 Uiso . . . . . .
H2 H 0.0145 0.4170 0.2339 0.0239 1.0000 Uiso . . . . . .
H21 H -0.0698 0.5870 0.2265 0.0246 1.0000 Uiso . . . . . .
H31 H -0.0863 0.7151 0.1604 0.0279 1.0000 Uiso . . . . . .
H41 H 0.1602 0.7604 0.1403 0.0278 1.0000 Uiso . . . . . .
H51 H 0.3352 0.6595 0.1916 0.0227 1.0000 Uiso . . . . . .
H71 H -0.1010 0.4755 0.1116 0.0219 1.0000 Uiso . . . . . .
H81 H -0.0883 0.6028 0.0475 0.0253 1.0000 Uiso . . . . . .
H91 H 0.1687 0.6325 0.0316 0.0259 1.0000 Uiso . . . . . .
H101 H 0.3174 0.5228 0.0841 0.0230 1.0000 Uiso . . . . . .
H121 H 0.3994 0.4507 0.3499 0.0284 1.0000 Uiso . . . . . .
H131 H 0.6379 0.4205 0.3567 0.0369 1.0000 Uiso . . . . . .
H141 H 0.7773 0.4549 0.2833 0.0379 1.0000 Uiso . . . . . .
H151 H 0.6803 0.5131 0.2025 0.0316 1.0000 Uiso . . . . . .
H161 H 0.4396 0.5401 0.1931 0.0237 1.0000 Uiso . . . . . .
H221 H 0.0304 0.4231 0.3413 0.0288 1.0000 Uiso . . . . . .
H231 H -0.0725 0.4600 0.4246 0.0379 1.0000 Uiso . . . . . .
H241 H -0.0186 0.5864 0.4673 0.0412 1.0000 Uiso . . . . . .
H251 H 0.1380 0.6761 0.4274 0.0378 1.0000 Uiso . . . . . .
H261 H 0.2340 0.6417 0.3422 0.0308 1.0000 Uiso . . . . . .
H321 H 0.3838 0.3128 0.2285 0.0266 1.0000 Uiso . . . . . .
H331 H 0.6143 0.2749 0.2189 0.0361 1.0000 Uiso . . . . . .
H341 H 0.7161 0.2968 0.1325 0.0387 1.0000 Uiso . . . . . .
H351 H 0.5829 0.3471 0.0566 0.0354 1.0000 Uiso . . . . . .
H361 H 0.3505 0.3821 0.0649 0.0271 1.0000 Uiso . . . . . .
H421 H 0.0504 0.3244 0.0497 0.0304 1.0000 Uiso . . . . . .
H431 H -0.0861 0.2125 0.0192 0.0379 1.0000 Uiso . . . . . .
H441 H -0.1655 0.1190 0.0839 0.0330 1.0000 Uiso . . . . . .
H451 H -0.1071 0.1357 0.1797 0.0299 1.0000 Uiso . . . . . .
H461 H 0.0303 0.2486 0.2100 0.0247 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.496(12)
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 . P1 . 1.923(3) yes
B1 . P2 . 1.926(3) yes
B1 . H1 . 1.062 no
B1 . H2 . 1.008 no
Br1 . Fe2 . 2.3269(6) yes
Br2 . Fe2 . 2.3423(6) yes
Br3 . Fe2 . 2.3300(6) yes
Br4 . Fe2 . 2.3139(6) yes
Fe1 . C1 . 2.032(3) yes
Fe1 . C2 . 2.037(3) yes
Fe1 . C3 . 2.062(3) yes
Fe1 . C4 . 2.066(3) yes
Fe1 . C5 . 2.063(3) yes
Fe1 . C6 . 2.050(3) yes
Fe1 . C7 . 2.051(3) yes
Fe1 . C8 . 2.062(3) yes
Fe1 . C9 . 2.063(3) yes
Fe1 . C10 . 2.046(3) yes
P1 . C1 . 1.789(3) yes
P1 . C11 . 1.808(3) yes
P1 . C21 . 1.808(3) yes
P2 . C6 . 1.795(3) yes
P2 . C31 . 1.806(3) yes
P2 . C41 . 1.811(3) yes
C1 . C2 . 1.438(4) yes
C1 . C5 . 1.440(4) yes
C2 . C3 . 1.426(4) yes
C2 . H21 . 0.963 no
C3 . C4 . 1.416(5) yes
C3 . H31 . 0.962 no
C4 . C5 . 1.420(4) yes
C4 . H41 . 0.971 no
C5 . H51 . 0.965 no
C6 . C7 . 1.436(4) yes
C6 . C10 . 1.442(4) yes
C7 . C8 . 1.425(4) yes
C7 . H71 . 0.954 no
C8 . C9 . 1.429(4) yes
C8 . H81 . 0.954 no
C9 . C10 . 1.418(4) yes
C9 . H91 . 0.953 no
C10 . H101 . 0.951 no
C11 . C12 . 1.393(4) yes
C11 . C16 . 1.397(4) yes
C12 . C13 . 1.397(5) yes
C12 . H121 . 0.914 no
C13 . C14 . 1.377(5) yes
C13 . H131 . 0.919 no
C14 . C15 . 1.385(5) yes
C14 . H141 . 0.923 no
C15 . C16 . 1.392(4) yes
C15 . H151 . 0.923 no
C16 . H161 . 0.925 no
C21 . C22 . 1.389(4) yes
C21 . C26 . 1.396(4) yes
C22 . C23 . 1.396(4) yes
C22 . H221 . 0.919 no
C23 . C24 . 1.381(5) yes
C23 . H231 . 0.923 no
C24 . C25 . 1.381(5) yes
C24 . H241 . 0.926 no
C25 . C26 . 1.397(4) yes
C25 . H251 . 0.916 no
C26 . H261 . 0.913 no
C31 . C32 . 1.389(4) yes
C31 . C36 . 1.407(4) yes
C32 . C33 . 1.386(4) yes
C32 . H321 . 0.920 no
C33 . C34 . 1.398(5) yes
C33 . H331 . 0.930 no
C34 . C35 . 1.382(5) yes
C34 . H341 . 0.921 no
C35 . C36 . 1.384(4) yes
C35 . H351 . 0.905 no
C36 . H361 . 0.919 no
C41 . C42 . 1.387(4) yes
C41 . C46 . 1.396(4) yes
C42 . C43 . 1.393(4) yes
C42 . H421 . 0.911 no
C43 . C44 . 1.383(5) yes
C43 . H431 . 0.922 no
C44 . C45 . 1.393(5) yes
C44 . H441 . 0.917 no
C45 . C46 . 1.388(4) yes
C45 . H451 . 0.924 no
C46 . H461 . 0.916 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 . B1 . P2 . 112.55(16) yes
P1 . B1 . H1 . 110.0 no
P2 . B1 . H1 . 107.9 no
P1 . B1 . H2 . 106.0 no
P2 . B1 . H2 . 106.4 no
H1 . B1 . H2 . 114.2 no
C1 . Fe1 . C2 . 41.41(11) yes
C1 . Fe1 . C3 . 68.92(11) yes
C2 . Fe1 . C3 . 40.71(12) yes
C1 . Fe1 . C4 . 68.57(11) yes
C2 . Fe1 . C4 . 68.19(12) yes
C3 . Fe1 . C4 . 40.12(13) yes
C1 . Fe1 . C5 . 41.18(11) yes
C2 . Fe1 . C5 . 68.93(12) yes
C3 . Fe1 . C5 . 68.08(12) yes
C4 . Fe1 . C5 . 40.25(12) yes
C1 . Fe1 . C6 . 108.97(11) yes
C2 . Fe1 . C6 . 121.28(12) yes
C3 . Fe1 . C6 . 155.35(12) yes
C4 . Fe1 . C6 . 163.85(12) yes
C5 . Fe1 . C6 . 127.51(11) yes
C1 . Fe1 . C7 . 125.97(11) yes
C2 . Fe1 . C7 . 106.80(12) yes
C3 . Fe1 . C7 . 119.02(12) yes
C4 . Fe1 . C7 . 153.42(12) yes
C5 . Fe1 . C7 . 164.58(11) yes
C1 . Fe1 . C8 . 162.14(12) yes
C2 . Fe1 . C8 . 123.58(12) yes
C3 . Fe1 . C8 . 105.65(12) yes
C4 . Fe1 . C8 . 118.94(12) yes
C5 . Fe1 . C8 . 154.21(12) yes
C1 . Fe1 . C9 . 156.56(12) yes
C2 . Fe1 . C9 . 160.32(12) yes
C3 . Fe1 . C9 . 123.50(12) yes
C4 . Fe1 . C9 . 107.07(12) yes
C5 . Fe1 . C9 . 120.65(12) yes
C1 . Fe1 . C10 . 122.17(11) yes
C2 . Fe1 . C10 . 157.63(12) yes
C3 . Fe1 . C10 . 160.87(12) yes
C4 . Fe1 . C10 . 125.48(12) yes
C5 . Fe1 . C10 . 108.93(12) yes
C6 . Fe1 . C7 . 41.01(11) yes
C6 . Fe1 . C8 . 68.46(11) yes
C7 . Fe1 . C8 . 40.54(11) yes
C6 . Fe1 . C9 . 68.46(11) yes
C7 . Fe1 . C9 . 68.39(12) yes
C8 . Fe1 . C9 . 40.52(12) yes
C6 . Fe1 . C10 . 41.22(11) yes
C7 . Fe1 . C10 . 69.04(11) yes
C8 . Fe1 . C10 . 68.38(12) yes
C9 . Fe1 . C10 . 40.38(12) yes
Br2 . Fe2 . Br3 . 109.89(2) yes
Br2 . Fe2 . Br1 . 109.48(2) yes
Br3 . Fe2 . Br1 . 107.62(2) yes
Br2 . Fe2 . Br4 . 110.29(2) yes
Br3 . Fe2 . Br4 . 109.78(2) yes
Br1 . Fe2 . Br4 . 109.74(2) yes
B1 . P1 . C1 . 112.03(13) yes
B1 . P1 . C11 . 111.78(13) yes
C1 . P1 . C11 . 110.87(13) yes
B1 . P1 . C21 . 108.96(13) yes
C1 . P1 . C21 . 104.23(13) yes
C11 . P1 . C21 . 108.62(13) yes
B1 . P2 . C6 . 112.70(13) yes
B1 . P2 . C31 . 115.42(13) yes
C6 . P2 . C31 . 108.06(13) yes
B1 . P2 . C41 . 106.97(13) yes
C6 . P2 . C41 . 106.30(13) yes
C31 . P2 . C41 . 106.86(12) yes
P1 . C1 . Fe1 . 123.19(15) yes
P1 . C1 . C2 . 120.8(2) yes
Fe1 . C1 . C2 . 69.51(16) yes
P1 . C1 . C5 . 131.7(2) yes
Fe1 . C1 . C5 . 70.57(16) yes
C2 . C1 . C5 . 107.4(2) yes
C1 . C2 . Fe1 . 69.08(15) yes
C1 . C2 . C3 . 107.9(3) yes
Fe1 . C2 . C3 . 70.58(17) yes
C1 . C2 . H21 . 124.7 no
Fe1 . C2 . H21 . 125.3 no
C3 . C2 . H21 . 127.4 no
C2 . C3 . Fe1 . 68.71(16) yes
C2 . C3 . C4 . 108.1(3) yes
Fe1 . C3 . C4 . 70.08(17) yes
C2 . C3 . H31 . 125.9 no
Fe1 . C3 . H31 . 124.5 no
C4 . C3 . H31 . 126.0 no
C3 . C4 . Fe1 . 69.80(18) yes
C3 . C4 . C5 . 109.0(3) yes
Fe1 . C4 . C5 . 69.77(16) yes
C3 . C4 . H41 . 124.1 no
Fe1 . C4 . H41 . 126.5 no
C5 . C4 . H41 . 127.0 no
C1 . C5 . C4 . 107.6(3) yes
C1 . C5 . Fe1 . 68.24(15) yes
C4 . C5 . Fe1 . 69.98(17) yes
C1 . C5 . H51 . 126.3 no
C4 . C5 . H51 . 126.1 no
Fe1 . C5 . H51 . 124.8 no
P2 . C6 . Fe1 . 123.70(14) yes
P2 . C6 . C7 . 123.1(2) yes
Fe1 . C6 . C7 . 69.52(16) yes
P2 . C6 . C10 . 129.3(2) yes
Fe1 . C6 . C10 . 69.24(16) yes
C7 . C6 . C10 . 107.5(2) yes
C6 . C7 . Fe1 . 69.47(16) yes
C6 . C7 . C8 . 107.9(2) yes
Fe1 . C7 . C8 . 70.16(17) yes
C6 . C7 . H71 . 126.0 no
Fe1 . C7 . H71 . 125.5 no
C8 . C7 . H71 . 126.1 no
C7 . C8 . Fe1 . 69.30(16) yes
C7 . C8 . C9 . 108.2(2) yes
Fe1 . C8 . C9 . 69.78(16) yes
C7 . C8 . H81 . 125.6 no
Fe1 . C8 . H81 . 125.4 no
C9 . C8 . H81 . 126.1 no
C8 . C9 . Fe1 . 69.70(16) yes
C8 . C9 . C10 . 108.4(3) yes
Fe1 . C9 . C10 . 69.16(16) yes
C8 . C9 . H91 . 125.1 no
Fe1 . C9 . H91 . 124.2 no
C10 . C9 . H91 . 126.4 no
C6 . C10 . C9 . 108.0(3) yes
C6 . C10 . Fe1 . 69.53(15) yes
C9 . C10 . Fe1 . 70.45(17) yes
C6 . C10 . H101 . 126.7 no
C9 . C10 . H101 . 125.3 no
Fe1 . C10 . H101 . 126.4 no
P1 . C11 . C12 . 118.0(2) yes
P1 . C11 . C16 . 121.8(2) yes
C12 . C11 . C16 . 119.7(3) yes
C11 . C12 . C13 . 119.8(3) yes
C11 . C12 . H121 . 120.2 no
C13 . C12 . H121 . 120.0 no
C12 . C13 . C14 . 120.4(3) yes
C12 . C13 . H131 . 120.2 no
C14 . C13 . H131 . 119.4 no
C13 . C14 . C15 . 120.0(3) yes
C13 . C14 . H141 . 121.3 no
C15 . C14 . H141 . 118.7 no
C14 . C15 . C16 . 120.4(3) yes
C14 . C15 . H151 . 118.8 no
C16 . C15 . H151 . 120.8 no
C11 . C16 . C15 . 119.7(3) yes
C11 . C16 . H161 . 120.0 no
C15 . C16 . H161 . 120.3 no
P1 . C21 . C22 . 120.7(2) yes
P1 . C21 . C26 . 118.6(2) yes
C22 . C21 . C26 . 120.5(3) yes
C21 . C22 . C23 . 119.5(3) yes
C21 . C22 . H221 . 119.9 no
C23 . C22 . H221 . 120.6 no
C22 . C23 . C24 . 120.1(3) yes
C22 . C23 . H231 . 119.7 no
C24 . C23 . H231 . 120.2 no
C23 . C24 . C25 . 120.6(3) yes
C23 . C24 . H241 . 119.6 no
C25 . C24 . H241 . 119.8 no
C24 . C25 . C26 . 120.2(3) yes
C24 . C25 . H251 . 120.5 no
C26 . C25 . H251 . 119.3 no
C25 . C26 . C21 . 119.1(3) yes
C25 . C26 . H261 . 121.5 no
C21 . C26 . H261 . 119.4 no
P2 . C31 . C32 . 119.1(2) yes
P2 . C31 . C36 . 120.9(2) yes
C32 . C31 . C36 . 120.0(3) yes
C31 . C32 . C33 . 120.1(3) yes
C31 . C32 . H321 . 120.4 no
C33 . C32 . H321 . 119.6 no
C32 . C33 . C34 . 119.6(3) yes
C32 . C33 . H331 . 119.7 no
C34 . C33 . H331 . 120.7 no
C33 . C34 . C35 . 120.4(3) yes
C33 . C34 . H341 . 119.9 no
C35 . C34 . H341 . 119.6 no
C34 . C35 . C36 . 120.3(3) yes
C34 . C35 . H351 . 119.8 no
C36 . C35 . H351 . 119.9 no
C31 . C36 . C35 . 119.5(3) yes
C31 . C36 . H361 . 120.1 no
C35 . C36 . H361 . 120.5 no
P2 . C41 . C42 . 121.1(2) yes
P2 . C41 . C46 . 118.9(2) yes
C42 . C41 . C46 . 119.9(3) yes
C41 . C42 . C43 . 120.1(3) yes
C41 . C42 . H421 . 120.3 no
C43 . C42 . H421 . 119.6 no
C42 . C43 . C44 . 120.0(3) yes
C42 . C43 . H431 . 119.8 no
C44 . C43 . H431 . 120.1 no
C43 . C44 . C45 . 120.0(3) yes
C43 . C44 . H441 . 119.3 no
C45 . C44 . H441 . 120.7 no
C44 . C45 . C46 . 120.1(3) yes
C44 . C45 . H451 . 119.5 no
C46 . C45 . H451 . 120.4 no
C41 . C46 . C45 . 119.8(3) yes
C41 . C46 . H461 . 119.7 no
C45 . C46 . H461 . 120.5 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 08/02/15 at 16:12:13
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
REM CONT O(1, OCC) F(100, OCC) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 08/02/15 at 16:12:13
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 0 4 x .


_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_jas127
_database_code_depnum_ccdc_archive 'CCDC 1058403'
_audit_update_record             
;
2015-04-08 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_audit_creation_date             13-08-24
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 'jas127 At 14:37 on 24/ 8'
_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                   13.2239(6)
_cell_length_b                   21.5110(9)
_cell_length_c                   14.3499(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.315(2)
_cell_angle_gamma                90
_cell_volume                     4016.0(3)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
As 0.0499 2.0058 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972
2.5310 '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'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 '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'


_cell_formula_units_Z            4

# Given Formula = C41 H43 As1 B1 F6 O1 P3 
# Dc =      1.40 Fooo =   1736.00 Mu =     10.26 M =    844.43
# Found Formula = C41 H43 As1 B1 F6 O1 P3 
# Dc =      1.40 FOOO =   1736.00 Mu =     10.26 M =    844.43

_chemical_formula_sum            'C41 H43 As1 B1 F6 O1 P3'
_chemical_formula_moiety         'C41 H41 B1 P3, As1 F6, H2 O1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         844.43


_cell_measurement_reflns_used    45439
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_max          0.370

_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    1.026

# 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 0.030
0 -1 0 0.030
0 0 1 0.160
0 0 -1 0.210
0 -5 1 0.060
0 -4 -1 0.080
0 6 1 0.051
-17 1 4 0.058
5 -1 -9 0.177


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  0.945
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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            55977
_reflns_number_total             7922
_diffrn_reflns_av_R_equivalents  0.165
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7922 
# Theoretical number of reflections is about 15904 


_diffrn_reflns_theta_min         2.704
_diffrn_reflns_theta_max         26.068
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        26.068
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              26
_reflns_limit_l_min              0
_reflns_limit_l_max              17

_oxford_diffrn_Wilson_B_factor   3.10
_oxford_diffrn_Wilson_scale      130.14

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

_refine_diff_density_min         -1.82
_refine_diff_density_max         1.36


# 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         7920
_refine_ls_number_restraints     36
_refine_ls_number_parameters     478
_oxford_refine_ls_R_factor_ref   0.1601
_refine_ls_wR_factor_ref         0.1932
_refine_ls_goodness_of_fit_ref   0.9314
_refine_ls_shift/su_max          0.0005213
_refine_ls_shift/su_mean         0.0000387


# The values computed from all data 
_oxford_reflns_number_all        7920
_refine_ls_R_factor_all          0.1601
_refine_ls_wR_factor_all         0.1932

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3988
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_gt          0.1597

# 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    mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.09P)² + 6.29P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
As1 As 0.13019(6) 0.60927(3) -0.20490(4) 0.0550 1.0000 Uani . . . . . .
B1 B -0.1134(6) 0.7546(3) 0.1702(5) 0.0470 1.0000 Uani . . . . . .
F1 F 0.0086(4) 0.6330(2) -0.2552(3) 0.1074 1.0000 Uani . . . . . .
F2 F 0.1102(4) 0.5496(3) -0.2823(4) 0.1255 1.0000 Uani . . . . . .
F3 F 0.2463(5) 0.5853(4) -0.1574(4) 0.1609 1.0000 Uani . . . . . .
F4 F 0.1769(5) 0.6507(3) -0.2857(4) 0.1572 1.0000 Uani . . . . . .
F5 F 0.1454(4) 0.6688(3) -0.1271(4) 0.1287 1.0000 Uani . . . . . .
F6 F 0.0739(5) 0.5710(3) -0.1269(3) 0.1386 1.0000 Uani . . . . . .
O101 O 0.4001(3) 0.6492(2) 0.2832(3) 0.0667 1.0000 Uani . . . . . .
P1 P 0.20616(13) 0.58268(8) 0.19758(11) 0.0508 1.0000 Uani . . . . . .
P2 P -0.12344(12) 0.67851(7) 0.23763(10) 0.0421 1.0000 Uani . . . . . .
P3 P -0.06056(12) 0.73921(7) 0.05555(10) 0.0435 1.0000 Uani . . . . . .
C1 C 0.0810(4) 0.5656(3) 0.1188(4) 0.0412 1.0000 Uani . . . . . .
C2 C -0.0219(4) 0.6257(3) 0.2182(4) 0.0428 1.0000 Uani . . . . . .
C3 C 0.0295(4) 0.6748(2) 0.0717(4) 0.0419 1.0000 Uani . . . . . .
C4 C -0.0056(4) 0.6145(3) 0.1157(4) 0.0402 1.0000 Uani . . . . . .
C5 C -0.1019(5) 0.5869(3) 0.0535(4) 0.0488 1.0000 Uani . . . . . .
C11 C 0.1890(4) 0.5549(3) 0.3145(4) 0.0466 1.0000 Uani . . . . . .
C12 C 0.1377(5) 0.5014(3) 0.3294(4) 0.0617 1.0000 Uani . . . . . .
C13 C 0.1202(6) 0.4853(4) 0.4192(5) 0.0804 1.0000 Uani . . . . . .
C14 C 0.1575(7) 0.5232(5) 0.4952(5) 0.0826 1.0000 Uani . . . . . .
C15 C 0.2092(6) 0.5752(4) 0.4817(5) 0.0778 1.0000 Uani . . . . . .
C16 C 0.2250(5) 0.5925(3) 0.3922(4) 0.0601 1.0000 Uani . . . . . .
C21 C 0.2866(5) 0.5226(3) 0.1578(4) 0.0515 1.0000 Uani . . . . . .
C22 C 0.3406(5) 0.4779(3) 0.2163(5) 0.0660 1.0000 Uani . . . . . .
C23 C 0.4077(6) 0.4374(4) 0.1842(7) 0.0835 1.0000 Uani . . . . . .
C24 C 0.4210(7) 0.4412(4) 0.0913(7) 0.0888 1.0000 Uani . . . . . .
C25 C 0.3694(6) 0.4854(4) 0.0317(6) 0.0810 1.0000 Uani . . . . . .
C26 C 0.3034(5) 0.5263(4) 0.0640(5) 0.0683 1.0000 Uani . . . . . .
C31 C -0.0970(4) 0.6960(3) 0.3627(4) 0.0443 1.0000 Uani . . . . . .
C32 C -0.0377(5) 0.6581(3) 0.4285(4) 0.0604 1.0000 Uani . . . . . .
C33 C -0.0186(6) 0.6735(3) 0.5226(5) 0.0684 1.0000 Uani . . . . . .
C34 C -0.0616(7) 0.7257(4) 0.5529(5) 0.0754 1.0000 Uani . . . . . .
C35 C -0.1217(6) 0.7634(4) 0.4888(5) 0.0769 1.0000 Uani . . . . . .
C36 C -0.1396(5) 0.7485(3) 0.3940(4) 0.0635 1.0000 Uani . . . . . .
C41 C -0.2462(5) 0.6390(3) 0.2191(4) 0.0534 1.0000 Uani . U . . . .
C42 C -0.2533(5) 0.5771(3) 0.2406(5) 0.0590 1.0000 Uani . U . . . .
C43 C -0.3471(6) 0.5486(4) 0.2343(5) 0.0712 1.0000 Uani . U . . . .
C44 C -0.4336(7) 0.5812(4) 0.2095(6) 0.0920 1.0000 Uani . U . . . .
C45 C -0.4286(7) 0.6428(5) 0.1887(7) 0.1158 1.0000 Uani . U . . . .
C46 C -0.3350(6) 0.6723(4) 0.1924(6) 0.0936 1.0000 Uani . U . . . .
C51 C 0.0122(5) 0.8071(3) 0.0318(4) 0.0458 1.0000 Uani . . . . . .
C52 C 0.0960(6) 0.8034(3) -0.0118(5) 0.0702 1.0000 Uani . . . . . .
C53 C 0.1495(7) 0.8568(4) -0.0277(6) 0.0883 1.0000 Uani . . . . . .
C54 C 0.1182(6) 0.9134(4) -0.0022(6) 0.0755 1.0000 Uani . . . . . .
C55 C 0.0365(6) 0.9175(3) 0.0431(5) 0.0746 1.0000 Uani . . . . . .
C56 C -0.0184(5) 0.8643(3) 0.0586(5) 0.0639 1.0000 Uani . . . . . .
C61 C -0.1573(5) 0.7273(3) -0.0493(4) 0.0488 1.0000 Uani . . . . . .
C62 C -0.1269(6) 0.7096(4) -0.1333(5) 0.0785 1.0000 Uani . . . . . .
C63 C -0.2008(6) 0.6997(5) -0.2143(5) 0.0930 1.0000 Uani . . . . . .
C64 C -0.3030(6) 0.7088(4) -0.2096(6) 0.0834 1.0000 Uani . . . . . .
C65 C -0.3320(6) 0.7255(4) -0.1283(6) 0.0735 1.0000 Uani . . . . . .
C66 C -0.2606(5) 0.7348(3) -0.0466(5) 0.0572 1.0000 Uani . . . . . .
H1 H -0.0551 0.7840 0.2164 0.0563 1.0000 Uiso R . . . . .
H2 H -0.1826 0.7840 0.1488 0.0715 1.0000 Uiso R . . . . .
H11 H 0.0953 0.5620 0.0554 0.0491 1.0000 Uiso R . . . . .
H12 H 0.0559 0.5265 0.1368 0.0489 1.0000 Uiso R . . . . .
H21 H 0.0413 0.6446 0.2511 0.0510 1.0000 Uiso R . . . . .
H22 H -0.0304 0.5861 0.2478 0.0508 1.0000 Uiso R . . . . .
H31 H 0.0911 0.6898 0.1139 0.0501 1.0000 Uiso R . . . . .
H32 H 0.0482 0.6638 0.0117 0.0498 1.0000 Uiso R . . . . .
H51 H -0.1186 0.5472 0.0766 0.0725 1.0000 Uiso R . . . . .
H52 H -0.0889 0.5816 -0.0099 0.0727 1.0000 Uiso R . . . . .
H53 H -0.1597 0.6139 0.0522 0.0727 1.0000 Uiso R . . . . .
H121 H 0.1139 0.4748 0.2786 0.0738 1.0000 Uiso R . . . . .
H131 H 0.0833 0.4495 0.4273 0.0970 1.0000 Uiso R . . . . .
H141 H 0.1476 0.5125 0.5557 0.0989 1.0000 Uiso R . . . . .
H151 H 0.2354 0.6003 0.5337 0.0927 1.0000 Uiso R . . . . .
H161 H 0.2594 0.6287 0.3833 0.0720 1.0000 Uiso R . . . . .
H221 H 0.3326 0.4753 0.2797 0.0788 1.0000 Uiso R . . . . .
H231 H 0.4426 0.4080 0.2253 0.0986 1.0000 Uiso R . . . . .
H241 H 0.4656 0.4135 0.0685 0.1059 1.0000 Uiso R . . . . .
H251 H 0.3798 0.4878 -0.0301 0.0970 1.0000 Uiso R . . . . .
H261 H 0.2696 0.5559 0.0243 0.0819 1.0000 Uiso R . . . . .
H321 H -0.0100 0.6225 0.4089 0.0719 1.0000 Uiso R . . . . .
H331 H 0.0241 0.6482 0.5659 0.0820 1.0000 Uiso R . . . . .
H341 H -0.0501 0.7359 0.6169 0.0910 1.0000 Uiso R . . . . .
H351 H -0.1511 0.7993 0.5094 0.0907 1.0000 Uiso R . . . . .
H361 H -0.1804 0.7733 0.3513 0.0768 1.0000 Uiso R . . . . .
H421 H -0.1938 0.5541 0.2597 0.0697 1.0000 Uiso R . . . . .
H431 H -0.3502 0.5064 0.2481 0.0860 1.0000 Uiso R . . . . .
H441 H -0.4974 0.5627 0.2070 0.1112 1.0000 Uiso R . . . . .
H451 H -0.4884 0.6657 0.1716 0.1750 1.0000 Uiso R . . . . .
H461 H -0.3326 0.7141 0.1764 0.1240 1.0000 Uiso R . . . . .
H521 H 0.1172 0.7650 -0.0301 0.0840 1.0000 Uiso R . . . . .
H531 H 0.2072 0.8535 -0.0560 0.1047 1.0000 Uiso R . . . . .
H541 H 0.1518 0.9494 -0.0153 0.0910 1.0000 Uiso R . . . . .
H551 H 0.0167 0.9558 0.0634 0.0900 1.0000 Uiso R . . . . .
H561 H -0.0763 0.8675 0.0875 0.0767 1.0000 Uiso R . . . . .
H621 H -0.0578 0.7042 -0.1358 0.0939 1.0000 Uiso R . . . . .
H631 H -0.1811 0.6869 -0.2696 0.1111 1.0000 Uiso R . . . . .
H641 H -0.3521 0.7032 -0.2642 0.0999 1.0000 Uiso R . . . . .
H651 H -0.4007 0.7310 -0.1273 0.0878 1.0000 Uiso R . . . . .
H661 H -0.2814 0.7454 0.0098 0.0680 1.0000 Uiso R . . . . .
H1011 H 0.4296 0.6782 0.3228 0.1025 1.0000 Uiso . . . . . .
H1012 H 0.3369 0.6455 0.2465 0.1024 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.11012(6)
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
As1 . F1 . 1.718(5) yes
As1 . F2 . 1.687(4) yes
As1 . F3 . 1.647(5) yes
As1 . F4 . 1.667(5) yes
As1 . F5 . 1.687(4) yes
As1 . F6 . 1.668(5) yes
B1 . P2 . 1.918(7) yes
B1 . P3 . 1.927(7) yes
B1 . H1 . 1.120 no
B1 . H2 . 1.109 no
O101 . H1011 . 0.885 no
O101 . H1012 . 0.908 no
P1 . C1 . 1.866(6) yes
P1 . C11 . 1.834(6) yes
P1 . C21 . 1.829(7) yes
P2 . C2 . 1.818(6) yes
P2 . C31 . 1.806(6) yes
P2 . C41 . 1.809(6) yes
P3 . C3 . 1.814(6) yes
P3 . C51 . 1.814(6) yes
P3 . C61 . 1.810(6) yes
C1 . C4 . 1.549(7) yes
C1 . H11 . 0.965 no
C1 . H12 . 0.957 no
C2 . C4 . 1.544(7) yes
C2 . H21 . 0.972 no
C2 . H22 . 0.966 no
C3 . C4 . 1.551(7) yes
C3 . H31 . 0.979 no
C3 . H32 . 0.967 no
C4 . C5 . 1.537(7) yes
C5 . H51 . 0.955 no
C5 . H52 . 0.963 no
C5 . H53 . 0.958 no
C11 . C12 . 1.371(9) yes
C11 . C16 . 1.390(8) yes
C12 . C13 . 1.394(9) yes
C12 . H121 . 0.936 no
C13 . C14 . 1.380(11) yes
C13 . H131 . 0.928 no
C14 . C15 . 1.343(11) yes
C14 . H141 . 0.930 no
C15 . C16 . 1.388(10) yes
C15 . H151 . 0.936 no
C16 . H161 . 0.923 no
C21 . C22 . 1.388(9) yes
C21 . C26 . 1.405(9) yes
C22 . C23 . 1.380(10) yes
C22 . H221 . 0.935 no
C23 . C24 . 1.378(11) yes
C23 . H231 . 0.931 no
C24 . C25 . 1.376(11) yes
C24 . H241 . 0.937 no
C25 . C26 . 1.375(10) yes
C25 . H251 . 0.924 no
C26 . H261 . 0.915 no
C31 . C32 . 1.380(8) yes
C31 . C36 . 1.373(8) yes
C32 . C33 . 1.369(9) yes
C32 . H321 . 0.915 no
C33 . C34 . 1.364(10) yes
C33 . H331 . 0.935 no
C34 . C35 . 1.370(10) yes
C34 . H341 . 0.930 no
C35 . C36 . 1.376(9) yes
C35 . H351 . 0.936 no
C36 . H361 . 0.913 no
C41 . C42 . 1.374(8) yes
C41 . C46 . 1.371(10) yes
C42 . C43 . 1.372(9) yes
C42 . H421 . 0.928 no
C43 . C44 . 1.335(10) yes
C43 . H431 . 0.930 no
C44 . C45 . 1.363(11) yes
C44 . H441 . 0.927 no
C45 . C46 . 1.383(11) yes
C45 . H451 . 0.926 no
C46 . H461 . 0.930 no
C51 . C52 . 1.369(9) yes
C51 . C56 . 1.372(9) yes
C52 . C53 . 1.390(10) yes
C52 . H521 . 0.925 no
C53 . C54 . 1.357(10) yes
C53 . H531 . 0.929 no
C54 . C55 . 1.360(10) yes
C54 . H541 . 0.929 no
C55 . C56 . 1.394(9) yes
C55 . H551 . 0.927 no
C56 . H561 . 0.936 no
C61 . C62 . 1.390(9) yes
C61 . C66 . 1.382(8) yes
C62 . C63 . 1.395(9) yes
C62 . H621 . 0.928 no
C63 . C64 . 1.379(10) yes
C63 . H631 . 0.920 no
C64 . C65 . 1.341(10) yes
C64 . H641 . 0.931 no
C65 . C66 . 1.381(9) yes
C65 . H651 . 0.918 no
C66 . H661 . 0.929 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
F1 . As1 . F2 . 85.7(2) yes
F1 . As1 . F3 . 179.0(3) yes
F2 . As1 . F3 . 93.4(3) yes
F1 . As1 . F4 . 89.1(3) yes
F2 . As1 . F4 . 89.0(3) yes
F3 . As1 . F4 . 91.2(4) yes
F1 . As1 . F5 . 92.5(3) yes
F2 . As1 . F5 . 177.8(3) yes
F3 . As1 . F5 . 88.4(3) yes
F4 . As1 . F5 . 92.3(3) yes
F1 . As1 . F6 . 86.1(3) yes
F2 . As1 . F6 . 91.8(3) yes
F3 . As1 . F6 . 93.6(4) yes
F4 . As1 . F6 . 175.1(3) yes
F5 . As1 . F6 . 86.8(3) yes
P2 . B1 . P3 . 110.7(3) yes
P2 . B1 . H1 . 106.6 no
P3 . B1 . H1 . 106.6 no
P2 . B1 . H2 . 119.9 no
P3 . B1 . H2 . 105.6 no
H1 . B1 . H2 . 106.7 no
H1011 . O101 . H1012 . 133.5 no
C1 . P1 . C11 . 104.4(3) yes
C1 . P1 . C21 . 100.1(3) yes
C11 . P1 . C21 . 103.3(3) yes
B1 . P2 . C2 . 109.7(3) yes
B1 . P2 . C31 . 107.8(3) yes
C2 . P2 . C31 . 105.4(3) yes
B1 . P2 . C41 . 117.9(3) yes
C2 . P2 . C41 . 110.6(3) yes
C31 . P2 . C41 . 104.6(3) yes
B1 . P3 . C3 . 110.6(3) yes
B1 . P3 . C51 . 107.9(3) yes
C3 . P3 . C51 . 106.3(3) yes
B1 . P3 . C61 . 115.0(3) yes
C3 . P3 . C61 . 110.4(3) yes
C51 . P3 . C61 . 106.1(3) yes
P1 . C1 . C4 . 117.1(4) yes
P1 . C1 . H11 . 106.5 no
C4 . C1 . H11 . 107.2 no
P1 . C1 . H12 . 108.8 no
C4 . C1 . H12 . 108.4 no
H11 . C1 . H12 . 108.6 no
P2 . C2 . C4 . 118.5(4) yes
P2 . C2 . H21 . 105.0 no
C4 . C2 . H21 . 105.8 no
P2 . C2 . H22 . 109.7 no
C4 . C2 . H22 . 109.1 no
H21 . C2 . H22 . 108.2 no
P3 . C3 . C4 . 117.0(4) yes
P3 . C3 . H31 . 106.4 no
C4 . C3 . H31 . 107.4 no
P3 . C3 . H32 . 109.9 no
C4 . C3 . H32 . 107.5 no
H31 . C3 . H32 . 108.3 no
C2 . C4 . C1 . 107.9(4) yes
C2 . C4 . C3 . 111.1(4) yes
C1 . C4 . C3 . 107.8(4) yes
C2 . C4 . C5 . 111.7(5) yes
C1 . C4 . C5 . 106.6(4) yes
C3 . C4 . C5 . 111.4(4) yes
C4 . C5 . H51 . 111.3 no
C4 . C5 . H52 . 108.9 no
H51 . C5 . H52 . 108.3 no
C4 . C5 . H53 . 110.6 no
H51 . C5 . H53 . 108.4 no
H52 . C5 . H53 . 109.2 no
P1 . C11 . C12 . 124.2(5) yes
P1 . C11 . C16 . 117.6(5) yes
C12 . C11 . C16 . 118.1(6) yes
C11 . C12 . C13 . 121.4(7) yes
C11 . C12 . H121 . 119.9 no
C13 . C12 . H121 . 118.7 no
C12 . C13 . C14 . 119.2(8) yes
C12 . C13 . H131 . 119.9 no
C14 . C13 . H131 . 120.9 no
C13 . C14 . C15 . 119.9(7) yes
C13 . C14 . H141 . 120.0 no
C15 . C14 . H141 . 120.1 no
C14 . C15 . C16 . 121.3(7) yes
C14 . C15 . H151 . 119.4 no
C16 . C15 . H151 . 119.3 no
C11 . C16 . C15 . 120.0(7) yes
C11 . C16 . H161 . 119.1 no
C15 . C16 . H161 . 120.9 no
P1 . C21 . C22 . 124.4(5) yes
P1 . C21 . C26 . 117.4(5) yes
C22 . C21 . C26 . 117.8(6) yes
C21 . C22 . C23 . 121.7(7) yes
C21 . C22 . H221 . 119.6 no
C23 . C22 . H221 . 118.6 no
C22 . C23 . C24 . 119.2(8) yes
C22 . C23 . H231 . 119.5 no
C24 . C23 . H231 . 121.3 no
C23 . C24 . C25 . 120.5(7) yes
C23 . C24 . H241 . 119.8 no
C25 . C24 . H241 . 119.7 no
C24 . C25 . C26 . 120.4(7) yes
C24 . C25 . H251 . 119.5 no
C26 . C25 . H251 . 120.0 no
C21 . C26 . C25 . 120.3(7) yes
C21 . C26 . H261 . 119.4 no
C25 . C26 . H261 . 120.2 no
P2 . C31 . C32 . 122.8(5) yes
P2 . C31 . C36 . 118.6(5) yes
C32 . C31 . C36 . 118.5(6) yes
C31 . C32 . C33 . 120.9(6) yes
C31 . C32 . H321 . 119.5 no
C33 . C32 . H321 . 119.5 no
C32 . C33 . C34 . 120.0(7) yes
C32 . C33 . H331 . 119.8 no
C34 . C33 . H331 . 120.2 no
C33 . C34 . C35 . 119.9(7) yes
C33 . C34 . H341 . 120.4 no
C35 . C34 . H341 . 119.7 no
C34 . C35 . C36 . 120.2(7) yes
C34 . C35 . H351 . 120.1 no
C36 . C35 . H351 . 119.7 no
C35 . C36 . C31 . 120.4(6) yes
C35 . C36 . H361 . 120.3 no
C31 . C36 . H361 . 119.3 no
P2 . C41 . C42 . 121.2(5) yes
P2 . C41 . C46 . 119.8(5) yes
C42 . C41 . C46 . 118.7(6) yes
C41 . C42 . C43 . 121.0(7) yes
C41 . C42 . H421 . 119.6 no
C43 . C42 . H421 . 119.4 no
C42 . C43 . C44 . 120.3(7) yes
C42 . C43 . H431 . 119.7 no
C44 . C43 . H431 . 120.1 no
C43 . C44 . C45 . 119.8(8) yes
C43 . C44 . H441 . 121.0 no
C45 . C44 . H441 . 119.3 no
C44 . C45 . C46 . 121.1(9) yes
C44 . C45 . H451 . 120.0 no
C46 . C45 . H451 . 118.9 no
C45 . C46 . C41 . 119.1(8) yes
C45 . C46 . H461 . 120.3 no
C41 . C46 . H461 . 120.6 no
P3 . C51 . C52 . 122.6(5) yes
P3 . C51 . C56 . 118.4(5) yes
C52 . C51 . C56 . 119.0(6) yes
C51 . C52 . C53 . 120.3(7) yes
C51 . C52 . H521 . 119.5 no
C53 . C52 . H521 . 120.2 no
C52 . C53 . C54 . 120.6(7) yes
C52 . C53 . H531 . 119.3 no
C54 . C53 . H531 . 120.1 no
C53 . C54 . C55 . 119.6(7) yes
C53 . C54 . H541 . 120.8 no
C55 . C54 . H541 . 119.6 no
C54 . C55 . C56 . 120.3(7) yes
C54 . C55 . H551 . 120.0 no
C56 . C55 . H551 . 119.7 no
C55 . C56 . C51 . 120.2(7) yes
C55 . C56 . H561 . 120.0 no
C51 . C56 . H561 . 119.8 no
P3 . C61 . C62 . 119.2(5) yes
P3 . C61 . C66 . 121.1(5) yes
C62 . C61 . C66 . 119.7(6) yes
C61 . C62 . C63 . 119.8(7) yes
C61 . C62 . H621 . 120.5 no
C63 . C62 . H621 . 119.7 no
C62 . C63 . C64 . 118.9(7) yes
C62 . C63 . H631 . 120.0 no
C64 . C63 . H631 . 121.0 no
C63 . C64 . C65 . 121.0(7) yes
C63 . C64 . H641 . 118.8 no
C65 . C64 . H641 . 120.2 no
C64 . C65 . C66 . 121.2(7) yes
C64 . C65 . H651 . 119.0 no
C66 . C65 . H651 . 119.8 no
C61 . C66 . C65 . 119.3(7) yes
C61 . C66 . H661 . 120.1 no
C65 . C66 . H661 . 120.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C16 . H161 . O101 . 130.00 0.923 2.583 3.255(10) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 24/08/13 at 15:54:11
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) H   (  53,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 24/08/13 at 15:54:11
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.01 = C(41) TO C(42) 
U(IJ) 0.0, 0.01 = C(42) TO C(43) 
U(IJ) 0.0, 0.01 = C(43) TO C(44) 
U(IJ) 0.0, 0.01 = C(44) TO C(45) 
U(IJ) 0.0, 0.01 = C(45) TO C(46) 
U(IJ) 0.0, 0.01 = C(46) TO C(41) 
REM DIST 1.0, 0.01 = O(101) TO H(1011) 
REM DIST 0.88, 0.01 = O(101) TO H(1012) 
REM ANGLE 109.0, 0.05 = H(1011) TO O(101) TO H(1012) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 0 2 x .
13 14 1 x .



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/acetone/pentane'
####################################################################### 
# 
# 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_jas124
_database_code_depnum_ccdc_archive 'CCDC 1058396'
_audit_update_record             
;
2015-04-08 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_audit_creation_date             13-07-22
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 'jas124 At 9:13 on 22/ 7'
_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                   14.6204(2)
_cell_length_b                   14.0880(3)
_cell_length_c                   14.7554(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.0115(15)
_cell_angle_gamma                90
_cell_volume                     2873.42(10)

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

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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            4

# Given Formula = C22 H23 B1 Br2 Cl6 N1 P1 
# Dc =      1.65 Fooo =   1416.00 Mu =     34.48 M =    715.74
# Found Formula = C22 H23 B1 Br2 Cl6 N1 P1 
# Dc =      1.65 FOOO =   1416.00 Mu =     34.48 M =    715.74

_chemical_formula_sum            'C22 H23 B1 Br2 Cl6 N1 P1'
_chemical_formula_moiety         'C20 H21 B1 Br1 N1 P1, Br1, 2(C1 H1 Cl3)'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         715.74


_cell_measurement_reflns_used    26216
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.160
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_max          0.290

_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    3.448

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.080
0 0 -1 0.080
9 10 0 0.112
-1 1 0 0.155
-12 -13 0 0.177
9 -10 0 0.125
0 -1 0 0.184


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_T_max  0.614
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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            52435
_reflns_number_total             6590
_diffrn_reflns_av_R_equivalents  0.078
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6590 
# Theoretical number of reflections is about 13200 


_diffrn_reflns_theta_min         2.792
_diffrn_reflns_theta_max         27.498
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.498
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -18
_reflns_limit_h_max              17
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   3.10
_oxford_diffrn_Wilson_scale      57.53

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

_refine_diff_density_min         -1.01
_refine_diff_density_max         1.93


# 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         6590
_refine_ls_number_restraints     0
_refine_ls_number_parameters     298
_oxford_refine_ls_R_factor_ref   0.0733
_refine_ls_wR_factor_ref         0.1020
_refine_ls_goodness_of_fit_ref   0.9651
_refine_ls_shift/su_max          0.0009067
_refine_ls_shift/su_mean         0.0000253


# The values computed from all data 
_oxford_reflns_number_all        6590
_refine_ls_R_factor_all          0.0733
_refine_ls_wR_factor_all         0.1020

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4632
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_gt          0.0900

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 4.58P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.1596(3) 0.1257(3) 0.1612(3) 0.0281 1.0000 Uani . . . . . .
Br1 Br 0.17617(3) 0.06539(3) 0.04635(3) 0.0391 1.0000 Uani . . . . . .
Br2 Br 0.46137(3) 0.67026(3) 0.30967(3) 0.0368 1.0000 Uani . . . . . .
Cl1 Cl 0.09884(8) 0.55588(9) 0.30192(10) 0.0605 1.0000 Uani . . . . . .
Cl2 Cl -0.09936(10) 0.54430(12) 0.18027(10) 0.0760 1.0000 Uani . . . . . .
Cl3 Cl -0.05249(10) 0.52764(11) 0.38406(10) 0.0721 1.0000 Uani . . . . . .
Cl4 Cl 0.27954(8) 0.75420(10) 0.39606(8) 0.0545 1.0000 Uani . . . . . .
Cl5 Cl 0.20470(9) 0.69288(10) 0.54529(9) 0.0594 1.0000 Uani . . . . . .
Cl6 Cl 0.23648(12) 0.89212(11) 0.52139(9) 0.0753 1.0000 Uani . . . . . .
N1 N 0.1024(2) 0.0595(2) 0.2148(2) 0.0267 1.0000 Uani . . . . . .
P1 P 0.08022(6) 0.23970(6) 0.13974(6) 0.0251 1.0000 Uani . . . . . .
C1 C 0.0517(2) 0.2178(2) 0.2472(2) 0.0273 1.0000 Uani . . . . . .
C2 C 0.0687(2) 0.1241(2) 0.2779(2) 0.0265 1.0000 Uani . . . . . .
C3 C 0.0528(3) 0.0931(3) 0.3601(3) 0.0334 1.0000 Uani . . . . . .
C4 C 0.0224(3) 0.1594(3) 0.4139(3) 0.0416 1.0000 Uani . . . . . .
C5 C 0.0080(3) 0.2534(3) 0.3861(3) 0.0403 1.0000 Uani . . . . . .
C6 C 0.0212(3) 0.2832(3) 0.3027(3) 0.0347 1.0000 Uani . . . . . .
C11 C -0.0287(2) 0.2410(2) 0.0375(2) 0.0256 1.0000 Uani . . . . . .
C12 C -0.0214(3) 0.2416(2) -0.0547(3) 0.0298 1.0000 Uani . . . . . .
C13 C -0.1041(3) 0.2397(3) -0.1338(3) 0.0337 1.0000 Uani . . . . . .
C14 C -0.1939(3) 0.2352(3) -0.1222(3) 0.0386 1.0000 Uani . . . . . .
C15 C -0.2016(3) 0.2330(3) -0.0313(3) 0.0392 1.0000 Uani . . . . . .
C16 C -0.1192(2) 0.2371(3) 0.0491(3) 0.0324 1.0000 Uani . . . . . .
C21 C 0.1455(2) 0.3496(2) 0.1459(3) 0.0268 1.0000 Uani . . . . . .
C22 C 0.1119(3) 0.4207(3) 0.0789(3) 0.0312 1.0000 Uani . . . . . .
C23 C 0.1650(3) 0.5036(3) 0.0870(3) 0.0356 1.0000 Uani . . . . . .
C24 C 0.2506(3) 0.5160(3) 0.1614(3) 0.0356 1.0000 Uani . . . . . .
C25 C 0.2837(3) 0.4453(3) 0.2286(3) 0.0376 1.0000 Uani . . . . . .
C26 C 0.2322(3) 0.3614(3) 0.2216(3) 0.0352 1.0000 Uani . . . . . .
C31 C 0.0158(3) 0.0096(3) 0.1469(3) 0.0317 1.0000 Uani . . . . . .
C41 C 0.1705(3) -0.0153(3) 0.2722(3) 0.0357 1.0000 Uani . . . . . .
C101 C -0.0209(3) 0.5820(3) 0.2915(3) 0.0436 1.0000 Uani . . . . . .
C201 C 0.2018(3) 0.7829(4) 0.4608(3) 0.0486 1.0000 Uani . . . . . .
H1 H 0.2315 0.1425 0.2121 0.0343 1.0000 Uiso R . . . . .
H31 H 0.0617 0.0299 0.3791 0.0428 1.0000 Uiso R . . . . .
H41 H 0.0110 0.1397 0.4696 0.0491 1.0000 Uiso R . . . . .
H51 H -0.0106 0.2970 0.4238 0.0481 1.0000 Uiso R . . . . .
H61 H 0.0099 0.3462 0.2832 0.0430 1.0000 Uiso R . . . . .
H121 H 0.0389 0.2431 -0.0630 0.0369 1.0000 Uiso R . . . . .
H131 H -0.0990 0.2408 -0.1945 0.0419 1.0000 Uiso R . . . . .
H141 H -0.2492 0.2333 -0.1761 0.0469 1.0000 Uiso R . . . . .
H151 H -0.2624 0.2293 -0.0236 0.0478 1.0000 Uiso R . . . . .
H161 H -0.1249 0.2370 0.1099 0.0391 1.0000 Uiso R . . . . .
H221 H 0.0541 0.4133 0.0284 0.0381 1.0000 Uiso R . . . . .
H231 H 0.1432 0.5515 0.0421 0.0423 1.0000 Uiso R . . . . .
H241 H 0.2859 0.5716 0.1660 0.0441 1.0000 Uiso R . . . . .
H251 H 0.3408 0.4535 0.2793 0.0452 1.0000 Uiso R . . . . .
H261 H 0.2549 0.3136 0.2662 0.0434 1.0000 Uiso R . . . . .
H311 H -0.0160 -0.0264 0.1837 0.0489 1.0000 Uiso R . . . . .
H312 H -0.0283 0.0551 0.1079 0.0489 1.0000 Uiso R . . . . .
H313 H 0.0369 -0.0324 0.1063 0.0489 1.0000 Uiso R . . . . .
H411 H 0.1355 -0.0599 0.2982 0.0539 1.0000 Uiso R . . . . .
H412 H 0.2205 0.0140 0.3238 0.0539 1.0000 Uiso R . . . . .
H413 H 0.2000 -0.0480 0.2309 0.0540 1.0000 Uiso R . . . . .
H1011 H -0.0273 0.6507 0.2962 0.0519 1.0000 Uiso R . . . . .
H2011 H 0.1358 0.7888 0.4164 0.0609 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.18680(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
B1 . Br1 . 1.980(4) yes
B1 . N1 . 1.621(5) yes
B1 . P1 . 1.946(4) yes
B1 . H1 . 1.100 no
Cl1 . C101 . 1.746(4) yes
Cl2 . C101 . 1.751(4) yes
Cl3 . C101 . 1.754(4) yes
Cl4 . C201 . 1.754(4) yes
Cl5 . C201 . 1.769(5) yes
Cl6 . C201 . 1.768(5) yes
N1 . C2 . 1.495(4) yes
N1 . C31 . 1.509(4) yes
N1 . C41 . 1.506(4) yes
P1 . C1 . 1.793(4) yes
P1 . C11 . 1.802(3) yes
P1 . C21 . 1.806(3) yes
C1 . C2 . 1.392(5) yes
C1 . C6 . 1.398(5) yes
C2 . C3 . 1.379(5) yes
C3 . C4 . 1.388(6) yes
C3 . H31 . 0.930 no
C4 . C5 . 1.382(6) yes
C4 . H41 . 0.933 no
C5 . C6 . 1.373(5) yes
C5 . H51 . 0.927 no
C6 . H61 . 0.930 no
C11 . C12 . 1.398(5) yes
C11 . C16 . 1.390(5) yes
C12 . C13 . 1.382(5) yes
C12 . H121 . 0.928 no
C13 . C14 . 1.378(5) yes
C13 . H131 . 0.923 no
C14 . C15 . 1.383(6) yes
C14 . H141 . 0.931 no
C15 . C16 . 1.389(5) yes
C15 . H151 . 0.934 no
C16 . H161 . 0.929 no
C21 . C22 . 1.381(5) yes
C21 . C26 . 1.399(5) yes
C22 . C23 . 1.386(5) yes
C22 . H221 . 0.932 no
C23 . C24 . 1.380(5) yes
C23 . H231 . 0.926 no
C24 . C25 . 1.377(5) yes
C24 . H241 . 0.928 no
C25 . C26 . 1.387(5) yes
C25 . H251 . 0.929 no
C26 . H261 . 0.924 no
C31 . H311 . 0.965 no
C31 . H312 . 0.958 no
C31 . H313 . 0.961 no
C41 . H411 . 0.965 no
C41 . H412 . 0.961 no
C41 . H413 . 0.971 no
C101 . H1011 . 0.977 no
C201 . H2011 . 0.978 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
Br1 . B1 . N1 . 113.4(2) yes
Br1 . B1 . P1 . 116.6(2) yes
N1 . B1 . P1 . 100.3(2) yes
Br1 . B1 . H1 . 108.7 no
N1 . B1 . H1 . 108.7 no
P1 . B1 . H1 . 108.7 no
B1 . N1 . C2 . 106.3(3) yes
B1 . N1 . C31 . 113.5(3) yes
C2 . N1 . C31 . 108.7(3) yes
B1 . N1 . C41 . 109.0(3) yes
C2 . N1 . C41 . 111.6(3) yes
C31 . N1 . C41 . 107.8(3) yes
B1 . P1 . C1 . 90.72(17) yes
B1 . P1 . C11 . 117.52(17) yes
C1 . P1 . C11 . 110.23(16) yes
B1 . P1 . C21 . 114.93(16) yes
C1 . P1 . C21 . 111.97(16) yes
C11 . P1 . C21 . 110.02(16) yes
P1 . C1 . C2 . 112.5(3) yes
P1 . C1 . C6 . 127.9(3) yes
C2 . C1 . C6 . 119.5(3) yes
N1 . C2 . C1 . 115.8(3) yes
N1 . C2 . C3 . 122.7(3) yes
C1 . C2 . C3 . 121.5(3) yes
C2 . C3 . C4 . 117.9(4) yes
C2 . C3 . H31 . 121.4 no
C4 . C3 . H31 . 120.7 no
C3 . C4 . C5 . 121.4(4) yes
C3 . C4 . H41 . 119.1 no
C5 . C4 . H41 . 119.5 no
C4 . C5 . C6 . 120.5(4) yes
C4 . C5 . H51 . 120.2 no
C6 . C5 . H51 . 119.3 no
C1 . C6 . C5 . 119.2(4) yes
C1 . C6 . H61 . 120.4 no
C5 . C6 . H61 . 120.5 no
P1 . C11 . C12 . 119.2(3) yes
P1 . C11 . C16 . 120.9(3) yes
C12 . C11 . C16 . 119.8(3) yes
C11 . C12 . C13 . 119.9(3) yes
C11 . C12 . H121 . 120.4 no
C13 . C12 . H121 . 119.7 no
C12 . C13 . C14 . 120.2(4) yes
C12 . C13 . H131 . 119.6 no
C14 . C13 . H131 . 120.2 no
C13 . C14 . C15 . 120.2(4) yes
C13 . C14 . H141 . 119.5 no
C15 . C14 . H141 . 120.3 no
C14 . C15 . C16 . 120.3(4) yes
C14 . C15 . H151 . 120.1 no
C16 . C15 . H151 . 119.6 no
C11 . C16 . C15 . 119.5(4) yes
C11 . C16 . H161 . 120.5 no
C15 . C16 . H161 . 120.0 no
P1 . C21 . C22 . 121.8(3) yes
P1 . C21 . C26 . 118.0(3) yes
C22 . C21 . C26 . 120.3(3) yes
C21 . C22 . C23 . 119.4(3) yes
C21 . C22 . H221 . 120.7 no
C23 . C22 . H221 . 119.9 no
C22 . C23 . C24 . 120.8(4) yes
C22 . C23 . H231 . 120.0 no
C24 . C23 . H231 . 119.2 no
C23 . C24 . C25 . 119.8(3) yes
C23 . C24 . H241 . 120.2 no
C25 . C24 . H241 . 120.0 no
C24 . C25 . C26 . 120.5(3) yes
C24 . C25 . H251 . 120.2 no
C26 . C25 . H251 . 119.3 no
C21 . C26 . C25 . 119.3(4) yes
C21 . C26 . H261 . 120.2 no
C25 . C26 . H261 . 120.5 no
N1 . C31 . H311 . 108.9 no
N1 . C31 . H312 . 110.0 no
H311 . C31 . H312 . 109.7 no
N1 . C31 . H313 . 109.2 no
H311 . C31 . H313 . 109.9 no
H312 . C31 . H313 . 109.2 no
N1 . C41 . H411 . 109.9 no
N1 . C41 . H412 . 109.7 no
H411 . C41 . H412 . 109.3 no
N1 . C41 . H413 . 109.1 no
H411 . C41 . H413 . 110.1 no
H412 . C41 . H413 . 108.7 no
Cl3 . C101 . Cl2 . 109.8(2) yes
Cl3 . C101 . Cl1 . 110.5(2) yes
Cl2 . C101 . Cl1 . 110.5(2) yes
Cl3 . C101 . H1011 . 108.8 no
Cl2 . C101 . H1011 . 108.6 no
Cl1 . C101 . H1011 . 108.6 no
Cl5 . C201 . Cl6 . 109.3(2) yes
Cl5 . C201 . Cl4 . 110.3(3) yes
Cl6 . C201 . Cl4 . 110.2(3) yes
Cl5 . C201 . H2011 . 109.0 no
Cl6 . C201 . H2011 . 108.9 no
Cl4 . C201 . H2011 . 109.1 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 22/07/13 at 09:36:43
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE B   (   1,X'S) H   (   1,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 201,X'S) H   (2011,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 22/07/13 at 09:36:43
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform/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_1
_database_code_depnum_ccdc_archive 'CCDC 943300'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 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                   11.13810(10)
_cell_length_b                   12.5367(2)
_cell_length_c                   22.3536(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.2547(8)
_cell_angle_gamma                90
_cell_volume                     3096.36(7)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            4

# Given Formula = C26 H51 B2 Br3 P2 
# Dc =      1.47 Fooo =   1408.00 Mu =     40.26 M =    686.97
# Found Formula = C26 H51 B2 Br3 P2 
# Dc =      1.47 FOOO =   1408.00 Mu =     40.26 M =    686.97

_chemical_formula_sum            'C26 H51 B2 Br3 P2'
_chemical_formula_moiety         'C26 H50 B1 P2, H1 B1 Br3'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         686.97


_cell_measurement_reflns_used    49823
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       lath
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.070
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_max          0.440

_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    4.026

# 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 0.240
0 1 0 0.090
0 -1 0 0.065
-1 0 10 0.030
1 0 -10 0.040
-6 -6 0 0.178
1 -4 0 0.055
8 -5 1 0.145


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_T_max  0.750
_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 (Farrugia, 1997)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            62272
_reflns_number_total             7097
_diffrn_reflns_av_R_equivalents  0.065
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7097 
# Theoretical number of reflections is about 14198 


_diffrn_reflns_theta_min         3.199
_diffrn_reflns_theta_max         27.480
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.480
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_oxford_diffrn_Wilson_B_factor   3.25
_oxford_diffrn_Wilson_scale      9.56

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

_refine_diff_density_min         -2.30
_refine_diff_density_max         0.85


# 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         7079
_refine_ls_number_restraints     176
_refine_ls_number_parameters     451
_oxford_refine_ls_R_factor_ref   0.0549
_refine_ls_wR_factor_ref         0.1251
_refine_ls_goodness_of_fit_ref   0.9925
_refine_ls_shift/su_max          0.0013843
_refine_ls_shift/su_mean         0.0000418


# The values computed from all data 
_oxford_reflns_number_all        7079
_refine_ls_R_factor_all          0.0549
_refine_ls_wR_factor_all         0.1251

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5874
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_gt          0.1172

# 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    refxyz # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 5.05P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.6301(3) 0.8814(3) 0.43219(15) 0.0302 1.0000 Uani . . . . . .
B2 B 0.8635(4) 0.4126(4) 0.5755(2) 0.0472 1.0000 Uani D . . . . .
Br1 Br 0.86146(4) 0.25114(3) 0.568905(18) 0.0510 1.0000 Uani D . . . . .
Br2 Br 0.70171(3) 0.46511(3) 0.597717(18) 0.0436 1.0000 Uani D . . . . .
Br3 Br 0.99294(5) 0.46070(4) 0.64068(3) 0.0870 1.0000 Uani D . . . . .
P1 P 0.69703(6) 0.77856(6) 0.49229(3) 0.0234 1.0000 Uani D . . . . .
P2 P 0.59385(6) 0.79067(6) 0.36168(3) 0.0243 1.0000 Uani D . . . . .
C1 C 0.7164(3) 0.6570(2) 0.44854(13) 0.0288 1.0000 Uani D . . . . .
C2 C 0.6230(3) 0.6549(2) 0.39107(13) 0.0288 1.0000 Uani D . . . . .
C11 C 0.5960(2) 0.7476(2) 0.54879(13) 0.0251 1.0000 Uani D . . . . .
C12 C 0.4847(3) 0.6853(3) 0.52024(14) 0.0335 1.0000 Uani D . . . . .
C13 C 0.3988(3) 0.6620(3) 0.56672(16) 0.0411 1.0000 Uani D . . . . .
C14 C 0.3613(3) 0.7633(3) 0.59627(16) 0.0391 1.0000 Uani D . . . . .
C15 C 0.4707(3) 0.8246(3) 0.62522(15) 0.0354 1.0000 Uani D . . . . .
C16 C 0.5583(3) 0.8489(3) 0.57975(15) 0.0345 1.0000 Uani D . . . . .
C21 C 0.8486(2) 0.8131(2) 0.52890(13) 0.0275 1.0000 Uani D . . . . .
C22 C 0.8998(3) 0.7286(3) 0.57471(17) 0.0382 1.0000 Uani D . . . . .
C23 C 1.0309(3) 0.7546(3) 0.59904(18) 0.0442 1.0000 Uani D . . . . .
C24 C 1.0440(3) 0.8665(3) 0.62550(16) 0.0397 1.0000 Uani D . . . . .
C25 C 0.9918(3) 0.9492(3) 0.57934(16) 0.0402 1.0000 Uani D . . . . .
C26 C 0.8594(3) 0.9256(3) 0.55647(15) 0.0343 1.0000 Uani D . . . . .
C31 C 0.4344(2) 0.7928(2) 0.32851(13) 0.0266 1.0000 Uani D . . . . .
C32 C 0.4112(3) 0.7215(3) 0.27252(15) 0.0356 1.0000 Uani D . . . . .
C33 C 0.2763(3) 0.7209(3) 0.24780(17) 0.0412 1.0000 Uani D . . . . .
C34 C 0.2301(3) 0.8336(3) 0.23458(16) 0.0408 1.0000 Uani D . . . . .
C35 C 0.2504(3) 0.9028(3) 0.29074(17) 0.0388 1.0000 Uani D . . . . .
C36 C 0.3848(3) 0.9057(3) 0.31615(17) 0.0381 1.0000 Uani D . . . . .
C41 C 0.6923(2) 0.8136(3) 0.30306(13) 0.0289 1.0000 Uani D . . . . .
C42 C 0.8240(3) 0.7825(3) 0.32543(16) 0.0382 1.0000 Uani D . . . . .
C43 C 0.9045(3) 0.7973(3) 0.27570(17) 0.0443 1.0000 Uani D . . . . .
C44 C 0.8999(3) 0.9117(3) 0.25244(17) 0.0436 1.0000 Uani D . . . . .
C45 C 0.7700(3) 0.9453(4) 0.23126(18) 0.0499 1.0000 Uani D . . . . .
C46 C 0.6871(3) 0.9284(3) 0.28023(17) 0.0450 1.0000 Uani D . . . . .
H1 H 0.552(3) 0.916(3) 0.4432(16) 0.0378 1.0000 Uiso . . . . . .
H2 H 0.698(4) 0.940(3) 0.4243(18) 0.0446 1.0000 Uiso . . . . . .
H11 H 0.706(2) 0.5939(16) 0.4723(9) 0.0340 1.0000 Uiso D . . . . .
H12 H 0.7984(17) 0.6569(19) 0.4374(10) 0.0340 1.0000 Uiso D . . . . .
H21 H 0.5478(17) 0.6277(18) 0.4012(10) 0.0340 1.0000 Uiso D . . . . .
H22 H 0.652(2) 0.6103(17) 0.3601(9) 0.0342 1.0000 Uiso D . . . . .
H111 H 0.6422(19) 0.7014(16) 0.5791(9) 0.0291 1.0000 Uiso D . . . . .
H121 H 0.442(2) 0.7296(18) 0.4887(10) 0.0400 1.0000 Uiso D . . . . .
H122 H 0.509(2) 0.6197(16) 0.5033(11) 0.0400 1.0000 Uiso D . . . . .
H131 H 0.440(2) 0.6170(18) 0.5970(9) 0.0489 1.0000 Uiso D . . . . .
H132 H 0.3294(18) 0.6238(19) 0.5477(11) 0.0490 1.0000 Uiso D . . . . .
H141 H 0.316(2) 0.8079(17) 0.5658(10) 0.0461 1.0000 Uiso D . . . . .
H142 H 0.311(2) 0.7450(19) 0.6268(10) 0.0461 1.0000 Uiso D . . . . .
H151 H 0.443(2) 0.8917(16) 0.6413(11) 0.0422 1.0000 Uiso D . . . . .
H152 H 0.512(2) 0.7828(19) 0.6583(10) 0.0419 1.0000 Uiso D . . . . .
H161 H 0.6296(18) 0.8831(19) 0.6006(10) 0.0419 1.0000 Uiso D . . . . .
H162 H 0.516(2) 0.8947(18) 0.5491(9) 0.0415 1.0000 Uiso D . . . . .
H211 H 0.8998(18) 0.8119(18) 0.4969(9) 0.0322 1.0000 Uiso D . . . . .
H221 H 0.853(2) 0.728(2) 0.6079(9) 0.0462 1.0000 Uiso D . . . . .
H222 H 0.895(2) 0.6601(16) 0.5567(11) 0.0460 1.0000 Uiso D . . . . .
H231 H 1.079(2) 0.750(2) 0.5658(10) 0.0512 1.0000 Uiso D . . . . .
H232 H 1.062(2) 0.7027(18) 0.6307(10) 0.0511 1.0000 Uiso D . . . . .
H241 H 1.1282(17) 0.8815(18) 0.6376(11) 0.0459 1.0000 Uiso D . . . . .
H242 H 1.003(2) 0.8716(18) 0.6608(9) 0.0460 1.0000 Uiso D . . . . .
H251 H 0.996(2) 1.0191(16) 0.5978(11) 0.0470 1.0000 Uiso D . . . . .
H252 H 1.038(2) 0.949(2) 0.5457(9) 0.0471 1.0000 Uiso D . . . . .
H261 H 0.814(2) 0.9289(19) 0.5899(9) 0.0414 1.0000 Uiso D . . . . .
H262 H 0.827(2) 0.9786(16) 0.5280(10) 0.0409 1.0000 Uiso D . . . . .
H311 H 0.3881(19) 0.7631(17) 0.3584(9) 0.0313 1.0000 Uiso D . . . . .
H321 H 0.459(2) 0.7474(19) 0.2423(9) 0.0430 1.0000 Uiso D . . . . .
H322 H 0.437(2) 0.6503(15) 0.2832(10) 0.0430 1.0000 Uiso D . . . . .
H331 H 0.232(2) 0.6884(19) 0.2778(10) 0.0480 1.0000 Uiso D . . . . .
H332 H 0.266(2) 0.6787(19) 0.2106(9) 0.0481 1.0000 Uiso D . . . . .
H341 H 0.1439(17) 0.8320(19) 0.2188(11) 0.0480 1.0000 Uiso D . . . . .
H342 H 0.275(2) 0.8647(18) 0.2046(10) 0.0480 1.0000 Uiso D . . . . .
H351 H 0.225(2) 0.9751(15) 0.2799(11) 0.0451 1.0000 Uiso D . . . . .
H352 H 0.205(2) 0.874(2) 0.3209(9) 0.0447 1.0000 Uiso D . . . . .
H361 H 0.393(2) 0.9448(18) 0.3536(9) 0.0452 1.0000 Uiso D . . . . .
H362 H 0.428(2) 0.9418(19) 0.2862(10) 0.0451 1.0000 Uiso D . . . . .
H411 H 0.6626(19) 0.7696(17) 0.2689(9) 0.0339 1.0000 Uiso D . . . . .
H421 H 0.854(2) 0.8270(19) 0.3592(10) 0.0459 1.0000 Uiso D . . . . .
H422 H 0.829(2) 0.7091(16) 0.3383(11) 0.0458 1.0000 Uiso D . . . . .
H431 H 0.879(2) 0.7487(18) 0.2433(10) 0.0530 1.0000 Uiso D . . . . .
H432 H 0.9875(17) 0.779(2) 0.2919(11) 0.0532 1.0000 Uiso D . . . . .
H441 H 0.934(2) 0.9592(18) 0.2856(10) 0.0510 1.0000 Uiso D . . . . .
H442 H 0.947(2) 0.917(2) 0.2187(10) 0.0511 1.0000 Uiso D . . . . .
H451 H 0.769(2) 1.0205(16) 0.2199(12) 0.0595 1.0000 Uiso D . . . . .
H452 H 0.739(2) 0.904(2) 0.1960(10) 0.0587 1.0000 Uiso D . . . . .
H461 H 0.6062(18) 0.945(2) 0.2619(11) 0.0549 1.0000 Uiso D . . . . .
H462 H 0.712(2) 0.9762(18) 0.3136(10) 0.0550 1.0000 Uiso D . . . . .
H3 H 0.897(3) 0.448(2) 0.5284(18) 0.0545 1.0000 Uiso D . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.4250(6)
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 . P1 . 1.942(3) yes
B1 . P2 . 1.945(3) yes
B1 . H1 . 1.03(4) no
B1 . H2 . 1.09(4) no
B2 . Br1 . 2.030(5) yes
B2 . Br2 . 2.038(4) yes
B2 . Br3 . 2.008(5) yes
B2 . H3 . 1.24(4) no
P1 . C1 . 1.838(3) yes
P1 . C11 . 1.836(3) yes
P1 . C21 . 1.832(3) yes
P2 . C2 . 1.839(3) yes
P2 . C31 . 1.837(3) yes
P2 . C41 . 1.834(3) yes
C1 . C2 . 1.548(4) yes
C1 . H11 . 0.968(18) no
C1 . H12 . 0.977(17) no
C2 . H21 . 0.958(17) no
C2 . H22 . 0.976(17) no
C11 . C12 . 1.535(4) yes
C11 . C16 . 1.530(4) yes
C11 . H111 . 0.986(17) no
C12 . C13 . 1.527(4) yes
C12 . H121 . 0.972(18) no
C12 . H122 . 0.959(18) no
C13 . C14 . 1.514(5) yes
C13 . H131 . 0.952(18) no
C13 . H132 . 0.962(18) no
C14 . C15 . 1.515(5) yes
C14 . H141 . 0.971(18) no
C14 . H142 . 0.965(18) no
C15 . C16 . 1.525(4) yes
C15 . H151 . 0.980(18) no
C15 . H152 . 0.973(18) no
C16 . H161 . 0.968(18) no
C16 . H162 . 0.970(18) no
C21 . C22 . 1.533(4) yes
C21 . C26 . 1.539(4) yes
C21 . H211 . 0.969(17) no
C22 . C23 . 1.528(4) yes
C22 . H221 . 0.962(18) no
C22 . H222 . 0.947(18) no
C23 . C24 . 1.522(5) yes
C23 . H231 . 0.972(18) no
C23 . H232 . 0.991(18) no
C24 . C25 . 1.525(5) yes
C24 . H241 . 0.961(18) no
C24 . H242 . 0.966(18) no
C25 . C26 . 1.527(4) yes
C25 . H251 . 0.968(18) no
C25 . H252 . 0.967(18) no
C26 . H261 . 0.953(18) no
C26 . H262 . 0.958(18) no
C31 . C32 . 1.533(4) yes
C31 . C36 . 1.532(4) yes
C31 . H311 . 0.968(17) no
C32 . C33 . 1.534(4) yes
C32 . H321 . 0.970(18) no
C32 . H322 . 0.958(18) no
C33 . C34 . 1.521(5) yes
C33 . H331 . 0.973(18) no
C33 . H332 . 0.981(18) no
C34 . C35 . 1.519(5) yes
C34 . H341 . 0.981(18) no
C34 . H342 . 0.966(18) no
C35 . C36 . 1.533(4) yes
C35 . H351 . 0.973(18) no
C35 . H352 . 0.964(18) no
C36 . H361 . 0.964(18) no
C36 . H362 . 0.986(18) no
C41 . C42 . 1.539(4) yes
C41 . C46 . 1.526(5) yes
C41 . H411 . 0.966(18) no
C42 . C43 . 1.526(4) yes
C42 . H421 . 0.963(18) no
C42 . H422 . 0.963(18) no
C43 . C44 . 1.524(5) yes
C43 . H431 . 0.962(18) no
C43 . H432 . 0.977(18) no
C44 . C45 . 1.523(5) yes
C44 . H441 . 0.989(18) no
C44 . H442 . 0.977(18) no
C45 . C46 . 1.534(4) yes
C45 . H451 . 0.977(18) no
C45 . H452 . 0.968(18) no
C46 . H461 . 0.964(18) no
C46 . H462 . 0.969(18) 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 . B1 . P2 . 101.20(16) yes
P1 . B1 . H1 . 112(2) no
P2 . B1 . H1 . 110(2) no
P1 . B1 . H2 . 110(2) no
P2 . B1 . H2 . 110(2) no
H1 . B1 . H2 . 112(3) no
Br1 . B2 . Br2 . 109.7(2) yes
Br1 . B2 . Br3 . 110.6(2) yes
Br2 . B2 . Br3 . 107.6(2) yes
Br1 . B2 . H3 . 107.2(13) no
Br2 . B2 . H3 . 117.5(13) no
Br3 . B2 . H3 . 104.0(13) no
B1 . P1 . C1 . 104.07(14) yes
B1 . P1 . C11 . 113.67(14) yes
C1 . P1 . C11 . 108.31(13) yes
B1 . P1 . C21 . 113.80(15) yes
C1 . P1 . C21 . 105.67(13) yes
C11 . P1 . C21 . 110.64(13) yes
B1 . P2 . C2 . 104.06(14) yes
B1 . P2 . C31 . 114.22(14) yes
C2 . P2 . C31 . 106.02(13) yes
B1 . P2 . C41 . 113.92(15) yes
C2 . P2 . C41 . 107.82(14) yes
C31 . P2 . C41 . 110.12(13) yes
P1 . C1 . C2 . 110.13(19) yes
P1 . C1 . H11 . 110.8(13) no
C2 . C1 . H11 . 108.9(13) no
P1 . C1 . H12 . 108.2(13) no
C2 . C1 . H12 . 109.9(13) no
H11 . C1 . H12 . 108.9(15) no
C1 . C2 . P2 . 110.5(2) yes
C1 . C2 . H21 . 109.0(13) no
P2 . C2 . H21 . 107.1(13) no
C1 . C2 . H22 . 110.6(13) no
P2 . C2 . H22 . 109.6(13) no
H21 . C2 . H22 . 110.0(15) no
P1 . C11 . C12 . 110.8(2) yes
P1 . C11 . C16 . 111.3(2) yes
C12 . C11 . C16 . 110.9(2) yes
P1 . C11 . H111 . 106.6(13) no
C12 . C11 . H111 . 108.1(13) no
C16 . C11 . H111 . 109.0(13) no
C11 . C12 . C13 . 110.9(3) yes
C11 . C12 . H121 . 107.8(14) no
C13 . C12 . H121 . 108.2(14) no
C11 . C12 . H122 . 110.4(14) no
C13 . C12 . H122 . 109.7(14) no
H121 . C12 . H122 . 109.8(16) no
C12 . C13 . C14 . 111.5(3) yes
C12 . C13 . H131 . 108.0(14) no
C14 . C13 . H131 . 108.8(14) no
C12 . C13 . H132 . 109.4(14) no
C14 . C13 . H132 . 111.1(14) no
H131 . C13 . H132 . 107.9(16) no
C13 . C14 . C15 . 111.1(3) yes
C13 . C14 . H141 . 108.9(14) no
C15 . C14 . H141 . 109.1(14) no
C13 . C14 . H142 . 109.0(14) no
C15 . C14 . H142 . 109.0(14) no
H141 . C14 . H142 . 109.7(16) no
C14 . C15 . C16 . 111.3(3) yes
C14 . C15 . H151 . 108.4(14) no
C16 . C15 . H151 . 109.4(14) no
C14 . C15 . H152 . 109.1(14) no
C16 . C15 . H152 . 109.6(14) no
H151 . C15 . H152 . 108.9(16) no
C11 . C16 . C15 . 111.8(3) yes
C11 . C16 . H161 . 109.2(14) no
C15 . C16 . H161 . 108.9(14) no
C11 . C16 . H162 . 108.0(14) no
C15 . C16 . H162 . 107.0(14) no
H161 . C16 . H162 . 112.0(16) no
P1 . C21 . C22 . 112.3(2) yes
P1 . C21 . C26 . 114.6(2) yes
C22 . C21 . C26 . 111.3(3) yes
P1 . C21 . H211 . 105.2(13) no
C22 . C21 . H211 . 106.2(13) no
C26 . C21 . H211 . 106.6(13) no
C21 . C22 . C23 . 110.4(3) yes
C21 . C22 . H221 . 109.0(14) no
C23 . C22 . H221 . 108.5(14) no
C21 . C22 . H222 . 110.2(14) no
C23 . C22 . H222 . 110.5(14) no
H221 . C22 . H222 . 108.2(16) no
C22 . C23 . C24 . 112.1(3) yes
C22 . C23 . H231 . 108.1(14) no
C24 . C23 . H231 . 108.2(14) no
C22 . C23 . H232 . 110.1(14) no
C24 . C23 . H232 . 108.7(14) no
H231 . C23 . H232 . 109.6(16) no
C23 . C24 . C25 . 110.7(3) yes
C23 . C24 . H241 . 109.4(14) no
C25 . C24 . H241 . 109.4(14) no
C23 . C24 . H242 . 110.2(14) no
C25 . C24 . H242 . 109.1(14) no
H241 . C24 . H242 . 108.0(16) no
C24 . C25 . C26 . 111.4(3) yes
C24 . C25 . H251 . 109.4(14) no
C26 . C25 . H251 . 108.3(14) no
C24 . C25 . H252 . 109.1(14) no
C26 . C25 . H252 . 109.2(14) no
H251 . C25 . H252 . 109.4(16) no
C21 . C26 . C25 . 109.6(3) yes
C21 . C26 . H261 . 109.3(14) no
C25 . C26 . H261 . 108.2(14) no
C21 . C26 . H262 . 111.5(14) no
C25 . C26 . H262 . 110.5(14) no
H261 . C26 . H262 . 107.6(16) no
P2 . C31 . C32 . 112.1(2) yes
P2 . C31 . C36 . 113.2(2) yes
C32 . C31 . C36 . 111.8(3) yes
P2 . C31 . H311 . 106.7(13) no
C32 . C31 . H311 . 106.8(13) no
C36 . C31 . H311 . 105.6(13) no
C31 . C32 . C33 . 110.7(3) yes
C31 . C32 . H321 . 108.8(14) no
C33 . C32 . H321 . 110.8(14) no
C31 . C32 . H322 . 109.0(14) no
C33 . C32 . H322 . 109.2(14) no
H321 . C32 . H322 . 108.3(16) no
C32 . C33 . C34 . 110.9(3) yes
C32 . C33 . H331 . 108.6(14) no
C34 . C33 . H331 . 109.4(14) no
C32 . C33 . H332 . 108.4(14) no
C34 . C33 . H332 . 109.6(14) no
H331 . C33 . H332 . 110.0(16) no
C33 . C34 . C35 . 111.0(3) yes
C33 . C34 . H341 . 110.0(14) no
C35 . C34 . H341 . 110.3(14) no
C33 . C34 . H342 . 108.5(14) no
C35 . C34 . H342 . 107.9(14) no
H341 . C34 . H342 . 109.0(16) no
C34 . C35 . C36 . 110.9(3) yes
C34 . C35 . H351 . 108.5(14) no
C36 . C35 . H351 . 108.3(14) no
C34 . C35 . H352 . 109.0(14) no
C36 . C35 . H352 . 109.0(14) no
H351 . C35 . H352 . 111.2(16) no
C35 . C36 . C31 . 110.9(3) yes
C35 . C36 . H361 . 108.7(14) no
C31 . C36 . H361 . 108.5(14) no
C35 . C36 . H362 . 107.5(14) no
C31 . C36 . H362 . 110.4(14) no
H361 . C36 . H362 . 110.7(16) no
P2 . C41 . C42 . 111.0(2) yes
P2 . C41 . C46 . 112.7(2) yes
C42 . C41 . C46 . 110.0(3) yes
P2 . C41 . H411 . 107.4(13) no
C42 . C41 . H411 . 109.2(13) no
C46 . C41 . H411 . 106.3(13) no
C41 . C42 . C43 . 110.9(3) yes
C41 . C42 . H421 . 109.3(14) no
C43 . C42 . H421 . 108.8(14) no
C41 . C42 . H422 . 110.8(14) no
C43 . C42 . H422 . 108.5(14) no
H421 . C42 . H422 . 108.5(16) no
C42 . C43 . C44 . 111.4(3) yes
C42 . C43 . H431 . 108.8(15) no
C44 . C43 . H431 . 110.2(14) no
C42 . C43 . H432 . 108.5(14) no
C44 . C43 . H432 . 109.7(14) no
H431 . C43 . H432 . 108.1(16) no
C43 . C44 . C45 . 110.8(3) yes
C43 . C44 . H441 . 108.5(14) no
C45 . C44 . H441 . 109.2(14) no
C43 . C44 . H442 . 109.1(14) no
C45 . C44 . H442 . 109.1(14) no
H441 . C44 . H442 . 110.1(16) no
C44 . C45 . C46 . 112.0(3) yes
C44 . C45 . H451 . 108.9(15) no
C46 . C45 . H451 . 109.4(15) no
C44 . C45 . H452 . 109.2(15) no
C46 . C45 . H452 . 109.0(15) no
H451 . C45 . H452 . 108.3(16) no
C45 . C46 . C41 . 111.6(3) yes
C45 . C46 . H461 . 106.3(14) no
C41 . C46 . H461 . 110.0(15) no
C45 . C46 . H462 . 109.2(15) no
C41 . C46 . H462 . 109.3(14) no
H461 . C46 . H462 . 110.4(16) no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 02/02/12 at 17:35:00
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT B    (    1 ,X'S,U'S)  UNTIL C    (   46 ) 
CONT H    (    1 ,X'S)  UNTIL H    (    3 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 02/02/12 at 17:35:00
#
#LIST     16                                                                    
ANGLE 0.0, 3. = MEAN BR(1) TO B(2) TO H(3), BR(2) TO B(2) TO H(3) 
ANGLE 0.0, 3. = MEAN BR(3) TO B(2) TO H(3), BR(1) TO B(2) TO H(3) 
ANGLE 0.0, 3. = MEAN BR(2) TO B(2) TO H(3), BR(3) TO B(2) TO H(3) 
REM DIST 1.04, 0.03 = B(1) TO H(1) 
REM DIST 1.04, 0.03 = B(1) TO H(2) 
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            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 1) TO H(12) 
CONT C ( 1) TO H(11) 
REST 0.034, 0.002 = H(12,U[ISO]) 
REST 0.034, 0.002 = H(11,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(12) TO C ( 1) TO P(1) 
CONT H(12) TO C ( 1) TO C(2) 
CONT H(11) TO C ( 1) TO P(1) 
CONT H(11) TO C ( 1) TO C(2) 
ANGLE 109.54, 2.0 = 
CONT H(12) TO C ( 1) TO H(11) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 2) TO H(21) 
CONT C ( 2) TO H(22) 
REST 0.034, 0.002 = H(21,U[ISO]) 
REST 0.034, 0.002 = H(22,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(21) TO C ( 2) TO C(1) 
CONT H(21) TO C ( 2) TO P(2) 
CONT H(22) TO C ( 2) TO C(1) 
CONT H(22) TO C ( 2) TO P(2) 
ANGLE 109.54, 2.0 = 
CONT H(21) TO C ( 2) TO H(22) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 11) TO H(111) 
REST 0.029, 0.002 = H(111,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(111) TO C ( 11) TO P(1) 
CONT H(111) TO C ( 11) TO C(12) 
CONT H(111) TO C ( 11) TO C(16) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 12) TO H(121) 
CONT C ( 12) TO H(122) 
REST 0.040, 0.002 = H(121,U[ISO]) 
REST 0.040, 0.002 = H(122,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) 
CONT H(122) TO C ( 12) TO C(11) 
CONT H(122) TO C ( 12) TO C(13) 
ANGLE 109.54, 2.0 = 
CONT H(121) TO C ( 12) TO H(122) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 13) TO H(131) 
CONT C ( 13) TO H(132) 
REST 0.049, 0.002 = H(131,U[ISO]) 
REST 0.049, 0.002 = H(132,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(131) TO C ( 13) TO C(12) 
CONT H(131) TO C ( 13) TO C(14) 
CONT H(132) TO C ( 13) TO C(12) 
CONT H(132) TO C ( 13) TO C(14) 
ANGLE 109.54, 2.0 = 
CONT H(131) TO C ( 13) TO H(132) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 14) TO H(142) 
CONT C ( 14) TO H(141) 
REST 0.046, 0.002 = H(142,U[ISO]) 
REST 0.046, 0.002 = H(141,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(142) TO C ( 14) TO C(13) 
CONT H(142) TO C ( 14) TO C(15) 
CONT H(141) TO C ( 14) TO C(13) 
CONT H(141) TO C ( 14) TO C(15) 
ANGLE 109.54, 2.0 = 
CONT H(142) TO C ( 14) TO H(141) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 15) TO H(151) 
CONT C ( 15) TO H(152) 
REST 0.042, 0.002 = H(151,U[ISO]) 
REST 0.042, 0.002 = H(152,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(151) TO C ( 15) TO C(14) 
CONT H(151) TO C ( 15) TO C(16) 
CONT H(152) TO C ( 15) TO C(14) 
CONT H(152) TO C ( 15) TO C(16) 
ANGLE 109.54, 2.0 = 
CONT H(151) TO C ( 15) TO H(152) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 16) TO H(161) 
CONT C ( 16) TO H(162) 
REST 0.042, 0.002 = H(161,U[ISO]) 
REST 0.042, 0.002 = H(162,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(161) TO C ( 16) TO C(11) 
CONT H(161) TO C ( 16) TO C(15) 
CONT H(162) TO C ( 16) TO C(11) 
CONT H(162) TO C ( 16) TO C(15) 
ANGLE 109.54, 2.0 = 
CONT H(161) TO C ( 16) TO H(162) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 21) TO H(211) 
REST 0.032, 0.002 = H(211,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(211) TO C ( 21) TO P(1) 
CONT H(211) TO C ( 21) TO C(22) 
CONT H(211) TO C ( 21) TO C(26) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 22) TO H(221) 
CONT C ( 22) TO H(222) 
REST 0.046, 0.002 = H(221,U[ISO]) 
REST 0.046, 0.002 = H(222,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) 
CONT H(222) TO C ( 22) TO C(21) 
CONT H(222) TO C ( 22) TO C(23) 
ANGLE 109.54, 2.0 = 
CONT H(221) TO C ( 22) TO H(222) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 23) TO H(232) 
CONT C ( 23) TO H(231) 
REST 0.051, 0.002 = H(232,U[ISO]) 
REST 0.051, 0.002 = H(231,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(232) TO C ( 23) TO C(22) 
CONT H(232) TO C ( 23) TO C(24) 
CONT H(231) TO C ( 23) TO C(22) 
CONT H(231) TO C ( 23) TO C(24) 
ANGLE 109.54, 2.0 = 
CONT H(232) TO C ( 23) TO H(231) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 24) TO H(241) 
CONT C ( 24) TO H(242) 
REST 0.046, 0.002 = H(241,U[ISO]) 
REST 0.046, 0.002 = H(242,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(241) TO C ( 24) TO C(23) 
CONT H(241) TO C ( 24) TO C(25) 
CONT H(242) TO C ( 24) TO C(23) 
CONT H(242) TO C ( 24) TO C(25) 
ANGLE 109.54, 2.0 = 
CONT H(241) TO C ( 24) TO H(242) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 25) TO H(251) 
CONT C ( 25) TO H(252) 
REST 0.047, 0.002 = H(251,U[ISO]) 
REST 0.047, 0.002 = H(252,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(251) TO C ( 25) TO C(24) 
CONT H(251) TO C ( 25) TO C(26) 
CONT H(252) TO C ( 25) TO C(24) 
CONT H(252) TO C ( 25) TO C(26) 
ANGLE 109.54, 2.0 = 
CONT H(251) TO C ( 25) TO H(252) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 26) TO H(261) 
CONT C ( 26) TO H(262) 
REST 0.041, 0.002 = H(261,U[ISO]) 
REST 0.041, 0.002 = H(262,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(261) TO C ( 26) TO C(25) 
CONT H(261) TO C ( 26) TO C(21) 
CONT H(262) TO C ( 26) TO C(25) 
CONT H(262) TO C ( 26) TO C(21) 
ANGLE 109.54, 2.0 = 
CONT H(261) TO C ( 26) TO H(262) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 31) TO H(311) 
REST 0.031, 0.002 = H(311,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(311) TO C ( 31) TO P(2) 
CONT H(311) TO C ( 31) TO C(32) 
CONT H(311) TO C ( 31) TO C(36) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 32) TO H(321) 
CONT C ( 32) TO H(322) 
REST 0.043, 0.002 = H(321,U[ISO]) 
REST 0.043, 0.002 = H(322,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) 
CONT H(322) TO C ( 32) TO C(31) 
CONT H(322) TO C ( 32) TO C(33) 
ANGLE 109.54, 2.0 = 
CONT H(321) TO C ( 32) TO H(322) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 33) TO H(331) 
CONT C ( 33) TO H(332) 
REST 0.048, 0.002 = H(331,U[ISO]) 
REST 0.048, 0.002 = H(332,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(331) TO C ( 33) TO C(32) 
CONT H(331) TO C ( 33) TO C(34) 
CONT H(332) TO C ( 33) TO C(32) 
CONT H(332) TO C ( 33) TO C(34) 
ANGLE 109.54, 2.0 = 
CONT H(331) TO C ( 33) TO H(332) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 34) TO H(342) 
CONT C ( 34) TO H(341) 
REST 0.048, 0.002 = H(342,U[ISO]) 
REST 0.048, 0.002 = H(341,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(342) TO C ( 34) TO C(33) 
CONT H(342) TO C ( 34) TO C(35) 
CONT H(341) TO C ( 34) TO C(33) 
CONT H(341) TO C ( 34) TO C(35) 
ANGLE 109.54, 2.0 = 
CONT H(342) TO C ( 34) TO H(341) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 35) TO H(351) 
CONT C ( 35) TO H(352) 
REST 0.045, 0.002 = H(351,U[ISO]) 
REST 0.045, 0.002 = H(352,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(351) TO C ( 35) TO C(34) 
CONT H(351) TO C ( 35) TO C(36) 
CONT H(352) TO C ( 35) TO C(34) 
CONT H(352) TO C ( 35) TO C(36) 
ANGLE 109.54, 2.0 = 
CONT H(351) TO C ( 35) TO H(352) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 36) TO H(361) 
CONT C ( 36) TO H(362) 
REST 0.045, 0.002 = H(361,U[ISO]) 
REST 0.045, 0.002 = H(362,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(361) TO C ( 36) TO C(35) 
CONT H(361) TO C ( 36) TO C(31) 
CONT H(362) TO C ( 36) TO C(35) 
CONT H(362) TO C ( 36) TO C(31) 
ANGLE 109.54, 2.0 = 
CONT H(361) TO C ( 36) TO H(362) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 41) TO H(411) 
REST 0.034, 0.002 = H(411,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(411) TO C ( 41) TO P(2) 
CONT H(411) TO C ( 41) TO C(42) 
CONT H(411) TO C ( 41) TO C(46) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 42) TO H(421) 
CONT C ( 42) TO H(422) 
REST 0.046, 0.002 = H(421,U[ISO]) 
REST 0.046, 0.002 = H(422,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) 
CONT H(422) TO C ( 42) TO C(41) 
CONT H(422) TO C ( 42) TO C(43) 
ANGLE 109.54, 2.0 = 
CONT H(421) TO C ( 42) TO H(422) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 43) TO H(432) 
CONT C ( 43) TO H(431) 
REST 0.053, 0.002 = H(432,U[ISO]) 
REST 0.053, 0.002 = H(431,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(432) TO C ( 43) TO C(42) 
CONT H(432) TO C ( 43) TO C(44) 
CONT H(431) TO C ( 43) TO C(42) 
CONT H(431) TO C ( 43) TO C(44) 
ANGLE 109.54, 2.0 = 
CONT H(432) TO C ( 43) TO H(431) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 44) TO H(441) 
CONT C ( 44) TO H(442) 
REST 0.051, 0.002 = H(441,U[ISO]) 
REST 0.051, 0.002 = H(442,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(441) TO C ( 44) TO C(43) 
CONT H(441) TO C ( 44) TO C(45) 
CONT H(442) TO C ( 44) TO C(43) 
CONT H(442) TO C ( 44) TO C(45) 
ANGLE 109.54, 2.0 = 
CONT H(441) TO C ( 44) TO H(442) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 45) TO H(451) 
CONT C ( 45) TO H(452) 
REST 0.059, 0.002 = H(451,U[ISO]) 
REST 0.059, 0.002 = H(452,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(451) TO C ( 45) TO C(44) 
CONT H(451) TO C ( 45) TO C(46) 
CONT H(452) TO C ( 45) TO C(44) 
CONT H(452) TO C ( 45) TO C(46) 
ANGLE 109.54, 2.0 = 
CONT H(451) TO C ( 45) TO H(452) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 46) TO H(462) 
CONT C ( 46) TO H(461) 
REST 0.055, 0.002 = H(462,U[ISO]) 
REST 0.055, 0.002 = H(461,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(462) TO C ( 46) TO C(45) 
CONT H(462) TO C ( 46) TO C(41) 
CONT H(461) TO C ( 46) TO C(45) 
CONT H(461) TO C ( 46) TO C(41) 
ANGLE 109.54, 2.0 = 
CONT H(462) TO C ( 46) TO H(461) 
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
-3 0 7 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_jas166(JSW418)
_database_code_depnum_ccdc_archive 'CCDC 1058392'
_audit_update_record             
;
2015-04-08 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_audit_creation_date             15-02-07
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'C:\Users\Jas\Desktop\jas166(JSW4 At 17:15 on'
_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                   10.3352(2)
_cell_length_b                   10.6422(2)
_cell_length_c                   15.0052(4)
_cell_angle_alpha                74.012(2)
_cell_angle_beta                 85.306(2)
_cell_angle_gamma                89.5144(19)
_cell_volume                     1581.08(6)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 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'
As -0.9300 1.0051 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972
2.5310 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 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'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe -1.1336 3.1974 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 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'


_cell_formula_units_Z            2

# Given Formula = C34 H30 As1 B1 F6 Fe1 P2 
# Dc =      1.59 Fooo =    764.00 Mu =     64.71 M =    756.13
# Found Formula = C34 H30 As1 B1 F6 Fe1 P2 
# Dc =      1.59 FOOO =    764.00 Mu =     64.71 M =    756.13

_chemical_formula_sum            'C34 H30 As1 B1 F6 Fe1 P2'
_chemical_formula_moiety         'C34 H30 B1 Fe1 P2, As1 F6'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         756.13


_cell_measurement_reflns_used    11300
_cell_measurement_theta_min      4
_cell_measurement_theta_max      72
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.084
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_max          0.271

_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    6.471

# Sheldrick geometric approximatio 0.31 0.58 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_T_max  0.58
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Agilent Technologies, 2013)'
_computing_cell_refinement       'CrysAlis PRO, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis PRO, (Agilent Technologies, 2013)'
_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      150
_diffrn_reflns_number            17516
_reflns_number_total             6249
_diffrn_reflns_av_R_equivalents  0.022
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6249 
# Theoretical number of reflections is about 12507 


_diffrn_reflns_theta_min         4.293
_diffrn_reflns_theta_max         72.343
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        72.343
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -12
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   1.84
_oxford_diffrn_Wilson_scale      0.06

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

_refine_diff_density_min         -0.44
_refine_diff_density_max         0.37


# 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         6249
_refine_ls_number_restraints     0
_refine_ls_number_parameters     407
_oxford_refine_ls_R_factor_ref   0.0265
_refine_ls_wR_factor_ref         0.0708
_refine_ls_goodness_of_fit_ref   0.9615
_refine_ls_shift/su_max          0.0015141
_refine_ls_shift/su_mean         0.0000280


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6249
_refine_ls_R_factor_all          0.0265
_refine_ls_wR_factor_all         0.0708

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6144
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_gt          0.0706

# 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 #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.166E+04 0.280E+04 0.178E+04 806. 202. 
;

# 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
As1 As 0.078104(18) 0.928691(17) 0.289763(13) 0.0275 1.0000 Uani . . . . . .
B1 B 0.41586(17) 0.39303(17) 0.17726(12) 0.0232 1.0000 Uani . . . . . .
F1 F 0.22188(11) 1.01440(11) 0.28068(9) 0.0428 1.0000 Uani . . . . . .
F2 F 0.14376(13) 0.79125(11) 0.35862(9) 0.0474 1.0000 Uani . . . . . .
F3 F 0.01040(12) 1.06502(11) 0.22006(9) 0.0412 1.0000 Uani . . . . . .
F4 F 0.13309(15) 0.88254(11) 0.19259(8) 0.0492 1.0000 Uani . . . . . .
F5 F -0.06435(13) 0.84439(12) 0.29825(10) 0.0542 1.0000 Uani . . . . . .
F6 F 0.02797(14) 0.97914(12) 0.38582(9) 0.0505 1.0000 Uani . . . . . .
Fe1 Fe 0.11839(2) 0.40755(2) 0.336521(16) 0.0197 1.0000 Uani . . . . . .
P1 P 0.26509(4) 0.47425(4) 0.11834(3) 0.0197 1.0000 Uani . . . . . .
P2 P 0.44399(4) 0.41302(4) 0.29784(3) 0.0211 1.0000 Uani . . . . . .
C1 C 0.12075(14) 0.47134(14) 0.19468(10) 0.0198 1.0000 Uani . . . . . .
C2 C 0.02810(16) 0.36636(16) 0.23099(11) 0.0246 1.0000 Uani . . . . . .
C3 C -0.06416(16) 0.40631(17) 0.29355(12) 0.0269 1.0000 Uani . . . . . .
C4 C -0.02950(15) 0.53435(16) 0.29603(11) 0.0247 1.0000 Uani . . . . . .
C5 C 0.08441(15) 0.57540(15) 0.23510(11) 0.0221 1.0000 Uani . . . . . .
C6 C 0.30131(15) 0.37190(15) 0.37603(10) 0.0229 1.0000 Uani . . . . . .
C7 C 0.23032(17) 0.25088(16) 0.39200(12) 0.0274 1.0000 Uani . . . . . .
C8 C 0.12062(17) 0.25356(18) 0.45464(12) 0.0318 1.0000 Uani . . . . . .
C9 C 0.12232(18) 0.37478(19) 0.47732(11) 0.0320 1.0000 Uani . . . . . .
C10 C 0.23362(17) 0.44867(17) 0.42951(11) 0.0273 1.0000 Uani . . . . . .
C11 C 0.28728(16) 0.64216(15) 0.05004(11) 0.0243 1.0000 Uani . . . . . .
C12 C 0.18053(17) 0.71362(17) 0.01232(12) 0.0295 1.0000 Uani . . . . . .
C13 C 0.1985(2) 0.83968(18) -0.04561(13) 0.0361 1.0000 Uani . . . . . .
C14 C 0.3217(2) 0.89515(18) -0.06536(14) 0.0405 1.0000 Uani . . . . . .
C15 C 0.4274(2) 0.82655(19) -0.02738(15) 0.0396 1.0000 Uani . . . . . .
C16 C 0.41064(17) 0.69956(17) 0.02955(13) 0.0308 1.0000 Uani . . . . . .
C21 C 0.23012(15) 0.38051(16) 0.03816(11) 0.0225 1.0000 Uani . . . . . .
C22 C 0.20912(17) 0.24653(17) 0.07324(12) 0.0277 1.0000 Uani . . . . . .
C23 C 0.18458(18) 0.17102(18) 0.01366(13) 0.0326 1.0000 Uani . . . . . .
C24 C 0.18507(19) 0.2299(2) -0.08141(13) 0.0362 1.0000 Uani . . . . . .
C25 C 0.20883(18) 0.3620(2) -0.11619(12) 0.0340 1.0000 Uani . . . . . .
C26 C 0.22962(16) 0.43932(18) -0.05723(11) 0.0276 1.0000 Uani . . . . . .
C31 C 0.49818(15) 0.57226(16) 0.30202(11) 0.0239 1.0000 Uani . . . . . .
C32 C 0.42687(17) 0.68104(17) 0.26049(13) 0.0308 1.0000 Uani . . . . . .
C33 C 0.46463(18) 0.80570(18) 0.26134(14) 0.0343 1.0000 Uani . . . . . .
C34 C 0.57536(19) 0.82153(18) 0.30402(13) 0.0345 1.0000 Uani . . . . . .
C35 C 0.64701(18) 0.7144(2) 0.34499(13) 0.0340 1.0000 Uani . . . . . .
C36 C 0.60941(16) 0.58957(18) 0.34499(12) 0.0283 1.0000 Uani . . . . . .
C41 C 0.56215(16) 0.29289(16) 0.34774(12) 0.0261 1.0000 Uani . . . . . .
C42 C 0.57304(19) 0.2583(2) 0.44353(14) 0.0380 1.0000 Uani . . . . . .
C43 C 0.6604(2) 0.1639(2) 0.48303(15) 0.0457 1.0000 Uani . . . . . .
C44 C 0.73634(19) 0.10288(19) 0.42717(16) 0.0415 1.0000 Uani . . . . . .
C45 C 0.72619(17) 0.13581(18) 0.33247(15) 0.0350 1.0000 Uani . . . . . .
C46 C 0.63922(16) 0.23137(17) 0.29193(13) 0.0290 1.0000 Uani . . . . . .
H1 H 0.5036 0.4196 0.1269 0.0350 1.0000 Uiso R . . . . .
H2 H 0.3943 0.2895 0.1953 0.0292 1.0000 Uiso R . . . . .
H21 H 0.0309 0.2827 0.2157 0.0289 1.0000 Uiso R . . . . .
H31 H -0.1349 0.3535 0.3309 0.0332 1.0000 Uiso R . . . . .
H41 H -0.0720 0.5836 0.3336 0.0309 1.0000 Uiso R . . . . .
H51 H 0.1290 0.6602 0.2220 0.0274 1.0000 Uiso R . . . . .
H71 H 0.2553 0.1797 0.3658 0.0341 1.0000 Uiso R . . . . .
H81 H 0.0564 0.1849 0.4775 0.0386 1.0000 Uiso R . . . . .
H91 H 0.0583 0.4025 0.5170 0.0376 1.0000 Uiso R . . . . .
H101 H 0.2603 0.5351 0.4304 0.0333 1.0000 Uiso R . . . . .
H121 H 0.0986 0.6763 0.0271 0.0352 1.0000 Uiso R . . . . .
H131 H 0.1273 0.8847 -0.0701 0.0435 1.0000 Uiso R . . . . .
H141 H 0.3359 0.9801 -0.1046 0.0487 1.0000 Uiso R . . . . .
H151 H 0.5124 0.8649 -0.0405 0.0484 1.0000 Uiso R . . . . .
H161 H 0.4860 0.6518 0.0536 0.0362 1.0000 Uiso R . . . . .
H221 H 0.2106 0.2046 0.1378 0.0327 1.0000 Uiso R . . . . .
H231 H 0.1674 0.0816 0.0393 0.0386 1.0000 Uiso R . . . . .
H241 H 0.1685 0.1786 -0.1207 0.0428 1.0000 Uiso R . . . . .
H251 H 0.2089 0.4031 -0.1807 0.0404 1.0000 Uiso R . . . . .
H261 H 0.2447 0.5303 -0.0822 0.0334 1.0000 Uiso R . . . . .
H321 H 0.3518 0.6700 0.2325 0.0367 1.0000 Uiso R . . . . .
H331 H 0.4145 0.8786 0.2348 0.0405 1.0000 Uiso R . . . . .
H341 H 0.6000 0.9035 0.3045 0.0407 1.0000 Uiso R . . . . .
H351 H 0.7213 0.7242 0.3742 0.0416 1.0000 Uiso R . . . . .
H361 H 0.6567 0.5177 0.3738 0.0334 1.0000 Uiso R . . . . .
H421 H 0.5195 0.2972 0.4812 0.0459 1.0000 Uiso R . . . . .
H431 H 0.6677 0.1398 0.5473 0.0549 1.0000 Uiso R . . . . .
H441 H 0.7945 0.0397 0.4547 0.0491 1.0000 Uiso R . . . . .
H451 H 0.7781 0.0972 0.2945 0.0415 1.0000 Uiso R . . . . .
H461 H 0.6317 0.2539 0.2284 0.0346 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       9.0(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          4.23(4)
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
As1 . F1 . 1.7263(11) yes
As1 . F2 . 1.7126(11) yes
As1 . F3 . 1.7190(11) yes
As1 . F4 . 1.7159(11) yes
As1 . F5 . 1.7081(12) yes
As1 . F6 . 1.7128(12) yes
B1 . P1 . 1.9335(17) yes
B1 . P2 . 1.9242(17) yes
B1 . H1 . 1.117 no
B1 . H2 . 1.080 no
Fe1 . C1 . 2.0462(14) yes
Fe1 . C2 . 2.0498(16) yes
Fe1 . C3 . 2.0445(16) yes
Fe1 . C4 . 2.0474(16) yes
Fe1 . C5 . 2.0517(15) yes
Fe1 . C6 . 2.0290(15) yes
Fe1 . C7 . 2.0424(16) yes
Fe1 . C8 . 2.0576(17) yes
Fe1 . C9 . 2.0481(16) yes
Fe1 . C10 . 2.0430(16) yes
P1 . C1 . 1.8001(15) yes
P1 . C11 . 1.8044(16) yes
P1 . C21 . 1.8200(15) yes
P2 . C6 . 1.7854(16) yes
P2 . C31 . 1.8083(16) yes
P2 . C41 . 1.8117(16) yes
C1 . C2 . 1.435(2) yes
C1 . C5 . 1.436(2) yes
C2 . C3 . 1.427(2) yes
C2 . H21 . 0.978 no
C3 . C4 . 1.423(2) yes
C3 . H31 . 0.965 no
C4 . C5 . 1.423(2) yes
C4 . H41 . 0.951 no
C5 . H51 . 0.980 no
C6 . C7 . 1.439(2) yes
C6 . C10 . 1.435(2) yes
C7 . C8 . 1.418(2) yes
C7 . H71 . 0.969 no
C8 . C9 . 1.422(3) yes
C8 . H81 . 0.961 no
C9 . C10 . 1.423(3) yes
C9 . H91 . 0.953 no
C10 . H101 . 0.967 no
C11 . C12 . 1.402(2) yes
C11 . C16 . 1.392(2) yes
C12 . C13 . 1.388(3) yes
C12 . H121 . 0.922 no
C13 . C14 . 1.383(3) yes
C13 . H131 . 0.920 no
C14 . C15 . 1.383(3) yes
C14 . H141 . 0.939 no
C15 . C16 . 1.389(3) yes
C15 . H151 . 0.954 no
C16 . H161 . 0.966 no
C21 . C22 . 1.389(2) yes
C21 . C26 . 1.396(2) yes
C22 . C23 . 1.395(2) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.391(3) yes
C23 . H231 . 0.935 no
C24 . C25 . 1.375(3) yes
C24 . H241 . 0.933 no
C25 . C26 . 1.393(2) yes
C25 . H251 . 0.946 no
C26 . H261 . 0.947 no
C31 . C32 . 1.391(2) yes
C31 . C36 . 1.401(2) yes
C32 . C33 . 1.390(2) yes
C32 . H321 . 0.935 no
C33 . C34 . 1.390(3) yes
C33 . H331 . 0.941 no
C34 . C35 . 1.379(3) yes
C34 . H341 . 0.914 no
C35 . C36 . 1.387(3) yes
C35 . H351 . 0.935 no
C36 . H361 . 0.926 no
C41 . C42 . 1.396(3) yes
C41 . C46 . 1.396(2) yes
C42 . C43 . 1.386(3) yes
C42 . H421 . 0.933 no
C43 . C44 . 1.387(3) yes
C43 . H431 . 0.937 no
C44 . C45 . 1.379(3) yes
C44 . H441 . 0.930 no
C45 . C46 . 1.395(2) yes
C45 . H451 . 0.925 no
C46 . H461 . 0.926 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
F1 . As1 . F2 . 90.92(6) yes
F1 . As1 . F3 . 89.96(6) yes
F2 . As1 . F3 . 179.03(6) yes
F1 . As1 . F4 . 88.80(6) yes
F2 . As1 . F4 . 89.95(6) yes
F3 . As1 . F4 . 89.65(6) yes
F1 . As1 . F5 . 179.72(6) yes
F2 . As1 . F5 . 89.34(7) yes
F3 . As1 . F5 . 89.79(6) yes
F4 . As1 . F5 . 91.08(7) yes
F1 . As1 . F6 . 89.05(6) yes
F2 . As1 . F6 . 90.58(6) yes
F3 . As1 . F6 . 89.85(6) yes
F4 . As1 . F6 . 177.79(6) yes
F5 . As1 . F6 . 91.06(7) yes
P1 . B1 . P2 . 117.92(9) yes
P1 . B1 . H1 . 109.3 no
P2 . B1 . H1 . 112.7 no
P1 . B1 . H2 . 104.3 no
P2 . B1 . H2 . 100.3 no
H1 . B1 . H2 . 111.6 no
C1 . Fe1 . C2 . 41.02(6) yes
C1 . Fe1 . C3 . 68.68(6) yes
C2 . Fe1 . C3 . 40.81(6) yes
C1 . Fe1 . C4 . 68.67(6) yes
C2 . Fe1 . C4 . 68.75(6) yes
C3 . Fe1 . C4 . 40.70(7) yes
C1 . Fe1 . C5 . 41.01(6) yes
C2 . Fe1 . C5 . 68.99(6) yes
C3 . Fe1 . C5 . 68.55(6) yes
C4 . Fe1 . C5 . 40.63(6) yes
C1 . Fe1 . C6 . 110.55(6) yes
C2 . Fe1 . C6 . 131.15(6) yes
C3 . Fe1 . C6 . 168.45(7) yes
C4 . Fe1 . C6 . 150.62(7) yes
C5 . Fe1 . C6 . 118.97(6) yes
C1 . Fe1 . C7 . 117.60(6) yes
C2 . Fe1 . C7 . 107.30(7) yes
C3 . Fe1 . C7 . 127.94(7) yes
C4 . Fe1 . C7 . 166.28(7) yes
C5 . Fe1 . C7 . 151.67(7) yes
C1 . Fe1 . C8 . 148.58(7) yes
C2 . Fe1 . C8 . 114.28(7) yes
C3 . Fe1 . C8 . 105.57(7) yes
C4 . Fe1 . C8 . 127.97(7) yes
C5 . Fe1 . C8 . 167.56(7) yes
C1 . Fe1 . C9 . 170.67(7) yes
C2 . Fe1 . C9 . 146.42(7) yes
C3 . Fe1 . C9 . 114.00(7) yes
C4 . Fe1 . C9 . 107.12(7) yes
C5 . Fe1 . C9 . 130.53(7) yes
C1 . Fe1 . C10 . 132.74(7) yes
C2 . Fe1 . C10 . 171.41(7) yes
C3 . Fe1 . C10 . 147.45(7) yes
C4 . Fe1 . C10 . 116.37(7) yes
C5 . Fe1 . C10 . 109.93(7) yes
C6 . Fe1 . C7 . 41.40(7) yes
C6 . Fe1 . C8 . 68.76(7) yes
C7 . Fe1 . C8 . 40.45(7) yes
C6 . Fe1 . C9 . 68.74(7) yes
C7 . Fe1 . C9 . 68.46(7) yes
C8 . Fe1 . C9 . 40.54(8) yes
C6 . Fe1 . C10 . 41.28(6) yes
C7 . Fe1 . C10 . 69.38(7) yes
C8 . Fe1 . C10 . 68.71(7) yes
C9 . Fe1 . C10 . 40.72(7) yes
B1 . P1 . C1 . 115.84(7) yes
B1 . P1 . C11 . 115.58(8) yes
C1 . P1 . C11 . 105.63(7) yes
B1 . P1 . C21 . 105.01(7) yes
C1 . P1 . C21 . 107.54(7) yes
C11 . P1 . C21 . 106.68(7) yes
B1 . P2 . C6 . 111.47(7) yes
B1 . P2 . C31 . 116.91(8) yes
C6 . P2 . C31 . 106.76(7) yes
B1 . P2 . C41 . 107.40(8) yes
C6 . P2 . C41 . 104.83(8) yes
C31 . P2 . C41 . 108.81(8) yes
P1 . C1 . Fe1 . 123.06(8) yes
P1 . C1 . C2 . 127.94(11) yes
Fe1 . C1 . C2 . 69.62(9) yes
P1 . C1 . C5 . 123.92(12) yes
Fe1 . C1 . C5 . 69.70(8) yes
C2 . C1 . C5 . 108.02(13) yes
C1 . C2 . Fe1 . 69.36(8) yes
C1 . C2 . C3 . 107.44(14) yes
Fe1 . C2 . C3 . 69.40(9) yes
C1 . C2 . H21 . 125.0 no
Fe1 . C2 . H21 . 125.5 no
C3 . C2 . H21 . 127.6 no
C2 . C3 . Fe1 . 69.80(9) yes
C2 . C3 . C4 . 108.49(14) yes
Fe1 . C3 . C4 . 69.76(9) yes
C2 . C3 . H31 . 125.8 no
Fe1 . C3 . H31 . 123.4 no
C4 . C3 . H31 . 125.6 no
C3 . C4 . Fe1 . 69.54(9) yes
C3 . C4 . C5 . 108.31(14) yes
Fe1 . C4 . C5 . 69.85(9) yes
C3 . C4 . H41 . 126.6 no
Fe1 . C4 . H41 . 124.3 no
C5 . C4 . H41 . 125.1 no
C1 . C5 . C4 . 107.74(14) yes
C1 . C5 . Fe1 . 69.29(8) yes
C4 . C5 . Fe1 . 69.52(9) yes
C1 . C5 . H51 . 126.1 no
C4 . C5 . H51 . 126.2 no
Fe1 . C5 . H51 . 127.6 no
P2 . C6 . Fe1 . 123.75(8) yes
P2 . C6 . C7 . 123.04(12) yes
Fe1 . C6 . C7 . 69.80(9) yes
P2 . C6 . C10 . 128.96(13) yes
Fe1 . C6 . C10 . 69.88(9) yes
C7 . C6 . C10 . 107.95(14) yes
C6 . C7 . Fe1 . 68.80(9) yes
C6 . C7 . C8 . 107.76(15) yes
Fe1 . C7 . C8 . 70.35(9) yes
C6 . C7 . H71 . 125.6 no
Fe1 . C7 . H71 . 127.7 no
C8 . C7 . H71 . 126.6 no
C7 . C8 . Fe1 . 69.20(9) yes
C7 . C8 . C9 . 108.23(16) yes
Fe1 . C8 . C9 . 69.37(9) yes
C7 . C8 . H81 . 125.5 no
Fe1 . C8 . H81 . 127.0 no
C9 . C8 . H81 . 126.3 no
C8 . C9 . Fe1 . 70.09(10) yes
C8 . C9 . C10 . 108.82(15) yes
Fe1 . C9 . C10 . 69.45(9) yes
C8 . C9 . H91 . 125.4 no
Fe1 . C9 . H91 . 125.5 no
C10 . C9 . H91 . 125.7 no
C6 . C10 . C9 . 107.24(15) yes
C6 . C10 . Fe1 . 68.83(9) yes
C9 . C10 . Fe1 . 69.84(10) yes
C6 . C10 . H101 . 124.7 no
C9 . C10 . H101 . 128.1 no
Fe1 . C10 . H101 . 125.5 no
P1 . C11 . C12 . 119.85(13) yes
P1 . C11 . C16 . 120.71(13) yes
C12 . C11 . C16 . 119.33(16) yes
C11 . C12 . C13 . 120.07(17) yes
C11 . C12 . H121 . 119.2 no
C13 . C12 . H121 . 120.7 no
C12 . C13 . C14 . 119.85(18) yes
C12 . C13 . H131 . 118.8 no
C14 . C13 . H131 . 121.4 no
C13 . C14 . C15 . 120.65(17) yes
C13 . C14 . H141 . 121.2 no
C15 . C14 . H141 . 118.2 no
C14 . C15 . C16 . 119.88(18) yes
C14 . C15 . H151 . 120.8 no
C16 . C15 . H151 . 119.3 no
C11 . C16 . C15 . 120.21(17) yes
C11 . C16 . H161 . 121.0 no
C15 . C16 . H161 . 118.8 no
P1 . C21 . C22 . 118.52(12) yes
P1 . C21 . C26 . 121.48(13) yes
C22 . C21 . C26 . 119.94(15) yes
C21 . C22 . C23 . 120.19(16) yes
C21 . C22 . H221 . 121.1 no
C23 . C22 . H221 . 118.7 no
C22 . C23 . C24 . 119.66(17) yes
C22 . C23 . H231 . 118.5 no
C24 . C23 . H231 . 121.8 no
C23 . C24 . C25 . 120.02(16) yes
C23 . C24 . H241 . 119.0 no
C25 . C24 . H241 . 120.9 no
C24 . C25 . C26 . 120.95(17) yes
C24 . C25 . H251 . 120.7 no
C26 . C25 . H251 . 118.3 no
C21 . C26 . C25 . 119.19(17) yes
C21 . C26 . H261 . 120.9 no
C25 . C26 . H261 . 119.9 no
P2 . C31 . C32 . 118.54(12) yes
P2 . C31 . C36 . 122.30(13) yes
C32 . C31 . C36 . 119.15(15) yes
C31 . C32 . C33 . 120.86(16) yes
C31 . C32 . H321 . 119.6 no
C33 . C32 . H321 . 119.6 no
C32 . C33 . C34 . 119.39(17) yes
C32 . C33 . H331 . 120.4 no
C34 . C33 . H331 . 120.1 no
C33 . C34 . C35 . 120.17(17) yes
C33 . C34 . H341 . 119.3 no
C35 . C34 . H341 . 120.5 no
C34 . C35 . C36 . 120.75(16) yes
C34 . C35 . H351 . 120.6 no
C36 . C35 . H351 . 118.6 no
C31 . C36 . C35 . 119.66(16) yes
C31 . C36 . H361 . 119.9 no
C35 . C36 . H361 . 120.5 no
P2 . C41 . C42 . 119.56(13) yes
P2 . C41 . C46 . 120.73(13) yes
C42 . C41 . C46 . 119.67(16) yes
C41 . C42 . C43 . 120.21(18) yes
C41 . C42 . H421 . 119.8 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 119.78(19) yes
C42 . C43 . H431 . 120.6 no
C44 . C43 . H431 . 119.6 no
C43 . C44 . C45 . 120.59(17) yes
C43 . C44 . H441 . 118.7 no
C45 . C44 . H441 . 120.7 no
C44 . C45 . C46 . 120.09(17) yes
C44 . C45 . H451 . 121.1 no
C46 . C45 . H451 . 118.8 no
C41 . C46 . C45 . 119.66(17) yes
C41 . C46 . H461 . 119.7 no
C45 . C46 . H461 . 120.6 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
C25 . H251 . C4 2_565 134.37(5) 0.946 2.598 3.328(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 07/02/15 at 17:35:35
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 07/02/15 at 17:35:35
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/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_1
_database_code_depnum_ccdc_archive 'CCDC 1530818'
_audit_update_record             
;
2017-02-03 deposited with the CCDC.
2017-05-12 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                   13.0162(3)
_cell_length_b                   21.4161(5)
_cell_length_c                   14.4005(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.8708(13)
_cell_angle_gamma                90
_cell_volume                     3976.41(14)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
As 0.0499 2.0058 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972
2.5310 '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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 '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'


_cell_formula_units_Z            4

# Given Formula = C41 H41 As1 B1 Br1 F6 O1 P3 
# Dc =      1.54 Fooo =   1731.20 Mu =     20.42 M =    922.32
# Found Formula = C41 H41.80 As1 B1 F6 O1 P3 
# Dc =      1.41 FOOO =   1731.20 Mu =     10.36 M =    843.22

_chemical_formula_sum            'C41 H41.80 As1 B1 F6 O1 P3'
_chemical_formula_moiety         'C41 H41 B1 O0.6 P3, As1 F6, H0.8 O0.4'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         843.22


_cell_measurement_reflns_used    108874
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      29
_cell_measurement_temperature    200

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.090
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.450

_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1731.200
_exptl_absorpt_coefficient_mu    1.036

# Sheldrick geometric approximatio 0.86 0.91 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.91

# 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    '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            17904
_reflns_number_total             9120
_diffrn_reflns_av_R_equivalents  0.030
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9120 
# Theoretical number of reflections is about 18290 


_diffrn_reflns_theta_min         2.745
_diffrn_reflns_theta_max         27.511
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        27.511
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              27
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   3.70
_oxford_diffrn_Wilson_scale      14.52

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

_refine_diff_density_min         -0.70
_refine_diff_density_max         0.96


# 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         9119
_refine_ls_number_restraints     200
_refine_ls_number_parameters     487
_oxford_refine_ls_R_factor_ref   0.0901
_refine_ls_wR_factor_ref         0.1517
_refine_ls_goodness_of_fit_ref   0.9869
_refine_ls_shift/su_max          0.0022377
_refine_ls_shift/su_mean         0.0000475


# The values computed from all data 
_oxford_reflns_number_all        9119
_refine_ls_R_factor_all          0.0901
_refine_ls_wR_factor_all         0.1517

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6292
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_gt          0.1343

# 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    mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 4.55P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
As1 As 0.37838(3) 0.607768(17) 0.70500(2) 0.0555 1.0000 Uani . . . . . .
B1 B 0.6159(3) 0.75686(18) 0.3168(3) 0.0496 1.0000 Uani . . . . . .
F1 F 0.3981(3) 0.54295(14) 0.7731(2) 0.1083 1.0000 Uani . . . . . .
F2 F 0.3641(3) 0.67285(15) 0.6375(3) 0.1257 1.0000 Uani . . . . . .
F3 F 0.2588(3) 0.5860(2) 0.6633(3) 0.1397 1.0000 Uani . . . . . .
F4 F 0.5023(2) 0.62936(15) 0.7501(2) 0.0983 1.0000 Uani . . . . . .
F5 F 0.3349(3) 0.6445(2) 0.7947(2) 0.1484 1.0000 Uani . . . . . .
F6 F 0.4306(3) 0.57169(16) 0.6184(2) 0.1216 1.0000 Uani . . . . . .
O1 O 0.2490(3) 0.64402(19) 0.3194(3) 0.0639 0.6000 Uani . . . . . .
O101 O 0.1064(4) 0.6523(2) 0.2159(4) 0.0455 0.4000 Uani . . . . . .
P1 P 0.29427(7) 0.58134(4) 0.30855(6) 0.0507 1.0000 Uani D . . . . .
P2 P 0.62838(7) 0.67951(4) 0.25230(6) 0.0445 1.0000 Uani D . . . . .
P3 P 0.56206(7) 0.74282(4) 0.43312(6) 0.0457 1.0000 Uani D . . . . .
C1 C 0.4209(3) 0.56697(14) 0.3796(2) 0.0447 1.0000 Uani D . . . . .
C2 C 0.5257(3) 0.62659(15) 0.2764(2) 0.0455 1.0000 Uani D . . . . .
C3 C 0.4716(3) 0.67748(15) 0.4224(2) 0.0454 1.0000 Uani D . . . . .
C4 C 0.5075(3) 0.61645(14) 0.3787(2) 0.0431 1.0000 Uani D . . . . .
C5 C 0.6051(3) 0.59022(16) 0.4382(2) 0.0503 1.0000 Uani D . . . . .
C11 C 0.3098(2) 0.55880(16) 0.1896(2) 0.0508 1.0000 Uani D . . . . .
C12 C 0.3617(3) 0.50536(18) 0.1682(3) 0.0599 1.0000 Uani D . . . . .
C13 C 0.3764(3) 0.4932(2) 0.0767(3) 0.0743 1.0000 Uani D . . . . .
C14 C 0.3385(3) 0.5347(3) 0.0064(3) 0.0803 1.0000 Uani D . . . . .
C15 C 0.2854(3) 0.5871(2) 0.0266(3) 0.0783 1.0000 Uani D . . . . .
C16 C 0.2712(3) 0.59947(18) 0.1170(3) 0.0643 1.0000 Uani D . . . . .
C21 C 0.2146(2) 0.52064(16) 0.3499(2) 0.0516 1.0000 Uani D . . . . .
C22 C 0.1643(3) 0.47460(17) 0.2929(3) 0.0650 1.0000 Uani D . . . . .
C23 C 0.0975(3) 0.43328(19) 0.3275(4) 0.0821 1.0000 Uani D . . . . .
C24 C 0.0808(3) 0.4360(2) 0.4197(4) 0.0888 1.0000 Uani D . . . . .
C25 C 0.1312(3) 0.4812(2) 0.4779(3) 0.0856 1.0000 Uani D . . . . .
C26 C 0.1962(3) 0.5240(2) 0.4426(3) 0.0691 1.0000 Uani D . . . . .
C31 C 0.6035(2) 0.69606(15) 0.1281(2) 0.0474 1.0000 Uani D . . . . .
C32 C 0.5448(3) 0.65623(17) 0.0658(2) 0.0596 1.0000 Uani D . . . . .
C33 C 0.5263(3) 0.6706(2) -0.0285(3) 0.0719 1.0000 Uani D . . . . .
C34 C 0.5673(3) 0.7242(2) -0.0608(3) 0.0782 1.0000 Uani D . . . . .
C35 C 0.6269(3) 0.7637(2) 0.0001(3) 0.0764 1.0000 Uani D . . . . .
C36 C 0.6439(3) 0.75019(17) 0.0949(3) 0.0627 1.0000 Uani D . . . . .
C41 C 0.7531(3) 0.64097(17) 0.2684(2) 0.0523 1.0000 Uani D . . . . .
C42 C 0.8426(3) 0.6766(2) 0.2855(3) 0.0884 1.0000 Uani D . . . . .
C43 C 0.9387(4) 0.6481(3) 0.2872(3) 0.1160 1.0000 Uani D . . . . .
C44 C 0.9458(4) 0.5844(3) 0.2744(3) 0.0981 1.0000 Uani D . . . . .
C45 C 0.8571(4) 0.5493(2) 0.2574(2) 0.0753 1.0000 Uani D . . . . .
C46 C 0.7611(3) 0.57742(17) 0.2526(2) 0.0607 1.0000 Uani D . . . . .
C51 C 0.4879(3) 0.81127(16) 0.4566(2) 0.0492 1.0000 Uani D . . . . .
C52 C 0.4017(3) 0.80816(19) 0.5024(3) 0.0715 1.0000 Uani D . . . . .
C53 C 0.3478(3) 0.8621(2) 0.5181(3) 0.0844 1.0000 Uani D . . . . .
C54 C 0.3817(3) 0.9190(2) 0.4905(3) 0.0754 1.0000 Uani D . . . . .
C55 C 0.4666(3) 0.92223(19) 0.4438(3) 0.0741 1.0000 Uani D . . . . .
C56 C 0.5197(3) 0.86883(18) 0.4257(2) 0.0617 1.0000 Uani D . . . . .
C61 C 0.6589(3) 0.73185(15) 0.5344(2) 0.0513 1.0000 Uani D . . . . .
C62 C 0.6277(3) 0.71923(18) 0.6206(3) 0.0755 1.0000 Uani D . . . . .
C63 C 0.7013(4) 0.71156(18) 0.6991(3) 0.0897 1.0000 Uani D . . . . .
C64 C 0.8049(4) 0.71715(17) 0.6912(3) 0.0807 1.0000 Uani D . . . . .
C65 C 0.8362(3) 0.72963(16) 0.6062(3) 0.0730 1.0000 Uani D . . . . .
C66 C 0.7633(3) 0.73734(14) 0.5272(3) 0.0587 1.0000 Uani D . . . . .
H1 H 0.5481 0.7828 0.2732 0.0578 1.0000 Uiso R . . . . .
H11 H 0.4475 0.5280 0.3613 0.0540 1.0000 Uiso DR . . . . .
H12 H 0.4074 0.5629 0.4435 0.0538 1.0000 Uiso DR . . . . .
H21 H 0.5376 0.5868 0.2490 0.0541 1.0000 Uiso DR . . . . .
H22 H 0.4627 0.6451 0.2425 0.0545 1.0000 Uiso DR . . . . .
H31 H 0.4534 0.6676 0.4837 0.0546 1.0000 Uiso DR . . . . .
H32 H 0.4094 0.6908 0.3828 0.0550 1.0000 Uiso DR . . . . .
H51 H 0.6246 0.5520 0.4116 0.0744 1.0000 Uiso DR . . . . .
H52 H 0.6621 0.6183 0.4400 0.0745 1.0000 Uiso DR . . . . .
H53 H 0.5906 0.5830 0.5006 0.0740 1.0000 Uiso DR . . . . .
H121 H 0.3866 0.4769 0.2156 0.0712 1.0000 Uiso DR . . . . .
H131 H 0.4108 0.4573 0.0642 0.0888 1.0000 Uiso DR . . . . .
H141 H 0.3499 0.5266 -0.0543 0.0959 1.0000 Uiso DR . . . . .
H151 H 0.2578 0.6134 -0.0212 0.0942 1.0000 Uiso DR . . . . .
H161 H 0.2357 0.6347 0.1303 0.0773 1.0000 Uiso DR . . . . .
H221 H 0.1745 0.4716 0.2303 0.0778 1.0000 Uiso DR . . . . .
H231 H 0.0629 0.4039 0.2877 0.0989 1.0000 Uiso DR . . . . .
H241 H 0.0353 0.4077 0.4425 0.1069 1.0000 Uiso DR . . . . .
H251 H 0.1227 0.4834 0.5401 0.1028 1.0000 Uiso DR . . . . .
H261 H 0.2277 0.5552 0.4811 0.0824 1.0000 Uiso DR . . . . .
H321 H 0.5176 0.6195 0.0876 0.0720 1.0000 Uiso DR . . . . .
H331 H 0.4858 0.6443 -0.0700 0.0857 1.0000 Uiso DR . . . . .
H341 H 0.5541 0.7337 -0.1248 0.0939 1.0000 Uiso DR . . . . .
H351 H 0.6568 0.7991 -0.0223 0.0917 1.0000 Uiso DR . . . . .
H361 H 0.6812 0.7772 0.1367 0.0746 1.0000 Uiso DR . . . . .
H421 H 0.8386 0.7191 0.2963 0.1057 1.0000 Uiso DR . . . . .
H431 H 0.9990 0.6724 0.2978 0.1390 1.0000 Uiso DR . . . . .
H441 H 1.0112 0.5653 0.2774 0.1178 1.0000 Uiso DR . . . . .
H451 H 0.8620 0.5078 0.2472 0.0901 1.0000 Uiso DR . . . . .
H461 H 0.7009 0.5537 0.2387 0.0729 1.0000 Uiso DR . . . . .
H521 H 0.3797 0.7704 0.5216 0.0858 1.0000 Uiso DR . . . . .
H531 H 0.2884 0.8599 0.5478 0.1011 1.0000 Uiso DR . . . . .
H541 H 0.3468 0.9560 0.5036 0.0900 1.0000 Uiso DR . . . . .
H551 H 0.4893 0.9614 0.4240 0.0891 1.0000 Uiso DR . . . . .
H561 H 0.5761 0.8716 0.3921 0.0739 1.0000 Uiso DR . . . . .
H621 H 0.5565 0.7155 0.6254 0.0905 1.0000 Uiso DR . . . . .
H631 H 0.6802 0.7015 0.7556 0.1080 1.0000 Uiso DR . . . . .
H641 H 0.8542 0.7117 0.7445 0.0970 1.0000 Uiso DR . . . . .
H651 H 0.9069 0.7338 0.6011 0.0872 1.0000 Uiso DR . . . . .
H661 H 0.7839 0.7463 0.4702 0.0707 1.0000 Uiso DR . . . . .
H2 H 0.6815 0.7832 0.3238 0.0713 1.0000 Uiso R . . . . .
H1011 H 0.1389 0.6319 0.2584 0.0693 0.4000 Uiso . . . . . .
H1012 H 0.0791 0.6302 0.1712 0.0698 0.4000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3052(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
As1 . F1 . 1.699(3) yes
As1 . F2 . 1.695(3) yes
As1 . F3 . 1.656(3) yes
As1 . F4 . 1.718(3) yes
As1 . F5 . 1.675(3) yes
As1 . F6 . 1.687(3) yes
B1 . P2 . 1.917(4) yes
B1 . P3 . 1.925(4) yes
B1 . H1 . 1.153 no
B1 . H2 . 1.018 no
O1 . P1 . 1.483(4) yes
O101 . H1011 . 0.822 no
O101 . H1012 . 0.838 no
P1 . C1 . 1.843(3) yes
P1 . C11 . 1.817(4) yes
P1 . C21 . 1.814(4) yes
P2 . C2 . 1.821(3) yes
P2 . C31 . 1.808(3) yes
P2 . C41 . 1.808(4) yes
P3 . C3 . 1.821(3) yes
P3 . C51 . 1.812(3) yes
P3 . C61 . 1.807(3) yes
C1 . C4 . 1.549(4) yes
C1 . H11 . 0.954 no
C1 . H12 . 0.965 no
C2 . C4 . 1.540(4) yes
C2 . H21 . 0.961 no
C2 . H22 . 0.979 no
C3 . C4 . 1.550(4) yes
C3 . H31 . 0.968 no
C3 . H32 . 0.967 no
C4 . C5 . 1.538(4) yes
C5 . H51 . 0.954 no
C5 . H52 . 0.953 no
C5 . H53 . 0.955 no
C11 . C12 . 1.385(5) yes
C11 . C16 . 1.400(5) yes
C12 . C13 . 1.381(5) yes
C12 . H121 . 0.940 no
C13 . C14 . 1.386(6) yes
C13 . H131 . 0.920 no
C14 . C15 . 1.370(7) yes
C14 . H141 . 0.923 no
C15 . C16 . 1.366(6) yes
C15 . H151 . 0.922 no
C16 . H161 . 0.918 no
C21 . C22 . 1.389(5) yes
C21 . C26 . 1.390(5) yes
C22 . C23 . 1.381(6) yes
C22 . H221 . 0.931 no
C23 . C24 . 1.376(7) yes
C23 . H231 . 0.926 no
C24 . C25 . 1.385(7) yes
C24 . H241 . 0.937 no
C25 . C26 . 1.390(6) yes
C25 . H251 . 0.918 no
C26 . H261 . 0.927 no
C31 . C32 . 1.389(5) yes
C31 . C36 . 1.385(5) yes
C32 . C33 . 1.380(5) yes
C32 . H321 . 0.935 no
C33 . C34 . 1.374(6) yes
C33 . H331 . 0.930 no
C34 . C35 . 1.379(6) yes
C34 . H341 . 0.937 no
C35 . C36 . 1.383(5) yes
C35 . H351 . 0.930 no
C36 . H361 . 0.924 no
C41 . C42 . 1.386(5) yes
C41 . C46 . 1.386(5) yes
C42 . C43 . 1.389(6) yes
C42 . H421 . 0.927 no
C43 . C44 . 1.382(7) yes
C43 . H431 . 0.936 no
C44 . C45 . 1.370(7) yes
C44 . H441 . 0.940 no
C45 . C46 . 1.381(6) yes
C45 . H451 . 0.906 no
C46 . H461 . 0.931 no
C51 . C52 . 1.380(5) yes
C51 . C56 . 1.393(5) yes
C52 . C53 . 1.386(6) yes
C52 . H521 . 0.913 no
C53 . C54 . 1.373(6) yes
C53 . H531 . 0.934 no
C54 . C55 . 1.372(6) yes
C54 . H541 . 0.945 no
C55 . C56 . 1.380(5) yes
C55 . H551 . 0.947 no
C56 . H561 . 0.935 no
C61 . C62 . 1.385(5) yes
C61 . C66 . 1.383(5) yes
C62 . C63 . 1.389(6) yes
C62 . H621 . 0.942 no
C63 . C64 . 1.374(6) yes
C63 . H631 . 0.920 no
C64 . C65 . 1.368(6) yes
C64 . H641 . 0.937 no
C65 . C66 . 1.388(5) yes
C65 . H651 . 0.938 no
C66 . H661 . 0.917 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
F1 . As1 . F2 . 177.63(16) yes
F1 . As1 . F3 . 92.30(17) yes
F2 . As1 . F3 . 89.95(18) yes
F1 . As1 . F4 . 86.65(15) yes
F2 . As1 . F4 . 91.11(17) yes
F3 . As1 . F4 . 178.87(15) yes
F1 . As1 . F5 . 88.8(2) yes
F2 . As1 . F5 . 92.0(2) yes
F3 . As1 . F5 . 90.7(2) yes
F4 . As1 . F5 . 88.93(19) yes
F1 . As1 . F6 . 90.47(17) yes
F2 . As1 . F6 . 88.66(17) yes
F3 . As1 . F6 . 93.3(2) yes
F4 . As1 . F6 . 87.15(17) yes
F5 . As1 . F6 . 176.0(2) yes
P2 . B1 . P3 . 110.6(2) yes
P2 . B1 . H1 . 105.2 no
P3 . B1 . H1 . 101.9 no
P2 . B1 . H2 . 113.7 no
P3 . B1 . H2 . 113.6 no
H1 . B1 . H2 . 110.9 no
H1011 . O101 . H1012 . 113.0 no
O1 . P1 . C1 . 115.5(2) yes
O1 . P1 . C11 . 115.9(2) yes
C1 . P1 . C11 . 105.82(15) yes
O1 . P1 . C21 . 111.1(2) yes
C1 . P1 . C21 . 101.89(15) yes
C11 . P1 . C21 . 105.16(16) yes
B1 . P2 . C2 . 109.39(16) yes
B1 . P2 . C31 . 107.13(16) yes
C2 . P2 . C31 . 105.88(15) yes
B1 . P2 . C41 . 117.83(17) yes
C2 . P2 . C41 . 111.15(16) yes
C31 . P2 . C41 . 104.62(14) yes
B1 . P3 . C3 . 110.75(16) yes
B1 . P3 . C51 . 107.60(17) yes
C3 . P3 . C51 . 106.42(15) yes
B1 . P3 . C61 . 115.19(18) yes
C3 . P3 . C61 . 109.84(16) yes
C51 . P3 . C61 . 106.57(14) yes
P1 . C1 . C4 . 118.6(2) yes
P1 . C1 . H11 . 108.9 no
C4 . C1 . H11 . 107.7 no
P1 . C1 . H12 . 106.2 no
C4 . C1 . H12 . 107.3 no
H11 . C1 . H12 . 107.7 no
P2 . C2 . C4 . 118.9(2) yes
P2 . C2 . H21 . 108.1 no
C4 . C2 . H21 . 108.8 no
P2 . C2 . H22 . 103.9 no
C4 . C2 . H22 . 107.9 no
H21 . C2 . H22 . 108.9 no
P3 . C3 . C4 . 117.0(2) yes
P3 . C3 . H31 . 109.1 no
C4 . C3 . H31 . 108.1 no
P3 . C3 . H32 . 107.6 no
C4 . C3 . H32 . 106.5 no
H31 . C3 . H32 . 108.2 no
C2 . C4 . C1 . 108.2(2) yes
C2 . C4 . C3 . 111.3(3) yes
C1 . C4 . C3 . 108.3(3) yes
C2 . C4 . C5 . 111.2(3) yes
C1 . C4 . C5 . 107.0(3) yes
C3 . C4 . C5 . 110.7(3) yes
C4 . C5 . H51 . 109.5 no
C4 . C5 . H52 . 111.4 no
H51 . C5 . H52 . 107.7 no
C4 . C5 . H53 . 109.2 no
H51 . C5 . H53 . 109.6 no
H52 . C5 . H53 . 109.4 no
P1 . C11 . C12 . 123.4(3) yes
P1 . C11 . C16 . 117.7(3) yes
C12 . C11 . C16 . 118.9(4) yes
C11 . C12 . C13 . 120.2(4) yes
C11 . C12 . H121 . 120.3 no
C13 . C12 . H121 . 119.5 no
C12 . C13 . C14 . 119.6(4) yes
C12 . C13 . H131 . 118.6 no
C14 . C13 . H131 . 121.8 no
C13 . C14 . C15 . 120.7(4) yes
C13 . C14 . H141 . 118.9 no
C15 . C14 . H141 . 120.4 no
C14 . C15 . C16 . 119.9(4) yes
C14 . C15 . H151 . 119.9 no
C16 . C15 . H151 . 120.2 no
C11 . C16 . C15 . 120.7(4) yes
C11 . C16 . H161 . 119.6 no
C15 . C16 . H161 . 119.7 no
P1 . C21 . C22 . 124.0(3) yes
P1 . C21 . C26 . 117.4(3) yes
C22 . C21 . C26 . 118.4(4) yes
C21 . C22 . C23 . 120.7(4) yes
C21 . C22 . H221 . 120.2 no
C23 . C22 . H221 . 119.1 no
C22 . C23 . C24 . 120.8(5) yes
C22 . C23 . H231 . 119.3 no
C24 . C23 . H231 . 119.8 no
C23 . C24 . C25 . 119.3(4) yes
C23 . C24 . H241 . 120.1 no
C25 . C24 . H241 . 120.7 no
C24 . C25 . C26 . 120.1(4) yes
C24 . C25 . H251 . 121.0 no
C26 . C25 . H251 . 118.9 no
C21 . C26 . C25 . 120.7(4) yes
C21 . C26 . H261 . 119.4 no
C25 . C26 . H261 . 120.0 no
P2 . C31 . C32 . 121.8(3) yes
P2 . C31 . C36 . 118.7(3) yes
C32 . C31 . C36 . 119.5(3) yes
C31 . C32 . C33 . 120.4(4) yes
C31 . C32 . H321 . 119.9 no
C33 . C32 . H321 . 119.7 no
C32 . C33 . C34 . 119.7(4) yes
C32 . C33 . H331 . 120.4 no
C34 . C33 . H331 . 119.9 no
C33 . C34 . C35 . 120.6(4) yes
C33 . C34 . H341 . 119.2 no
C35 . C34 . H341 . 120.2 no
C34 . C35 . C36 . 119.9(4) yes
C34 . C35 . H351 . 120.4 no
C36 . C35 . H351 . 119.7 no
C31 . C36 . C35 . 119.9(4) yes
C31 . C36 . H361 . 119.4 no
C35 . C36 . H361 . 120.7 no
P2 . C41 . C42 . 119.3(3) yes
P2 . C41 . C46 . 120.9(3) yes
C42 . C41 . C46 . 119.3(4) yes
C41 . C42 . C43 . 119.6(4) yes
C41 . C42 . H421 . 120.4 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 120.5(5) yes
C42 . C43 . H431 . 119.5 no
C44 . C43 . H431 . 120.1 no
C43 . C44 . C45 . 119.7(4) yes
C43 . C44 . H441 . 119.9 no
C45 . C44 . H441 . 120.5 no
C44 . C45 . C46 . 120.3(4) yes
C44 . C45 . H451 . 119.4 no
C46 . C45 . H451 . 120.2 no
C41 . C46 . C45 . 120.5(4) yes
C41 . C46 . H461 . 119.4 no
C45 . C46 . H461 . 120.1 no
P3 . C51 . C52 . 122.6(3) yes
P3 . C51 . C56 . 117.9(3) yes
C52 . C51 . C56 . 119.5(3) yes
C51 . C52 . C53 . 120.0(4) yes
C51 . C52 . H521 . 119.8 no
C53 . C52 . H521 . 120.2 no
C52 . C53 . C54 . 120.2(4) yes
C52 . C53 . H531 . 120.1 no
C54 . C53 . H531 . 119.7 no
C53 . C54 . C55 . 119.9(4) yes
C53 . C54 . H541 . 120.3 no
C55 . C54 . H541 . 119.8 no
C54 . C55 . C56 . 120.6(4) yes
C54 . C55 . H551 . 119.9 no
C56 . C55 . H551 . 119.5 no
C51 . C56 . C55 . 119.7(4) yes
C51 . C56 . H561 . 120.7 no
C55 . C56 . H561 . 119.7 no
P3 . C61 . C62 . 119.4(3) yes
P3 . C61 . C66 . 120.8(3) yes
C62 . C61 . C66 . 119.8(3) yes
C61 . C62 . C63 . 119.9(4) yes
C61 . C62 . H621 . 119.7 no
C63 . C62 . H621 . 120.4 no
C62 . C63 . C64 . 119.9(4) yes
C62 . C63 . H631 . 119.4 no
C64 . C63 . H631 . 120.6 no
C63 . C64 . C65 . 120.4(4) yes
C63 . C64 . H641 . 119.4 no
C65 . C64 . H641 . 120.2 no
C64 . C65 . C66 . 120.3(4) yes
C64 . C65 . H651 . 120.3 no
C66 . C65 . H651 . 119.4 no
C65 . C66 . C61 . 119.8(4) yes
C65 . C66 . H661 . 120.6 no
C61 . C66 . H661 . 119.6 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
C3 . H32 . O1 . 136.11(13) 0.967 2.382 3.152(6) yes
C16 . H161 . O101 . 133.47(16) 0.918 2.249 2.957(6) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 23/07/13 at 18:33:47
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
REM CONT O(1, OCC) O(101, OCC) 
REM EQUIV O(1, OCC) O(101, OCC) 
REM WEIGHT -1 O(1, OCC) 
RIDE B   (   1,X'S) H   (   2,X'S) H   (   1,X'S) 
RIDE C   (   1,X'S) H   (  12,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  53,X'S) H   (  51,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 23/07/13 at 18:33:47
#
#LIST     16                                                                    
REM DIST 1.0, 0.01 = O(101) TO H(1011) 
REM DIST 0.88, 0.01 = O(101) TO H(1012) 
REM ANGLE 109.0, 0.03 = H(1011) TO O(101) TO H(1012) 
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            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 1) TO H(12) 
CONT C ( 1) TO H(11) 
REST 0.053, 0.002 = H(12,U[ISO]) 
REST 0.053, 0.002 = H(11,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(12) TO C ( 1) TO P(1) 
CONT H(12) TO C ( 1) TO C(4) 
CONT H(11) TO C ( 1) TO P(1) 
CONT H(11) TO C ( 1) TO C(4) 
ANGLE 109.54, 2.0 = 
CONT H(12) TO C ( 1) TO H(11) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 2) TO H(22) 
CONT C ( 2) TO H(21) 
REST 0.053, 0.002 = H(22,U[ISO]) 
REST 0.053, 0.002 = H(21,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(22) TO C ( 2) TO P(2) 
CONT H(22) TO C ( 2) TO C(4) 
CONT H(21) TO C ( 2) TO P(2) 
CONT H(21) TO C ( 2) TO C(4) 
ANGLE 109.54, 2.0 = 
CONT H(22) TO C ( 2) TO H(21) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 3) TO H(31) 
CONT C ( 3) TO H(32) 
REST 0.054, 0.002 = H(31,U[ISO]) 
REST 0.054, 0.002 = H(32,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(31) TO C ( 3) TO P(3) 
CONT H(31) TO C ( 3) TO C(4) 
CONT H(32) TO C ( 3) TO P(3) 
CONT H(32) TO C ( 3) TO C(4) 
ANGLE 109.54, 2.0 = 
CONT H(31) TO C ( 3) TO H(32) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 5) TO H(52) 
CONT C ( 5) TO H(53) 
CONT C ( 5) TO H(51) 
REST 0.076, 0.002 = H(52,U[ISO]) 
REST 0.076, 0.002 = H(53,U[ISO]) 
REST 0.076, 0.002 = H(51,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(4) TO C ( 5) TO H(52) 
CONT C(4) TO C ( 5) TO H(53) 
CONT C(4) TO C ( 5) TO H(51) 
ANGLE 0.0, 2.0 = MEAN H(52) TO C ( 5) TO H(53) 
CONT H(52) TO C ( 5) TO H(51) 
CONT H(53) TO C ( 5) TO H(51) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 12) TO H(121) 
REST 0.073, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 13) TO H(131) 
REST 0.088, 0.002 = H(131,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(131) TO C ( 13) TO C(12) 
CONT H(131) TO C ( 13) TO C(14) 
PLANAR C ( 13) C(12) C(14) H(131) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 14) TO H(141) 
REST 0.091, 0.002 = H(141,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(141) TO C ( 14) TO C(13) 
CONT H(141) TO C ( 14) TO C(15) 
PLANAR C ( 14) C(13) C(15) H(141) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 15) TO H(151) 
REST 0.093, 0.002 = H(151,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(151) TO C ( 15) TO C(14) 
CONT H(151) TO C ( 15) TO C(16) 
PLANAR C ( 15) C(14) C(16) H(151) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 16) TO H(161) 
REST 0.078, 0.002 = H(161,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(161) TO C ( 16) TO C(11) 
CONT H(161) TO C ( 16) TO C(15) 
PLANAR C ( 16) C(11) C(15) H(161) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 22) TO H(221) 
REST 0.077, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 23) TO H(231) 
REST 0.099, 0.002 = H(231,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(231) TO C ( 23) TO C(22) 
CONT H(231) TO C ( 23) TO C(24) 
PLANAR C ( 23) C(22) C(24) H(231) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 24) TO H(241) 
REST 0.104, 0.002 = H(241,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(241) TO C ( 24) TO C(23) 
CONT H(241) TO C ( 24) TO C(25) 
PLANAR C ( 24) C(23) C(25) H(241) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 25) TO H(251) 
REST 0.102, 0.002 = H(251,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(251) TO C ( 25) TO C(24) 
CONT H(251) TO C ( 25) TO C(26) 
PLANAR C ( 25) C(24) C(26) H(251) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 26) TO H(261) 
REST 0.084, 0.002 = H(261,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(261) TO C ( 26) TO C(25) 
CONT H(261) TO C ( 26) TO C(21) 
PLANAR C ( 26) C(25) C(21) H(261) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 32) TO H(321) 
REST 0.070, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 33) TO H(331) 
REST 0.086, 0.002 = H(331,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(331) TO C ( 33) TO C(32) 
CONT H(331) TO C ( 33) TO C(34) 
PLANAR C ( 33) C(32) C(34) H(331) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 34) TO H(341) 
REST 0.089, 0.002 = H(341,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(341) TO C ( 34) TO C(33) 
CONT H(341) TO C ( 34) TO C(35) 
PLANAR C ( 34) C(33) C(35) H(341) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 35) TO H(351) 
REST 0.091, 0.002 = H(351,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(351) TO C ( 35) TO C(34) 
CONT H(351) TO C ( 35) TO C(36) 
PLANAR C ( 35) C(34) C(36) H(351) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 36) TO H(361) 
REST 0.074, 0.002 = H(361,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(361) TO C ( 36) TO C(31) 
CONT H(361) TO C ( 36) TO C(35) 
PLANAR C ( 36) C(31) C(35) H(361) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 42) TO H(421) 
REST 0.105, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 43) TO H(431) 
REST 0.130, 0.002 = H(431,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(431) TO C ( 43) TO C(42) 
CONT H(431) TO C ( 43) TO C(44) 
PLANAR C ( 43) C(42) C(44) H(431) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 44) TO H(441) 
REST 0.112, 0.002 = H(441,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(441) TO C ( 44) TO C(43) 
CONT H(441) TO C ( 44) TO C(45) 
PLANAR C ( 44) C(43) C(45) H(441) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 45) TO H(451) 
REST 0.088, 0.002 = H(451,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(451) TO C ( 45) TO C(44) 
CONT H(451) TO C ( 45) TO C(46) 
PLANAR C ( 45) C(44) C(46) H(451) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 46) TO H(461) 
REST 0.073, 0.002 = H(461,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(461) TO C ( 46) TO C(41) 
CONT H(461) TO C ( 46) TO C(45) 
PLANAR C ( 46) C(41) C(45) H(461) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 52) TO H(521) 
REST 0.083, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 53) TO H(531) 
REST 0.097, 0.002 = H(531,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(531) TO C ( 53) TO C(52) 
CONT H(531) TO C ( 53) TO C(54) 
PLANAR C ( 53) C(52) C(54) H(531) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 54) TO H(541) 
REST 0.088, 0.002 = H(541,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(541) TO C ( 54) TO C(53) 
CONT H(541) TO C ( 54) TO C(55) 
PLANAR C ( 54) C(53) C(55) H(541) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 55) TO H(551) 
REST 0.087, 0.002 = H(551,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(551) TO C ( 55) TO C(54) 
CONT H(551) TO C ( 55) TO C(56) 
PLANAR C ( 55) C(54) C(56) H(551) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 56) TO H(561) 
REST 0.075, 0.002 = H(561,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(561) TO C ( 56) TO C(55) 
CONT H(561) TO C ( 56) TO C(51) 
PLANAR C ( 56) C(55) C(51) H(561) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 62) TO H(621) 
REST 0.089, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 63) TO H(631) 
REST 0.103, 0.002 = H(631,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(631) TO C ( 63) TO C(62) 
CONT H(631) TO C ( 63) TO C(64) 
PLANAR C ( 63) C(62) C(64) H(631) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 64) TO H(641) 
REST 0.095, 0.002 = H(641,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(641) TO C ( 64) TO C(63) 
CONT H(641) TO C ( 64) TO C(65) 
PLANAR C ( 64) C(63) C(65) H(641) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 65) TO H(651) 
REST 0.087, 0.002 = H(651,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(651) TO C ( 65) TO C(64) 
CONT H(651) TO C ( 65) TO C(66) 
PLANAR C ( 65) C(64) C(66) H(651) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 66) TO H(661) 
REST 0.071, 0.002 = H(661,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(661) TO C ( 66) TO C(61) 
CONT H(661) TO C ( 66) TO C(65) 
PLANAR C ( 66) C(61) C(65) H(661) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 0 2 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 943298'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 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                   13.5244(3)
_cell_length_b                   12.0969(3)
_cell_length_c                   9.8466(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1610.94(6)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            4

# Given Formula = C12 H28 B1 Br1 P2 
# Dc =      1.34 Fooo =    680.00 Mu =     27.27 M =    162.51
# Found Formula = C12 H28 B1 Br1 P2 
# Dc =      1.34 FOOO =    680.00 Mu =     27.27 M =    162.51

_chemical_formula_sum            'C12 H28 B1 Br1 P2'
_chemical_formula_moiety         'C12 H28 B1 P2, Br1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         325.02


_cell_measurement_reflns_used    16490
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.140
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_max          0.270

_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    2.727

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -4 1 0.070
-1 4 -9 0.134
1 0 -7 0.146
-6 -7 1 0.080
8 1 0 0.081
4 8 -1 0.144
-2 1 0 0.090
-2 -1 8 0.150
8 -1 0 0.078
8 -9 0 0.090


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_T_max  0.703
_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       'φ & ω scans'

# 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            26642
_reflns_number_total             2352
_diffrn_reflns_av_R_equivalents  0.042
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 2352 
# Theoretical number of reflections is about 4712 


_diffrn_reflns_theta_min         3.012
_diffrn_reflns_theta_max         30.031
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        30.031
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_reflns_limit_h_min              0
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              17
_reflns_limit_l_min              0
_reflns_limit_l_max              13

_oxford_diffrn_Wilson_B_factor   2.69
_oxford_diffrn_Wilson_scale      2.81

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

_refine_diff_density_min         -0.47
_refine_diff_density_max         0.42


# 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         2348
_refine_ls_number_restraints     0
_refine_ls_number_parameters     75
_oxford_refine_ls_R_factor_ref   0.0386
_refine_ls_wR_factor_ref         0.0645
_refine_ls_goodness_of_fit_ref   0.9793
_refine_ls_shift/su_max          0.0002728
_refine_ls_shift/su_mean         0.0000243


# The values computed from all data 
_oxford_reflns_number_all        2348
_refine_ls_R_factor_all          0.0386
_refine_ls_wR_factor_all         0.0645

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1852
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_gt          0.0597

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 0.57P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.5000 0.2571(2) 0.2500 0.0393 1.0000 Uani S T . . . .
Br1 Br 0.5000 -0.078354(16) 0.2500 0.0378 1.0000 Uani S T . . . .
P1 P 0.43213(3) 0.17425(3) 0.38744(4) 0.0301 1.0000 Uani . . . . . .
C11 C 0.36365(10) 0.26621(11) 0.50065(13) 0.0288 1.0000 Uani . . . . . .
C12 C 0.43062(11) 0.35443(12) 0.56335(15) 0.0338 1.0000 Uani . . . . . .
C13 C 0.37158(12) 0.42842(13) 0.65969(17) 0.0392 1.0000 Uani . . . . . .
C14 C 0.28302(13) 0.48064(14) 0.58832(18) 0.0451 1.0000 Uani . . . . . .
C15 C 0.21736(12) 0.39277(16) 0.52477(18) 0.0444 1.0000 Uani . . . . . .
C16 C 0.27476(11) 0.31811(14) 0.42832(16) 0.0383 1.0000 Uani . . . . . .
H1 H 0.5549 0.3067 0.3006 0.0589 1.0000 Uiso . . . . . .
H11 H 0.3657 0.1056 0.3407 0.0434 1.0000 Uiso . . . . . .
H12 H 0.4876 0.1143 0.4653 0.0436 1.0000 Uiso . . . . . .
H111 H 0.3415 0.2195 0.5729 0.0341 1.0000 Uiso . . . . . .
H121 H 0.4579 0.3986 0.4909 0.0417 1.0000 Uiso . . . . . .
H122 H 0.4853 0.3207 0.6136 0.0417 1.0000 Uiso . . . . . .
H131 H 0.3492 0.3839 0.7370 0.0468 1.0000 Uiso . . . . . .
H132 H 0.4143 0.4853 0.6959 0.0467 1.0000 Uiso . . . . . .
H141 H 0.2457 0.5243 0.6525 0.0548 1.0000 Uiso . . . . . .
H142 H 0.3081 0.5290 0.5176 0.0543 1.0000 Uiso . . . . . .
H151 H 0.1643 0.4265 0.4749 0.0544 1.0000 Uiso . . . . . .
H152 H 0.1909 0.3462 0.5985 0.0519 1.0000 Uiso . . . . . .
H161 H 0.2967 0.3603 0.3515 0.0468 1.0000 Uiso . . . . . .
H162 H 0.2321 0.2603 0.3926 0.0474 1.0000 Uiso . . . . . .

_refine_ls_extinction_coef       120(12)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.6045(13)
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 . P1 6_655 1.9182(14) yes
B1 . H1 6_655 1.077 no
B1 . P1 . 1.9182(14) yes
B1 . H1 . 1.077 no
P1 . C11 . 1.8271(14) yes
P1 . H11 . 1.307 no
P1 . H12 . 1.294 no
C11 . C12 . 1.5298(19) yes
C11 . C16 . 1.532(2) yes
C11 . H111 . 0.957 no
C12 . C13 . 1.529(2) yes
C12 . H121 . 0.965 no
C12 . H122 . 0.979 no
C13 . C14 . 1.526(2) yes
C13 . H131 . 0.981 no
C13 . H132 . 0.967 no
C14 . C15 . 1.520(3) yes
C14 . H141 . 0.966 no
C14 . H142 . 0.970 no
C15 . C16 . 1.523(2) yes
C15 . H151 . 0.960 no
C15 . H152 . 0.985 no
C16 . H161 . 0.959 no
C16 . H162 . 0.973 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 6_655 B1 . H1 6_655 107.1 no
P1 6_655 B1 . P1 . 116.97(13) yes
H1 6_655 B1 . P1 . 106.7 no
P1 6_655 B1 . H1 . 106.7 no
H1 6_655 B1 . H1 . 112.4 no
P1 . B1 . H1 . 107.1 no
B1 . P1 . C11 . 110.78(8) yes
B1 . P1 . H11 . 114.4 no
C11 . P1 . H11 . 104.7 no
B1 . P1 . H12 . 115.7 no
C11 . P1 . H12 . 105.9 no
H11 . P1 . H12 . 104.5 no
P1 . C11 . C12 . 111.77(10) yes
P1 . C11 . C16 . 111.33(10) yes
C12 . C11 . C16 . 111.49(12) yes
P1 . C11 . H111 . 104.7 no
C12 . C11 . H111 . 107.3 no
C16 . C11 . H111 . 110.0 no
C11 . C12 . C13 . 110.46(12) yes
C11 . C12 . H121 . 108.3 no
C13 . C12 . H121 . 109.5 no
C11 . C12 . H122 . 111.1 no
C13 . C12 . H122 . 109.0 no
H121 . C12 . H122 . 108.4 no
C12 . C13 . C14 . 111.50(13) yes
C12 . C13 . H131 . 108.7 no
C14 . C13 . H131 . 110.0 no
C12 . C13 . H132 . 109.5 no
C14 . C13 . H132 . 110.1 no
H131 . C13 . H132 . 106.8 no
C13 . C14 . C15 . 111.03(14) yes
C13 . C14 . H141 . 109.6 no
C15 . C14 . H141 . 110.3 no
C13 . C14 . H142 . 107.8 no
C15 . C14 . H142 . 109.3 no
H141 . C14 . H142 . 108.8 no
C14 . C15 . C16 . 111.93(13) yes
C14 . C15 . H151 . 110.5 no
C16 . C15 . H151 . 108.3 no
C14 . C15 . H152 . 108.0 no
C16 . C15 . H152 . 107.8 no
H151 . C15 . H152 . 110.4 no
C11 . C16 . C15 . 110.68(12) yes
C11 . C16 . H161 . 110.0 no
C15 . C16 . H161 . 109.5 no
C11 . C16 . H162 . 109.8 no
C15 . C16 . H162 . 110.4 no
H161 . C16 . H162 . 106.3 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 01/11/11 at 17:43:57
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 01/11/11 at 17:43:57
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;



####################################################################### 
# 
# 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 943301'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;

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

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

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

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

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

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   12.8454(2)
_cell_length_b                   15.8917(3)
_cell_length_c                   14.0831(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.3055(11)
_cell_angle_gamma                90
_cell_volume                     2819.07(9)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'
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'


_cell_formula_units_Z            4

# Given Formula = C26 H26 B1 Br1 Cl0.50 P2 
# Dc =      1.20 Fooo =   1157.94 Mu =     16.29 M =    508.88
# Found Formula = C26.89 H27.79 B1 Br1 Cl1.79 P2 
# Dc =      1.34 FOOO =   1157.94 Mu =     17.54 M =    566.96

_chemical_formula_sum            'C26.89 H27.79 B1 Br1 Cl1.79 P2'
_chemical_formula_moiety         'C26 H26 B1 P2, Br1, C0.89 H1.79, Cl1.79'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         566.96


_cell_measurement_reflns_used    59767
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.210
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_max          0.370

_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1157.941
_exptl_absorpt_coefficient_mu    1.754
# 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 1 0.100
1 0 -1 0.110
-5 -1 -8 0.180
6 1 8 0.060
0 1 0 0.180
0 -1 0 0.190
-4 1 -5 0.148


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_T_max  0.718
_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 (Farrugia, 1997)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            56899
_reflns_number_total             6480
_diffrn_reflns_av_R_equivalents  0.040
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6480 
# Theoretical number of reflections is about 12998 


_diffrn_reflns_theta_min         2.714
_diffrn_reflns_theta_max         27.535
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        27.535
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   3.92
_oxford_diffrn_Wilson_scale      3.83

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

_refine_diff_density_min         -0.91
_refine_diff_density_max         0.98


# 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         6465
_refine_ls_number_restraints     10
_refine_ls_number_parameters     308
_oxford_refine_ls_R_factor_ref   0.0649
_refine_ls_wR_factor_ref         0.1540
_refine_ls_goodness_of_fit_ref   0.9833
_refine_ls_shift/su_max          0.0020679
_refine_ls_shift/su_mean         0.0000915


# The values computed from all data 
_oxford_reflns_number_all        6465
_refine_ls_R_factor_all          0.0649
_refine_ls_wR_factor_all         0.1540

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5240
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_gt          0.1437

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 3.53P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.5682(3) 0.7013(2) 0.7834(3) 0.0451 1.0000 Uani . . . . . .
Br1 Br 0.56949(3) 1.11132(2) 0.84833(3) 0.0550 1.0000 Uani . . . . . .
P1 P 0.56104(6) 0.81657(5) 0.73397(6) 0.0411 1.0000 Uani . . . . . .
P2 P 0.51050(6) 0.72085(5) 0.89832(6) 0.0393 1.0000 Uani . . . . . .
C1 C 0.4993(3) 0.8758(2) 0.8197(3) 0.0472 1.0000 Uani . . . . . .
C2 C 0.5318(3) 0.83277(19) 0.9192(2) 0.0449 1.0000 Uani . . . . . .
C11 C 0.4823(3) 0.8329(2) 0.6139(2) 0.0508 1.0000 Uani . . . . . .
C12 C 0.4464(3) 0.9135(3) 0.5853(3) 0.0689 1.0000 Uani . . . . . .
C13 C 0.3924(4) 0.9258(4) 0.4908(4) 0.0827 1.0000 Uani . . . . . .
C14 C 0.3736(4) 0.8610(5) 0.4274(4) 0.0877 1.0000 Uani . . . . . .
C15 C 0.4073(4) 0.7813(4) 0.4555(4) 0.0952 1.0000 Uani . . . . . .
C16 C 0.4623(4) 0.7680(3) 0.5503(3) 0.0711 1.0000 Uani . . . . . .
C21 C 0.6916(2) 0.8587(2) 0.7340(2) 0.0416 1.0000 Uani . . . . . .
C22 C 0.7128(3) 0.9438(2) 0.7474(3) 0.0527 1.0000 Uani . . . . . .
C23 C 0.8123(3) 0.9752(2) 0.7435(3) 0.0626 1.0000 Uani . . . . . .
C24 C 0.8914(3) 0.9215(3) 0.7259(3) 0.0606 1.0000 Uani . . . . . .
C25 C 0.8711(3) 0.8363(2) 0.7122(3) 0.0565 1.0000 Uani . . . . . .
C26 C 0.7713(3) 0.8051(2) 0.7158(2) 0.0481 1.0000 Uani . . . . . .
C31 C 0.3697(2) 0.70048(19) 0.8823(2) 0.0425 1.0000 Uani . . . . . .
C32 C 0.3163(3) 0.7212(3) 0.9558(3) 0.0587 1.0000 Uani . . . . . .
C33 C 0.2091(3) 0.7028(3) 0.9451(3) 0.0721 1.0000 Uani . . . . . .
C34 C 0.1551(3) 0.6653(3) 0.8617(3) 0.0636 1.0000 Uani . . . . . .
C35 C 0.2075(3) 0.6454(2) 0.7885(3) 0.0555 1.0000 Uani . . . . . .
C36 C 0.3149(3) 0.6629(2) 0.7980(2) 0.0484 1.0000 Uani . . . . . .
C41 C 0.5777(2) 0.66286(19) 1.0027(2) 0.0409 1.0000 Uani . . . . . .
C42 C 0.6043(3) 0.6998(2) 1.0938(3) 0.0517 1.0000 Uani . . . . . .
C43 C 0.6563(3) 0.6517(2) 1.1712(3) 0.0586 1.0000 Uani . . . . . .
C44 C 0.6808(3) 0.5685(2) 1.1583(3) 0.0563 1.0000 Uani . . . . . .
C45 C 0.6537(3) 0.5322(2) 1.0683(3) 0.0584 1.0000 Uani . . . . . .
C46 C 0.6019(3) 0.5785(2) 0.9897(3) 0.0524 1.0000 Uani . . . . . .
C50 C 0.8101(7) 1.0254(6) 1.0037(6) 0.1553 0.8925 Uani D . . . . .
Cl2 Cl 0.9034(3) 1.0822(3) 1.0651(3) 0.2251 0.8925 Uani D . . . . .
Cl10 Cl 0.8032(4) 0.9203(3) 1.0399(4) 0.1626 0.555(6) Uani D U P . . .
Cl11 Cl 0.7106(9) 0.9825(5) 1.0759(4) 0.1684 0.338(6) Uani D U P . . .
H1 H 0.5257 0.6637 0.7397 0.0537 1.0000 Uiso R . . . . .
H2 H 0.6391 0.6809 0.7984 0.0537 1.0000 Uiso R . . . . .
H11 H 0.4243 0.8751 0.7996 0.0555 1.0000 Uiso R . . . . .
H12 H 0.5238 0.9323 0.8235 0.0555 1.0000 Uiso R . . . . .
H21 H 0.4889 0.8528 0.9622 0.0529 1.0000 Uiso R . . . . .
H22 H 0.6044 0.8437 0.9459 0.0529 1.0000 Uiso R . . . . .
H121 H 0.4594 0.9592 0.6296 0.0798 1.0000 Uiso R . . . . .
H131 H 0.3680 0.9805 0.4703 0.0980 1.0000 Uiso R . . . . .
H141 H 0.3373 0.8706 0.3628 0.1036 1.0000 Uiso R . . . . .
H151 H 0.3924 0.7358 0.4111 0.1082 1.0000 Uiso R . . . . .
H161 H 0.4856 0.7128 0.5700 0.0857 1.0000 Uiso R . . . . .
H221 H 0.6585 0.9808 0.7589 0.0624 1.0000 Uiso R . . . . .
H231 H 0.8265 1.0336 0.7531 0.0749 1.0000 Uiso R . . . . .
H241 H 0.9598 0.9431 0.7234 0.0716 1.0000 Uiso R . . . . .
H251 H 0.9254 0.7995 0.7002 0.0657 1.0000 Uiso R . . . . .
H261 H 0.7571 0.7468 0.7056 0.0564 1.0000 Uiso R . . . . .
H321 H 0.3530 0.7477 1.0132 0.0687 1.0000 Uiso R . . . . .
H331 H 0.1726 0.7163 0.9956 0.0845 1.0000 Uiso R . . . . .
H341 H 0.0817 0.6528 0.8551 0.0754 1.0000 Uiso R . . . . .
H351 H 0.1699 0.6199 0.7309 0.0645 1.0000 Uiso R . . . . .
H361 H 0.3508 0.6490 0.7472 0.0563 1.0000 Uiso R . . . . .
H421 H 0.5873 0.7571 1.1028 0.0598 1.0000 Uiso R . . . . .
H431 H 0.6755 0.6766 1.2335 0.0684 1.0000 Uiso R . . . . .
H441 H 0.7156 0.5361 1.2119 0.0666 1.0000 Uiso R . . . . .
H451 H 0.6710 0.4750 1.0595 0.0681 1.0000 Uiso R . . . . .
H461 H 0.5829 0.5532 0.9275 0.0613 1.0000 Uiso R . . . . .
H501 H 0.8146 1.0264 0.9372 0.2001 0.5548 Uiso R . . . . .
H502 H 0.7454 1.0508 1.0117 0.2001 0.5548 Uiso R . . . . .
H511 H 0.7719 1.0583 0.9521 0.2001 0.3377 Uiso R . . . . .
H512 H 0.8412 0.9785 0.9781 0.2001 0.3377 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.6168(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
B1 . P1 . 1.955(4) yes
B1 . P2 . 1.933(4) yes
B1 . H1 . 0.950 no
B1 . H2 . 0.950 no
P1 . C1 . 1.830(3) yes
P1 . C11 . 1.811(3) yes
P1 . C21 . 1.806(3) yes
P2 . C2 . 1.815(3) yes
P2 . C31 . 1.807(3) yes
P2 . C41 . 1.805(3) yes
C1 . C2 . 1.540(5) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C2 . H21 . 0.950 no
C2 . H22 . 0.950 no
C11 . C12 . 1.394(6) yes
C11 . C16 . 1.357(6) yes
C12 . C13 . 1.389(6) yes
C12 . H121 . 0.950 no
C13 . C14 . 1.353(8) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.371(9) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.400(6) yes
C15 . H151 . 0.950 no
C16 . H161 . 0.950 no
C21 . C22 . 1.384(5) yes
C21 . C26 . 1.394(4) yes
C22 . C23 . 1.384(5) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.387(6) yes
C23 . H231 . 0.950 no
C24 . C25 . 1.386(6) yes
C24 . H241 . 0.950 no
C25 . C26 . 1.385(5) yes
C25 . H251 . 0.950 no
C26 . H261 . 0.950 no
C31 . C32 . 1.389(5) yes
C31 . C36 . 1.391(5) yes
C32 . C33 . 1.387(5) yes
C32 . H321 . 0.950 no
C33 . C34 . 1.377(6) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.373(6) yes
C34 . H341 . 0.950 no
C35 . C36 . 1.388(5) yes
C35 . H351 . 0.950 no
C36 . H361 . 0.950 no
C41 . C42 . 1.392(5) yes
C41 . C46 . 1.397(5) yes
C42 . C43 . 1.391(5) yes
C42 . H421 . 0.950 no
C43 . C44 . 1.378(5) yes
C43 . H431 . 0.950 no
C44 . C45 . 1.374(5) yes
C44 . H441 . 0.950 no
C45 . C46 . 1.386(5) yes
C45 . H451 . 0.950 no
C46 . H461 . 0.950 no
C50 . Cl2 . 1.610(8) yes
C50 . Cl10 . 1.754(9) yes
C50 . Cl11 . 1.908(13) yes
C50 . H501 . 0.950 no
C50 . H502 . 0.950 no
C50 . H511 . 0.950 no
C50 . H512 . 0.950 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 . B1 . P2 . 98.56(16) yes
P1 . B1 . H1 . 112.2 no
P2 . B1 . H1 . 112.2 no
P1 . B1 . H2 . 112.0 no
P2 . B1 . H2 . 112.1 no
H1 . B1 . H2 . 109.5 no
B1 . P1 . C1 . 104.05(15) yes
B1 . P1 . C11 . 116.45(17) yes
C1 . P1 . C11 . 107.93(16) yes
B1 . P1 . C21 . 111.62(16) yes
C1 . P1 . C21 . 109.37(15) yes
C11 . P1 . C21 . 107.21(15) yes
B1 . P2 . C2 . 102.85(15) yes
B1 . P2 . C31 . 113.94(16) yes
C2 . P2 . C31 . 108.13(15) yes
B1 . P2 . C41 . 113.54(15) yes
C2 . P2 . C41 . 109.62(15) yes
C31 . P2 . C41 . 108.48(14) yes
P1 . C1 . C2 . 107.3(2) yes
P1 . C1 . H11 . 110.1 no
C2 . C1 . H11 . 110.2 no
P1 . C1 . H12 . 109.9 no
C2 . C1 . H12 . 109.9 no
H11 . C1 . H12 . 109.5 no
C1 . C2 . P2 . 106.4(2) yes
C1 . C2 . H21 . 110.1 no
P2 . C2 . H21 . 110.1 no
C1 . C2 . H22 . 110.4 no
P2 . C2 . H22 . 110.3 no
H21 . C2 . H22 . 109.5 no
P1 . C11 . C12 . 119.6(3) yes
P1 . C11 . C16 . 120.4(3) yes
C12 . C11 . C16 . 120.0(4) yes
C11 . C12 . C13 . 118.7(5) yes
C11 . C12 . H121 . 120.5 no
C13 . C12 . H121 . 120.8 no
C12 . C13 . C14 . 121.1(5) yes
C12 . C13 . H131 . 119.5 no
C14 . C13 . H131 . 119.4 no
C13 . C14 . C15 . 120.5(4) yes
C13 . C14 . H141 . 120.0 no
C15 . C14 . H141 . 119.5 no
C14 . C15 . C16 . 119.1(5) yes
C14 . C15 . H151 . 120.1 no
C16 . C15 . H151 . 120.8 no
C15 . C16 . C11 . 120.6(5) yes
C15 . C16 . H161 . 119.3 no
C11 . C16 . H161 . 120.1 no
P1 . C21 . C22 . 121.3(2) yes
P1 . C21 . C26 . 119.2(3) yes
C22 . C21 . C26 . 119.4(3) yes
C21 . C22 . C23 . 120.4(3) yes
C21 . C22 . H221 . 119.7 no
C23 . C22 . H221 . 119.9 no
C22 . C23 . C24 . 120.0(4) yes
C22 . C23 . H231 . 120.0 no
C24 . C23 . H231 . 120.0 no
C23 . C24 . C25 . 120.1(3) yes
C23 . C24 . H241 . 120.0 no
C25 . C24 . H241 . 119.8 no
C24 . C25 . C26 . 119.7(3) yes
C24 . C25 . H251 . 120.1 no
C26 . C25 . H251 . 120.2 no
C21 . C26 . C25 . 120.4(3) yes
C21 . C26 . H261 . 119.8 no
C25 . C26 . H261 . 119.8 no
P2 . C31 . C32 . 119.6(3) yes
P2 . C31 . C36 . 120.6(3) yes
C32 . C31 . C36 . 119.8(3) yes
C31 . C32 . C33 . 119.6(4) yes
C31 . C32 . H321 . 120.3 no
C33 . C32 . H321 . 120.1 no
C32 . C33 . C34 . 120.5(4) yes
C32 . C33 . H331 . 119.7 no
C34 . C33 . H331 . 119.8 no
C33 . C34 . C35 . 120.1(3) yes
C33 . C34 . H341 . 119.9 no
C35 . C34 . H341 . 120.1 no
C34 . C35 . C36 . 120.4(3) yes
C34 . C35 . H351 . 119.8 no
C36 . C35 . H351 . 119.8 no
C31 . C36 . C35 . 119.7(3) yes
C31 . C36 . H361 . 120.2 no
C35 . C36 . H361 . 120.1 no
P2 . C41 . C42 . 121.8(2) yes
P2 . C41 . C46 . 117.8(2) yes
C42 . C41 . C46 . 120.4(3) yes
C41 . C42 . C43 . 118.9(3) yes
C41 . C42 . H421 . 120.4 no
C43 . C42 . H421 . 120.7 no
C42 . C43 . C44 . 120.8(3) yes
C42 . C43 . H431 . 119.5 no
C44 . C43 . H431 . 119.8 no
C43 . C44 . C45 . 120.1(3) yes
C43 . C44 . H441 . 120.0 no
C45 . C44 . H441 . 119.9 no
C44 . C45 . C46 . 120.6(3) yes
C44 . C45 . H451 . 120.0 no
C46 . C45 . H451 . 119.4 no
C41 . C46 . C45 . 119.2(3) yes
C41 . C46 . H461 . 120.2 no
C45 . C46 . H461 . 120.5 no
Cl2 . C50 . Cl10 . 116.9(4) yes
Cl2 . C50 . Cl11 . 114.9(6) yes
Cl2 . C50 . H501 . 109.7 no
Cl10 . C50 . H501 . 108.6 no
Cl2 . C50 . H502 . 106.0 no
Cl10 . C50 . H502 . 105.9 no
H501 . C50 . H502 . 109.5 no
Cl2 . C50 . H511 . 108.7 no
Cl11 . C50 . H511 . 107.8 no
Cl2 . C50 . H512 . 108.6 no
Cl11 . C50 . H512 . 107.3 no
H511 . C50 . H512 . 109.5 no

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 11/08/11 at 11:50:03
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT CL(10, OCC) CL(11, OCC) 
EQUIV CL(10, OCC) CL(11, OCC) 
WEIGHT -1 CL(10, OCC) 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
CONT H   ( 511,X'S) H   ( 512,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 11/08/11 at 11:50:03
#
#LIST     16                                                                    
U(IJ) 0.0, 0.02 = CL(10) TO CL(11) 
DIST 0.0, 0.05 = MEAN C(50) TO CL(10), C(50) TO CL(11) 
ANGLE 0.0, 3. = MEAN CL(10) TO C(50) TO CL(2), CL(11) TO C(50) TO CL(2) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;



####################################################################### 
# 
# 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_jas134
_database_code_depnum_ccdc_archive 'CCDC 1530819'
_audit_update_record             
;
2017-02-03 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_audit_creation_date             13-09-19
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 'jas134 At 9:26 on 19/ 9'
_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                   12.7639(3)
_cell_length_b                   21.4218(5)
_cell_length_c                   14.4115(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.4493(13)
_cell_angle_gamma                90
_cell_volume                     3922.67(14)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
As 0.0499 2.0058 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972
2.5310 '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'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 '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'


_cell_formula_units_Z            4

# Given Formula = C41 H41 As1 B1 F6 O1 P3 
# Dc =      1.43 Fooo =   1728.00 Mu =     10.50 M =    842.42
# Found Formula = C41 H41 As1 B1 F6 O1 P3 
# Dc =      1.43 FOOO =   1728.00 Mu =     10.50 M =    842.42

_chemical_formula_sum            'C41 H41 As1 B1 F6 O1 P3'
_chemical_formula_moiety         'C41 H41 B1 O1 P3, As1 F6'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         842.42


_cell_measurement_reflns_used    39007
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25
_cell_measurement_temperature    200

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_max          0.280

_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    1.050

# Absorption correction 

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

# 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    '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            58122
_reflns_number_total             6921
_diffrn_reflns_av_R_equivalents  0.084
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6921 
# Theoretical number of reflections is about 13858 


_diffrn_reflns_theta_min         2.787
_diffrn_reflns_theta_max         25.025
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        25.025
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              25
_reflns_limit_l_min              0
_reflns_limit_l_max              17

_oxford_diffrn_Wilson_B_factor   3.45
_oxford_diffrn_Wilson_scale      43.07

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

_refine_diff_density_min         -0.70
_refine_diff_density_max         1.12


# 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         6919
_refine_ls_number_restraints     201
_refine_ls_number_parameters     478
_oxford_refine_ls_R_factor_ref   0.0783
_refine_ls_wR_factor_ref         0.1347
_refine_ls_goodness_of_fit_ref   0.9475
_refine_ls_shift/su_max          0.0015747
_refine_ls_shift/su_mean         0.0000327


# The values computed from all data 
_oxford_reflns_number_all        6919
_refine_ls_R_factor_all          0.0783
_refine_ls_wR_factor_all         0.1347

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4974
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_gt          0.1224

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 5.45P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
As1 As 0.38114(4) 0.60629(2) 1.20550(3) 0.0469 1.0000 Uani . . . . . .
B1 B 0.6197(4) 0.7580(2) 0.8040(3) 0.0412 1.0000 Uani . . . . . .
F1 F 0.4260(4) 0.57004(19) 1.1146(2) 0.1238 1.0000 Uani . . . . . .
F2 F 0.3663(3) 0.67193(18) 1.1412(3) 0.1258 1.0000 Uani . . . . . .
F3 F 0.5095(2) 0.62527(16) 1.2416(2) 0.0912 1.0000 Uani . . . . . .
F4 F 0.3434(3) 0.6425(2) 1.3002(3) 0.1397 1.0000 Uani . . . . . .
F5 F 0.4007(3) 0.54087(16) 1.2711(2) 0.1018 1.0000 Uani . . . . . .
F6 F 0.2566(3) 0.5882(2) 1.1735(3) 0.1223 1.0000 Uani . . . . . .
O1 O 0.2471(2) 0.64311(13) 0.8247(2) 0.0527 1.0000 Uani . . . . . .
P1 P 0.29297(8) 0.58015(5) 0.81502(7) 0.0380 1.0000 Uani D . . . . .
P2 P 0.63290(8) 0.67940(5) 0.74226(6) 0.0368 1.0000 Uani D . . . . .
P3 P 0.56337(8) 0.74600(5) 0.92211(7) 0.0384 1.0000 Uani D . . . . .
C1 C 0.4212(3) 0.56940(17) 0.8802(2) 0.0377 1.0000 Uani D . . . . .
C2 C 0.5287(3) 0.62731(17) 0.7708(2) 0.0369 1.0000 Uani D . . . . .
C3 C 0.4710(3) 0.68124(17) 0.9166(2) 0.0387 1.0000 Uani D . . . . .
C4 C 0.5090(3) 0.61918(16) 0.8743(2) 0.0354 1.0000 Uani D . . . . .
C5 C 0.6078(3) 0.59431(19) 0.9321(3) 0.0434 1.0000 Uani D . . . . .
C11 C 0.3080(3) 0.56016(17) 0.6946(3) 0.0401 1.0000 Uani D . . . . .
C12 C 0.2661(3) 0.60122(18) 0.6253(3) 0.0474 1.0000 Uani D . . . . .
C13 C 0.2814(3) 0.5896(2) 0.5327(3) 0.0583 1.0000 Uani D . . . . .
C14 C 0.3363(3) 0.5381(2) 0.5089(3) 0.0627 1.0000 Uani D . . . . .
C15 C 0.3764(3) 0.4969(2) 0.5765(3) 0.0598 1.0000 Uani D . . . . .
C16 C 0.3625(3) 0.50789(18) 0.6694(3) 0.0488 1.0000 Uani D . . . . .
C21 C 0.2151(3) 0.51877(18) 0.8603(3) 0.0435 1.0000 Uani D . . . . .
C22 C 0.1685(3) 0.47103(19) 0.8055(3) 0.0585 1.0000 Uani D . . . . .
C23 C 0.1032(3) 0.4285(2) 0.8427(4) 0.0773 1.0000 Uani D . . . . .
C24 C 0.0852(3) 0.4315(2) 0.9348(4) 0.0793 1.0000 Uani D . . . . .
C25 C 0.1317(3) 0.4779(3) 0.9899(4) 0.0767 1.0000 Uani D . . . . .
C26 C 0.1954(3) 0.5220(2) 0.9529(3) 0.0612 1.0000 Uani D . . . . .
C31 C 0.6087(3) 0.69436(17) 0.6187(3) 0.0404 1.0000 Uani D . . . . .
C32 C 0.6485(3) 0.7481(2) 0.5820(3) 0.0511 1.0000 Uani D . . . . .
C33 C 0.6305(3) 0.7611(2) 0.4875(3) 0.0617 1.0000 Uani D . . . . .
C34 C 0.5711(3) 0.7203(2) 0.4303(3) 0.0664 1.0000 Uani D . . . . .
C35 C 0.5299(3) 0.6671(2) 0.4656(3) 0.0599 1.0000 Uani D . . . . .
C36 C 0.5499(3) 0.65367(19) 0.5596(3) 0.0511 1.0000 Uani D . . . . .
C41 C 0.7591(3) 0.64098(18) 0.7565(2) 0.0405 1.0000 Uani D . . . . .
C42 C 0.8498(3) 0.6769(2) 0.7711(3) 0.0602 1.0000 Uani D . . . . .
C43 C 0.9478(4) 0.6484(3) 0.7731(3) 0.0778 1.0000 Uani D . . . . .
C44 C 0.9552(4) 0.5852(3) 0.7613(3) 0.0740 1.0000 Uani D . . . . .
C45 C 0.8658(4) 0.5491(2) 0.7467(2) 0.0647 1.0000 Uani D . . . . .
C46 C 0.7680(3) 0.5770(2) 0.7437(2) 0.0500 1.0000 Uani D . . . . .
C51 C 0.4892(3) 0.81517(18) 0.9442(2) 0.0415 1.0000 Uani D . . . . .
C52 C 0.3999(3) 0.8143(2) 0.9918(3) 0.0643 1.0000 Uani D . . . . .
C53 C 0.3474(4) 0.8694(2) 1.0071(3) 0.0752 1.0000 Uani D . . . . .
C54 C 0.3831(4) 0.9247(2) 0.9771(3) 0.0669 1.0000 Uani D . . . . .
C55 C 0.4712(4) 0.9267(2) 0.9285(3) 0.0619 1.0000 Uani D . . . . .
C56 C 0.5240(3) 0.8722(2) 0.9118(3) 0.0535 1.0000 Uani D . . . . .
C61 C 0.6597(3) 0.73668(16) 1.0214(3) 0.0416 1.0000 Uani D . . . . .
C62 C 0.6266(4) 0.72529(18) 1.1092(3) 0.0572 1.0000 Uani D . . . . .
C63 C 0.7005(4) 0.71922(17) 1.1857(3) 0.0677 1.0000 Uani D . . . . .
C64 C 0.8058(4) 0.72414(16) 1.1752(3) 0.0629 1.0000 Uani D . . . . .
C65 C 0.8386(4) 0.73440(16) 1.0884(4) 0.0617 1.0000 Uani D . . . . .
C66 C 0.7660(3) 0.74111(16) 1.0114(3) 0.0504 1.0000 Uani D . . . . .
H1 H 0.5514 0.7826 0.7591 0.0646 1.0000 Uiso R . . . . .
H2 H 0.6980 0.7884 0.8138 0.0640 1.0000 Uiso R . . . . .
H11 H 0.4077 0.5664 0.9448 0.0452 1.0000 Uiso DR . . . . .
H12 H 0.4494 0.5293 0.8604 0.0457 1.0000 Uiso DR . . . . .
H21 H 0.5430 0.5864 0.7458 0.0428 1.0000 Uiso DR . . . . .
H22 H 0.4641 0.6449 0.7386 0.0432 1.0000 Uiso DR . . . . .
H31 H 0.4534 0.6725 0.9799 0.0464 1.0000 Uiso DR . . . . .
H32 H 0.4072 0.6947 0.8790 0.0462 1.0000 Uiso DR . . . . .
H51 H 0.6256 0.5542 0.9077 0.0640 1.0000 Uiso DR . . . . .
H52 H 0.6658 0.6219 0.9274 0.0641 1.0000 Uiso DR . . . . .
H53 H 0.5941 0.5897 0.9966 0.0636 1.0000 Uiso DR . . . . .
H121 H 0.2268 0.6362 0.6418 0.0586 1.0000 Uiso DR . . . . .
H131 H 0.2535 0.6168 0.4862 0.0686 1.0000 Uiso DR . . . . .
H141 H 0.3467 0.5311 0.4459 0.0735 1.0000 Uiso DR . . . . .
H151 H 0.4131 0.4614 0.5597 0.0734 1.0000 Uiso DR . . . . .
H161 H 0.3898 0.4796 0.7154 0.0584 1.0000 Uiso DR . . . . .
H221 H 0.1823 0.4684 0.7429 0.0698 1.0000 Uiso DR . . . . .
H231 H 0.0687 0.3974 0.8058 0.0915 1.0000 Uiso DR . . . . .
H241 H 0.0421 0.4017 0.9601 0.0913 1.0000 Uiso DR . . . . .
H251 H 0.1199 0.4800 1.0532 0.0902 1.0000 Uiso DR . . . . .
H261 H 0.2262 0.5542 0.9898 0.0747 1.0000 Uiso DR . . . . .
H321 H 0.6874 0.7760 0.6215 0.0605 1.0000 Uiso DR . . . . .
H331 H 0.6585 0.7977 0.4626 0.0731 1.0000 Uiso DR . . . . .
H341 H 0.5577 0.7291 0.3665 0.0756 1.0000 Uiso DR . . . . .
H351 H 0.4889 0.6399 0.4259 0.0704 1.0000 Uiso DR . . . . .
H361 H 0.5237 0.6168 0.5842 0.0601 1.0000 Uiso DR . . . . .
H421 H 0.8442 0.7201 0.7796 0.0705 1.0000 Uiso DR . . . . .
H431 H 1.0101 0.6721 0.7830 0.0893 1.0000 Uiso DR . . . . .
H441 H 1.0223 0.5666 0.7640 0.0845 1.0000 Uiso DR . . . . .
H451 H 0.8716 0.5053 0.7374 0.0776 1.0000 Uiso DR . . . . .
H461 H 0.7074 0.5525 0.7341 0.0596 1.0000 Uiso DR . . . . .
H521 H 0.3746 0.7762 1.0126 0.0765 1.0000 Uiso DR . . . . .
H531 H 0.2863 0.8683 1.0384 0.0876 1.0000 Uiso DR . . . . .
H541 H 0.3472 0.9618 0.9881 0.0796 1.0000 Uiso DR . . . . .
H551 H 0.4952 0.9652 0.9069 0.0736 1.0000 Uiso DR . . . . .
H561 H 0.5842 0.8734 0.8779 0.0643 1.0000 Uiso DR . . . . .
H621 H 0.5533 0.7213 1.1163 0.0674 1.0000 Uiso DR . . . . .
H631 H 0.6786 0.7115 1.2445 0.0805 1.0000 Uiso DR . . . . .
H641 H 0.8556 0.7211 1.2271 0.0745 1.0000 Uiso DR . . . . .
H651 H 0.9117 0.7371 1.0821 0.0742 1.0000 Uiso DR . . . . .
H661 H 0.7892 0.7493 0.9515 0.0604 1.0000 Uiso DR . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.16982(10)
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
As1 . F1 . 1.670(3) yes
As1 . F2 . 1.685(3) yes
As1 . F3 . 1.720(3) yes
As1 . F4 . 1.679(3) yes
As1 . F5 . 1.696(3) yes
As1 . F6 . 1.659(3) yes
B1 . P2 . 1.919(4) yes
B1 . P3 . 1.926(4) yes
B1 . H1 . 1.161 no
B1 . H2 . 1.190 no
O1 . P1 . 1.482(3) yes
P1 . C1 . 1.822(4) yes
P1 . C11 . 1.816(4) yes
P1 . C21 . 1.807(4) yes
P2 . C2 . 1.812(4) yes
P2 . C31 . 1.807(4) yes
P2 . C41 . 1.804(4) yes
P3 . C3 . 1.817(4) yes
P3 . C51 . 1.803(4) yes
P3 . C61 . 1.807(4) yes
C1 . C4 . 1.555(5) yes
C1 . H11 . 0.964 no
C1 . H12 . 0.984 no
C2 . C4 . 1.547(5) yes
C2 . H21 . 0.971 no
C2 . H22 . 0.983 no
C3 . C4 . 1.559(5) yes
C3 . H31 . 0.978 no
C3 . H32 . 0.978 no
C4 . C5 . 1.539(5) yes
C5 . H51 . 0.963 no
C5 . H52 . 0.956 no
C5 . H53 . 0.966 no
C11 . C12 . 1.398(5) yes
C11 . C16 . 1.384(5) yes
C12 . C13 . 1.390(6) yes
C12 . H121 . 0.944 no
C13 . C14 . 1.366(7) yes
C13 . H131 . 0.934 no
C14 . C15 . 1.378(7) yes
C14 . H141 . 0.942 no
C15 . C16 . 1.387(6) yes
C15 . H151 . 0.936 no
C16 . H161 . 0.941 no
C21 . C22 . 1.391(6) yes
C21 . C26 . 1.382(6) yes
C22 . C23 . 1.377(6) yes
C22 . H221 . 0.937 no
C23 . C24 . 1.370(7) yes
C23 . H231 . 0.936 no
C24 . C25 . 1.372(8) yes
C24 . H241 . 0.940 no
C25 . C26 . 1.385(7) yes
C25 . H251 . 0.939 no
C26 . H261 . 0.936 no
C31 . C32 . 1.384(5) yes
C31 . C36 . 1.388(6) yes
C32 . C33 . 1.386(6) yes
C32 . H321 . 0.935 no
C33 . C34 . 1.378(7) yes
C33 . H331 . 0.948 no
C34 . C35 . 1.372(7) yes
C34 . H341 . 0.938 no
C35 . C36 . 1.385(6) yes
C35 . H351 . 0.941 no
C36 . H361 . 0.941 no
C41 . C42 . 1.389(6) yes
C41 . C46 . 1.389(6) yes
C42 . C43 . 1.389(6) yes
C42 . H421 . 0.939 no
C43 . C44 . 1.367(7) yes
C43 . H431 . 0.944 no
C44 . C45 . 1.378(7) yes
C44 . H441 . 0.943 no
C45 . C46 . 1.381(6) yes
C45 . H451 . 0.950 no
C46 . H461 . 0.934 no
C51 . C52 . 1.385(6) yes
C51 . C56 . 1.395(6) yes
C52 . C53 . 1.384(6) yes
C52 . H521 . 0.939 no
C53 . C54 . 1.356(7) yes
C53 . H531 . 0.937 no
C54 . C55 . 1.382(7) yes
C54 . H541 . 0.938 no
C55 . C56 . 1.382(6) yes
C55 . H551 . 0.942 no
C56 . H561 . 0.949 no
C61 . C62 . 1.393(6) yes
C61 . C66 . 1.382(5) yes
C62 . C63 . 1.388(6) yes
C62 . H621 . 0.955 no
C63 . C64 . 1.371(7) yes
C63 . H631 . 0.933 no
C64 . C65 . 1.374(7) yes
C64 . H641 . 0.937 no
C65 . C66 . 1.385(6) yes
C65 . H651 . 0.948 no
C66 . H661 . 0.954 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
F1 . As1 . F2 . 89.2(2) yes
F1 . As1 . F3 . 87.7(2) yes
F2 . As1 . F3 . 91.35(18) yes
F1 . As1 . F4 . 176.6(2) yes
F2 . As1 . F4 . 92.0(2) yes
F3 . As1 . F4 . 89.0(2) yes
F1 . As1 . F5 . 90.6(2) yes
F2 . As1 . F5 . 177.95(18) yes
F3 . As1 . F5 . 86.60(16) yes
F4 . As1 . F5 . 88.1(2) yes
F1 . As1 . F6 . 93.7(2) yes
F2 . As1 . F6 . 89.3(2) yes
F3 . As1 . F6 . 178.51(19) yes
F4 . As1 . F6 . 89.6(2) yes
F5 . As1 . F6 . 92.77(18) yes
P2 . B1 . P3 . 110.5(2) yes
P2 . B1 . H1 . 103.5 no
P3 . B1 . H1 . 103.3 no
P2 . B1 . H2 . 115.1 no
P3 . B1 . H2 . 110.4 no
H1 . B1 . H2 . 113.3 no
O1 . P1 . C1 . 114.21(17) yes
O1 . P1 . C11 . 112.52(17) yes
C1 . P1 . C11 . 106.96(17) yes
O1 . P1 . C21 . 113.12(17) yes
C1 . P1 . C21 . 102.66(16) yes
C11 . P1 . C21 . 106.59(17) yes
B1 . P2 . C2 . 109.65(18) yes
B1 . P2 . C31 . 106.68(18) yes
C2 . P2 . C31 . 105.79(17) yes
B1 . P2 . C41 . 117.67(19) yes
C2 . P2 . C41 . 111.08(18) yes
C31 . P2 . C41 . 105.11(15) yes
B1 . P3 . C3 . 110.99(18) yes
B1 . P3 . C51 . 107.04(19) yes
C3 . P3 . C51 . 106.60(17) yes
B1 . P3 . C61 . 115.6(2) yes
C3 . P3 . C61 . 109.87(17) yes
C51 . P3 . C61 . 106.25(16) yes
P1 . C1 . C4 . 120.1(3) yes
P1 . C1 . H11 . 105.8 no
C4 . C1 . H11 . 107.1 no
P1 . C1 . H12 . 107.2 no
C4 . C1 . H12 . 107.3 no
H11 . C1 . H12 . 109.0 no
P2 . C2 . C4 . 118.6(2) yes
P2 . C2 . H21 . 107.7 no
C4 . C2 . H21 . 108.0 no
P2 . C2 . H22 . 104.9 no
C4 . C2 . H22 . 107.0 no
H21 . C2 . H22 . 110.5 no
P3 . C3 . C4 . 116.3(3) yes
P3 . C3 . H31 . 108.1 no
C4 . C3 . H31 . 108.0 no
P3 . C3 . H32 . 107.6 no
C4 . C3 . H32 . 107.9 no
H31 . C3 . H32 . 108.6 no
C2 . C4 . C1 . 108.3(3) yes
C2 . C4 . C3 . 111.5(3) yes
C1 . C4 . C3 . 108.1(3) yes
C2 . C4 . C5 . 111.1(3) yes
C1 . C4 . C5 . 106.9(3) yes
C3 . C4 . C5 . 110.7(3) yes
C4 . C5 . H51 . 108.7 no
C4 . C5 . H52 . 110.4 no
H51 . C5 . H52 . 108.3 no
C4 . C5 . H53 . 110.0 no
H51 . C5 . H53 . 109.3 no
H52 . C5 . H53 . 110.1 no
P1 . C11 . C12 . 117.8(3) yes
P1 . C11 . C16 . 122.9(3) yes
C12 . C11 . C16 . 119.3(4) yes
C11 . C12 . C13 . 119.5(4) yes
C11 . C12 . H121 . 119.7 no
C13 . C12 . H121 . 120.7 no
C12 . C13 . C14 . 120.6(4) yes
C12 . C13 . H131 . 119.9 no
C14 . C13 . H131 . 119.6 no
C13 . C14 . C15 . 120.3(4) yes
C13 . C14 . H141 . 119.6 no
C15 . C14 . H141 . 120.2 no
C14 . C15 . C16 . 120.0(4) yes
C14 . C15 . H151 . 119.9 no
C16 . C15 . H151 . 120.1 no
C15 . C16 . C11 . 120.3(4) yes
C15 . C16 . H161 . 119.9 no
C11 . C16 . H161 . 119.8 no
P1 . C21 . C22 . 123.4(3) yes
P1 . C21 . C26 . 118.0(3) yes
C22 . C21 . C26 . 118.5(4) yes
C21 . C22 . C23 . 120.5(5) yes
C21 . C22 . H221 . 118.8 no
C23 . C22 . H221 . 120.7 no
C22 . C23 . C24 . 120.6(5) yes
C22 . C23 . H231 . 121.3 no
C24 . C23 . H231 . 118.1 no
C23 . C24 . C25 . 119.4(5) yes
C23 . C24 . H241 . 120.1 no
C25 . C24 . H241 . 120.4 no
C24 . C25 . C26 . 120.5(5) yes
C24 . C25 . H251 . 119.7 no
C26 . C25 . H251 . 119.8 no
C25 . C26 . C21 . 120.4(5) yes
C25 . C26 . H261 . 120.9 no
C21 . C26 . H261 . 118.7 no
P2 . C31 . C32 . 119.3(3) yes
P2 . C31 . C36 . 121.7(3) yes
C32 . C31 . C36 . 119.0(4) yes
C31 . C32 . C33 . 120.6(4) yes
C31 . C32 . H321 . 119.4 no
C33 . C32 . H321 . 120.0 no
C32 . C33 . C34 . 119.5(4) yes
C32 . C33 . H331 . 120.3 no
C34 . C33 . H331 . 120.2 no
C33 . C34 . C35 . 120.8(4) yes
C33 . C34 . H341 . 119.8 no
C35 . C34 . H341 . 119.3 no
C34 . C35 . C36 . 119.6(4) yes
C34 . C35 . H351 . 120.0 no
C36 . C35 . H351 . 120.4 no
C31 . C36 . C35 . 120.5(4) yes
C31 . C36 . H361 . 119.1 no
C35 . C36 . H361 . 120.3 no
P2 . C41 . C42 . 119.2(3) yes
P2 . C41 . C46 . 121.2(3) yes
C42 . C41 . C46 . 119.2(4) yes
C41 . C42 . C43 . 119.7(4) yes
C41 . C42 . H421 . 119.5 no
C43 . C42 . H421 . 120.8 no
C42 . C43 . C44 . 120.3(5) yes
C42 . C43 . H431 . 120.7 no
C44 . C43 . H431 . 119.0 no
C43 . C44 . C45 . 120.6(5) yes
C43 . C44 . H441 . 119.1 no
C45 . C44 . H441 . 120.2 no
C44 . C45 . C46 . 119.6(5) yes
C44 . C45 . H451 . 120.1 no
C46 . C45 . H451 . 120.3 no
C41 . C46 . C45 . 120.6(4) yes
C41 . C46 . H461 . 119.8 no
C45 . C46 . H461 . 119.6 no
P3 . C51 . C52 . 123.2(3) yes
P3 . C51 . C56 . 118.1(3) yes
C52 . C51 . C56 . 118.7(4) yes
C51 . C52 . C53 . 120.1(4) yes
C51 . C52 . H521 . 119.6 no
C53 . C52 . H521 . 120.3 no
C52 . C53 . C54 . 120.7(4) yes
C52 . C53 . H531 . 119.6 no
C54 . C53 . H531 . 119.6 no
C53 . C54 . C55 . 120.2(4) yes
C53 . C54 . H541 . 120.2 no
C55 . C54 . H541 . 119.5 no
C54 . C55 . C56 . 119.7(4) yes
C54 . C55 . H551 . 120.0 no
C56 . C55 . H551 . 120.3 no
C51 . C56 . C55 . 120.4(4) yes
C51 . C56 . H561 . 119.7 no
C55 . C56 . H561 . 119.9 no
P3 . C61 . C62 . 119.8(3) yes
P3 . C61 . C66 . 120.7(3) yes
C62 . C61 . C66 . 119.5(4) yes
C61 . C62 . C63 . 119.7(4) yes
C61 . C62 . H621 . 119.9 no
C63 . C62 . H621 . 120.4 no
C62 . C63 . C64 . 120.4(4) yes
C62 . C63 . H631 . 119.9 no
C64 . C63 . H631 . 119.7 no
C63 . C64 . C65 . 120.0(4) yes
C63 . C64 . H641 . 120.3 no
C65 . C64 . H641 . 119.7 no
C64 . C65 . C66 . 120.5(4) yes
C64 . C65 . H651 . 119.0 no
C66 . C65 . H651 . 120.4 no
C65 . C66 . C61 . 119.9(4) yes
C65 . C66 . H661 . 120.2 no
C61 . C66 . H661 . 119.9 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
C3 . H32 . O1 . 133.00 0.978 2.388 3.142(6) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/09/13 at 09:55:49
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  53,X'S) H   (  51,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/09/13 at 09:55:49
#
#LIST     16                                                                    
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            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 1) TO H(12) 
CONT C ( 1) TO H(11) 
REST 0.045, 0.002 = H(12,U[ISO]) 
REST 0.045, 0.002 = H(11,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(12) TO C ( 1) TO P(1) 
CONT H(12) TO C ( 1) TO C(4) 
CONT H(11) TO C ( 1) TO P(1) 
CONT H(11) TO C ( 1) TO C(4) 
ANGLE 109.54, 2.0 = 
CONT H(12) TO C ( 1) TO H(11) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 2) TO H(22) 
CONT C ( 2) TO H(21) 
REST 0.043, 0.002 = H(22,U[ISO]) 
REST 0.043, 0.002 = H(21,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(22) TO C ( 2) TO P(2) 
CONT H(22) TO C ( 2) TO C(4) 
CONT H(21) TO C ( 2) TO P(2) 
CONT H(21) TO C ( 2) TO C(4) 
ANGLE 109.54, 2.0 = 
CONT H(22) TO C ( 2) TO H(21) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 3) TO H(31) 
CONT C ( 3) TO H(32) 
REST 0.046, 0.002 = H(31,U[ISO]) 
REST 0.046, 0.002 = H(32,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(31) TO C ( 3) TO P(3) 
CONT H(31) TO C ( 3) TO C(4) 
CONT H(32) TO C ( 3) TO P(3) 
CONT H(32) TO C ( 3) TO C(4) 
ANGLE 109.54, 2.0 = 
CONT H(31) TO C ( 3) TO H(32) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 5) TO H(52) 
CONT C ( 5) TO H(53) 
CONT C ( 5) TO H(51) 
REST 0.064, 0.002 = H(52,U[ISO]) 
REST 0.064, 0.002 = H(53,U[ISO]) 
REST 0.064, 0.002 = H(51,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(4) TO C ( 5) TO H(52) 
CONT C(4) TO C ( 5) TO H(53) 
CONT C(4) TO C ( 5) TO H(51) 
ANGLE 0.0, 2.0 = MEAN H(52) TO C ( 5) TO H(53) 
CONT H(52) TO C ( 5) TO H(51) 
CONT H(53) TO C ( 5) TO H(51) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 12) TO H(121) 
REST 0.058, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 13) TO H(131) 
REST 0.068, 0.002 = H(131,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(131) TO C ( 13) TO C(12) 
CONT H(131) TO C ( 13) TO C(14) 
PLANAR C ( 13) C(12) C(14) H(131) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 14) TO H(141) 
REST 0.073, 0.002 = H(141,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(141) TO C ( 14) TO C(13) 
CONT H(141) TO C ( 14) TO C(15) 
PLANAR C ( 14) C(13) C(15) H(141) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 15) TO H(151) 
REST 0.073, 0.002 = H(151,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(151) TO C ( 15) TO C(14) 
CONT H(151) TO C ( 15) TO C(16) 
PLANAR C ( 15) C(14) C(16) H(151) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 16) TO H(161) 
REST 0.058, 0.002 = H(161,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(161) TO C ( 16) TO C(15) 
CONT H(161) TO C ( 16) TO C(11) 
PLANAR C ( 16) C(15) C(11) H(161) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 22) TO H(221) 
REST 0.069, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 23) TO H(231) 
REST 0.091, 0.002 = H(231,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(231) TO C ( 23) TO C(22) 
CONT H(231) TO C ( 23) TO C(24) 
PLANAR C ( 23) C(22) C(24) H(231) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 24) TO H(241) 
REST 0.091, 0.002 = H(241,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(241) TO C ( 24) TO C(23) 
CONT H(241) TO C ( 24) TO C(25) 
PLANAR C ( 24) C(23) C(25) H(241) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 25) TO H(251) 
REST 0.090, 0.002 = H(251,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(251) TO C ( 25) TO C(24) 
CONT H(251) TO C ( 25) TO C(26) 
PLANAR C ( 25) C(24) C(26) H(251) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 26) TO H(261) 
REST 0.074, 0.002 = H(261,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(261) TO C ( 26) TO C(21) 
CONT H(261) TO C ( 26) TO C(25) 
PLANAR C ( 26) C(21) C(25) H(261) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 32) TO H(321) 
REST 0.060, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 33) TO H(331) 
REST 0.073, 0.002 = H(331,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(331) TO C ( 33) TO C(32) 
CONT H(331) TO C ( 33) TO C(34) 
PLANAR C ( 33) C(32) C(34) H(331) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 34) TO H(341) 
REST 0.075, 0.002 = H(341,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(341) TO C ( 34) TO C(33) 
CONT H(341) TO C ( 34) TO C(35) 
PLANAR C ( 34) C(33) C(35) H(341) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 35) TO H(351) 
REST 0.070, 0.002 = H(351,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(351) TO C ( 35) TO C(34) 
CONT H(351) TO C ( 35) TO C(36) 
PLANAR C ( 35) C(34) C(36) H(351) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 36) TO H(361) 
REST 0.060, 0.002 = H(361,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(361) TO C ( 36) TO C(35) 
CONT H(361) TO C ( 36) TO C(31) 
PLANAR C ( 36) C(35) C(31) H(361) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 42) TO H(421) 
REST 0.070, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 43) TO H(431) 
REST 0.089, 0.002 = H(431,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(431) TO C ( 43) TO C(42) 
CONT H(431) TO C ( 43) TO C(44) 
PLANAR C ( 43) C(42) C(44) H(431) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 44) TO H(441) 
REST 0.084, 0.002 = H(441,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(441) TO C ( 44) TO C(43) 
CONT H(441) TO C ( 44) TO C(45) 
PLANAR C ( 44) C(43) C(45) H(441) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 45) TO H(451) 
REST 0.077, 0.002 = H(451,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(451) TO C ( 45) TO C(44) 
CONT H(451) TO C ( 45) TO C(46) 
PLANAR C ( 45) C(44) C(46) H(451) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 46) TO H(461) 
REST 0.059, 0.002 = H(461,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(461) TO C ( 46) TO C(45) 
CONT H(461) TO C ( 46) TO C(41) 
PLANAR C ( 46) C(45) C(41) H(461) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 52) TO H(521) 
REST 0.076, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 53) TO H(531) 
REST 0.087, 0.002 = H(531,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(531) TO C ( 53) TO C(52) 
CONT H(531) TO C ( 53) TO C(54) 
PLANAR C ( 53) C(52) C(54) H(531) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 54) TO H(541) 
REST 0.079, 0.002 = H(541,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(541) TO C ( 54) TO C(53) 
CONT H(541) TO C ( 54) TO C(55) 
PLANAR C ( 54) C(53) C(55) H(541) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 55) TO H(551) 
REST 0.073, 0.002 = H(551,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(551) TO C ( 55) TO C(54) 
CONT H(551) TO C ( 55) TO C(56) 
PLANAR C ( 55) C(54) C(56) H(551) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 56) TO H(561) 
REST 0.064, 0.002 = H(561,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(561) TO C ( 56) TO C(51) 
CONT H(561) TO C ( 56) TO C(55) 
PLANAR C ( 56) C(51) C(55) H(561) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 62) TO H(621) 
REST 0.067, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 63) TO H(631) 
REST 0.080, 0.002 = H(631,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(631) TO C ( 63) TO C(62) 
CONT H(631) TO C ( 63) TO C(64) 
PLANAR C ( 63) C(62) C(64) H(631) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 64) TO H(641) 
REST 0.074, 0.002 = H(641,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(641) TO C ( 64) TO C(63) 
CONT H(641) TO C ( 64) TO C(65) 
PLANAR C ( 64) C(63) C(65) H(641) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 65) TO H(651) 
REST 0.074, 0.002 = H(651,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(651) TO C ( 65) TO C(64) 
CONT H(651) TO C ( 65) TO C(66) 
PLANAR C ( 65) C(64) C(66) H(651) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 66) TO H(661) 
REST 0.060, 0.002 = H(661,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(661) TO C ( 66) TO C(65) 
CONT H(661) TO C ( 66) TO C(61) 
PLANAR C ( 66) C(65) C(61) H(661) 
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
-8 4 4 x .
-5 12 2 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 943306'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 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                   27.9522(14)
_cell_length_b                   13.3162(8)
_cell_length_c                   10.5732(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.950(3)
_cell_angle_gamma                90
_cell_volume                     3933.2(4)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
As 0.0499 2.0058 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972
2.5310 '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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            4

# Given Formula = C42 H44 As2 B1 Br1 P2 
# Dc =      1.44 Fooo =   1728.00 Mu =     28.25 M =    425.66
# Found Formula = C42 H44 As2 B1 Br1 P2 
# Dc =      1.44 FOOO =   1728.00 Mu =     28.25 M =    425.66

_chemical_formula_sum            'C42 H44 As2 B1 Br1 P2'
_chemical_formula_moiety         'C42 H44 As2 B1 P2, Br1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         851.32


_cell_measurement_reflns_used    52052
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_max          0.210

_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    2.825

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.050
0 -1 0 0.160
-2 0 1 0.040
-4 0 -1 0.030
4 0 1 0.030
5 -1 -3 0.073


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_T_max  0.846
_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 (Farrugia, 1997)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            26436
_reflns_number_total             3481
_diffrn_reflns_av_R_equivalents  0.082
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3481 
# Theoretical number of reflections is about 6960 


_diffrn_reflns_theta_min         2.548
_diffrn_reflns_theta_max         25.041
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        25.041
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -33
_reflns_limit_h_max              33
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   4.89
_oxford_diffrn_Wilson_scale      28.37

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

_refine_diff_density_min         -0.68
_refine_diff_density_max         1.27


# 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         3481
_refine_ls_number_restraints     0
_refine_ls_number_parameters     232
_oxford_refine_ls_R_factor_ref   0.0749
_refine_ls_wR_factor_ref         0.1283
_refine_ls_goodness_of_fit_ref   1.0423
_refine_ls_shift/su_max          0.0018379
_refine_ls_shift/su_mean         0.0001181


# The values computed from all data 
_oxford_reflns_number_all        3481
_refine_ls_R_factor_all          0.0749
_refine_ls_wR_factor_all         0.1283

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2768
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_gt          0.1212

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² +35.67P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
As1 As 0.65596(2) 0.48017(6) 0.58117(6) 0.0669 1.0000 Uani . . . . . .
B1 B 0.4657(7) 0.336(2) 0.323(2) 0.0744 0.5000 Uani . . . . . .
Br1 Br 0.5000 0.36793(8) 0.7500 0.0763 1.0000 Uani S T . . . .
P1 P 0.53569(6) 0.32500(15) 0.35286(15) 0.0648 1.0000 Uani . . . . . .
C1 C 0.5543(7) 0.3665(14) 0.1915(15) 0.0690 0.5000 Uani . . . . . .
C2 C 0.5259(6) 0.3258(15) 0.0946(16) 0.1001 0.5000 Uani . . . . . .
C3 C 0.5669(2) 0.4139(5) 0.4534(6) 0.0702 1.0000 Uani . . . . . .
C4 C 0.6199(2) 0.4096(5) 0.4420(6) 0.0684 1.0000 Uani . . . . . .
C11 C 0.5536(2) 0.2000(5) 0.4009(6) 0.0677 1.0000 Uani . . . . . .
C12 C 0.5787(3) 0.1367(7) 0.3231(8) 0.1011 1.0000 Uani . . . . . .
C13 C 0.5893(4) 0.0404(9) 0.3610(11) 0.1349 1.0000 Uani . . . . . .
C14 C 0.5752(4) 0.0088(8) 0.4749(12) 0.1164 1.0000 Uani . . . . . .
C15 C 0.5511(3) 0.0685(8) 0.5545(10) 0.1106 1.0000 Uani . . . . . .
C16 C 0.5397(3) 0.1675(6) 0.5173(8) 0.0857 1.0000 Uani . . . . . .
C21 C 0.7189(2) 0.4369(5) 0.5310(6) 0.0610 1.0000 Uani . . . . . .
C22 C 0.7385(2) 0.4628(5) 0.4162(6) 0.0680 1.0000 Uani . . . . . .
C23 C 0.7827(3) 0.4292(6) 0.3823(8) 0.0848 1.0000 Uani . . . . . .
C24 C 0.8087(3) 0.3663(7) 0.4656(8) 0.0967 1.0000 Uani . . . . . .
C25 C 0.7912(3) 0.3416(6) 0.5789(8) 0.0951 1.0000 Uani . . . . . .
C26 C 0.7459(3) 0.3743(6) 0.6114(6) 0.0796 1.0000 Uani . . . . . .
C31 C 0.6589(2) 0.6173(5) 0.5177(6) 0.0616 1.0000 Uani . . . . . .
C32 C 0.6322(3) 0.6530(5) 0.4138(6) 0.0728 1.0000 Uani . . . . . .
C33 C 0.6378(3) 0.7544(7) 0.3781(7) 0.0926 1.0000 Uani . . . . . .
C34 C 0.6671(3) 0.8158(6) 0.4464(8) 0.0924 1.0000 Uani . . . . . .
C35 C 0.6928(3) 0.7820(7) 0.5508(8) 0.0930 1.0000 Uani . . . . . .
C36 C 0.6882(3) 0.6830(6) 0.5863(7) 0.0784 1.0000 Uani . . . . . .
H1 H 0.4517 0.4091 0.3549 0.0888 0.5000 Uiso R . . . . .
H2 H 0.4460 0.2752 0.3686 0.0888 0.5000 Uiso R . . . . .
H11 H 0.5865 0.3461 0.1804 0.0830 0.5000 Uiso R . . . . .
H12 H 0.5524 0.4376 0.1870 0.0830 0.5000 Uiso R . . . . .
H21 H 0.5280 0.3656 0.0205 0.1202 0.5000 Uiso R . . . . .
H22 H 0.5359 0.2592 0.0770 0.1202 0.5000 Uiso R . . . . .
H31 H 0.5594 0.4003 0.5388 0.0842 1.0000 Uiso R . . . . .
H32 H 0.5562 0.4795 0.4313 0.0842 1.0000 Uiso R . . . . .
H41 H 0.6278 0.4397 0.3640 0.0821 1.0000 Uiso R . . . . .
H42 H 0.6294 0.3412 0.4423 0.0821 1.0000 Uiso R . . . . .
H121 H 0.5887 0.1600 0.2432 0.1214 1.0000 Uiso R . . . . .
H131 H 0.6064 -0.0033 0.3077 0.1618 1.0000 Uiso R . . . . .
H141 H 0.5824 -0.0580 0.5004 0.1397 1.0000 Uiso R . . . . .
H151 H 0.5420 0.0440 0.6346 0.1328 1.0000 Uiso R . . . . .
H161 H 0.5227 0.2107 0.5714 0.1029 1.0000 Uiso R . . . . .
H221 H 0.7207 0.5050 0.3595 0.0817 1.0000 Uiso R . . . . .
H231 H 0.7955 0.4483 0.3037 0.1017 1.0000 Uiso R . . . . .
H241 H 0.8389 0.3408 0.4422 0.1160 1.0000 Uiso R . . . . .
H251 H 0.8098 0.3018 0.6366 0.1141 1.0000 Uiso R . . . . .
H261 H 0.7332 0.3537 0.6895 0.0955 1.0000 Uiso R . . . . .
H321 H 0.6108 0.6102 0.3678 0.0873 1.0000 Uiso R . . . . .
H331 H 0.6209 0.7795 0.3054 0.1112 1.0000 Uiso R . . . . .
H341 H 0.6700 0.8840 0.4217 0.1109 1.0000 Uiso R . . . . .
H351 H 0.7134 0.8260 0.5977 0.1117 1.0000 Uiso R . . . . .
H361 H 0.7054 0.6593 0.6593 0.0941 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       111(11)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.2305(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
As1 . C4 . 1.991(6) yes
As1 . C21 . 1.942(6) yes
As1 . C31 . 1.948(7) yes
B1 . P1 5_655 1.87(2) yes
B1 . P1 . 1.978(19) yes
B1 . H1 . 1.100 no
B1 . H2 . 1.100 no
P1 . C2 5_655 1.826(15) yes
P1 . C1 . 1.884(15) yes
P1 . C3 . 1.797(6) yes
P1 . C11 . 1.806(7) yes
C1 . C2 . 1.39(2) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C2 . H21 . 0.950 no
C2 . H22 . 0.950 no
C3 . C4 . 1.492(9) yes
C3 . H31 . 0.950 no
C3 . H32 . 0.950 no
C4 . H41 . 0.950 no
C4 . H42 . 0.950 no
C11 . C12 . 1.386(9) yes
C11 . C16 . 1.373(10) yes
C12 . C13 . 1.372(13) yes
C12 . H121 . 0.950 no
C13 . C14 . 1.348(14) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.353(13) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.408(11) yes
C15 . H151 . 0.950 no
C16 . H161 . 0.950 no
C21 . C22 . 1.391(8) yes
C21 . C26 . 1.394(9) yes
C22 . C23 . 1.375(9) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.400(11) yes
C23 . H231 . 0.950 no
C24 . C25 . 1.350(11) yes
C24 . H241 . 0.950 no
C25 . C26 . 1.394(10) yes
C25 . H251 . 0.950 no
C26 . H261 . 0.950 no
C31 . C32 . 1.390(9) yes
C31 . C36 . 1.386(9) yes
C32 . C33 . 1.412(10) yes
C32 . H321 . 0.950 no
C33 . C34 . 1.348(11) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.372(11) yes
C34 . H341 . 0.950 no
C35 . C36 . 1.377(10) yes
C35 . H351 . 0.950 no
C36 . H361 . 0.950 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
C4 . As1 . C21 . 95.7(3) yes
C4 . As1 . C31 . 102.3(3) yes
C21 . As1 . C31 . 97.8(3) yes
P1 5_655 B1 . P1 . 97.9(10) yes
P1 5_655 B1 . H1 . 112.2 no
P1 5_655 B1 . H2 . 112.4 no
P1 . B1 . H1 . 112.2 no
P1 . B1 . H2 . 112.3 no
H1 . B1 . H2 . 109.5 no
C2 5_655 P1 . B1 5_655 108.4(7) yes
B1 . P1 . C1 . 97.9(8) yes
B1 . P1 . C3 . 120.0(8) yes
C2 5_655 P1 . C3 . 105.0(7) yes
B1 5_655 P1 . C3 . 122.0(7) yes
C1 . P1 . C3 . 101.5(6) yes
B1 . P1 . C11 . 112.2(8) yes
C2 5_655 P1 . C11 . 100.0(6) yes
B1 5_655 P1 . C11 . 110.6(9) yes
C1 . P1 . C11 . 116.3(6) yes
C3 . P1 . C11 . 108.5(3) yes
P1 . C1 . C2 . 112.6(13) yes
P1 . C1 . H11 . 108.6 no
C2 . C1 . H11 . 108.6 no
P1 . C1 . H12 . 108.7 no
C2 . C1 . H12 . 108.8 no
H11 . C1 . H12 . 109.5 no
P1 5_655 C2 . C1 . 107.5(13) yes
P1 5_655 C2 . H21 . 109.9 no
C1 . C2 . H21 . 109.9 no
P1 5_655 C2 . H22 . 110.0 no
C1 . C2 . H22 . 110.1 no
H21 . C2 . H22 . 109.5 no
P1 . C3 . C4 . 113.0(5) yes
P1 . C3 . H31 . 108.6 no
C4 . C3 . H31 . 108.6 no
P1 . C3 . H32 . 108.6 no
C4 . C3 . H32 . 108.6 no
H31 . C3 . H32 . 109.5 no
C3 . C4 . As1 . 113.7(4) yes
C3 . C4 . H41 . 108.4 no
As1 . C4 . H41 . 108.4 no
C3 . C4 . H42 . 108.4 no
As1 . C4 . H42 . 108.4 no
H41 . C4 . H42 . 109.5 no
P1 . C11 . C12 . 122.3(6) yes
P1 . C11 . C16 . 117.3(5) yes
C12 . C11 . C16 . 120.3(8) yes
C11 . C12 . C13 . 120.3(9) yes
C11 . C12 . H121 . 119.9 no
C13 . C12 . H121 . 119.9 no
C12 . C13 . C14 . 119.0(10) yes
C12 . C13 . H131 . 120.5 no
C14 . C13 . H131 . 120.5 no
C13 . C14 . C15 . 122.7(10) yes
C13 . C14 . H141 . 118.7 no
C15 . C14 . H141 . 118.7 no
C14 . C15 . C16 . 119.2(10) yes
C14 . C15 . H151 . 120.4 no
C16 . C15 . H151 . 120.4 no
C15 . C16 . C11 . 118.5(8) yes
C15 . C16 . H161 . 120.7 no
C11 . C16 . H161 . 120.7 no
As1 . C21 . C22 . 123.5(5) yes
As1 . C21 . C26 . 119.2(5) yes
C22 . C21 . C26 . 117.4(6) yes
C21 . C22 . C23 . 122.1(7) yes
C21 . C22 . H221 . 119.0 no
C23 . C22 . H221 . 119.0 no
C22 . C23 . C24 . 118.8(7) yes
C22 . C23 . H231 . 120.6 no
C24 . C23 . H231 . 120.6 no
C23 . C24 . C25 . 120.6(8) yes
C23 . C24 . H241 . 119.7 no
C25 . C24 . H241 . 119.7 no
C24 . C25 . C26 . 120.1(8) yes
C24 . C25 . H251 . 120.0 no
C26 . C25 . H251 . 120.0 no
C25 . C26 . C21 . 121.0(7) yes
C25 . C26 . H261 . 119.5 no
C21 . C26 . H261 . 119.5 no
As1 . C31 . C32 . 124.4(5) yes
As1 . C31 . C36 . 116.3(5) yes
C32 . C31 . C36 . 119.2(7) yes
C31 . C32 . C33 . 118.5(7) yes
C31 . C32 . H321 . 120.7 no
C33 . C32 . H321 . 120.7 no
C32 . C33 . C34 . 120.5(8) yes
C32 . C33 . H331 . 119.8 no
C34 . C33 . H331 . 119.8 no
C33 . C34 . C35 . 121.6(8) yes
C33 . C34 . H341 . 119.2 no
C35 . C34 . H341 . 119.2 no
C34 . C35 . C36 . 118.8(8) yes
C34 . C35 . H351 . 120.6 no
C36 . C35 . H351 . 120.6 no
C31 . C36 . C35 . 121.4(7) yes
C31 . C36 . H361 . 119.3 no
C35 . C36 . H361 . 119.3 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 05/12/11 at 14:14:11
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE B   (   1,X'S) H   (  1,X'S) H   (  2,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 05/12/11 at 14:14:11
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;





####################################################################### 
# 
# 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 1058398'
_audit_update_record             
;
2015-04-08 deposited with the CCDC.
2017-05-12 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                   9.5770(2)
_cell_length_b                   7.34050(10)
_cell_length_c                   27.7205(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.4547(10)
_cell_angle_gamma                90
_cell_volume                     1927.57(6)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            4

# Given Formula = C20 H22 B1 Br1 N1 P1 
# Dc =      1.37 Fooo =    816.00 Mu =     22.16 M =    398.09
# Found Formula = C20 H22 B1 Br1 N1 P1 
# Dc =      1.37 FOOO =    816.00 Mu =     22.16 M =    398.09

_chemical_formula_sum            'C20 H22 B1 Br1 N1 P1'
_chemical_formula_moiety         'C20 H22 B1 N1 P1, Br1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         398.09


_cell_measurement_reflns_used    61482
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.040
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_max          0.240

_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    2.216

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.090
0 0 1 0.010
0 0 -1 0.030
-6 -4 1 0.051
7 -5 0 0.160
10 5 -1 0.122


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_T_max  0.916
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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            31237
_reflns_number_total             4427
_diffrn_reflns_av_R_equivalents  0.035
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4427 
# Theoretical number of reflections is about 8832 


_diffrn_reflns_theta_min         2.860
_diffrn_reflns_theta_max         27.473
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.473
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              9
_reflns_limit_l_min              0
_reflns_limit_l_max              35

_oxford_diffrn_Wilson_B_factor   3.02
_oxford_diffrn_Wilson_scale      6.57

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

_refine_diff_density_min         -0.72
_refine_diff_density_max         0.73


# 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         4425
_refine_ls_number_restraints     0
_refine_ls_number_parameters     305
_oxford_refine_ls_R_factor_ref   0.0452
_refine_ls_wR_factor_ref         0.0817
_refine_ls_goodness_of_fit_ref   0.9906
_refine_ls_shift/su_max          0.0008562
_refine_ls_shift/su_mean         0.0000656


# The values computed from all data 
_oxford_reflns_number_all        4425
_refine_ls_R_factor_all          0.0452
_refine_ls_wR_factor_all         0.0817

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3637
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_gt          0.0757

# 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    mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 1.54P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.5114(2) 0.9010(4) 0.62543(9) 0.0316 1.0000 Uani . . . . . .
Br1 Br 0.77871(3) 0.44246(3) 0.655128(9) 0.0489 1.0000 Uani . . . . . .
N1 N 0.53836(16) 0.9047(2) 0.68455(6) 0.0261 1.0000 Uani . . . . . .
P1 P 0.33608(5) 0.76316(7) 0.613018(18) 0.0263 1.0000 Uani . . . . . .
C1 C 0.36305(19) 0.6584(3) 0.67233(7) 0.0245 1.0000 Uani . . . . . .
C2 C 0.46962(19) 0.7444(3) 0.70398(7) 0.0243 1.0000 Uani . . . . . .
C3 C 0.5038(2) 0.6869(3) 0.75171(7) 0.0302 1.0000 Uani . . . . . .
C4 C 0.4317(2) 0.5398(3) 0.76753(8) 0.0327 1.0000 Uani . . . . . .
C5 C 0.3266(2) 0.4522(3) 0.73647(8) 0.0320 1.0000 Uani . . . . . .
C6 C 0.2910(2) 0.5105(3) 0.68879(8) 0.0302 1.0000 Uani . . . . . .
C11 C 0.1697(2) 0.8813(3) 0.60479(7) 0.0295 1.0000 Uani . . . . . .
C12 C 0.0450(2) 0.7904(3) 0.61076(8) 0.0333 1.0000 Uani . . . . . .
C13 C -0.0820(2) 0.8829(4) 0.60357(8) 0.0409 1.0000 Uani . . . . . .
C14 C -0.0864(3) 1.0641(4) 0.59086(10) 0.0509 1.0000 Uani . . . . . .
C15 C 0.0355(3) 1.1545(4) 0.58499(12) 0.0596 1.0000 Uani . . . . . .
C16 C 0.1642(3) 1.0643(3) 0.59182(10) 0.0460 1.0000 Uani . . . . . .
C21 C 0.3288(2) 0.5902(3) 0.56653(7) 0.0290 1.0000 Uani . . . . . .
C22 C 0.2261(3) 0.5953(4) 0.52520(8) 0.0427 1.0000 Uani . . . . . .
C23 C 0.2289(3) 0.4657(4) 0.48896(9) 0.0531 1.0000 Uani . . . . . .
C24 C 0.3313(3) 0.3326(4) 0.49370(9) 0.0462 1.0000 Uani . . . . . .
C25 C 0.4331(3) 0.3280(3) 0.53431(8) 0.0395 1.0000 Uani . . . . . .
C26 C 0.4328(2) 0.4566(3) 0.57100(8) 0.0338 1.0000 Uani . . . . . .
C31 C 0.4781(3) 1.0752(3) 0.70352(10) 0.0374 1.0000 Uani . . . . . .
C41 C 0.6957(2) 0.9069(3) 0.70159(8) 0.0322 1.0000 Uani . . . . . .
H1 H 0.528(3) 1.049(3) 0.6029(9) 0.045(7) 1.0000 Uiso . . . . . .
H2 H 0.586(2) 0.806(3) 0.6128(8) 0.037(6) 1.0000 Uiso . . . . . .
H31 H 0.571(3) 0.747(3) 0.7731(9) 0.038(6) 1.0000 Uiso . . . . . .
H41 H 0.460(2) 0.497(3) 0.8004(9) 0.038(6) 1.0000 Uiso . . . . . .
H51 H 0.282(2) 0.357(3) 0.7479(8) 0.035(6) 1.0000 Uiso . . . . . .
H61 H 0.219(3) 0.452(3) 0.6683(9) 0.041(7) 1.0000 Uiso . . . . . .
H121 H 0.048(3) 0.663(4) 0.6209(9) 0.043(7) 1.0000 Uiso . . . . . .
H131 H -0.165(3) 0.823(3) 0.6092(9) 0.041(7) 1.0000 Uiso . . . . . .
H141 H -0.171(3) 1.126(4) 0.5876(10) 0.060(8) 1.0000 Uiso . . . . . .
H151 H 0.035(3) 1.275(4) 0.5766(11) 0.063(9) 1.0000 Uiso . . . . . .
H161 H 0.246(3) 1.123(4) 0.5873(10) 0.056(8) 1.0000 Uiso . . . . . .
H221 H 0.155(3) 0.692(4) 0.5212(10) 0.052(7) 1.0000 Uiso . . . . . .
H231 H 0.166(3) 0.470(5) 0.4619(13) 0.074(10) 1.0000 Uiso . . . . . .
H241 H 0.335(3) 0.242(4) 0.4687(11) 0.068(9) 1.0000 Uiso . . . . . .
H251 H 0.506(3) 0.237(4) 0.5376(9) 0.042(7) 1.0000 Uiso . . . . . .
H261 H 0.507(3) 0.458(3) 0.5990(10) 0.043(7) 1.0000 Uiso . . . . . .
H311 H 0.492(3) 1.073(3) 0.7376(10) 0.038(7) 1.0000 Uiso . . . . . .
H312 H 0.525(2) 1.174(4) 0.6905(9) 0.038(6) 1.0000 Uiso . . . . . .
H313 H 0.376(3) 1.077(3) 0.6907(9) 0.043(7) 1.0000 Uiso . . . . . .
H411 H 0.733(2) 0.797(3) 0.6929(8) 0.032(6) 1.0000 Uiso . . . . . .
H412 H 0.715(2) 0.925(3) 0.7369(9) 0.033(6) 1.0000 Uiso . . . . . .
H413 H 0.732(2) 1.011(4) 0.6844(9) 0.036(6) 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.4422(5)
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 . N1 . 1.621(3) yes
B1 . P1 . 1.947(2) yes
B1 . H1 . 1.27(2) no
B1 . H2 . 1.09(2) no
N1 . C2 . 1.488(2) yes
N1 . C31 . 1.505(3) yes
N1 . C41 . 1.511(3) yes
P1 . C1 . 1.7989(19) yes
P1 . C11 . 1.799(2) yes
P1 . C21 . 1.803(2) yes
C1 . C2 . 1.395(3) yes
C1 . C6 . 1.398(3) yes
C2 . C3 . 1.381(3) yes
C3 . C4 . 1.387(3) yes
C3 . H31 . 0.92(2) no
C4 . C5 . 1.383(3) yes
C4 . H41 . 0.96(2) no
C5 . C6 . 1.383(3) yes
C5 . H51 . 0.90(3) no
C6 . H61 . 0.93(3) no
C11 . C12 . 1.399(3) yes
C11 . C16 . 1.389(3) yes
C12 . C13 . 1.382(3) yes
C12 . H121 . 0.98(3) no
C13 . C14 . 1.376(4) yes
C13 . H131 . 0.94(3) no
C14 . C15 . 1.373(4) yes
C14 . H141 . 0.93(3) no
C15 . C16 . 1.388(4) yes
C15 . H151 . 0.92(3) no
C16 . H161 . 0.92(3) no
C21 . C22 . 1.397(3) yes
C21 . C26 . 1.390(3) yes
C22 . C23 . 1.387(4) yes
C22 . H221 . 0.98(3) no
C23 . C24 . 1.377(4) yes
C23 . H231 . 0.89(3) no
C24 . C25 . 1.377(3) yes
C24 . H241 . 0.96(3) no
C25 . C26 . 1.388(3) yes
C25 . H251 . 0.96(3) no
C26 . H261 . 0.97(3) no
C31 . H311 . 0.93(3) no
C31 . H312 . 0.95(3) no
C31 . H313 . 0.99(3) no
C41 . H411 . 0.92(2) no
C41 . H412 . 0.98(2) no
C41 . H413 . 0.99(3) 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
N1 . B1 . P1 . 101.08(13) yes
N1 . B1 . H1 . 118.0(12) no
P1 . B1 . H1 . 121.3(11) no
N1 . B1 . H2 . 108.6(12) no
P1 . B1 . H2 . 101.6(12) no
H1 . B1 . H2 . 104.7(17) no
B1 . N1 . C2 . 109.85(15) yes
B1 . N1 . C31 . 110.80(17) yes
C2 . N1 . C31 . 108.58(15) yes
B1 . N1 . C41 . 108.61(15) yes
C2 . N1 . C41 . 111.68(15) yes
C31 . N1 . C41 . 107.31(17) yes
B1 . P1 . C1 . 93.23(9) yes
B1 . P1 . C11 . 119.79(11) yes
C1 . P1 . C11 . 109.11(9) yes
B1 . P1 . C21 . 115.70(10) yes
C1 . P1 . C21 . 109.72(9) yes
C11 . P1 . C21 . 107.96(9) yes
P1 . C1 . C2 . 112.03(14) yes
P1 . C1 . C6 . 128.22(15) yes
C2 . C1 . C6 . 119.75(18) yes
N1 . C2 . C1 . 116.86(16) yes
N1 . C2 . C3 . 122.21(17) yes
C1 . C2 . C3 . 120.87(18) yes
C2 . C3 . C4 . 118.77(19) yes
C2 . C3 . H31 . 120.9(15) no
C4 . C3 . H31 . 120.3(15) no
C3 . C4 . C5 . 121.0(2) yes
C3 . C4 . H41 . 118.0(15) no
C5 . C4 . H41 . 120.9(15) no
C4 . C5 . C6 . 120.3(2) yes
C4 . C5 . H51 . 118.7(15) no
C6 . C5 . H51 . 121.0(15) no
C1 . C6 . C5 . 119.22(19) yes
C1 . C6 . H61 . 120.9(15) no
C5 . C6 . H61 . 119.9(15) no
P1 . C11 . C12 . 120.72(17) yes
P1 . C11 . C16 . 119.85(17) yes
C12 . C11 . C16 . 119.4(2) yes
C11 . C12 . C13 . 119.8(2) yes
C11 . C12 . H121 . 120.1(14) no
C13 . C12 . H121 . 120.1(14) no
C12 . C13 . C14 . 120.3(2) yes
C12 . C13 . H131 . 119.6(16) no
C14 . C13 . H131 . 120.0(16) no
C13 . C14 . C15 . 120.3(2) yes
C13 . C14 . H141 . 119.7(19) no
C15 . C14 . H141 . 120.0(19) no
C14 . C15 . C16 . 120.4(3) yes
C14 . C15 . H151 . 121.4(19) no
C16 . C15 . H151 . 118.1(19) no
C11 . C16 . C15 . 119.7(2) yes
C11 . C16 . H161 . 118.9(18) no
C15 . C16 . H161 . 121.3(18) no
P1 . C21 . C22 . 121.05(17) yes
P1 . C21 . C26 . 118.76(15) yes
C22 . C21 . C26 . 120.1(2) yes
C21 . C22 . C23 . 119.3(2) yes
C21 . C22 . H221 . 120.4(16) no
C23 . C22 . H221 . 120.2(16) no
C22 . C23 . C24 . 120.5(2) yes
C22 . C23 . H231 . 120(2) no
C24 . C23 . H231 . 119(2) no
C23 . C24 . C25 . 120.3(2) yes
C23 . C24 . H241 . 121.2(18) no
C25 . C24 . H241 . 118.5(18) no
C24 . C25 . C26 . 120.3(2) yes
C24 . C25 . H251 . 120.8(15) no
C26 . C25 . H251 . 118.9(15) no
C21 . C26 . C25 . 119.6(2) yes
C21 . C26 . H261 . 119.3(15) no
C25 . C26 . H261 . 121.1(15) no
N1 . C31 . H311 . 109.7(15) no
N1 . C31 . H312 . 106.0(14) no
H311 . C31 . H312 . 113(2) no
N1 . C31 . H313 . 107.0(14) no
H311 . C31 . H313 . 110(2) no
H312 . C31 . H313 . 111(2) no
N1 . C41 . H411 . 108.2(14) no
N1 . C41 . H412 . 110.1(13) no
H411 . C41 . H412 . 110.9(19) no
N1 . C41 . H413 . 105.3(14) no
H411 . C41 . H413 . 111.7(19) no
H412 . C41 . H413 . 110.5(19) no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 30/06/13 at 13:33:45
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT B    (    1 ,X'S,U'S)  UNTIL C    (   41 ) 
CONT H    (    1 ,X'S,U[ISO])  UNTIL H    (  413 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 30/06/13 at 13:33:45
#
#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
-5 3 9 x .
0 3 9 x .


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/pentane'
####################################################################### 
# 
# 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 943305'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;

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

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

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

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

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

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   10.2490(2)
_cell_length_b                   19.1746(7)
_cell_length_c                   15.1472(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.516(2)
_cell_angle_gamma                90
_cell_volume                     2975.69(16)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 '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'
Sb -0.5866 1.5461 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.2825
4.5909 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C24 H48 B1 F6 P2 Sb1 
# Dc =      1.44 Fooo =   1320.00 Mu =     10.84 M =    645.14
# Found Formula = C24 H46 B1 F6 P2 Sb1 
# Dc =      1.44 FOOO =   1320.00 Mu =     10.83 M =    643.13

_chemical_formula_sum            'C24 H46 B1 F6 P2 Sb1'
_chemical_formula_moiety         'C24 H46 B1 P2, F6 Sb1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         643.13


_cell_measurement_reflns_used    18651
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      29
_cell_measurement_temperature    200

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.410

_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    1.083

# 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 0.220
-1 0 0 0.190
0 1 0 0.050
0 -1 0 0.080
0 -10 -9 0.075
0 10 -11 0.060
0 7 6 0.037
0 -5 4 0.055
4 -5 4 0.153
4 -10 -9 0.135
9 7 6 0.174
2 5 -4 0.137


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.897
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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            33770
_reflns_number_total             6792
_diffrn_reflns_av_R_equivalents  0.057
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6792 
# Theoretical number of reflections is about 13675 


_diffrn_reflns_theta_min         2.598
_diffrn_reflns_theta_max         27.502
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        25.302
_diffrn_measured_fraction_theta_full 0.994


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              24
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   2.97
_oxford_diffrn_Wilson_scale      38.67

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

_refine_diff_density_min         -2.23
_refine_diff_density_max         2.67


# 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         6784
_refine_ls_number_restraints     0
_refine_ls_number_parameters     308
_oxford_refine_ls_R_factor_ref   0.0833
_refine_ls_wR_factor_ref         0.1504
_refine_ls_goodness_of_fit_ref   0.9380
_refine_ls_shift/su_max          0.0003246
_refine_ls_shift/su_mean         0.0000421


# The values computed from all data 
_oxford_reflns_number_all        6784
_refine_ls_R_factor_all          0.0833
_refine_ls_wR_factor_all         0.1504

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4882
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_gt          0.1234

# 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: 
 17.2 25.0 11.8 2.87 
;

# 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 0.7631(6) 0.4010(3) 0.1258(4) 0.0365 1.0000 Uani . . . . . .
F1 F 0.0298(6) 0.1525(3) 0.1017(4) 0.1149 1.0000 Uani . . . . . .
F2 F 0.0768(5) 0.2807(3) 0.1281(4) 0.0948 1.0000 Uani . . . . . .
F3 F 0.1685(6) 0.1869(3) 0.2401(3) 0.1152 1.0000 Uani . . . . . .
F4 F 0.3285(5) 0.2558(4) 0.1417(6) 0.1429 1.0000 Uani . . . . . .
F5 F 0.1858(7) 0.2142(4) -0.0010(3) 0.1328 1.0000 Uani . . . . . .
F6 F 0.2828(8) 0.1242(4) 0.1113(5) 0.1568 1.0000 Uani . . . . . .
P1 P 0.82661(12) 0.35354(6) 0.23095(8) 0.0300 1.0000 Uani . . . . . .
P2 P 0.83010(11) 0.36830(6) 0.01664(8) 0.0303 1.0000 Uani . . . . . .
Sb1 Sb 0.18348(4) 0.20389(2) 0.11857(3) 0.0517 1.0000 Uani . . . . . .
C11 C 0.7838(4) 0.2615(2) 0.2403(3) 0.0314 1.0000 Uani . . . . . .
C12 C 0.6363(5) 0.2491(3) 0.2472(4) 0.0388 1.0000 Uani . . . . . .
C13 C 0.6080(6) 0.1710(3) 0.2492(4) 0.0474 1.0000 Uani . . . . . .
C14 C 0.6808(6) 0.1352(3) 0.3250(4) 0.0506 1.0000 Uani . . . . . .
C15 C 0.8268(6) 0.1485(3) 0.3208(4) 0.0484 1.0000 Uani . . . . . .
C16 C 0.8579(5) 0.2267(3) 0.3182(3) 0.0394 1.0000 Uani . . . . . .
C21 C 0.7778(5) 0.4021(2) 0.3292(3) 0.0327 1.0000 Uani . . . . . .
C22 C 0.6406(5) 0.4328(3) 0.3183(4) 0.0395 1.0000 Uani . . . . . .
C23 C 0.6016(6) 0.4706(3) 0.4022(4) 0.0473 1.0000 Uani . . . . . .
C24 C 0.6996(6) 0.5266(3) 0.4273(4) 0.0463 1.0000 Uani . . . . . .
C25 C 0.8382(6) 0.4974(3) 0.4361(4) 0.0483 1.0000 Uani . . . . . .
C26 C 0.8771(5) 0.4591(3) 0.3521(3) 0.0390 1.0000 Uani . . . . . .
C31 C 0.7956(4) 0.2776(2) -0.0099(3) 0.0301 1.0000 Uani . . . . . .
C32 C 0.6491(5) 0.2615(3) -0.0178(3) 0.0381 1.0000 Uani . . . . . .
C33 C 0.6282(5) 0.1836(3) -0.0324(4) 0.0471 1.0000 Uani . . . . . .
C34 C 0.6977(5) 0.1582(3) -0.1137(4) 0.0446 1.0000 Uani . . . . . .
C35 C 0.8423(5) 0.1754(3) -0.1087(3) 0.0397 1.0000 Uani . . . . . .
C36 C 0.8654(5) 0.2533(3) -0.0924(3) 0.0382 1.0000 Uani . . . . . .
C41 C 0.7762(5) 0.4240(3) -0.0754(3) 0.0381 1.0000 Uani . . . . . .
C42 C 0.6368(6) 0.4482(3) -0.0678(4) 0.0560 1.0000 Uani . . . . . .
C43 C 0.5933(7) 0.4911(4) -0.1487(5) 0.0651 1.0000 Uani . . . . . .
C44 C 0.6843(8) 0.5528(4) -0.1603(6) 0.0834 1.0000 Uani . . . . . .
C45 C 0.8237(8) 0.5297(5) -0.1681(7) 0.0976 1.0000 Uani . . . . . .
C46 C 0.8671(7) 0.4860(4) -0.0869(5) 0.0682 1.0000 Uani . . . . . .
H1 H 0.7881 0.4555 0.1323 0.0439 1.0000 Uiso R . . . . .
H2 H 0.6582 0.3954 0.1223 0.0439 1.0000 Uiso R . . . . .
H111 H 0.8108 0.2391 0.1879 0.0377 1.0000 Uiso R . . . . .
H121 H 0.6065 0.2699 0.2999 0.0466 1.0000 Uiso R . . . . .
H122 H 0.5922 0.2695 0.1977 0.0466 1.0000 Uiso R . . . . .
H131 H 0.6341 0.1509 0.1951 0.0569 1.0000 Uiso R . . . . .
H132 H 0.5169 0.1642 0.2556 0.0569 1.0000 Uiso R . . . . .
H141 H 0.6499 0.1527 0.3793 0.0607 1.0000 Uiso R . . . . .
H142 H 0.6652 0.0864 0.3218 0.0607 1.0000 Uiso R . . . . .
H151 H 0.8688 0.1286 0.3714 0.0581 1.0000 Uiso R . . . . .
H152 H 0.8588 0.1272 0.2691 0.0581 1.0000 Uiso R . . . . .
H161 H 0.9491 0.2329 0.3114 0.0473 1.0000 Uiso R . . . . .
H162 H 0.8324 0.2477 0.3718 0.0473 1.0000 Uiso R . . . . .
H211 H 0.7771 0.3703 0.3773 0.0392 1.0000 Uiso R . . . . .
H221 H 0.6392 0.4650 0.2705 0.0474 1.0000 Uiso R . . . . .
H222 H 0.5803 0.3963 0.3061 0.0474 1.0000 Uiso R . . . . .
H231 H 0.5971 0.4378 0.4490 0.0568 1.0000 Uiso R . . . . .
H232 H 0.5184 0.4915 0.3926 0.0568 1.0000 Uiso R . . . . .
H241 H 0.6763 0.5463 0.4822 0.0556 1.0000 Uiso R . . . . .
H242 H 0.6975 0.5617 0.3831 0.0556 1.0000 Uiso R . . . . .
H251 H 0.8974 0.5348 0.4468 0.0580 1.0000 Uiso R . . . . .
H252 H 0.8426 0.4657 0.4843 0.0580 1.0000 Uiso R . . . . .
H261 H 0.9607 0.4386 0.3612 0.0468 1.0000 Uiso R . . . . .
H262 H 0.8800 0.4915 0.3047 0.0468 1.0000 Uiso R . . . . .
H311 H 0.8296 0.2505 0.0380 0.0361 1.0000 Uiso R . . . . .
H321 H 0.6119 0.2866 -0.0664 0.0457 1.0000 Uiso R . . . . .
H322 H 0.6081 0.2754 0.0349 0.0457 1.0000 Uiso R . . . . .
H331 H 0.6612 0.1589 0.0179 0.0566 1.0000 Uiso R . . . . .
H332 H 0.5374 0.1747 -0.0398 0.0566 1.0000 Uiso R . . . . .
H341 H 0.6596 0.1800 -0.1645 0.0536 1.0000 Uiso R . . . . .
H342 H 0.6875 0.1091 -0.1183 0.0536 1.0000 Uiso R . . . . .
H351 H 0.8805 0.1626 -0.1628 0.0476 1.0000 Uiso R . . . . .
H352 H 0.8822 0.1497 -0.0617 0.0476 1.0000 Uiso R . . . . .
H361 H 0.9564 0.2615 -0.0847 0.0458 1.0000 Uiso R . . . . .
H362 H 0.8330 0.2790 -0.1420 0.0458 1.0000 Uiso R . . . . .
H411 H 0.7802 0.3967 -0.1276 0.0457 1.0000 Uiso R . . . . .
H421 H 0.6300 0.4762 -0.0164 0.0672 1.0000 Uiso R . . . . .
H422 H 0.5816 0.4087 -0.0632 0.0672 1.0000 Uiso R . . . . .
H431 H 0.5071 0.5076 -0.1408 0.0781 1.0000 Uiso R . . . . .
H432 H 0.5951 0.4624 -0.1998 0.0781 1.0000 Uiso R . . . . .
H441 H 0.6586 0.5773 -0.2124 0.1001 1.0000 Uiso R . . . . .
H442 H 0.6780 0.5828 -0.1107 0.1001 1.0000 Uiso R . . . . .
H451 H 0.8782 0.5696 -0.1720 0.1171 1.0000 Uiso R . . . . .
H452 H 0.8315 0.5022 -0.2199 0.1171 1.0000 Uiso R . . . . .
H461 H 0.9534 0.4696 -0.0948 0.0818 1.0000 Uiso R . . . . .
H462 H 0.8653 0.5145 -0.0356 0.0818 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       57(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.19792(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
B1 . P1 . 1.932(5) yes
B1 . P2 . 1.912(6) yes
B1 . H1 . 1.080 no
B1 . H2 . 1.080 no
F1 . Sb1 . 1.870(5) yes
F2 . Sb1 . 1.842(4) yes
F3 . Sb1 . 1.880(5) yes
F4 . Sb1 . 1.815(5) yes
F5 . Sb1 . 1.823(5) yes
F6 . Sb1 . 1.842(5) yes
P1 . C11 . 1.825(5) yes
P1 . C21 . 1.835(5) yes
P2 . C31 . 1.818(5) yes
P2 . C41 . 1.829(5) yes
C11 . C12 . 1.536(6) yes
C11 . C16 . 1.539(6) yes
C11 . H111 . 0.950 no
C12 . C13 . 1.526(7) yes
C12 . H121 . 0.950 no
C12 . H122 . 0.950 no
C13 . C14 . 1.518(8) yes
C13 . H131 . 0.950 no
C13 . H132 . 0.950 no
C14 . C15 . 1.521(8) yes
C14 . H141 . 0.950 no
C14 . H142 . 0.950 no
C15 . C16 . 1.533(7) yes
C15 . H151 . 0.950 no
C15 . H152 . 0.950 no
C16 . H161 . 0.950 no
C16 . H162 . 0.950 no
C21 . C22 . 1.530(6) yes
C21 . C26 . 1.527(7) yes
C21 . H211 . 0.950 no
C22 . C23 . 1.525(7) yes
C22 . H221 . 0.950 no
C22 . H222 . 0.950 no
C23 . C24 . 1.512(8) yes
C23 . H231 . 0.950 no
C23 . H232 . 0.950 no
C24 . C25 . 1.530(8) yes
C24 . H241 . 0.950 no
C24 . H242 . 0.950 no
C25 . C26 . 1.531(7) yes
C25 . H251 . 0.950 no
C25 . H252 . 0.950 no
C26 . H261 . 0.950 no
C26 . H262 . 0.950 no
C31 . C32 . 1.534(6) yes
C31 . C36 . 1.529(6) yes
C31 . H311 . 0.950 no
C32 . C33 . 1.525(7) yes
C32 . H321 . 0.950 no
C32 . H322 . 0.950 no
C33 . C34 . 1.519(8) yes
C33 . H331 . 0.950 no
C33 . H332 . 0.950 no
C34 . C35 . 1.518(7) yes
C34 . H341 . 0.950 no
C34 . H342 . 0.950 no
C35 . C36 . 1.531(7) yes
C35 . H351 . 0.950 no
C35 . H352 . 0.950 no
C36 . H361 . 0.950 no
C36 . H362 . 0.950 no
C41 . C42 . 1.510(8) yes
C41 . C46 . 1.524(8) yes
C41 . H411 . 0.950 no
C42 . C43 . 1.531(8) yes
C42 . H421 . 0.950 no
C42 . H422 . 0.950 no
C43 . C44 . 1.519(10) yes
C43 . H431 . 0.950 no
C43 . H432 . 0.950 no
C44 . C45 . 1.503(12) yes
C44 . H441 . 0.950 no
C44 . H442 . 0.950 no
C45 . C46 . 1.543(9) yes
C45 . H451 . 0.950 no
C45 . H452 . 0.950 no
C46 . H461 . 0.950 no
C46 . H462 . 0.950 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 . B1 . P2 . 116.0(3) yes
P1 . B1 . H1 . 107.8 no
P2 . B1 . H1 . 107.8 no
P1 . B1 . H2 . 107.8 no
P2 . B1 . H2 . 107.8 no
H1 . B1 . H2 . 109.5 no
B1 . P1 . C11 . 116.3(2) yes
B1 . P1 . C21 . 109.7(2) yes
C11 . P1 . C21 . 110.9(2) yes
B1 . P2 . C31 . 115.6(2) yes
B1 . P2 . C41 . 111.1(2) yes
C31 . P2 . C41 . 109.7(2) yes
F3 . Sb1 . F1 . 87.3(3) yes
F3 . Sb1 . F2 . 89.9(3) yes
F1 . Sb1 . F2 . 86.1(3) yes
F3 . Sb1 . F6 . 88.5(3) yes
F1 . Sb1 . F6 . 91.1(3) yes
F2 . Sb1 . F6 . 176.9(4) yes
F3 . Sb1 . F5 . 174.5(3) yes
F1 . Sb1 . F5 . 87.4(3) yes
F2 . Sb1 . F5 . 90.8(3) yes
F6 . Sb1 . F5 . 90.5(3) yes
F3 . Sb1 . F4 . 89.6(3) yes
F1 . Sb1 . F4 . 176.2(3) yes
F2 . Sb1 . F4 . 91.8(3) yes
F6 . Sb1 . F4 . 90.9(4) yes
F5 . Sb1 . F4 . 95.8(4) yes
P1 . C11 . C12 . 113.2(3) yes
P1 . C11 . C16 . 111.3(3) yes
C12 . C11 . C16 . 110.3(4) yes
P1 . C11 . H111 . 107.2 no
C12 . C11 . H111 . 107.2 no
C16 . C11 . H111 . 107.2 no
C11 . C12 . C13 . 110.0(4) yes
C11 . C12 . H121 . 109.3 no
C13 . C12 . H121 . 109.3 no
C11 . C12 . H122 . 109.3 no
C13 . C12 . H122 . 109.3 no
H121 . C12 . H122 . 109.5 no
C12 . C13 . C14 . 111.6(5) yes
C12 . C13 . H131 . 108.9 no
C14 . C13 . H131 . 108.9 no
C12 . C13 . H132 . 108.9 no
C14 . C13 . H132 . 108.9 no
H131 . C13 . H132 . 109.5 no
C13 . C14 . C15 . 110.9(5) yes
C13 . C14 . H141 . 109.1 no
C15 . C14 . H141 . 109.1 no
C13 . C14 . H142 . 109.1 no
C15 . C14 . H142 . 109.1 no
H141 . C14 . H142 . 109.5 no
C14 . C15 . C16 . 111.8(4) yes
C14 . C15 . H151 . 108.9 no
C16 . C15 . H151 . 108.9 no
C14 . C15 . H152 . 108.9 no
C16 . C15 . H152 . 108.9 no
H151 . C15 . H152 . 109.5 no
C11 . C16 . C15 . 110.1(4) yes
C11 . C16 . H161 . 109.3 no
C15 . C16 . H161 . 109.3 no
C11 . C16 . H162 . 109.3 no
C15 . C16 . H162 . 109.3 no
H161 . C16 . H162 . 109.5 no
P1 . C21 . C22 . 112.2(3) yes
P1 . C21 . C26 . 110.7(3) yes
C22 . C21 . C26 . 110.7(4) yes
P1 . C21 . H211 . 107.7 no
C22 . C21 . H211 . 107.7 no
C26 . C21 . H211 . 107.7 no
C21 . C22 . C23 . 110.7(4) yes
C21 . C22 . H221 . 109.2 no
C23 . C22 . H221 . 109.2 no
C21 . C22 . H222 . 109.2 no
C23 . C22 . H222 . 109.2 no
H221 . C22 . H222 . 109.5 no
C22 . C23 . C24 . 111.1(4) yes
C22 . C23 . H231 . 109.1 no
C24 . C23 . H231 . 109.1 no
C22 . C23 . H232 . 109.1 no
C24 . C23 . H232 . 109.1 no
H231 . C23 . H232 . 109.5 no
C23 . C24 . C25 . 111.8(4) yes
C23 . C24 . H241 . 108.9 no
C25 . C24 . H241 . 108.9 no
C23 . C24 . H242 . 108.9 no
C25 . C24 . H242 . 108.9 no
H241 . C24 . H242 . 109.5 no
C24 . C25 . C26 . 111.4(4) yes
C24 . C25 . H251 . 109.0 no
C26 . C25 . H251 . 109.0 no
C24 . C25 . H252 . 109.0 no
C26 . C25 . H252 . 109.0 no
H251 . C25 . H252 . 109.5 no
C25 . C26 . C21 . 110.2(4) yes
C25 . C26 . H261 . 109.3 no
C21 . C26 . H261 . 109.3 no
C25 . C26 . H262 . 109.3 no
C21 . C26 . H262 . 109.3 no
H261 . C26 . H262 . 109.5 no
P2 . C31 . C32 . 113.1(3) yes
P2 . C31 . C36 . 112.3(3) yes
C32 . C31 . C36 . 110.7(4) yes
P2 . C31 . H311 . 106.8 no
C32 . C31 . H311 . 106.8 no
C36 . C31 . H311 . 106.8 no
C31 . C32 . C33 . 109.9(4) yes
C31 . C32 . H321 . 109.4 no
C33 . C32 . H321 . 109.4 no
C31 . C32 . H322 . 109.4 no
C33 . C32 . H322 . 109.4 no
H321 . C32 . H322 . 109.5 no
C32 . C33 . C34 . 111.3(5) yes
C32 . C33 . H331 . 109.0 no
C34 . C33 . H331 . 109.0 no
C32 . C33 . H332 . 109.0 no
C34 . C33 . H332 . 109.0 no
H331 . C33 . H332 . 109.5 no
C33 . C34 . C35 . 111.6(4) yes
C33 . C34 . H341 . 108.9 no
C35 . C34 . H341 . 108.9 no
C33 . C34 . H342 . 108.9 no
C35 . C34 . H342 . 108.9 no
H341 . C34 . H342 . 109.5 no
C34 . C35 . C36 . 111.5(4) yes
C34 . C35 . H351 . 109.0 no
C36 . C35 . H351 . 109.0 no
C34 . C35 . H352 . 109.0 no
C36 . C35 . H352 . 109.0 no
H351 . C35 . H352 . 109.5 no
C35 . C36 . C31 . 110.7(4) yes
C35 . C36 . H361 . 109.2 no
C31 . C36 . H361 . 109.2 no
C35 . C36 . H362 . 109.1 no
C31 . C36 . H362 . 109.2 no
H361 . C36 . H362 . 109.5 no
P2 . C41 . C42 . 112.9(4) yes
P2 . C41 . C46 . 111.7(4) yes
C42 . C41 . C46 . 110.5(5) yes
P2 . C41 . H411 . 107.1 no
C42 . C41 . H411 . 107.1 no
C46 . C41 . H411 . 107.1 no
C41 . C42 . C43 . 111.1(5) yes
C41 . C42 . H421 . 109.1 no
C43 . C42 . H421 . 109.1 no
C41 . C42 . H422 . 109.1 no
C43 . C42 . H422 . 109.1 no
H421 . C42 . H422 . 109.5 no
C42 . C43 . C44 . 110.1(6) yes
C42 . C43 . H431 . 109.3 no
C44 . C43 . H431 . 109.3 no
C42 . C43 . H432 . 109.3 no
C44 . C43 . H432 . 109.3 no
H431 . C43 . H432 . 109.5 no
C43 . C44 . C45 . 111.5(6) yes
C43 . C44 . H441 . 109.0 no
C45 . C44 . H441 . 109.0 no
C43 . C44 . H442 . 109.0 no
C45 . C44 . H442 . 109.0 no
H441 . C44 . H442 . 109.5 no
C44 . C45 . C46 . 110.6(7) yes
C44 . C45 . H451 . 109.2 no
C46 . C45 . H451 . 109.2 no
C44 . C45 . H452 . 109.2 no
C46 . C45 . H452 . 109.2 no
H451 . C45 . H452 . 109.5 no
C45 . C46 . C41 . 110.5(6) yes
C45 . C46 . H461 . 109.2 no
C41 . C46 . H461 . 109.2 no
C45 . C46 . H462 . 109.2 no
C41 . C46 . H462 . 109.2 no
H461 . C46 . H462 . 109.5 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 27/05/13 at 11:55:51
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 27/05/13 at 11:55:51
#
#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 17 11 x .
1 1 1 x .
-1 0 5 x .
1 2 0 x .
0 0 4 x .
2 5 1 x .
-1 2 5 x .
1 0 5 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 943297'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 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                   8.30660(10)
_cell_length_b                   18.0004(3)
_cell_length_c                   15.1242(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.2060(9)
_cell_angle_gamma                90
_cell_volume                     2243.54(6)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            4

# Given Formula = C24 H24 B1 Br1 P2 
# Dc =      1.38 Fooo =    952.00 Mu =     19.82 M =    465.12
# Found Formula = C24 H24 B1 Br1 P2 
# Dc =      1.38 FOOO =    952.00 Mu =     19.82 M =    465.12

_chemical_formula_sum            'C24 H24 B1 Br1 P2'
_chemical_formula_moiety         'C24 H24 B1 P2, Br1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         465.12


_cell_measurement_reflns_used    25261
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.140
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.290

_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    1.982

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 2 3 0.090
0 -4 3 0.086
-1 -1 -2 0.060
2 9 -3 0.030
-1 5 6 0.060
3 -4 -4 0.110
0 3 4 0.056


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_T_max  0.818
_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 (Farrugia, 1997)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            46433
_reflns_number_total             5139
_diffrn_reflns_av_R_equivalents  0.045
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 5139 
# Theoretical number of reflections is about 10288 


_diffrn_reflns_theta_min         2.639
_diffrn_reflns_theta_max         27.480
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.480
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   2.95
_oxford_diffrn_Wilson_scale      7.21

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

_refine_diff_density_min         -0.65
_refine_diff_density_max         0.64


# 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         5124
_refine_ls_number_restraints     0
_refine_ls_number_parameters     254
_oxford_refine_ls_R_factor_ref   0.0400
_refine_ls_wR_factor_ref         0.0773
_refine_ls_goodness_of_fit_ref   0.9679
_refine_ls_shift/su_max          0.0004848
_refine_ls_shift/su_mean         0.0000489


# The values computed from all data 
_oxford_reflns_number_all        5124
_refine_ls_R_factor_all          0.0400
_refine_ls_wR_factor_all         0.0773

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4263
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_gt          0.0723

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 1.09P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.8185(3) 0.60256(13) 0.27918(14) 0.0350 1.0000 Uani . . . . . .
Br1 Br 0.61609(2) 0.409032(10) 0.191816(13) 0.0390 1.0000 Uani . . . . . .
P1 P 0.78757(6) 0.60301(3) 0.15072(3) 0.0294 1.0000 Uani . . . . . .
P2 P 0.61437(6) 0.59322(2) 0.32581(3) 0.0300 1.0000 Uani . . . . . .
C11 C 0.9788(2) 0.58433(10) 0.10995(12) 0.0313 1.0000 Uani . . . . . .
C12 C 1.0573(3) 0.51773(11) 0.13511(14) 0.0405 1.0000 Uani . . . . . .
C13 C 1.2057(3) 0.50193(12) 0.10681(15) 0.0459 1.0000 Uani . . . . . .
C14 C 1.2745(2) 0.55164(13) 0.05334(14) 0.0471 1.0000 Uani . . . . . .
C15 C 1.1972(3) 0.61706(14) 0.02758(16) 0.0512 1.0000 Uani . . . . . .
C16 C 1.0489(2) 0.63412(12) 0.05623(14) 0.0417 1.0000 Uani . . . . . .
C21 C 0.7013(2) 0.68606(10) 0.09861(12) 0.0319 1.0000 Uani . . . . . .
C22 C 0.6118(2) 0.68173(11) 0.01408(13) 0.0371 1.0000 Uani . . . . . .
C23 C 0.5435(3) 0.74536(12) -0.02610(14) 0.0467 1.0000 Uani . . . . . .
C24 C 0.5613(3) 0.81282(13) 0.01775(17) 0.0559 1.0000 Uani . . . . . .
C25 C 0.6516(3) 0.81748(12) 0.10110(17) 0.0567 1.0000 Uani . . . . . .
C26 C 0.7217(3) 0.75452(11) 0.14164(14) 0.0427 1.0000 Uani . . . . . .
C31 C 0.6490(2) 0.57421(10) 0.44438(12) 0.0333 1.0000 Uani . . . . . .
C32 C 0.5658(3) 0.61258(13) 0.50398(14) 0.0448 1.0000 Uani . . . . . .
C33 C 0.5972(3) 0.59820(13) 0.59473(15) 0.0528 1.0000 Uani . . . . . .
C34 C 0.7124(3) 0.54607(13) 0.62544(14) 0.0486 1.0000 Uani . . . . . .
C35 C 0.7926(3) 0.50701(13) 0.56689(15) 0.0501 1.0000 Uani . . . . . .
C36 C 0.7621(3) 0.52076(12) 0.47602(14) 0.0439 1.0000 Uani . . . . . .
C41 C 0.4849(2) 0.67324(10) 0.30950(12) 0.0316 1.0000 Uani . . . . . .
C42 C 0.3225(2) 0.66622(12) 0.27539(14) 0.0431 1.0000 Uani . . . . . .
C43 C 0.2252(3) 0.72873(13) 0.26627(17) 0.0532 1.0000 Uani . . . . . .
C44 C 0.2868(3) 0.79755(12) 0.29078(15) 0.0484 1.0000 Uani . . . . . .
C45 C 0.4497(3) 0.80498(12) 0.32394(16) 0.0487 1.0000 Uani . . . . . .
C46 C 0.5482(3) 0.74285(11) 0.33290(15) 0.0437 1.0000 Uani . . . . . .
H121 H 1.0067 0.4843 0.1695 0.0491 1.0000 Uiso R . . . . .
H131 H 1.2582 0.4576 0.1236 0.0552 1.0000 Uiso R . . . . .
H141 H 1.3737 0.5405 0.0340 0.0568 1.0000 Uiso R . . . . .
H151 H 1.2434 0.6495 -0.0092 0.0621 1.0000 Uiso R . . . . .
H161 H 0.9961 0.6790 0.0392 0.0498 1.0000 Uiso R . . . . .
H221 H 0.5965 0.6364 -0.0149 0.0444 1.0000 Uiso R . . . . .
H231 H 0.4845 0.7419 -0.0836 0.0565 1.0000 Uiso R . . . . .
H241 H 0.5118 0.8563 -0.0085 0.0676 1.0000 Uiso R . . . . .
H251 H 0.6660 0.8641 0.1307 0.0682 1.0000 Uiso R . . . . .
H261 H 0.7822 0.7578 0.1992 0.0513 1.0000 Uiso R . . . . .
H321 H 0.4907 0.6488 0.4839 0.0542 1.0000 Uiso R . . . . .
H331 H 0.5400 0.6229 0.6358 0.0624 1.0000 Uiso R . . . . .
H341 H 0.7349 0.5362 0.6861 0.0576 1.0000 Uiso R . . . . .
H351 H 0.8669 0.4703 0.5883 0.0605 1.0000 Uiso R . . . . .
H361 H 0.8153 0.4941 0.4357 0.0533 1.0000 Uiso R . . . . .
H421 H 0.2789 0.6193 0.2581 0.0526 1.0000 Uiso R . . . . .
H431 H 0.1143 0.7241 0.2434 0.0647 1.0000 Uiso R . . . . .
H441 H 0.2186 0.8396 0.2861 0.0580 1.0000 Uiso R . . . . .
H451 H 0.4921 0.8517 0.3416 0.0581 1.0000 Uiso R . . . . .
H461 H 0.6582 0.7480 0.3545 0.0527 1.0000 Uiso R . . . . .
H11 H 0.6911 0.5505 0.1199 0.0354 1.0000 Uiso R . . . . .
H2 H 0.8827 0.6536 0.3064 0.0468 1.0000 Uiso R . . . . .
H1 H 0.8884 0.5564 0.2992 0.0697 1.0000 Uiso R . . . . .
H21 H 0.5261 0.5406 0.2879 0.0505 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       170(15)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.4228(5)
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 . P1 . 1.928(2) yes
B1 . P2 . 1.923(2) yes
B1 . H2 . 1.116 no
B1 . H1 . 1.038 no
P1 . C11 . 1.8061(18) yes
P1 . C21 . 1.7965(18) yes
P1 . H11 . 1.288 no
P2 . C31 . 1.8128(19) yes
P2 . C41 . 1.7961(18) yes
P2 . H21 . 1.287 no
C11 . C12 . 1.395(3) yes
C11 . C16 . 1.386(3) yes
C12 . C13 . 1.384(3) yes
C12 . H121 . 0.929 no
C13 . C14 . 1.377(3) yes
C13 . H131 . 0.929 no
C14 . C15 . 1.374(3) yes
C14 . H141 . 0.930 no
C15 . C16 . 1.390(3) yes
C15 . H151 . 0.923 no
C16 . H161 . 0.940 no
C21 . C22 . 1.398(3) yes
C21 . C26 . 1.394(3) yes
C22 . C23 . 1.384(3) yes
C22 . H221 . 0.927 no
C23 . C24 . 1.383(3) yes
C23 . H231 . 0.946 no
C24 . C25 . 1.386(3) yes
C24 . H241 . 0.948 no
C25 . C26 . 1.382(3) yes
C25 . H251 . 0.952 no
C26 . H261 . 0.950 no
C31 . C32 . 1.387(3) yes
C31 . C36 . 1.387(3) yes
C32 . C33 . 1.389(3) yes
C32 . H321 . 0.927 no
C33 . C34 . 1.379(3) yes
C33 . H331 . 0.940 no
C34 . C35 . 1.368(3) yes
C34 . H341 . 0.931 no
C35 . C36 . 1.388(3) yes
C35 . H351 . 0.935 no
C36 . H361 . 0.930 no
C41 . C42 . 1.388(3) yes
C41 . C46 . 1.387(3) yes
C42 . C43 . 1.382(3) yes
C42 . H421 . 0.943 no
C43 . C44 . 1.373(3) yes
C43 . H431 . 0.946 no
C44 . C45 . 1.389(3) yes
C44 . H441 . 0.943 no
C45 . C46 . 1.382(3) yes
C45 . H451 . 0.938 no
C46 . H461 . 0.935 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 . B1 . P2 . 110.97(11) yes
P1 . B1 . H2 . 111.4 no
P2 . B1 . H2 . 109.8 no
P1 . B1 . H1 . 107.3 no
P2 . B1 . H1 . 108.0 no
H2 . B1 . H1 . 109.2 no
B1 . P1 . C11 . 109.38(9) yes
B1 . P1 . C21 . 116.17(9) yes
C11 . P1 . C21 . 108.95(8) yes
B1 . P1 . H11 . 111.1 no
C11 . P1 . H11 . 105.9 no
C21 . P1 . H11 . 104.8 no
B1 . P2 . C31 . 109.95(9) yes
B1 . P2 . C41 . 114.81(9) yes
C31 . P2 . C41 . 107.78(8) yes
B1 . P2 . H21 . 112.3 no
C31 . P2 . H21 . 108.2 no
C41 . P2 . H21 . 103.3 no
P1 . C11 . C12 . 117.92(14) yes
P1 . C11 . C16 . 122.12(14) yes
C12 . C11 . C16 . 119.96(18) yes
C11 . C12 . C13 . 119.76(19) yes
C11 . C12 . H121 . 118.7 no
C13 . C12 . H121 . 121.6 no
C12 . C13 . C14 . 120.0(2) yes
C12 . C13 . H131 . 119.8 no
C14 . C13 . H131 . 120.2 no
C13 . C14 . C15 . 120.63(19) yes
C13 . C14 . H141 . 119.6 no
C15 . C14 . H141 . 119.8 no
C14 . C15 . C16 . 120.1(2) yes
C14 . C15 . H151 . 119.8 no
C16 . C15 . H151 . 120.0 no
C15 . C16 . C11 . 119.57(19) yes
C15 . C16 . H161 . 120.4 no
C11 . C16 . H161 . 120.1 no
P1 . C21 . C22 . 119.46(14) yes
P1 . C21 . C26 . 120.81(14) yes
C22 . C21 . C26 . 119.72(17) yes
C21 . C22 . C23 . 119.79(19) yes
C21 . C22 . H221 . 120.4 no
C23 . C22 . H221 . 119.8 no
C22 . C23 . C24 . 120.19(19) yes
C22 . C23 . H231 . 119.0 no
C24 . C23 . H231 . 120.8 no
C23 . C24 . C25 . 120.2(2) yes
C23 . C24 . H241 . 120.6 no
C25 . C24 . H241 . 119.2 no
C24 . C25 . C26 . 120.2(2) yes
C24 . C25 . H251 . 120.2 no
C26 . C25 . H251 . 119.5 no
C21 . C26 . C25 . 119.86(19) yes
C21 . C26 . H261 . 120.1 no
C25 . C26 . H261 . 120.0 no
P2 . C31 . C32 . 121.24(15) yes
P2 . C31 . C36 . 119.27(15) yes
C32 . C31 . C36 . 119.49(18) yes
C31 . C32 . C33 . 120.2(2) yes
C31 . C32 . H321 . 120.4 no
C33 . C32 . H321 . 119.4 no
C32 . C33 . C34 . 119.7(2) yes
C32 . C33 . H331 . 121.1 no
C34 . C33 . H331 . 119.1 no
C33 . C34 . C35 . 120.4(2) yes
C33 . C34 . H341 . 120.5 no
C35 . C34 . H341 . 119.1 no
C34 . C35 . C36 . 120.4(2) yes
C34 . C35 . H351 . 119.6 no
C36 . C35 . H351 . 120.0 no
C35 . C36 . C31 . 119.79(19) yes
C35 . C36 . H361 . 120.9 no
C31 . C36 . H361 . 119.3 no
P2 . C41 . C42 . 121.01(14) yes
P2 . C41 . C46 . 119.20(14) yes
C42 . C41 . C46 . 119.78(18) yes
C41 . C42 . C43 . 119.47(19) yes
C41 . C42 . H421 . 120.4 no
C43 . C42 . H421 . 120.1 no
C42 . C43 . C44 . 120.9(2) yes
C42 . C43 . H431 . 119.7 no
C44 . C43 . H431 . 119.4 no
C43 . C44 . C45 . 119.82(19) yes
C43 . C44 . H441 . 120.2 no
C45 . C44 . H441 . 119.9 no
C44 . C45 . C46 . 119.7(2) yes
C44 . C45 . H451 . 120.2 no
C46 . C45 . H451 . 120.1 no
C41 . C46 . C45 . 120.31(19) yes
C41 . C46 . H461 . 120.1 no
C45 . C46 . H461 . 119.6 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 24/09/11 at 11:19:44
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE B   (   1,X'S) H   (   2,X'S) H   (   1,X'S) 
RIDE P   (   1,X'S) H   (  11,X'S) 
RIDE P   (   2,X'S) H   (  21,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 24/09/11 at 11:19:44
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;



####################################################################### 
# 
# 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 943302'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 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                   13.7686(6)
_cell_length_b                   14.0695(5)
_cell_length_c                   14.3983(6)
_cell_angle_alpha                98.002(2)
_cell_angle_beta                 114.3643(19)
_cell_angle_gamma                113.651(2)
_cell_volume                     2166.66(18)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'
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'


_cell_formula_units_Z            2

# Given Formula = C43 H45 B1 Br1 Cl4 P3 
# Dc =      1.36 Fooo =    744.00 Mu =     13.36 M =    887.28
# Found Formula = C41 H41 B1 Br1 P3 
# Dc =      1.10 FOOO =    744.00 Mu =     10.83 M =    717.41

_chemical_formula_sum            'C41 H41 B1 Br1 P3'
_chemical_formula_moiety         'C41 H41 B1 P3, Br1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         717.41


_cell_measurement_reflns_used    36206
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25
_cell_measurement_temperature    200

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_max          0.340

_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    1.083

# 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 0.110
0 1 0 0.160
0 0 1 0.090
0 0 -1 0.080
1 -3 2 0.104
4 2 -1 0.106
0 1 -2 0.056
5 -1 -4 0.096
-3 1 1 0.060
-1 -1 3 0.085


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_T_max  0.859
_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 (Farrugia, 1997)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            7713
_reflns_number_total             7713
_diffrn_reflns_av_R_equivalents  0.047
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7713 
# Theoretical number of reflections is about 15597 


_diffrn_reflns_theta_min         2.673
_diffrn_reflns_theta_max         25.192
_diffrn_measured_fraction_theta_max 0.988

_diffrn_reflns_theta_full        25.192
_diffrn_measured_fraction_theta_full 0.988


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

_oxford_diffrn_Wilson_B_factor   3.85
_oxford_diffrn_Wilson_scale      3.94

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

_refine_diff_density_min         -0.92
_refine_diff_density_max         0.82


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

# 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 0.016 0.000 0.500 479 100 ' '
_platon_squeeze_details          
;
;

# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7713
_refine_ls_number_restraints     0
_refine_ls_number_parameters     415
_oxford_refine_ls_R_factor_ref   0.0590
_refine_ls_wR_factor_ref         0.1504
_refine_ls_goodness_of_fit_ref   1.0032
_refine_ls_shift/su_max          0.0002009
_refine_ls_shift/su_mean         0.0000101


# The values computed from all data 
_oxford_reflns_number_all        7713
_refine_ls_R_factor_all          0.0590
_refine_ls_wR_factor_all         0.1504

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6309
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_gt          0.1418

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 2.85P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B -0.0068(4) 0.3362(3) -0.0620(3) 0.0405 1.0000 Uani . . . . . .
Br1 Br -0.12766(4) -0.04058(3) -0.25354(3) 0.0551 1.0000 Uani . . . . . .
P1 P 0.44267(9) 0.38626(8) 0.16899(8) 0.0423 1.0000 Uani . . . . . .
P2 P 0.13312(8) 0.36864(7) -0.07879(7) 0.0377 1.0000 Uani . . . . . .
P3 P -0.00560(8) 0.26393(7) 0.04288(7) 0.0359 1.0000 Uani . . . . . .
C1 C 0.2844(3) 0.3225(3) 0.1466(3) 0.0394 1.0000 Uani . . . . . .
C2 C 0.1718(3) 0.2598(3) -0.0633(3) 0.0399 1.0000 Uani . . . . . .
C3 C 0.0564(3) 0.1736(3) 0.0318(3) 0.0386 1.0000 Uani . . . . . .
C4 C 0.1825(3) 0.2249(3) 0.0367(3) 0.0386 1.0000 Uani . . . . . .
C5 C 0.2126(4) 0.1312(3) 0.0273(3) 0.0466 1.0000 Uani . . . . . .
C11 C 0.5221(4) 0.5190(3) 0.2813(3) 0.0480 1.0000 Uani . . . . . .
C12 C 0.6373(4) 0.5992(4) 0.3049(4) 0.0640 1.0000 Uani . . . . . .
C13 C 0.7039(6) 0.7010(4) 0.3877(5) 0.0894 1.0000 Uani . . . . . .
C14 C 0.6572(6) 0.7281(5) 0.4458(5) 0.0969 1.0000 Uani . . . . . .
C15 C 0.5443(7) 0.6511(6) 0.4244(5) 0.1012 1.0000 Uani . . . . . .
C16 C 0.4749(5) 0.5458(4) 0.3430(4) 0.0733 1.0000 Uani . . . . . .
C21 C 0.5131(3) 0.3147(3) 0.2462(3) 0.0440 1.0000 Uani . . . . . .
C22 C 0.6003(4) 0.3034(4) 0.2289(4) 0.0592 1.0000 Uani . . . . . .
C23 C 0.6672(4) 0.2602(4) 0.2911(4) 0.0671 1.0000 Uani . . . . . .
C24 C 0.6477(4) 0.2280(4) 0.3693(4) 0.0650 1.0000 Uani . . . . . .
C25 C 0.5581(5) 0.2355(4) 0.3849(4) 0.0677 1.0000 Uani . . . . . .
C26 C 0.4911(4) 0.2779(4) 0.3237(3) 0.0588 1.0000 Uani . . . . . .
C31 C 0.2678(3) 0.5052(3) 0.0089(3) 0.0408 1.0000 Uani . . . . . .
C32 C 0.3751(4) 0.5407(3) 0.0036(3) 0.0485 1.0000 Uani . . . . . .
C33 C 0.4755(4) 0.6467(3) 0.0690(4) 0.0552 1.0000 Uani . . . . . .
C34 C 0.4707(4) 0.7177(3) 0.1412(4) 0.0603 1.0000 Uani . . . . . .
C35 C 0.3659(4) 0.6846(3) 0.1470(4) 0.0633 1.0000 Uani . . . . . .
C36 C 0.2646(4) 0.5788(3) 0.0809(3) 0.0531 1.0000 Uani . . . . . .
C41 C 0.0889(3) 0.3605(3) -0.2185(3) 0.0433 1.0000 Uani . . . . . .
C42 C 0.1298(4) 0.4562(4) -0.2428(3) 0.0575 1.0000 Uani . . . . . .
C43 C 0.0891(5) 0.4472(5) -0.3518(4) 0.0732 1.0000 Uani . . . . . .
C44 C 0.0103(5) 0.3441(5) -0.4346(4) 0.0709 1.0000 Uani . . . . . .
C45 C -0.0327(5) 0.2502(4) -0.4121(4) 0.0705 1.0000 Uani . . . . . .
C46 C 0.0068(4) 0.2570(4) -0.3035(3) 0.0589 1.0000 Uani . . . . . .
C51 C 0.0719(3) 0.3524(3) 0.1846(3) 0.0389 1.0000 Uani . . . . . .
C52 C 0.0867(4) 0.4581(3) 0.2095(3) 0.0490 1.0000 Uani . . . . . .
C53 C 0.1422(4) 0.5262(3) 0.3177(4) 0.0611 1.0000 Uani . . . . . .
C54 C 0.1838(4) 0.4878(4) 0.4005(3) 0.0647 1.0000 Uani . . . . . .
C55 C 0.1688(4) 0.3821(4) 0.3766(3) 0.0613 1.0000 Uani . . . . . .
C56 C 0.1125(4) 0.3142(3) 0.2687(3) 0.0488 1.0000 Uani . . . . . .
C61 C -0.1668(3) 0.1773(3) 0.0017(3) 0.0399 1.0000 Uani . . . . . .
C62 C -0.2142(4) 0.2034(3) 0.0633(3) 0.0523 1.0000 Uani . . . . . .
C63 C -0.3392(4) 0.1429(4) 0.0241(4) 0.0644 1.0000 Uani . . . . . .
C64 C -0.4182(4) 0.0557(4) -0.0761(4) 0.0620 1.0000 Uani . . . . . .
C65 C -0.3713(4) 0.0290(3) -0.1366(4) 0.0599 1.0000 Uani . . . . . .
C66 C -0.2464(4) 0.0905(3) -0.0991(3) 0.0491 1.0000 Uani . . . . . .
H11 H 0.2654 0.3819 0.1502 0.0460 1.0000 Uiso R . . . . .
H12 H 0.2820 0.2958 0.2045 0.0473 1.0000 Uiso R . . . . .
H21 H 0.2480 0.2825 -0.0622 0.0480 1.0000 Uiso R . . . . .
H22 H 0.1065 0.1939 -0.1269 0.0478 1.0000 Uiso R . . . . .
H31 H 0.0631 0.1423 0.0874 0.0460 1.0000 Uiso R . . . . .
H32 H -0.0028 0.1172 -0.0388 0.0461 1.0000 Uiso R . . . . .
H53 H 0.1451 0.0698 -0.0389 0.0693 1.0000 Uiso R . . . . .
H52 H 0.2868 0.1581 0.0252 0.0696 1.0000 Uiso R . . . . .
H51 H 0.2226 0.1098 0.0895 0.0694 1.0000 Uiso R . . . . .
H121 H 0.6685 0.5826 0.2634 0.0774 1.0000 Uiso R . . . . .
H131 H 0.7817 0.7517 0.4036 0.1070 1.0000 Uiso R . . . . .
H141 H 0.6998 0.7972 0.4972 0.1157 1.0000 Uiso R . . . . .
H151 H 0.5113 0.6671 0.4641 0.1212 1.0000 Uiso R . . . . .
H161 H 0.3981 0.4936 0.3304 0.0881 1.0000 Uiso R . . . . .
H221 H 0.6153 0.3261 0.1756 0.0713 1.0000 Uiso R . . . . .
H231 H 0.7253 0.2506 0.2786 0.0811 1.0000 Uiso R . . . . .
H241 H 0.6960 0.2032 0.4139 0.0776 1.0000 Uiso R . . . . .
H251 H 0.5422 0.2103 0.4372 0.0809 1.0000 Uiso R . . . . .
H261 H 0.4293 0.2811 0.3345 0.0710 1.0000 Uiso R . . . . .
H321 H 0.3795 0.4920 -0.0443 0.0577 1.0000 Uiso R . . . . .
H331 H 0.5453 0.6702 0.0633 0.0662 1.0000 Uiso R . . . . .
H341 H 0.5397 0.7883 0.1857 0.0720 1.0000 Uiso R . . . . .
H351 H 0.3626 0.7335 0.1950 0.0760 1.0000 Uiso R . . . . .
H361 H 0.1933 0.5560 0.0851 0.0640 1.0000 Uiso R . . . . .
H421 H 0.1847 0.5264 -0.1872 0.0689 1.0000 Uiso R . . . . .
H431 H 0.1163 0.5113 -0.3676 0.0878 1.0000 Uiso R . . . . .
H441 H -0.0153 0.3373 -0.5075 0.0850 1.0000 Uiso R . . . . .
H451 H -0.0893 0.1828 -0.4687 0.0847 1.0000 Uiso R . . . . .
H461 H -0.0209 0.1926 -0.2868 0.0707 1.0000 Uiso R . . . . .
H521 H 0.0608 0.4851 0.1532 0.0590 1.0000 Uiso R . . . . .
H531 H 0.1516 0.5982 0.3346 0.0731 1.0000 Uiso R . . . . .
H541 H 0.2196 0.5329 0.4722 0.0782 1.0000 Uiso R . . . . .
H551 H 0.1968 0.3571 0.4333 0.0740 1.0000 Uiso R . . . . .
H561 H 0.1008 0.2429 0.2524 0.0583 1.0000 Uiso R . . . . .
H621 H -0.1624 0.2617 0.1301 0.0628 1.0000 Uiso R . . . . .
H631 H -0.3712 0.1624 0.0660 0.0769 1.0000 Uiso R . . . . .
H641 H -0.5032 0.0155 -0.1038 0.0738 1.0000 Uiso R . . . . .
H651 H -0.4229 -0.0297 -0.2031 0.0718 1.0000 Uiso R . . . . .
H661 H -0.2162 0.0730 -0.1406 0.0589 1.0000 Uiso R . . . . .
H1 H -0.0845 0.2671 -0.1409 0.0565 1.0000 Uiso R . . . . .
H2 H -0.0130 0.4099 -0.0441 0.0449 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       94.354
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.6437(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
B1 . P2 . 1.921(4) yes
B1 . P3 . 1.932(4) yes
B1 . H1 . 1.112 no
B1 . H2 . 1.079 no
P1 . C1 . 1.852(4) yes
P1 . C11 . 1.833(4) yes
P1 . C21 . 1.842(4) yes
P2 . C2 . 1.825(3) yes
P2 . C31 . 1.805(4) yes
P2 . C41 . 1.817(3) yes
P3 . C3 . 1.816(3) yes
P3 . C51 . 1.812(3) yes
P3 . C61 . 1.818(3) yes
C1 . C4 . 1.541(5) yes
C1 . H11 . 0.971 no
C1 . H12 . 0.967 no
C2 . C4 . 1.554(5) yes
C2 . H21 . 0.959 no
C2 . H22 . 0.960 no
C3 . C4 . 1.555(5) yes
C3 . H31 . 0.956 no
C3 . H32 . 0.949 no
C4 . C5 . 1.538(5) yes
C5 . H53 . 0.956 no
C5 . H52 . 0.952 no
C5 . H51 . 0.957 no
C11 . C12 . 1.384(6) yes
C11 . C16 . 1.391(6) yes
C12 . C13 . 1.372(7) yes
C12 . H121 . 0.921 no
C13 . C14 . 1.346(9) yes
C13 . H131 . 0.921 no
C14 . C15 . 1.358(9) yes
C14 . H141 . 0.906 no
C15 . C16 . 1.391(7) yes
C15 . H151 . 0.920 no
C16 . H161 . 0.934 no
C21 . C22 . 1.385(5) yes
C21 . C26 . 1.385(6) yes
C22 . C23 . 1.394(6) yes
C22 . H221 . 0.938 no
C23 . C24 . 1.356(7) yes
C23 . H231 . 0.943 no
C24 . C25 . 1.382(7) yes
C24 . H241 . 0.935 no
C25 . C26 . 1.379(6) yes
C25 . H251 . 0.941 no
C26 . H261 . 0.942 no
C31 . C32 . 1.396(5) yes
C31 . C36 . 1.387(5) yes
C32 . C33 . 1.380(5) yes
C32 . H321 . 0.940 no
C33 . C34 . 1.378(6) yes
C33 . H331 . 0.927 no
C34 . C35 . 1.370(6) yes
C34 . H341 . 0.930 no
C35 . C36 . 1.383(6) yes
C35 . H351 . 0.933 no
C36 . H361 . 0.933 no
C41 . C42 . 1.391(5) yes
C41 . C46 . 1.392(6) yes
C42 . C43 . 1.398(6) yes
C42 . H421 . 0.932 no
C43 . C44 . 1.375(7) yes
C43 . H431 . 0.929 no
C44 . C45 . 1.360(7) yes
C44 . H441 . 0.936 no
C45 . C46 . 1.403(6) yes
C45 . H451 . 0.916 no
C46 . H461 . 0.940 no
C51 . C52 . 1.390(5) yes
C51 . C56 . 1.390(5) yes
C52 . C53 . 1.393(6) yes
C52 . H521 . 0.941 no
C53 . C54 . 1.381(6) yes
C53 . H531 . 0.950 no
C54 . C55 . 1.387(6) yes
C54 . H541 . 0.926 no
C55 . C56 . 1.388(6) yes
C55 . H551 . 0.932 no
C56 . H561 . 0.927 no
C61 . C62 . 1.389(5) yes
C61 . C66 . 1.385(5) yes
C62 . C63 . 1.376(6) yes
C62 . H621 . 0.924 no
C63 . C64 . 1.382(6) yes
C63 . H631 . 0.952 no
C64 . C65 . 1.373(6) yes
C64 . H641 . 0.932 no
C65 . C66 . 1.381(6) yes
C65 . H651 . 0.922 no
C66 . H661 . 0.915 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
P2 . B1 . P3 . 111.2(2) yes
P2 . B1 . H1 . 102.0 no
P3 . B1 . H1 . 102.3 no
P2 . B1 . H2 . 110.7 no
P3 . B1 . H2 . 113.7 no
H1 . B1 . H2 . 116.0 no
C1 . P1 . C11 . 101.36(17) yes
C1 . P1 . C21 . 104.87(16) yes
C11 . P1 . C21 . 98.82(16) yes
B1 . P2 . C2 . 109.48(17) yes
B1 . P2 . C31 . 115.38(17) yes
C2 . P2 . C31 . 111.02(17) yes
B1 . P2 . C41 . 108.79(17) yes
C2 . P2 . C41 . 105.31(16) yes
C31 . P2 . C41 . 106.30(16) yes
B1 . P3 . C3 . 108.89(16) yes
B1 . P3 . C51 . 117.37(17) yes
C3 . P3 . C51 . 110.23(16) yes
B1 . P3 . C61 . 106.00(17) yes
C3 . P3 . C61 . 108.27(16) yes
C51 . P3 . C61 . 105.64(16) yes
P1 . C1 . C4 . 115.4(2) yes
P1 . C1 . H11 . 105.9 no
C4 . C1 . H11 . 108.8 no
P1 . C1 . H12 . 110.6 no
C4 . C1 . H12 . 107.6 no
H11 . C1 . H12 . 108.3 no
P2 . C2 . C4 . 118.2(2) yes
P2 . C2 . H21 . 108.1 no
C4 . C2 . H21 . 108.7 no
P2 . C2 . H22 . 106.6 no
C4 . C2 . H22 . 105.8 no
H21 . C2 . H22 . 109.2 no
P3 . C3 . C4 . 117.6(2) yes
P3 . C3 . H31 . 108.9 no
C4 . C3 . H31 . 108.7 no
P3 . C3 . H32 . 104.7 no
C4 . C3 . H32 . 106.1 no
H31 . C3 . H32 . 110.7 no
C1 . C4 . C2 . 112.3(3) yes
C1 . C4 . C3 . 110.2(3) yes
C2 . C4 . C3 . 111.2(3) yes
C1 . C4 . C5 . 109.8(3) yes
C2 . C4 . C5 . 106.8(3) yes
C3 . C4 . C5 . 106.2(3) yes
C4 . C5 . H53 . 108.0 no
C4 . C5 . H52 . 108.6 no
H53 . C5 . H52 . 110.2 no
C4 . C5 . H51 . 108.6 no
H53 . C5 . H51 . 110.5 no
H52 . C5 . H51 . 110.7 no
P1 . C11 . C12 . 117.1(3) yes
P1 . C11 . C16 . 125.2(3) yes
C12 . C11 . C16 . 117.7(4) yes
C11 . C12 . C13 . 121.3(5) yes
C11 . C12 . H121 . 118.2 no
C13 . C12 . H121 . 120.4 no
C12 . C13 . C14 . 121.0(6) yes
C12 . C13 . H131 . 119.5 no
C14 . C13 . H131 . 119.5 no
C13 . C14 . C15 . 118.9(5) yes
C13 . C14 . H141 . 120.3 no
C15 . C14 . H141 . 120.8 no
C14 . C15 . C16 . 121.9(6) yes
C14 . C15 . H151 . 120.5 no
C16 . C15 . H151 . 117.6 no
C15 . C16 . C11 . 119.0(5) yes
C15 . C16 . H161 . 120.6 no
C11 . C16 . H161 . 120.3 no
P1 . C21 . C22 . 116.3(3) yes
P1 . C21 . C26 . 125.4(3) yes
C22 . C21 . C26 . 118.2(4) yes
C21 . C22 . C23 . 120.6(4) yes
C21 . C22 . H221 . 119.7 no
C23 . C22 . H221 . 119.7 no
C22 . C23 . C24 . 120.6(4) yes
C22 . C23 . H231 . 121.0 no
C24 . C23 . H231 . 118.4 no
C23 . C24 . C25 . 119.4(4) yes
C23 . C24 . H241 . 120.5 no
C25 . C24 . H241 . 120.1 no
C24 . C25 . C26 . 120.5(5) yes
C24 . C25 . H251 . 119.4 no
C26 . C25 . H251 . 120.1 no
C21 . C26 . C25 . 120.7(4) yes
C21 . C26 . H261 . 119.9 no
C25 . C26 . H261 . 119.4 no
P2 . C31 . C32 . 121.4(3) yes
P2 . C31 . C36 . 120.0(3) yes
C32 . C31 . C36 . 118.6(3) yes
C31 . C32 . C33 . 120.3(4) yes
C31 . C32 . H321 . 120.0 no
C33 . C32 . H321 . 119.6 no
C32 . C33 . C34 . 120.0(4) yes
C32 . C33 . H331 . 119.6 no
C34 . C33 . H331 . 120.4 no
C33 . C34 . C35 . 120.5(4) yes
C33 . C34 . H341 . 118.9 no
C35 . C34 . H341 . 120.6 no
C34 . C35 . C36 . 119.8(4) yes
C34 . C35 . H351 . 120.2 no
C36 . C35 . H351 . 120.0 no
C31 . C36 . C35 . 120.8(4) yes
C31 . C36 . H361 . 119.3 no
C35 . C36 . H361 . 119.9 no
P2 . C41 . C42 . 121.2(3) yes
P2 . C41 . C46 . 119.2(3) yes
C42 . C41 . C46 . 119.4(4) yes
C41 . C42 . C43 . 119.7(4) yes
C41 . C42 . H421 . 120.9 no
C43 . C42 . H421 . 119.4 no
C42 . C43 . C44 . 120.2(4) yes
C42 . C43 . H431 . 119.4 no
C44 . C43 . H431 . 120.4 no
C43 . C44 . C45 . 120.6(4) yes
C43 . C44 . H441 . 120.6 no
C45 . C44 . H441 . 118.8 no
C44 . C45 . C46 . 120.3(5) yes
C44 . C45 . H451 . 119.3 no
C46 . C45 . H451 . 120.4 no
C45 . C46 . C41 . 119.7(4) yes
C45 . C46 . H461 . 121.1 no
C41 . C46 . H461 . 119.2 no
P3 . C51 . C52 . 119.7(3) yes
P3 . C51 . C56 . 120.8(3) yes
C52 . C51 . C56 . 119.4(3) yes
C51 . C52 . C53 . 120.8(4) yes
C51 . C52 . H521 . 119.9 no
C53 . C52 . H521 . 119.3 no
C52 . C53 . C54 . 119.2(4) yes
C52 . C53 . H531 . 120.7 no
C54 . C53 . H531 . 120.1 no
C53 . C54 . C55 . 120.6(4) yes
C53 . C54 . H541 . 118.9 no
C55 . C54 . H541 . 120.5 no
C54 . C55 . C56 . 120.1(4) yes
C54 . C55 . H551 . 119.7 no
C56 . C55 . H551 . 120.3 no
C51 . C56 . C55 . 120.0(4) yes
C51 . C56 . H561 . 119.8 no
C55 . C56 . H561 . 120.2 no
P3 . C61 . C62 . 121.4(3) yes
P3 . C61 . C66 . 118.9(3) yes
C62 . C61 . C66 . 119.3(3) yes
C61 . C62 . C63 . 119.9(4) yes
C61 . C62 . H621 . 120.3 no
C63 . C62 . H621 . 119.9 no
C62 . C63 . C64 . 120.6(4) yes
C62 . C63 . H631 . 119.3 no
C64 . C63 . H631 . 120.0 no
C63 . C64 . C65 . 119.6(4) yes
C63 . C64 . H641 . 121.0 no
C65 . C64 . H641 . 119.4 no
C64 . C65 . C66 . 120.3(4) yes
C64 . C65 . H651 . 120.5 no
C66 . C65 . H651 . 119.2 no
C61 . C66 . C65 . 120.2(4) yes
C61 . C66 . H661 . 120.0 no
C65 . C66 . H661 . 119.8 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 21/11/11 at 15:07:51
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
REM CONT EXTPARAM 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   5,X'S) H   (  53,X'S) H   (  52,X'S) H   (  51,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 21/11/11 at 15:07:51
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# start Validation Reply Form
_vrf_PLAT602_jas045              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        !
RESPONSE: The asymmetric unit cell contained one molecule of 
JSW151 as well as two disordered molecules of DCM. The disorder
of the DCM molecules could not be resolved and subsequently 
Platon Squeeze was used to refine the structure.
;
# end Validation Reply Form




####################################################################### 
# 
# 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 943304'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 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                   11.8318(3)
_cell_length_b                   13.6868(3)
_cell_length_c                   20.5375(4)
_cell_angle_alpha                102.0817(13)
_cell_angle_beta                 99.8011(10)
_cell_angle_gamma                92.5268(11)
_cell_volume                     3193.71(13)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'
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'


_cell_formula_units_Z            2

# Given Formula = C53 H100 B2 Br4 Cl2 P4 
# Dc =      1.32 Fooo =   1324.00 Mu =     27.35 M =   1273.42
# Found Formula = C53 H100 B2 Br4 Cl2 P4 
# Dc =      1.32 FOOO =   1324.00 Mu =     27.35 M =   1273.41

_chemical_formula_sum            'C53 H100 B2 Br4 Cl2 P4'
_chemical_formula_moiety         '2(C26 H49 B1 Br1 P2), 2(Br), C1 H2 Cl2'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         1273.41


_cell_measurement_reflns_used    100672
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.160
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_max          0.280

_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1324
_exptl_absorpt_coefficient_mu    2.735

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -1 1 0.090
1 -4 -6 0.040
-1 4 6 0.130
3 1 -2 0.054
0 -1 5 0.142
-1 5 -1 0.108
0 -2 3 0.135
-1 3 -4 0.129


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 150 30 ' '
2 0.509 0.958 0.088 40 2 ' '
3 0.491 0.042 0.911 39 2 ' '
_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    '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            66125
_reflns_number_total             14614
_diffrn_reflns_av_R_equivalents  0.057
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 14614 
# Theoretical number of reflections is about 29433 


_diffrn_reflns_theta_min         2.718
_diffrn_reflns_theta_max         27.529
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        26.978
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              -17
_reflns_limit_k_max              17
_reflns_limit_l_min              0
_reflns_limit_l_max              26

_oxford_diffrn_Wilson_B_factor   3.42
_oxford_diffrn_Wilson_scale      12.70

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

_refine_diff_density_min         -1.55
_refine_diff_density_max         1.12


# 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         14574
_refine_ls_number_restraints     247
_refine_ls_number_parameters     586
_oxford_refine_ls_R_factor_ref   0.0706
_refine_ls_wR_factor_ref         0.1320
_refine_ls_goodness_of_fit_ref   0.9776
_refine_ls_shift/su_max          0.0009927
_refine_ls_shift/su_mean         0.0001392


# The values computed from all data 
_oxford_reflns_number_all        14574
_refine_ls_R_factor_all          0.0706
_refine_ls_wR_factor_all         0.1320

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10760
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_gt          0.1182

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 3.99P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.8676(3) 0.6405(3) 0.78805(18) 0.0337 1.0000 Uani . . . . . .
B2 B 0.4763(3) 0.8812(3) 0.71464(19) 0.0348 1.0000 Uani . . . . . .
Br1 Br 0.94353(3) 0.72142(3) 0.733658(19) 0.0462 1.0000 Uani . . . . . .
Br2 Br 0.51707(4) 0.75872(3) 0.74894(2) 0.0537 1.0000 Uani . . . . . .
Br3 Br 0.31874(4) 0.81520(3) 0.422581(19) 0.0558 1.0000 Uani . . . . . .
Br4 Br 0.85472(3) 0.63165(3) 1.08431(2) 0.0500 1.0000 Uani . . . . . .
Cl1 Cl 0.49443(19) 0.50440(13) 0.89742(10) 0.1136 1.0000 Uani D . . . . .
Cl2 Cl 0.47422(12) 0.28773(11) 0.85046(7) 0.0811 1.0000 Uani D . . . . .
P1 P 0.92015(7) 0.65669(6) 0.88553(4) 0.0321 1.0000 Uani D . . . . .
P2 P 0.86627(7) 0.49482(6) 0.75711(4) 0.0292 1.0000 Uani D . . . . .
P3 P 0.31947(7) 0.87570(6) 0.66470(4) 0.0308 1.0000 Uani D . . . . .
P4 P 0.56380(7) 0.93497(6) 0.65655(4) 0.0314 1.0000 Uani D . . . . .
C1 C 0.8589(3) 0.5359(2) 0.89379(17) 0.0359 1.0000 Uani D . . . . .
C2 C 0.8865(3) 0.4530(2) 0.83677(16) 0.0324 1.0000 Uani D . . . . .
C3 C 0.3386(3) 0.9410(2) 0.59785(16) 0.0344 1.0000 Uani D . . . . .
C4 C 0.4530(3) 1.0057(2) 0.61873(18) 0.0368 1.0000 Uani D . . . . .
C11 C 1.0755(3) 0.6599(3) 0.91655(17) 0.0366 1.0000 Uani D . . . . .
C12 C 1.1484(3) 0.7355(4) 0.8930(2) 0.0610 1.0000 Uani D . . . . .
C13 C 1.2760(4) 0.7232(4) 0.9136(2) 0.0695 1.0000 Uani D . . . . .
C14 C 1.3087(4) 0.7345(4) 0.9902(2) 0.0607 1.0000 Uani D . . . . .
C15 C 1.2353(3) 0.6605(3) 1.0141(2) 0.0529 1.0000 Uani D . . . . .
C16 C 1.1071(3) 0.6724(3) 0.99353(18) 0.0445 1.0000 Uani D . . . . .
C21 C 0.8538(3) 0.7572(3) 0.93584(17) 0.0401 1.0000 Uani D . . . . .
C22 C 0.7236(4) 0.7363(3) 0.9253(2) 0.0560 1.0000 Uani D . . . . .
C23 C 0.6688(4) 0.8220(4) 0.9664(3) 0.0729 1.0000 Uani D . . . . .
C24 C 0.7016(6) 0.9226(4) 0.9525(3) 0.0963 1.0000 Uani D . . . . .
C25 C 0.8317(6) 0.9428(3) 0.9641(3) 0.0852 1.0000 Uani D . . . . .
C26 C 0.8851(5) 0.8591(3) 0.9204(2) 0.0640 1.0000 Uani D . . . . .
C31 C 0.9796(3) 0.4484(3) 0.71113(17) 0.0358 1.0000 Uani D . . . . .
C32 C 1.0992(3) 0.4953(3) 0.7488(2) 0.0423 1.0000 Uani D . . . . .
C33 C 1.1914(3) 0.4594(3) 0.7086(2) 0.0556 1.0000 Uani D . . . . .
C34 C 1.1909(3) 0.3465(3) 0.6942(2) 0.0549 1.0000 Uani D . . . . .
C35 C 1.0728(4) 0.2971(4) 0.6584(2) 0.0605 1.0000 Uani D . . . . .
C36 C 0.9777(3) 0.3334(3) 0.6968(2) 0.0475 1.0000 Uani D . . . . .
C41 C 0.7265(3) 0.4433(2) 0.70561(16) 0.0314 1.0000 Uani D . . . . .
C42 C 0.6304(3) 0.4485(3) 0.74740(17) 0.0374 1.0000 Uani D . . . . .
C43 C 0.5162(3) 0.4038(3) 0.70288(19) 0.0436 1.0000 Uani D . . . . .
C44 C 0.4841(3) 0.4575(3) 0.64564(19) 0.0446 1.0000 Uani D . . . . .
C45 C 0.5775(3) 0.4556(3) 0.60351(18) 0.0426 1.0000 Uani D . . . . .
C46 C 0.6954(3) 0.4979(3) 0.64732(17) 0.0377 1.0000 Uani D . . . . .
C51 C 0.2477(3) 0.7509(2) 0.62562(16) 0.0339 1.0000 Uani D . . . . .
C52 C 0.1269(3) 0.7562(3) 0.5857(2) 0.0452 1.0000 Uani D . . . . .
C53 C 0.0700(3) 0.6513(3) 0.5522(2) 0.0545 1.0000 Uani D . . . . .
C54 C 0.1433(3) 0.5921(3) 0.5073(2) 0.0511 1.0000 Uani D . . . . .
C55 C 0.2615(3) 0.5844(2) 0.54731(18) 0.0407 1.0000 Uani D . . . . .
C56 C 0.3209(3) 0.6881(2) 0.58040(17) 0.0365 1.0000 Uani D . . . . .
C61 C 0.2292(3) 0.9461(2) 0.71878(17) 0.0349 1.0000 Uani D . . . . .
C62 C 0.2348(4) 0.9070(3) 0.78441(19) 0.0463 1.0000 Uani D . . . . .
C63 C 0.1601(4) 0.9647(3) 0.8298(2) 0.0589 1.0000 Uani D . . . . .
C64 C 0.1896(4) 1.0770(3) 0.8443(2) 0.0536 1.0000 Uani D . . . . .
C65 C 0.1855(4) 1.1153(3) 0.7805(2) 0.0463 1.0000 Uani D . . . . .
C66 C 0.2626(3) 1.0598(2) 0.73535(18) 0.0393 1.0000 Uani D . . . . .
C71 C 0.6049(3) 0.8459(2) 0.58647(17) 0.0362 1.0000 Uani D . . . . .
C72 C 0.6818(5) 0.7684(3) 0.6083(2) 0.0657 1.0000 Uani D . . . . .
C73 C 0.7057(5) 0.6925(3) 0.5474(2) 0.0642 1.0000 Uani D . . . . .
C74 C 0.7578(3) 0.7423(3) 0.5000(2) 0.0476 1.0000 Uani D . . . . .
C75 C 0.6804(5) 0.8193(3) 0.4776(2) 0.0636 1.0000 Uani D . . . . .
C76 C 0.6574(5) 0.8964(3) 0.5382(2) 0.0647 1.0000 Uani D . . . . .
C81 C 0.6849(3) 1.0220(2) 0.70504(17) 0.0370 1.0000 Uani D . . . . .
C82 C 0.7595(3) 0.9729(3) 0.7568(2) 0.0534 1.0000 Uani D . . . . .
C83 C 0.8617(4) 1.0462(3) 0.7973(2) 0.0626 1.0000 Uani D . . . . .
C84 C 0.8229(4) 1.1441(3) 0.8326(2) 0.0585 1.0000 Uani D . . . . .
C85 C 0.7457(4) 1.1912(3) 0.7828(2) 0.0532 1.0000 Uani D . . . . .
C86 C 0.6450(3) 1.1198(3) 0.7420(2) 0.0444 1.0000 Uani D . . . . .
C100 C 0.4411(5) 0.3898(5) 0.9085(3) 0.0860 1.0000 Uani D . . . . .
H1 H 0.7761 0.6576 0.7814 0.0406 1.0000 Uiso R . . . . .
H2 H 0.4818 0.9420 0.7605 0.0421 1.0000 Uiso R . . . . .
H11 H 0.8915 0.5233 0.9365 0.0432 1.0000 Uiso DR . . . . .
H12 H 0.7779 0.5369 0.8902 0.0432 1.0000 Uiso DR . . . . .
H21 H 0.9641 0.4380 0.8480 0.0389 1.0000 Uiso DR . . . . .
H22 H 0.8366 0.3945 0.8318 0.0389 1.0000 Uiso DR . . . . .
H31 H 0.2772 0.9824 0.5911 0.0413 1.0000 Uiso DR . . . . .
H32 H 0.3391 0.8933 0.5570 0.0413 1.0000 Uiso DR . . . . .
H41 H 0.4448 1.0647 0.6508 0.0444 1.0000 Uiso DR . . . . .
H42 H 0.4745 1.0236 0.5800 0.0444 1.0000 Uiso DR . . . . .
H111 H 1.0976 0.5958 0.8975 0.0440 1.0000 Uiso DR . . . . .
H121 H 1.1328 0.8014 0.9131 0.0734 1.0000 Uiso DR . . . . .
H122 H 1.1293 0.7252 0.8451 0.0734 1.0000 Uiso DR . . . . .
H131 H 1.3199 0.7728 0.9002 0.0838 1.0000 Uiso DR . . . . .
H132 H 1.2923 0.6585 0.8915 0.0838 1.0000 Uiso DR . . . . .
H141 H 1.3873 0.7227 1.0014 0.0726 1.0000 Uiso DR . . . . .
H142 H 1.2973 0.8007 1.0121 0.0726 1.0000 Uiso DR . . . . .
H151 H 1.2543 0.6716 1.0620 0.0635 1.0000 Uiso DR . . . . .
H152 H 1.2507 0.5943 0.9945 0.0635 1.0000 Uiso DR . . . . .
H161 H 1.0904 0.7372 1.0151 0.0535 1.0000 Uiso DR . . . . .
H162 H 1.0633 0.6229 1.0071 0.0535 1.0000 Uiso DR . . . . .
H211 H 0.8840 0.7606 0.9823 0.0481 1.0000 Uiso DR . . . . .
H221 H 0.7066 0.6762 0.9391 0.0673 1.0000 Uiso DR . . . . .
H222 H 0.6922 0.7287 0.8786 0.0673 1.0000 Uiso DR . . . . .
H231 H 0.6935 0.8243 1.0132 0.0873 1.0000 Uiso DR . . . . .
H232 H 0.5874 0.8093 0.9551 0.0873 1.0000 Uiso DR . . . . .
H241 H 0.6711 0.9736 0.9819 0.1154 1.0000 Uiso DR . . . . .
H242 H 0.6703 0.9230 0.9068 0.1154 1.0000 Uiso DR . . . . .
H251 H 0.8626 0.9467 1.0105 0.1017 1.0000 Uiso DR . . . . .
H252 H 0.8498 1.0048 0.9527 0.1017 1.0000 Uiso DR . . . . .
H261 H 0.9664 0.8724 0.9297 0.0770 1.0000 Uiso DR . . . . .
H262 H 0.8568 0.8572 0.8740 0.0770 1.0000 Uiso DR . . . . .
H311 H 0.9659 0.4675 0.6688 0.0430 1.0000 Uiso DR . . . . .
H321 H 1.1149 0.4770 0.7914 0.0508 1.0000 Uiso DR . . . . .
H322 H 1.1002 0.5662 0.7558 0.0508 1.0000 Uiso DR . . . . .
H331 H 1.2645 0.4881 0.7337 0.0665 1.0000 Uiso DR . . . . .
H332 H 1.1775 0.4802 0.6668 0.0665 1.0000 Uiso DR . . . . .
H341 H 1.2110 0.3259 0.7359 0.0660 1.0000 Uiso DR . . . . .
H342 H 1.2458 0.3261 0.6664 0.0660 1.0000 Uiso DR . . . . .
H351 H 1.0736 0.2267 0.6538 0.0726 1.0000 Uiso DR . . . . .
H352 H 1.0568 0.3120 0.6147 0.0726 1.0000 Uiso DR . . . . .
H361 H 0.9887 0.3125 0.7385 0.0571 1.0000 Uiso DR . . . . .
H362 H 0.9052 0.3052 0.6704 0.0571 1.0000 Uiso DR . . . . .
H411 H 0.7324 0.3747 0.6862 0.0377 1.0000 Uiso DR . . . . .
H421 H 0.6493 0.4120 0.7818 0.0450 1.0000 Uiso DR . . . . .
H422 H 0.6238 0.5165 0.7676 0.0450 1.0000 Uiso DR . . . . .
H431 H 0.4579 0.4098 0.7297 0.0524 1.0000 Uiso DR . . . . .
H432 H 0.5220 0.3350 0.6842 0.0524 1.0000 Uiso DR . . . . .
H441 H 0.4730 0.5253 0.6643 0.0535 1.0000 Uiso DR . . . . .
H442 H 0.4146 0.4256 0.6174 0.0535 1.0000 Uiso DR . . . . .
H451 H 0.5576 0.4949 0.5708 0.0512 1.0000 Uiso DR . . . . .
H452 H 0.5829 0.3883 0.5811 0.0512 1.0000 Uiso DR . . . . .
H461 H 0.6927 0.5672 0.6658 0.0454 1.0000 Uiso DR . . . . .
H462 H 0.7526 0.4893 0.6198 0.0454 1.0000 Uiso DR . . . . .
H511 H 0.2393 0.7179 0.6611 0.0408 1.0000 Uiso DR . . . . .
H521 H 0.0809 0.7894 0.6158 0.0544 1.0000 Uiso DR . . . . .
H522 H 0.1327 0.7928 0.5518 0.0544 1.0000 Uiso DR . . . . .
H531 H 0.0586 0.6167 0.5864 0.0653 1.0000 Uiso DR . . . . .
H532 H -0.0023 0.6571 0.5255 0.0653 1.0000 Uiso DR . . . . .
H541 H 0.1516 0.6248 0.4717 0.0614 1.0000 Uiso DR . . . . .
H542 H 0.1067 0.5266 0.4888 0.0614 1.0000 Uiso DR . . . . .
H551 H 0.2535 0.5487 0.5815 0.0489 1.0000 Uiso DR . . . . .
H552 H 0.3070 0.5493 0.5176 0.0489 1.0000 Uiso DR . . . . .
H561 H 0.3926 0.6811 0.6072 0.0438 1.0000 Uiso DR . . . . .
H562 H 0.3338 0.7218 0.5460 0.0438 1.0000 Uiso DR . . . . .
H611 H 0.1519 0.9347 0.6950 0.0419 1.0000 Uiso DR . . . . .
H621 H 0.3122 0.9151 0.8079 0.0556 1.0000 Uiso DR . . . . .
H622 H 0.2083 0.8379 0.7731 0.0556 1.0000 Uiso DR . . . . .
H631 H 0.1709 0.9435 0.8714 0.0712 1.0000 Uiso DR . . . . .
H632 H 0.0818 0.9504 0.8080 0.0712 1.0000 Uiso DR . . . . .
H641 H 0.1361 1.1097 0.8692 0.0645 1.0000 Uiso DR . . . . .
H642 H 0.2650 1.0921 0.8705 0.0645 1.0000 Uiso DR . . . . .
H651 H 0.2105 1.1847 0.7922 0.0555 1.0000 Uiso DR . . . . .
H652 H 0.1085 1.1061 0.7563 0.0555 1.0000 Uiso DR . . . . .
H661 H 0.3404 1.0727 0.7581 0.0473 1.0000 Uiso DR . . . . .
H662 H 0.2543 1.0829 0.6944 0.0473 1.0000 Uiso DR . . . . .
H711 H 0.5355 0.8097 0.5609 0.0435 1.0000 Uiso DR . . . . .
H721 H 0.7528 0.8015 0.6337 0.0791 1.0000 Uiso DR . . . . .
H722 H 0.6451 0.7340 0.6357 0.0791 1.0000 Uiso DR . . . . .
H731 H 0.7572 0.6476 0.5630 0.0771 1.0000 Uiso DR . . . . .
H732 H 0.6352 0.6562 0.5237 0.0771 1.0000 Uiso DR . . . . .
H741 H 0.8309 0.7748 0.5225 0.0571 1.0000 Uiso DR . . . . .
H742 H 0.7668 0.6932 0.4615 0.0571 1.0000 Uiso DR . . . . .
H751 H 0.7165 0.8529 0.4495 0.0766 1.0000 Uiso DR . . . . .
H752 H 0.6091 0.7859 0.4527 0.0766 1.0000 Uiso DR . . . . .
H761 H 0.7280 0.9327 0.5616 0.0777 1.0000 Uiso DR . . . . .
H762 H 0.6058 0.9413 0.5226 0.0777 1.0000 Uiso DR . . . . .
H811 H 0.7311 1.0376 0.6745 0.0445 1.0000 Uiso DR . . . . .
H821 H 0.7138 0.9552 0.7870 0.0641 1.0000 Uiso DR . . . . .
H822 H 0.7878 0.9144 0.7333 0.0641 1.0000 Uiso DR . . . . .
H831 H 0.9036 1.0160 0.8305 0.0750 1.0000 Uiso DR . . . . .
H832 H 0.9101 1.0598 0.7673 0.0750 1.0000 Uiso DR . . . . .
H841 H 0.8886 1.1892 0.8534 0.0703 1.0000 Uiso DR . . . . .
H842 H 0.7815 1.1318 0.8662 0.0703 1.0000 Uiso DR . . . . .
H851 H 0.7169 1.2487 0.8072 0.0639 1.0000 Uiso DR . . . . .
H852 H 0.7900 1.2109 0.7525 0.0639 1.0000 Uiso DR . . . . .
H861 H 0.5968 1.1047 0.7718 0.0532 1.0000 Uiso DR . . . . .
H862 H 0.6028 1.1511 0.7096 0.0532 1.0000 Uiso DR . . . . .
H1001 H 0.4729 0.3830 0.9529 0.1029 1.0000 Uiso DR . . . . .
H1002 H 0.3598 0.3892 0.9037 0.1029 1.0000 Uiso DR . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3598(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
B1 . Br1 . 2.013(4) yes
B1 . P1 . 1.955(4) yes
B1 . P2 . 1.960(4) yes
B1 . H1 . 1.110 no
B2 . Br2 . 1.997(4) yes
B2 . P3 . 1.952(4) yes
B2 . P4 . 1.938(4) yes
B2 . H2 . 1.110 no
Cl1 . C100 . 1.738(6) yes
Cl2 . C100 . 1.743(6) yes
P1 . C1 . 1.828(3) yes
P1 . C11 . 1.835(3) yes
P1 . C21 . 1.831(4) yes
P2 . C2 . 1.826(3) yes
P2 . C31 . 1.829(3) yes
P2 . C41 . 1.827(3) yes
P3 . C3 . 1.827(3) yes
P3 . C51 . 1.830(3) yes
P3 . C61 . 1.830(3) yes
P4 . C4 . 1.828(3) yes
P4 . C71 . 1.830(3) yes
P4 . C81 . 1.825(3) yes
C1 . C2 . 1.540(5) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C2 . H21 . 0.950 no
C2 . H22 . 0.950 no
C3 . C4 . 1.529(5) yes
C3 . H31 . 0.950 no
C3 . H32 . 0.950 no
C4 . H41 . 0.950 no
C4 . H42 . 0.950 no
C11 . C12 . 1.523(5) yes
C11 . C16 . 1.532(5) yes
C11 . H111 . 0.950 no
C12 . C13 . 1.524(6) yes
C12 . H121 . 0.950 no
C12 . H122 . 0.950 no
C13 . C14 . 1.528(6) yes
C13 . H131 . 0.950 no
C13 . H132 . 0.950 no
C14 . C15 . 1.516(6) yes
C14 . H141 . 0.950 no
C14 . H142 . 0.950 no
C15 . C16 . 1.529(5) yes
C15 . H151 . 0.950 no
C15 . H152 . 0.950 no
C16 . H161 . 0.950 no
C16 . H162 . 0.950 no
C21 . C22 . 1.524(5) yes
C21 . C26 . 1.538(5) yes
C21 . H211 . 0.950 no
C22 . C23 . 1.532(6) yes
C22 . H221 . 0.950 no
C22 . H222 . 0.950 no
C23 . C24 . 1.511(8) yes
C23 . H231 . 0.950 no
C23 . H232 . 0.950 no
C24 . C25 . 1.521(9) yes
C24 . H241 . 0.950 no
C24 . H242 . 0.950 no
C25 . C26 . 1.530(6) yes
C25 . H251 . 0.950 no
C25 . H252 . 0.950 no
C26 . H261 . 0.950 no
C26 . H262 . 0.950 no
C31 . C32 . 1.534(5) yes
C31 . C36 . 1.537(5) yes
C31 . H311 . 0.950 no
C32 . C33 . 1.516(5) yes
C32 . H321 . 0.950 no
C32 . H322 . 0.950 no
C33 . C34 . 1.511(6) yes
C33 . H331 . 0.950 no
C33 . H332 . 0.950 no
C34 . C35 . 1.520(6) yes
C34 . H341 . 0.950 no
C34 . H342 . 0.950 no
C35 . C36 . 1.524(5) yes
C35 . H351 . 0.950 no
C35 . H352 . 0.950 no
C36 . H361 . 0.950 no
C36 . H362 . 0.950 no
C41 . C42 . 1.532(5) yes
C41 . C46 . 1.541(4) yes
C41 . H411 . 0.950 no
C42 . C43 . 1.520(5) yes
C42 . H421 . 0.950 no
C42 . H422 . 0.950 no
C43 . C44 . 1.517(5) yes
C43 . H431 . 0.950 no
C43 . H432 . 0.950 no
C44 . C45 . 1.513(5) yes
C44 . H441 . 0.950 no
C44 . H442 . 0.950 no
C45 . C46 . 1.540(5) yes
C45 . H451 . 0.950 no
C45 . H452 . 0.950 no
C46 . H461 . 0.950 no
C46 . H462 . 0.950 no
C51 . C52 . 1.534(5) yes
C51 . C56 . 1.536(5) yes
C51 . H511 . 0.950 no
C52 . C53 . 1.527(5) yes
C52 . H521 . 0.950 no
C52 . H522 . 0.950 no
C53 . C54 . 1.510(6) yes
C53 . H531 . 0.950 no
C53 . H532 . 0.950 no
C54 . C55 . 1.516(5) yes
C54 . H541 . 0.950 no
C54 . H542 . 0.950 no
C55 . C56 . 1.523(5) yes
C55 . H551 . 0.950 no
C55 . H552 . 0.950 no
C56 . H561 . 0.950 no
C56 . H562 . 0.950 no
C61 . C62 . 1.544(5) yes
C61 . C66 . 1.540(4) yes
C61 . H611 . 0.950 no
C62 . C63 . 1.518(5) yes
C62 . H621 . 0.950 no
C62 . H622 . 0.950 no
C63 . C64 . 1.516(5) yes
C63 . H631 . 0.950 no
C63 . H632 . 0.950 no
C64 . C65 . 1.505(5) yes
C64 . H641 . 0.950 no
C64 . H642 . 0.950 no
C65 . C66 . 1.524(5) yes
C65 . H651 . 0.950 no
C65 . H652 . 0.950 no
C66 . H661 . 0.950 no
C66 . H662 . 0.950 no
C71 . C72 . 1.516(5) yes
C71 . C76 . 1.518(5) yes
C71 . H711 . 0.950 no
C72 . C73 . 1.524(6) yes
C72 . H721 . 0.950 no
C72 . H722 . 0.950 no
C73 . C74 . 1.494(6) yes
C73 . H731 . 0.950 no
C73 . H732 . 0.950 no
C74 . C75 . 1.519(5) yes
C74 . H741 . 0.950 no
C74 . H742 . 0.950 no
C75 . C76 . 1.525(6) yes
C75 . H751 . 0.950 no
C75 . H752 . 0.950 no
C76 . H761 . 0.950 no
C76 . H762 . 0.950 no
C81 . C82 . 1.547(5) yes
C81 . C86 . 1.531(5) yes
C81 . H811 . 0.950 no
C82 . C83 . 1.536(5) yes
C82 . H821 . 0.950 no
C82 . H822 . 0.950 no
C83 . C84 . 1.514(6) yes
C83 . H831 . 0.950 no
C83 . H832 . 0.950 no
C84 . C85 . 1.519(6) yes
C84 . H841 . 0.950 no
C84 . H842 . 0.950 no
C85 . C86 . 1.513(5) yes
C85 . H851 . 0.950 no
C85 . H852 . 0.950 no
C86 . H861 . 0.950 no
C86 . H862 . 0.950 no
C100 . H1001 . 0.950 no
C100 . H1002 . 0.950 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
Br1 . B1 . P1 . 121.75(19) yes
Br1 . B1 . P2 . 114.84(19) yes
P1 . B1 . P2 . 101.01(16) yes
Br1 . B1 . H1 . 106.0 no
P1 . B1 . H1 . 106.0 no
P2 . B1 . H1 . 106.0 no
Br2 . B2 . P3 . 115.36(19) yes
Br2 . B2 . P4 . 122.3(2) yes
P3 . B2 . P4 . 101.37(17) yes
Br2 . B2 . H2 . 105.5 no
P3 . B2 . H2 . 105.5 no
P4 . B2 . H2 . 105.5 no
B1 . P1 . C1 . 97.86(15) yes
B1 . P1 . C11 . 117.68(16) yes
C1 . P1 . C11 . 105.86(15) yes
B1 . P1 . C21 . 112.85(16) yes
C1 . P1 . C21 . 108.89(16) yes
C11 . P1 . C21 . 112.12(16) yes
B1 . P2 . C2 . 102.20(15) yes
B1 . P2 . C31 . 116.97(16) yes
C2 . P2 . C31 . 108.33(15) yes
B1 . P2 . C41 . 110.29(15) yes
C2 . P2 . C41 . 109.94(14) yes
C31 . P2 . C41 . 108.83(15) yes
B2 . P3 . C3 . 102.48(15) yes
B2 . P3 . C51 . 116.69(16) yes
C3 . P3 . C51 . 108.75(15) yes
B2 . P3 . C61 . 110.24(16) yes
C3 . P3 . C61 . 109.14(15) yes
C51 . P3 . C61 . 109.18(15) yes
B2 . P4 . C4 . 98.32(16) yes
B2 . P4 . C71 . 117.37(16) yes
C4 . P4 . C71 . 106.58(16) yes
B2 . P4 . C81 . 112.09(16) yes
C4 . P4 . C81 . 109.04(16) yes
C71 . P4 . C81 . 112.10(16) yes
P1 . C1 . C2 . 108.9(2) yes
P1 . C1 . H11 . 109.6 no
C2 . C1 . H11 . 109.6 no
P1 . C1 . H12 . 109.6 no
C2 . C1 . H12 . 109.6 no
H11 . C1 . H12 . 109.5 no
C1 . C2 . P2 . 110.0(2) yes
C1 . C2 . H21 . 109.3 no
P2 . C2 . H21 . 109.3 no
C1 . C2 . H22 . 109.3 no
P2 . C2 . H22 . 109.3 no
H21 . C2 . H22 . 109.5 no
P3 . C3 . C4 . 109.3(2) yes
P3 . C3 . H31 . 109.5 no
C4 . C3 . H31 . 109.5 no
P3 . C3 . H32 . 109.5 no
C4 . C3 . H32 . 109.5 no
H31 . C3 . H32 . 109.5 no
C3 . C4 . P4 . 109.3(2) yes
C3 . C4 . H41 . 109.5 no
P4 . C4 . H41 . 109.5 no
C3 . C4 . H42 . 109.5 no
P4 . C4 . H42 . 109.5 no
H41 . C4 . H42 . 109.5 no
P1 . C11 . C12 . 114.5(2) yes
P1 . C11 . C16 . 113.3(2) yes
C12 . C11 . C16 . 110.4(3) yes
P1 . C11 . H111 . 105.9 no
C12 . C11 . H111 . 105.9 no
C16 . C11 . H111 . 105.9 no
C11 . C12 . C13 . 110.6(3) yes
C11 . C12 . H121 . 109.2 no
C13 . C12 . H121 . 109.2 no
C11 . C12 . H122 . 109.2 no
C13 . C12 . H122 . 109.2 no
H121 . C12 . H122 . 109.5 no
C12 . C13 . C14 . 110.7(4) yes
C12 . C13 . H131 . 109.2 no
C14 . C13 . H131 . 109.1 no
C12 . C13 . H132 . 109.1 no
C14 . C13 . H132 . 109.2 no
H131 . C13 . H132 . 109.5 no
C13 . C14 . C15 . 110.8(3) yes
C13 . C14 . H141 . 109.2 no
C15 . C14 . H141 . 109.2 no
C13 . C14 . H142 . 109.2 no
C15 . C14 . H142 . 109.1 no
H141 . C14 . H142 . 109.5 no
C14 . C15 . C16 . 111.3(3) yes
C14 . C15 . H151 . 109.0 no
C16 . C15 . H151 . 109.0 no
C14 . C15 . H152 . 109.0 no
C16 . C15 . H152 . 109.0 no
H151 . C15 . H152 . 109.5 no
C11 . C16 . C15 . 110.0(3) yes
C11 . C16 . H161 . 109.3 no
C15 . C16 . H161 . 109.4 no
C11 . C16 . H162 . 109.3 no
C15 . C16 . H162 . 109.3 no
H161 . C16 . H162 . 109.5 no
P1 . C21 . C22 . 112.0(3) yes
P1 . C21 . C26 . 111.0(3) yes
C22 . C21 . C26 . 110.6(3) yes
P1 . C21 . H211 . 107.7 no
C22 . C21 . H211 . 107.7 no
C26 . C21 . H211 . 107.7 no
C21 . C22 . C23 . 111.5(4) yes
C21 . C22 . H221 . 109.0 no
C23 . C22 . H221 . 109.0 no
C21 . C22 . H222 . 109.0 no
C23 . C22 . H222 . 109.0 no
H221 . C22 . H222 . 109.5 no
C22 . C23 . C24 . 112.3(4) yes
C22 . C23 . H231 . 108.7 no
C24 . C23 . H231 . 108.8 no
C22 . C23 . H232 . 108.8 no
C24 . C23 . H232 . 108.7 no
H231 . C23 . H232 . 109.5 no
C23 . C24 . C25 . 110.9(4) yes
C23 . C24 . H241 . 109.1 no
C25 . C24 . H241 . 109.1 no
C23 . C24 . H242 . 109.1 no
C25 . C24 . H242 . 109.2 no
H241 . C24 . H242 . 109.5 no
C24 . C25 . C26 . 110.9(5) yes
C24 . C25 . H251 . 109.2 no
C26 . C25 . H251 . 109.1 no
C24 . C25 . H252 . 109.1 no
C26 . C25 . H252 . 109.2 no
H251 . C25 . H252 . 109.5 no
C21 . C26 . C25 . 110.5(4) yes
C21 . C26 . H261 . 109.3 no
C25 . C26 . H261 . 109.2 no
C21 . C26 . H262 . 109.2 no
C25 . C26 . H262 . 109.2 no
H261 . C26 . H262 . 109.5 no
P2 . C31 . C32 . 111.8(2) yes
P2 . C31 . C36 . 112.0(2) yes
C32 . C31 . C36 . 109.9(3) yes
P2 . C31 . H311 . 107.7 no
C32 . C31 . H311 . 107.6 no
C36 . C31 . H311 . 107.7 no
C31 . C32 . C33 . 111.0(3) yes
C31 . C32 . H321 . 109.1 no
C33 . C32 . H321 . 109.1 no
C31 . C32 . H322 . 109.1 no
C33 . C32 . H322 . 109.1 no
H321 . C32 . H322 . 109.5 no
C32 . C33 . C34 . 111.2(3) yes
C32 . C33 . H331 . 109.1 no
C34 . C33 . H331 . 109.1 no
C32 . C33 . H332 . 109.0 no
C34 . C33 . H332 . 109.0 no
H331 . C33 . H332 . 109.5 no
C33 . C34 . C35 . 111.0(3) yes
C33 . C34 . H341 . 109.1 no
C35 . C34 . H341 . 109.1 no
C33 . C34 . H342 . 109.1 no
C35 . C34 . H342 . 109.1 no
H341 . C34 . H342 . 109.5 no
C34 . C35 . C36 . 112.5(4) yes
C34 . C35 . H351 . 108.8 no
C36 . C35 . H351 . 108.6 no
C34 . C35 . H352 . 108.7 no
C36 . C35 . H352 . 108.7 no
H351 . C35 . H352 . 109.5 no
C31 . C36 . C35 . 110.7(3) yes
C31 . C36 . H361 . 109.1 no
C35 . C36 . H361 . 109.2 no
C31 . C36 . H362 . 109.1 no
C35 . C36 . H362 . 109.2 no
H361 . C36 . H362 . 109.5 no
P2 . C41 . C42 . 112.5(2) yes
P2 . C41 . C46 . 110.3(2) yes
C42 . C41 . C46 . 110.1(3) yes
P2 . C41 . H411 . 107.9 no
C42 . C41 . H411 . 107.9 no
C46 . C41 . H411 . 107.9 no
C41 . C42 . C43 . 110.8(3) yes
C41 . C42 . H421 . 109.1 no
C43 . C42 . H421 . 109.2 no
C41 . C42 . H422 . 109.1 no
C43 . C42 . H422 . 109.2 no
H421 . C42 . H422 . 109.5 no
C42 . C43 . C44 . 111.2(3) yes
C42 . C43 . H431 . 109.0 no
C44 . C43 . H431 . 109.0 no
C42 . C43 . H432 . 109.1 no
C44 . C43 . H432 . 109.0 no
H431 . C43 . H432 . 109.5 no
C43 . C44 . C45 . 111.3(3) yes
C43 . C44 . H441 . 109.0 no
C45 . C44 . H441 . 109.0 no
C43 . C44 . H442 . 109.1 no
C45 . C44 . H442 . 109.1 no
H441 . C44 . H442 . 109.5 no
C44 . C45 . C46 . 111.8(3) yes
C44 . C45 . H451 . 108.9 no
C46 . C45 . H451 . 108.9 no
C44 . C45 . H452 . 108.8 no
C46 . C45 . H452 . 108.9 no
H451 . C45 . H452 . 109.5 no
C45 . C46 . C41 . 111.0(3) yes
C45 . C46 . H461 . 109.1 no
C41 . C46 . H461 . 109.1 no
C45 . C46 . H462 . 109.1 no
C41 . C46 . H462 . 109.1 no
H461 . C46 . H462 . 109.5 no
P3 . C51 . C52 . 112.0(2) yes
P3 . C51 . C56 . 111.2(2) yes
C52 . C51 . C56 . 110.8(3) yes
P3 . C51 . H511 . 107.6 no
C52 . C51 . H511 . 107.6 no
C56 . C51 . H511 . 107.5 no
C51 . C52 . C53 . 111.0(3) yes
C51 . C52 . H521 . 109.1 no
C53 . C52 . H521 . 109.1 no
C51 . C52 . H522 . 109.1 no
C53 . C52 . H522 . 109.1 no
H521 . C52 . H522 . 109.5 no
C52 . C53 . C54 . 111.5(3) yes
C52 . C53 . H531 . 109.0 no
C54 . C53 . H531 . 108.9 no
C52 . C53 . H532 . 109.0 no
C54 . C53 . H532 . 109.0 no
H531 . C53 . H532 . 109.5 no
C53 . C54 . C55 . 110.8(3) yes
C53 . C54 . H541 . 109.1 no
C55 . C54 . H541 . 109.1 no
C53 . C54 . H542 . 109.2 no
C55 . C54 . H542 . 109.2 no
H541 . C54 . H542 . 109.5 no
C54 . C55 . C56 . 110.7(3) yes
C54 . C55 . H551 . 109.1 no
C56 . C55 . H551 . 109.1 no
C54 . C55 . H552 . 109.2 no
C56 . C55 . H552 . 109.2 no
H551 . C55 . H552 . 109.5 no
C51 . C56 . C55 . 111.6(3) yes
C51 . C56 . H561 . 109.0 no
C55 . C56 . H561 . 109.0 no
C51 . C56 . H562 . 108.9 no
C55 . C56 . H562 . 108.9 no
H561 . C56 . H562 . 109.5 no
P3 . C61 . C62 . 110.0(2) yes
P3 . C61 . C66 . 112.3(2) yes
C62 . C61 . C66 . 110.7(3) yes
P3 . C61 . H611 . 107.9 no
C62 . C61 . H611 . 107.9 no
C66 . C61 . H611 . 107.9 no
C61 . C62 . C63 . 110.6(3) yes
C61 . C62 . H621 . 109.2 no
C63 . C62 . H621 . 109.1 no
C61 . C62 . H622 . 109.2 no
C63 . C62 . H622 . 109.2 no
H621 . C62 . H622 . 109.5 no
C62 . C63 . C64 . 112.3(3) yes
C62 . C63 . H631 . 108.8 no
C64 . C63 . H631 . 108.8 no
C62 . C63 . H632 . 108.8 no
C64 . C63 . H632 . 108.7 no
H631 . C63 . H632 . 109.5 no
C63 . C64 . C65 . 112.2(3) yes
C63 . C64 . H641 . 108.8 no
C65 . C64 . H641 . 108.8 no
C63 . C64 . H642 . 108.7 no
C65 . C64 . H642 . 108.8 no
H641 . C64 . H642 . 109.5 no
C64 . C65 . C66 . 111.4(3) yes
C64 . C65 . H651 . 109.0 no
C66 . C65 . H651 . 109.0 no
C64 . C65 . H652 . 108.9 no
C66 . C65 . H652 . 109.0 no
H651 . C65 . H652 . 109.5 no
C61 . C66 . C65 . 110.5(3) yes
C61 . C66 . H661 . 109.2 no
C65 . C66 . H661 . 109.3 no
C61 . C66 . H662 . 109.2 no
C65 . C66 . H662 . 109.2 no
H661 . C66 . H662 . 109.5 no
P4 . C71 . C72 . 114.3(3) yes
P4 . C71 . C76 . 113.2(2) yes
C72 . C71 . C76 . 110.0(3) yes
P4 . C71 . H711 . 106.2 no
C72 . C71 . H711 . 106.2 no
C76 . C71 . H711 . 106.2 no
C71 . C72 . C73 . 111.5(3) yes
C71 . C72 . H721 . 108.9 no
C73 . C72 . H721 . 108.9 no
C71 . C72 . H722 . 109.0 no
C73 . C72 . H722 . 109.0 no
H721 . C72 . H722 . 109.5 no
C72 . C73 . C74 . 111.8(3) yes
C72 . C73 . H731 . 108.9 no
C74 . C73 . H731 . 108.9 no
C72 . C73 . H732 . 108.8 no
C74 . C73 . H732 . 108.9 no
H731 . C73 . H732 . 109.5 no
C73 . C74 . C75 . 110.0(3) yes
C73 . C74 . H741 . 109.3 no
C75 . C74 . H741 . 109.3 no
C73 . C74 . H742 . 109.4 no
C75 . C74 . H742 . 109.4 no
H741 . C74 . H742 . 109.5 no
C74 . C75 . C76 . 111.3(3) yes
C74 . C75 . H751 . 109.1 no
C76 . C75 . H751 . 109.1 no
C74 . C75 . H752 . 109.0 no
C76 . C75 . H752 . 108.9 no
H751 . C75 . H752 . 109.5 no
C75 . C76 . C71 . 111.1(3) yes
C75 . C76 . H761 . 109.0 no
C71 . C76 . H761 . 109.1 no
C75 . C76 . H762 . 109.1 no
C71 . C76 . H762 . 109.1 no
H761 . C76 . H762 . 109.5 no
P4 . C81 . C82 . 110.5(2) yes
P4 . C81 . C86 . 111.9(2) yes
C82 . C81 . C86 . 109.6(3) yes
P4 . C81 . H811 . 108.3 no
C82 . C81 . H811 . 108.3 no
C86 . C81 . H811 . 108.2 no
C81 . C82 . C83 . 110.3(3) yes
C81 . C82 . H821 . 109.2 no
C83 . C82 . H821 . 109.3 no
C81 . C82 . H822 . 109.3 no
C83 . C82 . H822 . 109.2 no
H821 . C82 . H822 . 109.5 no
C82 . C83 . C84 . 112.0(3) yes
C82 . C83 . H831 . 108.8 no
C84 . C83 . H831 . 108.8 no
C82 . C83 . H832 . 108.9 no
C84 . C83 . H832 . 108.9 no
H831 . C83 . H832 . 109.5 no
C83 . C84 . C85 . 111.2(4) yes
C83 . C84 . H841 . 109.0 no
C85 . C84 . H841 . 109.0 no
C83 . C84 . H842 . 109.1 no
C85 . C84 . H842 . 109.0 no
H841 . C84 . H842 . 109.5 no
C84 . C85 . C86 . 112.3(3) yes
C84 . C85 . H851 . 108.8 no
C86 . C85 . H851 . 108.8 no
C84 . C85 . H852 . 108.7 no
C86 . C85 . H852 . 108.7 no
H851 . C85 . H852 . 109.5 no
C81 . C86 . C85 . 111.7(3) yes
C81 . C86 . H861 . 108.9 no
C85 . C86 . H861 . 108.9 no
C81 . C86 . H862 . 108.9 no
C85 . C86 . H862 . 108.9 no
H861 . C86 . H862 . 109.5 no
Cl2 . C100 . Cl1 . 113.2(3) yes
Cl2 . C100 . H1001 . 108.5 no
Cl1 . C100 . H1001 . 108.6 no
Cl2 . C100 . H1002 . 108.5 no
Cl1 . C100 . H1002 . 108.5 no
H1001 . C100 . H1002 . 109.5 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 29/02/12 at 12:17:02
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE B   (   1,X'S) H   (   1,X'S) 
RIDE B   (   2,X'S) H   (   2,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) H   ( 642,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,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   ( 741,X'S) H   ( 742,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) H   ( 752,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) H   ( 822,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) H   ( 832,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) H   ( 842,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) H   ( 852,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) H   ( 862,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) H   (1002,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 29/02/12 at 12:17:02
#
#LIST     16                                                                    
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            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 1) TO H(12) 
CONT C ( 1) TO H(11) 
REST 0.042, 0.002 = H(12,U[ISO]) 
REST 0.042, 0.002 = H(11,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(12) TO C ( 1) TO P(1) 
CONT H(12) TO C ( 1) TO C(2) 
CONT H(11) TO C ( 1) TO P(1) 
CONT H(11) TO C ( 1) TO C(2) 
ANGLE 109.54, 2.0 = 
CONT H(12) TO C ( 1) TO H(11) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 2) TO H(21) 
CONT C ( 2) TO H(22) 
REST 0.040, 0.002 = H(21,U[ISO]) 
REST 0.040, 0.002 = H(22,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(21) TO C ( 2) TO C(1) 
CONT H(21) TO C ( 2) TO P(2) 
CONT H(22) TO C ( 2) TO C(1) 
CONT H(22) TO C ( 2) TO P(2) 
ANGLE 109.54, 2.0 = 
CONT H(21) TO C ( 2) TO H(22) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 3) TO H(31) 
CONT C ( 3) TO H(32) 
REST 0.041, 0.002 = H(31,U[ISO]) 
REST 0.041, 0.002 = H(32,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(31) TO C ( 3) TO P(3) 
CONT H(31) TO C ( 3) TO C(4) 
CONT H(32) TO C ( 3) TO P(3) 
CONT H(32) TO C ( 3) TO C(4) 
ANGLE 109.54, 2.0 = 
CONT H(31) TO C ( 3) TO H(32) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 4) TO H(42) 
CONT C ( 4) TO H(41) 
REST 0.046, 0.002 = H(42,U[ISO]) 
REST 0.046, 0.002 = H(41,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(42) TO C ( 4) TO C(3) 
CONT H(42) TO C ( 4) TO P(4) 
CONT H(41) TO C ( 4) TO C(3) 
CONT H(41) TO C ( 4) TO P(4) 
ANGLE 109.54, 2.0 = 
CONT H(42) TO C ( 4) TO H(41) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 11) TO H(111) 
REST 0.042, 0.002 = H(111,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(111) TO C ( 11) TO P(1) 
CONT H(111) TO C ( 11) TO C(12) 
CONT H(111) TO C ( 11) TO C(16) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 12) TO H(122) 
CONT C ( 12) TO H(121) 
REST 0.078, 0.002 = H(122,U[ISO]) 
REST 0.078, 0.002 = H(121,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(122) TO C ( 12) TO C(11) 
CONT H(122) TO C ( 12) TO C(13) 
CONT H(121) TO C ( 12) TO C(11) 
CONT H(121) TO C ( 12) TO C(13) 
ANGLE 109.54, 2.0 = 
CONT H(122) TO C ( 12) TO H(121) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 13) TO H(131) 
CONT C ( 13) TO H(132) 
REST 0.091, 0.002 = H(131,U[ISO]) 
REST 0.091, 0.002 = H(132,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(131) TO C ( 13) TO C(12) 
CONT H(131) TO C ( 13) TO C(14) 
CONT H(132) TO C ( 13) TO C(12) 
CONT H(132) TO C ( 13) TO C(14) 
ANGLE 109.54, 2.0 = 
CONT H(131) TO C ( 13) TO H(132) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 14) TO H(141) 
CONT C ( 14) TO H(142) 
REST 0.072, 0.002 = H(141,U[ISO]) 
REST 0.072, 0.002 = H(142,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(141) TO C ( 14) TO C(13) 
CONT H(141) TO C ( 14) TO C(15) 
CONT H(142) TO C ( 14) TO C(13) 
CONT H(142) TO C ( 14) TO C(15) 
ANGLE 109.54, 2.0 = 
CONT H(141) TO C ( 14) TO H(142) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 15) TO H(152) 
CONT C ( 15) TO H(151) 
REST 0.064, 0.002 = H(152,U[ISO]) 
REST 0.064, 0.002 = H(151,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(152) TO C ( 15) TO C(14) 
CONT H(152) TO C ( 15) TO C(16) 
CONT H(151) TO C ( 15) TO C(14) 
CONT H(151) TO C ( 15) TO C(16) 
ANGLE 109.54, 2.0 = 
CONT H(152) TO C ( 15) TO H(151) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 16) TO H(161) 
CONT C ( 16) TO H(162) 
REST 0.052, 0.002 = H(161,U[ISO]) 
REST 0.052, 0.002 = H(162,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(161) TO C ( 16) TO C(11) 
CONT H(161) TO C ( 16) TO C(15) 
CONT H(162) TO C ( 16) TO C(11) 
CONT H(162) TO C ( 16) TO C(15) 
ANGLE 109.54, 2.0 = 
CONT H(161) TO C ( 16) TO H(162) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 21) TO H(211) 
REST 0.047, 0.002 = H(211,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(211) TO C ( 21) TO P(1) 
CONT H(211) TO C ( 21) TO C(22) 
CONT H(211) TO C ( 21) TO C(26) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 22) TO H(221) 
CONT C ( 22) TO H(222) 
REST 0.067, 0.002 = H(221,U[ISO]) 
REST 0.067, 0.002 = H(222,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) 
CONT H(222) TO C ( 22) TO C(21) 
CONT H(222) TO C ( 22) TO C(23) 
ANGLE 109.54, 2.0 = 
CONT H(221) TO C ( 22) TO H(222) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 23) TO H(231) 
CONT C ( 23) TO H(232) 
REST 0.085, 0.002 = H(231,U[ISO]) 
REST 0.085, 0.002 = H(232,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(231) TO C ( 23) TO C(22) 
CONT H(231) TO C ( 23) TO C(24) 
CONT H(232) TO C ( 23) TO C(22) 
CONT H(232) TO C ( 23) TO C(24) 
ANGLE 109.54, 2.0 = 
CONT H(231) TO C ( 23) TO H(232) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 24) TO H(241) 
CONT C ( 24) TO H(242) 
REST 0.105, 0.002 = H(241,U[ISO]) 
REST 0.105, 0.002 = H(242,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(241) TO C ( 24) TO C(23) 
CONT H(241) TO C ( 24) TO C(25) 
CONT H(242) TO C ( 24) TO C(23) 
CONT H(242) TO C ( 24) TO C(25) 
ANGLE 109.54, 2.0 = 
CONT H(241) TO C ( 24) TO H(242) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 25) TO H(251) 
CONT C ( 25) TO H(252) 
REST 0.109, 0.002 = H(251,U[ISO]) 
REST 0.109, 0.002 = H(252,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(251) TO C ( 25) TO C(24) 
CONT H(251) TO C ( 25) TO C(26) 
CONT H(252) TO C ( 25) TO C(24) 
CONT H(252) TO C ( 25) TO C(26) 
ANGLE 109.54, 2.0 = 
CONT H(251) TO C ( 25) TO H(252) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 26) TO H(262) 
CONT C ( 26) TO H(261) 
REST 0.077, 0.002 = H(262,U[ISO]) 
REST 0.077, 0.002 = H(261,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(262) TO C ( 26) TO C(25) 
CONT H(262) TO C ( 26) TO C(21) 
CONT H(261) TO C ( 26) TO C(25) 
CONT H(261) TO C ( 26) TO C(21) 
ANGLE 109.54, 2.0 = 
CONT H(262) TO C ( 26) TO H(261) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 31) TO H(311) 
REST 0.044, 0.002 = H(311,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(311) TO C ( 31) TO P(2) 
CONT H(311) TO C ( 31) TO C(32) 
CONT H(311) TO C ( 31) TO C(36) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 32) TO H(322) 
CONT C ( 32) TO H(321) 
REST 0.050, 0.002 = H(322,U[ISO]) 
REST 0.050, 0.002 = H(321,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(322) TO C ( 32) TO C(31) 
CONT H(322) TO C ( 32) TO C(33) 
CONT H(321) TO C ( 32) TO C(31) 
CONT H(321) TO C ( 32) TO C(33) 
ANGLE 109.54, 2.0 = 
CONT H(322) TO C ( 32) TO H(321) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 33) TO H(331) 
CONT C ( 33) TO H(332) 
REST 0.064, 0.002 = H(331,U[ISO]) 
REST 0.064, 0.002 = H(332,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(331) TO C ( 33) TO C(32) 
CONT H(331) TO C ( 33) TO C(34) 
CONT H(332) TO C ( 33) TO C(32) 
CONT H(332) TO C ( 33) TO C(34) 
ANGLE 109.54, 2.0 = 
CONT H(331) TO C ( 33) TO H(332) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 34) TO H(341) 
CONT C ( 34) TO H(342) 
REST 0.067, 0.002 = H(341,U[ISO]) 
REST 0.067, 0.002 = H(342,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(341) TO C ( 34) TO C(33) 
CONT H(341) TO C ( 34) TO C(35) 
CONT H(342) TO C ( 34) TO C(33) 
CONT H(342) TO C ( 34) TO C(35) 
ANGLE 109.54, 2.0 = 
CONT H(341) TO C ( 34) TO H(342) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 35) TO H(352) 
CONT C ( 35) TO H(351) 
REST 0.074, 0.002 = H(352,U[ISO]) 
REST 0.074, 0.002 = H(351,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(352) TO C ( 35) TO C(34) 
CONT H(352) TO C ( 35) TO C(36) 
CONT H(351) TO C ( 35) TO C(34) 
CONT H(351) TO C ( 35) TO C(36) 
ANGLE 109.54, 2.0 = 
CONT H(352) TO C ( 35) TO H(351) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 36) TO H(361) 
CONT C ( 36) TO H(362) 
REST 0.060, 0.002 = H(361,U[ISO]) 
REST 0.060, 0.002 = H(362,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(361) TO C ( 36) TO C(31) 
CONT H(361) TO C ( 36) TO C(35) 
CONT H(362) TO C ( 36) TO C(31) 
CONT H(362) TO C ( 36) TO C(35) 
ANGLE 109.54, 2.0 = 
CONT H(361) TO C ( 36) TO H(362) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 41) TO H(411) 
REST 0.038, 0.002 = H(411,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(411) TO C ( 41) TO P(2) 
CONT H(411) TO C ( 41) TO C(42) 
CONT H(411) TO C ( 41) TO C(46) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 42) TO H(421) 
CONT C ( 42) TO H(422) 
REST 0.045, 0.002 = H(421,U[ISO]) 
REST 0.045, 0.002 = H(422,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) 
CONT H(422) TO C ( 42) TO C(41) 
CONT H(422) TO C ( 42) TO C(43) 
ANGLE 109.54, 2.0 = 
CONT H(421) TO C ( 42) TO H(422) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 43) TO H(431) 
CONT C ( 43) TO H(432) 
REST 0.052, 0.002 = H(431,U[ISO]) 
REST 0.052, 0.002 = H(432,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(431) TO C ( 43) TO C(42) 
CONT H(431) TO C ( 43) TO C(44) 
CONT H(432) TO C ( 43) TO C(42) 
CONT H(432) TO C ( 43) TO C(44) 
ANGLE 109.54, 2.0 = 
CONT H(431) TO C ( 43) TO H(432) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 44) TO H(442) 
CONT C ( 44) TO H(441) 
REST 0.050, 0.002 = H(442,U[ISO]) 
REST 0.050, 0.002 = H(441,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(442) TO C ( 44) TO C(43) 
CONT H(442) TO C ( 44) TO C(45) 
CONT H(441) TO C ( 44) TO C(43) 
CONT H(441) TO C ( 44) TO C(45) 
ANGLE 109.54, 2.0 = 
CONT H(442) TO C ( 44) TO H(441) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 45) TO H(452) 
CONT C ( 45) TO H(451) 
REST 0.050, 0.002 = H(452,U[ISO]) 
REST 0.050, 0.002 = H(451,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(452) TO C ( 45) TO C(44) 
CONT H(452) TO C ( 45) TO C(46) 
CONT H(451) TO C ( 45) TO C(44) 
CONT H(451) TO C ( 45) TO C(46) 
ANGLE 109.54, 2.0 = 
CONT H(452) TO C ( 45) TO H(451) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 46) TO H(462) 
CONT C ( 46) TO H(461) 
REST 0.045, 0.002 = H(462,U[ISO]) 
REST 0.045, 0.002 = H(461,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(462) TO C ( 46) TO C(41) 
CONT H(462) TO C ( 46) TO C(45) 
CONT H(461) TO C ( 46) TO C(41) 
CONT H(461) TO C ( 46) TO C(45) 
ANGLE 109.54, 2.0 = 
CONT H(462) TO C ( 46) TO H(461) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 51) TO H(511) 
REST 0.039, 0.002 = H(511,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(511) TO C ( 51) TO P(3) 
CONT H(511) TO C ( 51) TO C(52) 
CONT H(511) TO C ( 51) TO C(56) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 52) TO H(522) 
CONT C ( 52) TO H(521) 
REST 0.055, 0.002 = H(522,U[ISO]) 
REST 0.055, 0.002 = H(521,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(522) TO C ( 52) TO C(51) 
CONT H(522) TO C ( 52) TO C(53) 
CONT H(521) TO C ( 52) TO C(51) 
CONT H(521) TO C ( 52) TO C(53) 
ANGLE 109.54, 2.0 = 
CONT H(522) TO C ( 52) TO H(521) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 53) TO H(531) 
CONT C ( 53) TO H(532) 
REST 0.065, 0.002 = H(531,U[ISO]) 
REST 0.065, 0.002 = H(532,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(531) TO C ( 53) TO C(52) 
CONT H(531) TO C ( 53) TO C(54) 
CONT H(532) TO C ( 53) TO C(52) 
CONT H(532) TO C ( 53) TO C(54) 
ANGLE 109.54, 2.0 = 
CONT H(531) TO C ( 53) TO H(532) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 54) TO H(541) 
CONT C ( 54) TO H(542) 
REST 0.063, 0.002 = H(541,U[ISO]) 
REST 0.063, 0.002 = H(542,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(541) TO C ( 54) TO C(53) 
CONT H(541) TO C ( 54) TO C(55) 
CONT H(542) TO C ( 54) TO C(53) 
CONT H(542) TO C ( 54) TO C(55) 
ANGLE 109.54, 2.0 = 
CONT H(541) TO C ( 54) TO H(542) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 55) TO H(552) 
CONT C ( 55) TO H(551) 
REST 0.049, 0.002 = H(552,U[ISO]) 
REST 0.049, 0.002 = H(551,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(552) TO C ( 55) TO C(54) 
CONT H(552) TO C ( 55) TO C(56) 
CONT H(551) TO C ( 55) TO C(54) 
CONT H(551) TO C ( 55) TO C(56) 
ANGLE 109.54, 2.0 = 
CONT H(552) TO C ( 55) TO H(551) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 56) TO H(561) 
CONT C ( 56) TO H(562) 
REST 0.043, 0.002 = H(561,U[ISO]) 
REST 0.043, 0.002 = H(562,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(561) TO C ( 56) TO C(51) 
CONT H(561) TO C ( 56) TO C(55) 
CONT H(562) TO C ( 56) TO C(51) 
CONT H(562) TO C ( 56) TO C(55) 
ANGLE 109.54, 2.0 = 
CONT H(561) TO C ( 56) TO H(562) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 61) TO H(611) 
REST 0.042, 0.002 = H(611,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(611) TO C ( 61) TO P(3) 
CONT H(611) TO C ( 61) TO C(62) 
CONT H(611) TO C ( 61) TO C(66) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 62) TO H(621) 
CONT C ( 62) TO H(622) 
REST 0.056, 0.002 = H(621,U[ISO]) 
REST 0.056, 0.002 = H(622,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) 
CONT H(622) TO C ( 62) TO C(61) 
CONT H(622) TO C ( 62) TO C(63) 
ANGLE 109.54, 2.0 = 
CONT H(621) TO C ( 62) TO H(622) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 63) TO H(631) 
CONT C ( 63) TO H(632) 
REST 0.076, 0.002 = H(631,U[ISO]) 
REST 0.076, 0.002 = H(632,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(631) TO C ( 63) TO C(62) 
CONT H(631) TO C ( 63) TO C(64) 
CONT H(632) TO C ( 63) TO C(62) 
CONT H(632) TO C ( 63) TO C(64) 
ANGLE 109.54, 2.0 = 
CONT H(631) TO C ( 63) TO H(632) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 64) TO H(642) 
CONT C ( 64) TO H(641) 
REST 0.070, 0.002 = H(642,U[ISO]) 
REST 0.070, 0.002 = H(641,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(642) TO C ( 64) TO C(63) 
CONT H(642) TO C ( 64) TO C(65) 
CONT H(641) TO C ( 64) TO C(63) 
CONT H(641) TO C ( 64) TO C(65) 
ANGLE 109.54, 2.0 = 
CONT H(642) TO C ( 64) TO H(641) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 65) TO H(651) 
CONT C ( 65) TO H(652) 
REST 0.057, 0.002 = H(651,U[ISO]) 
REST 0.057, 0.002 = H(652,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(651) TO C ( 65) TO C(64) 
CONT H(651) TO C ( 65) TO C(66) 
CONT H(652) TO C ( 65) TO C(64) 
CONT H(652) TO C ( 65) TO C(66) 
ANGLE 109.54, 2.0 = 
CONT H(651) TO C ( 65) TO H(652) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 66) TO H(661) 
CONT C ( 66) TO H(662) 
REST 0.047, 0.002 = H(661,U[ISO]) 
REST 0.047, 0.002 = H(662,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(661) TO C ( 66) TO C(61) 
CONT H(661) TO C ( 66) TO C(65) 
CONT H(662) TO C ( 66) TO C(61) 
CONT H(662) TO C ( 66) TO C(65) 
ANGLE 109.54, 2.0 = 
CONT H(661) TO C ( 66) TO H(662) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 71) TO H(711) 
REST 0.044, 0.002 = H(711,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(711) TO C ( 71) TO P(4) 
CONT H(711) TO C ( 71) TO C(72) 
CONT H(711) TO C ( 71) TO C(76) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 72) TO H(722) 
CONT C ( 72) TO H(721) 
REST 0.081, 0.002 = H(722,U[ISO]) 
REST 0.081, 0.002 = H(721,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(722) TO C ( 72) TO C(71) 
CONT H(722) TO C ( 72) TO C(73) 
CONT H(721) TO C ( 72) TO C(71) 
CONT H(721) TO C ( 72) TO C(73) 
ANGLE 109.54, 2.0 = 
CONT H(722) TO C ( 72) TO H(721) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 73) TO H(731) 
CONT C ( 73) TO H(732) 
REST 0.080, 0.002 = H(731,U[ISO]) 
REST 0.080, 0.002 = H(732,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(731) TO C ( 73) TO C(72) 
CONT H(731) TO C ( 73) TO C(74) 
CONT H(732) TO C ( 73) TO C(72) 
CONT H(732) TO C ( 73) TO C(74) 
ANGLE 109.54, 2.0 = 
CONT H(731) TO C ( 73) TO H(732) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 74) TO H(741) 
CONT C ( 74) TO H(742) 
REST 0.057, 0.002 = H(741,U[ISO]) 
REST 0.057, 0.002 = H(742,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(741) TO C ( 74) TO C(73) 
CONT H(741) TO C ( 74) TO C(75) 
CONT H(742) TO C ( 74) TO C(73) 
CONT H(742) TO C ( 74) TO C(75) 
ANGLE 109.54, 2.0 = 
CONT H(741) TO C ( 74) TO H(742) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 75) TO H(752) 
CONT C ( 75) TO H(751) 
REST 0.076, 0.002 = H(752,U[ISO]) 
REST 0.076, 0.002 = H(751,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(752) TO C ( 75) TO C(74) 
CONT H(752) TO C ( 75) TO C(76) 
CONT H(751) TO C ( 75) TO C(74) 
CONT H(751) TO C ( 75) TO C(76) 
ANGLE 109.54, 2.0 = 
CONT H(752) TO C ( 75) TO H(751) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 76) TO H(761) 
CONT C ( 76) TO H(762) 
REST 0.080, 0.002 = H(761,U[ISO]) 
REST 0.080, 0.002 = H(762,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(761) TO C ( 76) TO C(71) 
CONT H(761) TO C ( 76) TO C(75) 
CONT H(762) TO C ( 76) TO C(71) 
CONT H(762) TO C ( 76) TO C(75) 
ANGLE 109.54, 2.0 = 
CONT H(761) TO C ( 76) TO H(762) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 81) TO H(811) 
REST 0.043, 0.002 = H(811,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(811) TO C ( 81) TO P(4) 
CONT H(811) TO C ( 81) TO C(82) 
CONT H(811) TO C ( 81) TO C(86) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 82) TO H(821) 
CONT C ( 82) TO H(822) 
REST 0.060, 0.002 = H(821,U[ISO]) 
REST 0.060, 0.002 = H(822,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(821) TO C ( 82) TO C(81) 
CONT H(821) TO C ( 82) TO C(83) 
CONT H(822) TO C ( 82) TO C(81) 
CONT H(822) TO C ( 82) TO C(83) 
ANGLE 109.54, 2.0 = 
CONT H(821) TO C ( 82) TO H(822) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 83) TO H(831) 
CONT C ( 83) TO H(832) 
REST 0.074, 0.002 = H(831,U[ISO]) 
REST 0.074, 0.002 = H(832,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(831) TO C ( 83) TO C(82) 
CONT H(831) TO C ( 83) TO C(84) 
CONT H(832) TO C ( 83) TO C(82) 
CONT H(832) TO C ( 83) TO C(84) 
ANGLE 109.54, 2.0 = 
CONT H(831) TO C ( 83) TO H(832) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 84) TO H(842) 
CONT C ( 84) TO H(841) 
REST 0.070, 0.002 = H(842,U[ISO]) 
REST 0.070, 0.002 = H(841,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(842) TO C ( 84) TO C(83) 
CONT H(842) TO C ( 84) TO C(85) 
CONT H(841) TO C ( 84) TO C(83) 
CONT H(841) TO C ( 84) TO C(85) 
ANGLE 109.54, 2.0 = 
CONT H(842) TO C ( 84) TO H(841) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 85) TO H(851) 
CONT C ( 85) TO H(852) 
REST 0.069, 0.002 = H(851,U[ISO]) 
REST 0.069, 0.002 = H(852,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(851) TO C ( 85) TO C(84) 
CONT H(851) TO C ( 85) TO C(86) 
CONT H(852) TO C ( 85) TO C(84) 
CONT H(852) TO C ( 85) TO C(86) 
ANGLE 109.54, 2.0 = 
CONT H(851) TO C ( 85) TO H(852) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 86) TO H(861) 
CONT C ( 86) TO H(862) 
REST 0.051, 0.002 = H(861,U[ISO]) 
REST 0.051, 0.002 = H(862,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(861) TO C ( 86) TO C(81) 
CONT H(861) TO C ( 86) TO C(85) 
CONT H(862) TO C ( 86) TO C(81) 
CONT H(862) TO C ( 86) TO C(85) 
ANGLE 109.54, 2.0 = 
CONT H(861) TO C ( 86) TO H(862) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 100) TO H(1002) 
CONT C ( 100) TO H(1001) 
REST 0.100, 0.002 = H(1002,U[ISO]) 
REST 0.100, 0.002 = H(1001,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(1002) TO C ( 100) TO CL(2) 
CONT H(1002) TO C ( 100) TO CL(1) 
CONT H(1001) TO C ( 100) TO CL(2) 
CONT H(1001) TO C ( 100) TO CL(1) 
ANGLE 109.54, 2.0 = 
CONT H(1002) TO C ( 100) TO H(1001) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;





####################################################################### 
# 
# 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 943296'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 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                   11.1026(3)
_cell_length_b                   12.0068(3)
_cell_length_c                   12.5924(3)
_cell_angle_alpha                117.0693(11)
_cell_angle_beta                 109.9315(14)
_cell_angle_gamma                96.4193(13)
_cell_volume                     1331.87(7)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            2

# Given Formula = C24 H48 B1 Br1 P2 
# Dc =      1.22 Fooo =    524.00 Mu =     16.72 M =    489.31
# Found Formula = C24 H48 B1 Br1 P2 
# Dc =      1.22 FOOO =    524.00 Mu =     16.72 M =    489.31

_chemical_formula_sum            'C24 H48 B1 Br1 P2'
_chemical_formula_moiety         'C24 H48 B1 P2, Br1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         489.31


_cell_measurement_reflns_used    18303
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      28
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.230
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_max          0.360

_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             524
_exptl_absorpt_coefficient_mu    1.672

# 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 0.110
-1 0 0 0.220
0 0 -1 0.120
-1 0 2 0.050
1 -7 8 0.095
-2 8 -7 0.130
1 1 -2 0.110
-1 -7 8 0.090
7 -1 -6 0.135
1 4 0 0.051


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_T_max  0.811
_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 (Farrugia, 1997)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            29869
_reflns_number_total             6125
_diffrn_reflns_av_R_equivalents  0.055
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6125 
# Theoretical number of reflections is about 12303 


_diffrn_reflns_theta_min         2.651
_diffrn_reflns_theta_max         27.552
_diffrn_measured_fraction_theta_max 0.994

_diffrn_reflns_theta_full        27.001
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -14
_reflns_limit_h_max              13
_reflns_limit_k_min              -15
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.84
_oxford_diffrn_Wilson_scale      4.28

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

_refine_diff_density_min         -0.61
_refine_diff_density_max         0.46


# 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         6108
_refine_ls_number_restraints     0
_refine_ls_number_parameters     254
_oxford_refine_ls_R_factor_ref   0.0448
_refine_ls_wR_factor_ref         0.0764
_refine_ls_goodness_of_fit_ref   0.9794
_refine_ls_shift/su_max          0.0005369
_refine_ls_shift/su_mean         0.0000199


# The values computed from all data 
_oxford_reflns_number_all        6108
_refine_ls_R_factor_all          0.0448
_refine_ls_wR_factor_all         0.0764

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5022
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_gt          0.0717

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 0.65P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.4771(2) 0.0649(2) 0.2341(2) 0.0323 1.0000 Uani . . . . . .
Br1 Br 0.15743(2) 0.32247(2) 0.27157(2) 0.0429 1.0000 Uani . . . . . .
P1 P 0.53944(5) 0.24170(4) 0.38606(4) 0.0276 1.0000 Uani . . . . . .
P2 P 0.28893(4) 0.01182(4) 0.11281(4) 0.0267 1.0000 Uani . . . . . .
C11 C 0.72079(17) 0.29750(17) 0.48956(17) 0.0290 1.0000 Uani . . . . . .
C12 C 0.7995(2) 0.2990(2) 0.4107(2) 0.0414 1.0000 Uani . . . . . .
C13 C 0.9518(2) 0.3494(3) 0.5001(2) 0.0517 1.0000 Uani . . . . . .
C14 C 0.9919(2) 0.2708(3) 0.5640(2) 0.0535 1.0000 Uani . . . . . .
C15 C 0.9122(2) 0.2685(3) 0.6404(2) 0.0531 1.0000 Uani . . . . . .
C16 C 0.7602(2) 0.2154(2) 0.5511(2) 0.0438 1.0000 Uani . . . . . .
C21 C 0.44504(18) 0.26796(18) 0.48411(18) 0.0314 1.0000 Uani . . . . . .
C22 C 0.5135(2) 0.40219(19) 0.6147(2) 0.0413 1.0000 Uani . . . . . .
C23 C 0.4216(2) 0.4282(2) 0.6838(2) 0.0480 1.0000 Uani . . . . . .
C24 C 0.3857(2) 0.3197(2) 0.7084(2) 0.0474 1.0000 Uani . . . . . .
C25 C 0.3189(2) 0.1857(2) 0.5789(3) 0.0533 1.0000 Uani . . . . . .
C26 C 0.4087(2) 0.1570(2) 0.5067(2) 0.0453 1.0000 Uani . . . . . .
C31 C 0.26443(18) 0.05492(17) -0.01281(17) 0.0303 1.0000 Uani . . . . . .
C32 C 0.34584(19) 0.19867(19) 0.04834(19) 0.0351 1.0000 Uani . . . . . .
C33 C 0.3251(2) 0.2305(2) -0.0598(2) 0.0427 1.0000 Uani . . . . . .
C34 C 0.1757(2) 0.2012(2) -0.1430(2) 0.0438 1.0000 Uani . . . . . .
C35 C 0.0961(2) 0.0584(2) -0.2030(2) 0.0440 1.0000 Uani . . . . . .
C36 C 0.11426(19) 0.0262(2) -0.0957(2) 0.0382 1.0000 Uani . . . . . .
C41 C 0.20998(17) -0.16613(17) 0.02644(17) 0.0290 1.0000 Uani . . . . . .
C42 C 0.2853(2) -0.24078(19) -0.0485(2) 0.0411 1.0000 Uani . . . . . .
C43 C 0.2167(3) -0.3896(2) -0.1232(2) 0.0498 1.0000 Uani . . . . . .
C44 C 0.2070(2) -0.4318(2) -0.0287(2) 0.0513 1.0000 Uani . . . . . .
C45 C 0.1327(3) -0.3573(2) 0.0461(2) 0.0546 1.0000 Uani . . . . . .
C46 C 0.2001(2) -0.2081(2) 0.1215(2) 0.0443 1.0000 Uani . . . . . .
H1 H 0.5334 0.0519 0.1727 0.0500 1.0000 Uiso R . . . . .
H2 H 0.4862 0.0009 0.2779 0.0500 1.0000 Uiso R . . . . .
H11 H 0.5200 0.3242 0.3450 0.0500 1.0000 Uiso R . . . . .
H21 H 0.2131 0.0690 0.1763 0.0500 1.0000 Uiso R . . . . .
H111 H 0.7443 0.3894 0.5625 0.0344 1.0000 Uiso R . . . . .
H121 H 0.7757 0.2090 0.3355 0.0505 1.0000 Uiso R . . . . .
H122 H 0.7746 0.3570 0.3766 0.0504 1.0000 Uiso R . . . . .
H131 H 0.9748 0.4422 0.5712 0.0623 1.0000 Uiso R . . . . .
H132 H 1.0011 0.3462 0.4485 0.0625 1.0000 Uiso R . . . . .
H141 H 1.0900 0.3102 0.6250 0.0633 1.0000 Uiso R . . . . .
H142 H 0.9734 0.1784 0.4949 0.0637 1.0000 Uiso R . . . . .
H151 H 0.9383 0.2142 0.6785 0.0661 1.0000 Uiso R . . . . .
H152 H 0.9358 0.3613 0.7124 0.0666 1.0000 Uiso R . . . . .
H161 H 0.7097 0.2175 0.6034 0.0534 1.0000 Uiso R . . . . .
H162 H 0.7370 0.1232 0.4782 0.0529 1.0000 Uiso R . . . . .
H211 H 0.3592 0.2739 0.4314 0.0364 1.0000 Uiso R . . . . .
H221 H 0.5320 0.4721 0.5952 0.0504 1.0000 Uiso R . . . . .
H222 H 0.5973 0.3995 0.6738 0.0504 1.0000 Uiso R . . . . .
H231 H 0.3363 0.4287 0.6223 0.0583 1.0000 Uiso R . . . . .
H232 H 0.4653 0.5133 0.7675 0.0583 1.0000 Uiso R . . . . .
H241 H 0.4685 0.3175 0.7673 0.0564 1.0000 Uiso R . . . . .
H242 H 0.3254 0.3359 0.7514 0.0560 1.0000 Uiso R . . . . .
H251 H 0.3004 0.1157 0.5974 0.0657 1.0000 Uiso R . . . . .
H252 H 0.2333 0.1856 0.5197 0.0654 1.0000 Uiso R . . . . .
H261 H 0.4921 0.1513 0.5620 0.0564 1.0000 Uiso R . . . . .
H262 H 0.3601 0.0720 0.4193 0.0566 1.0000 Uiso R . . . . .
H311 H 0.2987 -0.0037 -0.0726 0.0372 1.0000 Uiso R . . . . .
H321 H 0.3160 0.2566 0.1116 0.0426 1.0000 Uiso R . . . . .
H322 H 0.4419 0.2123 0.0965 0.0423 1.0000 Uiso R . . . . .
H331 H 0.3601 0.1745 -0.1199 0.0513 1.0000 Uiso R . . . . .
H332 H 0.3736 0.3248 -0.0196 0.0517 1.0000 Uiso R . . . . .
H341 H 0.1643 0.2187 -0.2147 0.0532 1.0000 Uiso R . . . . .
H342 H 0.1384 0.2586 -0.0858 0.0526 1.0000 Uiso R . . . . .
H351 H 0.1287 0.0006 -0.2640 0.0530 1.0000 Uiso R . . . . .
H352 H -0.0005 0.0422 -0.2537 0.0533 1.0000 Uiso R . . . . .
H361 H 0.0682 -0.0658 -0.1353 0.0464 1.0000 Uiso R . . . . .
H362 H 0.0796 0.0827 -0.0360 0.0461 1.0000 Uiso R . . . . .
H411 H 0.1190 -0.1869 -0.0392 0.0356 1.0000 Uiso R . . . . .
H421 H 0.2856 -0.2153 -0.1134 0.0498 1.0000 Uiso R . . . . .
H422 H 0.3776 -0.2178 0.0177 0.0494 1.0000 Uiso R . . . . .
H431 H 0.1233 -0.4126 -0.1908 0.0592 1.0000 Uiso R . . . . .
H432 H 0.2694 -0.4363 -0.1662 0.0600 1.0000 Uiso R . . . . .
H441 H 0.1600 -0.5268 -0.0780 0.0588 1.0000 Uiso R . . . . .
H442 H 0.2983 -0.4131 0.0359 0.0595 1.0000 Uiso R . . . . .
H451 H 0.1314 -0.3842 0.1082 0.0675 1.0000 Uiso R . . . . .
H452 H 0.0395 -0.3807 -0.0192 0.0674 1.0000 Uiso R . . . . .
H461 H 0.2922 -0.1860 0.1885 0.0532 1.0000 Uiso R . . . . .
H462 H 0.1466 -0.1628 0.1640 0.0532 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       80(10)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.5789(8)
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 . P1 . 1.928(2) yes
B1 . P2 . 1.935(2) yes
B1 . H1 . 1.120 no
B1 . H2 . 1.127 no
P1 . C11 . 1.8210(17) yes
P1 . C21 . 1.8233(19) yes
P1 . H11 . 1.316 no
P2 . C31 . 1.8241(18) yes
P2 . C41 . 1.8255(17) yes
P2 . H21 . 1.381 no
C11 . C12 . 1.534(3) yes
C11 . C16 . 1.524(3) yes
C11 . H111 . 0.989 no
C12 . C13 . 1.532(3) yes
C12 . H121 . 0.984 no
C12 . H122 . 0.990 no
C13 . C14 . 1.509(3) yes
C13 . H131 . 0.991 no
C13 . H132 . 0.974 no
C14 . C15 . 1.520(3) yes
C14 . H141 . 0.991 no
C14 . H142 . 0.989 no
C15 . C16 . 1.527(3) yes
C15 . H151 . 0.986 no
C15 . H152 . 0.993 no
C16 . H161 . 0.995 no
C16 . H162 . 0.992 no
C21 . C22 . 1.530(3) yes
C21 . C26 . 1.524(3) yes
C21 . H211 . 0.990 no
C22 . C23 . 1.526(3) yes
C22 . H221 . 0.995 no
C22 . H222 . 0.989 no
C23 . C24 . 1.511(3) yes
C23 . H231 . 1.001 no
C23 . H232 . 0.975 no
C24 . C25 . 1.523(3) yes
C24 . H241 . 0.977 no
C24 . H242 . 0.980 no
C25 . C26 . 1.533(3) yes
C25 . H251 . 0.988 no
C25 . H252 . 0.986 no
C26 . H261 . 0.982 no
C26 . H262 . 0.996 no
C31 . C32 . 1.535(3) yes
C31 . C36 . 1.532(2) yes
C31 . H311 . 0.990 no
C32 . C33 . 1.528(3) yes
C32 . H321 . 0.978 no
C32 . H322 . 0.980 no
C33 . C34 . 1.524(3) yes
C33 . H331 . 0.985 no
C33 . H332 . 0.992 no
C34 . C35 . 1.522(3) yes
C34 . H341 . 0.988 no
C34 . H342 . 0.990 no
C35 . C36 . 1.524(3) yes
C35 . H351 . 0.982 no
C35 . H352 . 0.984 no
C36 . H361 . 0.964 no
C36 . H362 . 0.983 no
C41 . C42 . 1.526(3) yes
C41 . C46 . 1.525(3) yes
C41 . H411 . 0.976 no
C42 . C43 . 1.528(3) yes
C42 . H421 . 0.995 no
C42 . H422 . 0.983 no
C43 . C44 . 1.519(3) yes
C43 . H431 . 0.998 no
C43 . H432 . 0.982 no
C44 . C45 . 1.516(3) yes
C44 . H441 . 0.979 no
C44 . H442 . 0.980 no
C45 . C46 . 1.529(3) yes
C45 . H451 . 0.975 no
C45 . H452 . 0.985 no
C46 . H461 . 0.988 no
C46 . H462 . 0.979 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 . B1 . P2 . 112.42(10) yes
P1 . B1 . H1 . 113.4 no
P2 . B1 . H1 . 105.4 no
P1 . B1 . H2 . 104.1 no
P2 . B1 . H2 . 107.7 no
H1 . B1 . H2 . 113.9 no
B1 . P1 . C11 . 112.03(8) yes
B1 . P1 . C21 . 114.47(9) yes
C11 . P1 . C21 . 111.70(8) yes
B1 . P1 . H11 . 109.3 no
C11 . P1 . H11 . 105.3 no
C21 . P1 . H11 . 103.3 no
B1 . P2 . C31 . 113.16(9) yes
B1 . P2 . C41 . 110.92(9) yes
C31 . P2 . C41 . 107.77(8) yes
B1 . P2 . H21 . 112.9 no
C31 . P2 . H21 . 105.7 no
C41 . P2 . H21 . 105.9 no
P1 . C11 . C12 . 110.82(12) yes
P1 . C11 . C16 . 112.06(13) yes
C12 . C11 . C16 . 111.11(16) yes
P1 . C11 . H111 . 106.5 no
C12 . C11 . H111 . 107.9 no
C16 . C11 . H111 . 108.2 no
C11 . C12 . C13 . 110.16(16) yes
C11 . C12 . H121 . 109.7 no
C13 . C12 . H121 . 108.6 no
C11 . C12 . H122 . 108.5 no
C13 . C12 . H122 . 110.3 no
H121 . C12 . H122 . 109.5 no
C12 . C13 . C14 . 111.94(19) yes
C12 . C13 . H131 . 107.4 no
C14 . C13 . H131 . 108.5 no
C12 . C13 . H132 . 109.8 no
C14 . C13 . H132 . 109.9 no
H131 . C13 . H132 . 109.2 no
C13 . C14 . C15 . 111.31(18) yes
C13 . C14 . H141 . 109.1 no
C15 . C14 . H141 . 109.8 no
C13 . C14 . H142 . 109.9 no
C15 . C14 . H142 . 107.7 no
H141 . C14 . H142 . 109.0 no
C14 . C15 . C16 . 111.18(19) yes
C14 . C15 . H151 . 109.5 no
C16 . C15 . H151 . 110.3 no
C14 . C15 . H152 . 106.6 no
C16 . C15 . H152 . 108.8 no
H151 . C15 . H152 . 110.3 no
C15 . C16 . C11 . 110.20(17) yes
C15 . C16 . H161 . 110.1 no
C11 . C16 . H161 . 109.8 no
C15 . C16 . H162 . 108.7 no
C11 . C16 . H162 . 108.5 no
H161 . C16 . H162 . 109.6 no
P1 . C21 . C22 . 111.64(13) yes
P1 . C21 . C26 . 115.38(13) yes
C22 . C21 . C26 . 111.67(17) yes
P1 . C21 . H211 . 104.9 no
C22 . C21 . H211 . 105.1 no
C26 . C21 . H211 . 107.3 no
C21 . C22 . C23 . 109.77(16) yes
C21 . C22 . H221 . 109.1 no
C23 . C22 . H221 . 109.9 no
C21 . C22 . H222 . 108.4 no
C23 . C22 . H222 . 107.6 no
H221 . C22 . H222 . 112.0 no
C22 . C23 . C24 . 111.18(18) yes
C22 . C23 . H231 . 107.0 no
C24 . C23 . H231 . 108.3 no
C22 . C23 . H232 . 110.0 no
C24 . C23 . H232 . 110.2 no
H231 . C23 . H232 . 110.1 no
C23 . C24 . C25 . 110.95(19) yes
C23 . C24 . H241 . 108.9 no
C25 . C24 . H241 . 108.2 no
C23 . C24 . H242 . 111.0 no
C25 . C24 . H242 . 109.5 no
H241 . C24 . H242 . 108.3 no
C24 . C25 . C26 . 111.39(18) yes
C24 . C25 . H251 . 109.8 no
C26 . C25 . H251 . 109.1 no
C24 . C25 . H252 . 109.0 no
C26 . C25 . H252 . 107.9 no
H251 . C25 . H252 . 109.7 no
C25 . C26 . C21 . 109.91(17) yes
C25 . C26 . H261 . 108.9 no
C21 . C26 . H261 . 109.0 no
C25 . C26 . H262 . 109.8 no
C21 . C26 . H262 . 109.4 no
H261 . C26 . H262 . 109.8 no
P2 . C31 . C32 . 112.01(12) yes
P2 . C31 . C36 . 111.30(13) yes
C32 . C31 . C36 . 111.17(15) yes
P2 . C31 . H311 . 105.6 no
C32 . C31 . H311 . 108.5 no
C36 . C31 . H311 . 108.0 no
C31 . C32 . C33 . 110.58(16) yes
C31 . C32 . H321 . 108.6 no
C33 . C32 . H321 . 110.0 no
C31 . C32 . H322 . 109.0 no
C33 . C32 . H322 . 110.0 no
H321 . C32 . H322 . 108.6 no
C32 . C33 . C34 . 111.33(17) yes
C32 . C33 . H331 . 108.9 no
C34 . C33 . H331 . 107.7 no
C32 . C33 . H332 . 110.4 no
C34 . C33 . H332 . 109.0 no
H331 . C33 . H332 . 109.6 no
C33 . C34 . C35 . 110.92(17) yes
C33 . C34 . H341 . 110.0 no
C35 . C34 . H341 . 109.7 no
C33 . C34 . H342 . 109.6 no
C35 . C34 . H342 . 107.9 no
H341 . C34 . H342 . 108.8 no
C34 . C35 . C36 . 111.31(17) yes
C34 . C35 . H351 . 108.6 no
C36 . C35 . H351 . 109.0 no
C34 . C35 . H352 . 109.7 no
C36 . C35 . H352 . 109.5 no
H351 . C35 . H352 . 108.7 no
C31 . C36 . C35 . 110.32(16) yes
C31 . C36 . H361 . 108.2 no
C35 . C36 . H361 . 110.5 no
C31 . C36 . H362 . 108.0 no
C35 . C36 . H362 . 108.9 no
H361 . C36 . H362 . 110.9 no
P2 . C41 . C42 . 110.75(12) yes
P2 . C41 . C46 . 111.65(12) yes
C42 . C41 . C46 . 111.12(16) yes
P2 . C41 . H411 . 106.4 no
C42 . C41 . H411 . 107.7 no
C46 . C41 . H411 . 109.0 no
C41 . C42 . C43 . 110.43(17) yes
C41 . C42 . H421 . 109.3 no
C43 . C42 . H421 . 109.1 no
C41 . C42 . H422 . 107.5 no
C43 . C42 . H422 . 109.0 no
H421 . C42 . H422 . 111.5 no
C42 . C43 . C44 . 110.94(18) yes
C42 . C43 . H431 . 108.7 no
C44 . C43 . H431 . 108.6 no
C42 . C43 . H432 . 109.5 no
C44 . C43 . H432 . 108.5 no
H431 . C43 . H432 . 110.6 no
C43 . C44 . C45 . 110.88(18) yes
C43 . C44 . H441 . 110.2 no
C45 . C44 . H441 . 109.4 no
C43 . C44 . H442 . 109.2 no
C45 . C44 . H442 . 108.6 no
H441 . C44 . H442 . 108.5 no
C44 . C45 . C46 . 111.31(19) yes
C44 . C45 . H451 . 108.7 no
C46 . C45 . H451 . 109.9 no
C44 . C45 . H452 . 108.0 no
C46 . C45 . H452 . 109.0 no
H451 . C45 . H452 . 109.8 no
C45 . C46 . C41 . 110.37(17) yes
C45 . C46 . H461 . 108.0 no
C41 . C46 . H461 . 108.9 no
C45 . C46 . H462 . 109.4 no
C41 . C46 . H462 . 109.3 no
H461 . C46 . H462 . 111.0 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 01/11/11 at 17:42:02
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 422,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE P   (   2,X'S) H   (  21,X'S) 
RIDE P   (   1,X'S) H   (  11,X'S) 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 01/11/11 at 17:42:02
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


####################################################################### 
# 
# 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 943299'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;

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

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

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

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

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

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   12.5325(4)
_cell_length_b                   13.6104(5)
_cell_length_c                   12.3150(3)
_cell_angle_alpha                90
_cell_angle_beta                 119.5074(16)
_cell_angle_gamma                90
_cell_volume                     1828.13(10)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            4

# Given Formula = C16 H24 B1 Br1 P2 
# Dc =      1.34 Fooo =    760.00 Mu =     24.12 M =    369.03
# Found Formula = C16 H24 B1 Br1 P2 
# Dc =      1.34 FOOO =    760.00 Mu =     24.12 M =    369.03

_chemical_formula_sum            'C16 H24 B1 Br1 P2'
_chemical_formula_moiety         'C16 H24 B1 P2, Br1'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         369.03


_cell_measurement_reflns_used    10394
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.130
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_max          0.400

_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    2.412

# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 9 3 0.050
-10 -9 -3 0.110
4 -10 1 0.060
-2 6 -1 0.067
4 1 -4 0.175
-6 2 6 0.190
6 5 1 0.045


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_T_max  0.753
_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 (Farrugia, 1997)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            17592
_reflns_number_total             4040
_diffrn_reflns_av_R_equivalents  0.051
# Number of reflections without Friedels Law is 4040 
# Number of reflections with Friedels Law is 2091 
# Theoretical number of reflections is about 2097 


_diffrn_reflns_theta_min         2.993
_diffrn_reflns_theta_max         27.488
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.488
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              17
_reflns_limit_l_min              -14
_reflns_limit_l_max              15

_oxford_diffrn_Wilson_B_factor   2.70
_oxford_diffrn_Wilson_scale      28.68

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

_refine_diff_density_min         -1.18
_refine_diff_density_max         1.17


# 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         4027
_refine_ls_number_restraints     2
_refine_ls_number_parameters     183
_oxford_refine_ls_R_factor_ref   0.0401
_refine_ls_wR_factor_ref         0.0603
_refine_ls_goodness_of_fit_ref   0.9862
_refine_ls_shift/su_max          0.0008190
_refine_ls_shift/su_mean         0.0000308


# The values computed from all data 
_oxford_reflns_number_all        4027
_refine_ls_R_factor_all          0.0401
_refine_ls_wR_factor_all         0.0603

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3496
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_gt          0.0568

_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_abs_structure_details 'Flack (1983), 1949 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= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² + 1.52P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.6203(3) 0.6129(2) 0.8589(3) 0.0328 1.0000 Uani . . . . . .
Br1 Br 0.47906(8) 0.763699(19) 0.39780(8) 0.0353 1.0000 Uani . . . . . .
P1 P 0.62349(10) 0.52781(5) 0.73568(10) 0.0300 1.0000 Uani . . . . . .
P2 P 0.54589(10) 0.73876(5) 0.79810(9) 0.0274 1.0000 Uani . . . . . .
C1 C 0.7047(3) 0.5754(3) 0.6609(3) 0.0434 1.0000 Uani . . . . . .
C2 C 0.7033(3) 0.4169(2) 0.8165(3) 0.0461 1.0000 Uani . . . . . .
C3 C 0.3900(3) 0.7327(3) 0.6730(3) 0.0442 1.0000 Uani . . . . . .
C4 C 0.6284(3) 0.8100(2) 0.7410(3) 0.0418 1.0000 Uani . . . . . .
C11 C 0.4751(3) 0.4861(2) 0.6161(2) 0.0275 1.0000 Uani . . . . . .
C12 C 0.4103(3) 0.4208(2) 0.6497(3) 0.0328 1.0000 Uani . . . . . .
C13 C 0.3009(3) 0.3814(2) 0.5590(3) 0.0382 1.0000 Uani . . . . . .
C14 C 0.2548(3) 0.4056(2) 0.4355(3) 0.0389 1.0000 Uani . . . . . .
C15 C 0.3174(3) 0.4717(2) 0.4015(3) 0.0352 1.0000 Uani . . . . . .
C16 C 0.4260(3) 0.5127(2) 0.4908(3) 0.0297 1.0000 Uani . . . . . .
C21 C 0.5412(3) 0.8078(2) 0.9219(3) 0.0285 1.0000 Uani . . . . . .
C22 C 0.5199(3) 0.7606(2) 1.0093(3) 0.0377 1.0000 Uani . . . . . .
C23 C 0.5084(3) 0.8132(2) 1.0984(3) 0.0416 1.0000 Uani . . . . . .
C24 C 0.5191(3) 0.9139(2) 1.1026(3) 0.0354 1.0000 Uani . . . . . .
C25 C 0.5407(3) 0.9628(2) 1.0172(3) 0.0444 1.0000 Uani . . . . . .
C26 C 0.5520(3) 0.9098(2) 0.9276(3) 0.0402 1.0000 Uani . . . . . .
H1 H 0.7288 0.6190 0.9427 0.0494 1.0000 Uiso R . . . . .
H2 H 0.5711 0.5719 0.8961 0.0455 1.0000 Uiso R . . . . .
H11 H 0.6574 0.6259 0.6052 0.0645 1.0000 Uiso R . . . . .
H12 H 0.7810 0.6002 0.7229 0.0644 1.0000 Uiso R . . . . .
H13 H 0.7168 0.5235 0.6152 0.0646 1.0000 Uiso R . . . . .
H21 H 0.6630 0.3880 0.8584 0.0684 1.0000 Uiso R . . . . .
H22 H 0.7866 0.4325 0.8791 0.0682 1.0000 Uiso R . . . . .
H23 H 0.7042 0.3708 0.7589 0.0686 1.0000 Uiso R . . . . .
H31 H 0.3431 0.6941 0.7004 0.0655 1.0000 Uiso R . . . . .
H32 H 0.3581 0.7980 0.6534 0.0658 1.0000 Uiso R . . . . .
H33 H 0.3875 0.7031 0.6024 0.0654 1.0000 Uiso R . . . . .
H41 H 0.7142 0.8103 0.8005 0.0626 1.0000 Uiso R . . . . .
H42 H 0.5985 0.8761 0.7256 0.0627 1.0000 Uiso R . . . . .
H43 H 0.6152 0.7813 0.6643 0.0630 1.0000 Uiso R . . . . .
H121 H 0.4414 0.4013 0.7334 0.0391 1.0000 Uiso R . . . . .
H131 H 0.2582 0.3363 0.5822 0.0454 1.0000 Uiso R . . . . .
H141 H 0.1824 0.3769 0.3753 0.0470 1.0000 Uiso R . . . . .
H151 H 0.2857 0.4872 0.3164 0.0416 1.0000 Uiso R . . . . .
H161 H 0.4661 0.5586 0.4687 0.0363 1.0000 Uiso R . . . . .
H221 H 0.5127 0.6933 1.0069 0.0454 1.0000 Uiso R . . . . .
H231 H 0.4946 0.7812 1.1579 0.0499 1.0000 Uiso R . . . . .
H241 H 0.5100 0.9504 1.1626 0.0432 1.0000 Uiso R . . . . .
H251 H 0.5464 1.0311 1.0189 0.0532 1.0000 Uiso R . . . . .
H261 H 0.5652 0.9442 0.8696 0.0481 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       77(6)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.21949(13)
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 . P1 . 1.924(3) yes
B1 . P2 . 1.918(3) yes
B1 . H1 . 1.241 no
B1 . H2 . 1.086 no
P1 . C1 . 1.796(3) yes
P1 . C2 . 1.814(3) yes
P1 . C11 . 1.803(3) yes
P2 . C3 . 1.798(3) yes
P2 . C4 . 1.794(3) yes
P2 . C21 . 1.816(3) yes
C1 . H11 . 0.946 no
C1 . H12 . 0.944 no
C1 . H13 . 0.961 no
C2 . H21 . 0.967 no
C2 . H22 . 0.967 no
C2 . H23 . 0.950 no
C3 . H31 . 0.965 no
C3 . H32 . 0.956 no
C3 . H33 . 0.945 no
C4 . H41 . 0.958 no
C4 . H42 . 0.957 no
C4 . H43 . 0.959 no
C11 . C12 . 1.398(4) yes
C11 . C16 . 1.398(4) yes
C12 . C13 . 1.381(4) yes
C12 . H121 . 0.943 no
C13 . C14 . 1.375(4) yes
C13 . H131 . 0.947 no
C14 . C15 . 1.387(4) yes
C14 . H141 . 0.929 no
C15 . C16 . 1.378(4) yes
C15 . H151 . 0.943 no
C16 . H161 . 0.923 no
C21 . C22 . 1.388(4) yes
C21 . C26 . 1.393(4) yes
C22 . C23 . 1.375(4) yes
C22 . H221 . 0.920 no
C23 . C24 . 1.376(4) yes
C23 . H231 . 0.940 no
C24 . C25 . 1.379(4) yes
C24 . H241 . 0.943 no
C25 . C26 . 1.383(4) yes
C25 . H251 . 0.932 no
C26 . H261 . 0.934 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 . B1 . P2 . 115.13(16) yes
P1 . B1 . H1 . 104.9 no
P2 . B1 . H1 . 112.8 no
P1 . B1 . H2 . 105.1 no
P2 . B1 . H2 . 110.8 no
H1 . B1 . H2 . 107.5 no
B1 . P1 . C1 . 115.10(15) yes
B1 . P1 . C2 . 106.76(15) yes
C1 . P1 . C2 . 106.41(17) yes
B1 . P1 . C11 . 114.83(14) yes
C1 . P1 . C11 . 108.15(14) yes
C2 . P1 . C11 . 104.73(15) yes
B1 . P2 . C3 . 114.08(16) yes
B1 . P2 . C4 . 111.85(16) yes
C3 . P2 . C4 . 106.37(17) yes
B1 . P2 . C21 . 110.19(13) yes
C3 . P2 . C21 . 105.79(14) yes
C4 . P2 . C21 . 108.20(14) yes
P1 . C1 . H11 . 108.8 no
P1 . C1 . H12 . 108.5 no
H11 . C1 . H12 . 110.5 no
P1 . C1 . H13 . 109.2 no
H11 . C1 . H13 . 109.4 no
H12 . C1 . H13 . 110.3 no
P1 . C2 . H21 . 109.8 no
P1 . C2 . H22 . 109.9 no
H21 . C2 . H22 . 107.8 no
P1 . C2 . H23 . 110.2 no
H21 . C2 . H23 . 109.3 no
H22 . C2 . H23 . 109.7 no
P2 . C3 . H31 . 108.5 no
P2 . C3 . H32 . 108.5 no
H31 . C3 . H32 . 110.1 no
P2 . C3 . H33 . 109.7 no
H31 . C3 . H33 . 109.8 no
H32 . C3 . H33 . 110.1 no
P2 . C4 . H41 . 110.4 no
P2 . C4 . H42 . 109.9 no
H41 . C4 . H42 . 109.3 no
P2 . C4 . H43 . 108.3 no
H41 . C4 . H43 . 109.9 no
H42 . C4 . H43 . 109.1 no
P1 . C11 . C12 . 118.3(2) yes
P1 . C11 . C16 . 122.4(2) yes
C12 . C11 . C16 . 119.2(3) yes
C11 . C12 . C13 . 119.8(3) yes
C11 . C12 . H121 . 121.0 no
C13 . C12 . H121 . 119.1 no
C12 . C13 . C14 . 120.7(3) yes
C12 . C13 . H131 . 119.4 no
C14 . C13 . H131 . 119.8 no
C13 . C14 . C15 . 119.9(3) yes
C13 . C14 . H141 . 119.7 no
C15 . C14 . H141 . 120.5 no
C14 . C15 . C16 . 120.3(3) yes
C14 . C15 . H151 . 119.3 no
C16 . C15 . H151 . 120.4 no
C11 . C16 . C15 . 120.1(3) yes
C11 . C16 . H161 . 119.5 no
C15 . C16 . H161 . 120.4 no
P2 . C21 . C22 . 120.7(2) yes
P2 . C21 . C26 . 121.0(2) yes
C22 . C21 . C26 . 118.2(3) yes
C21 . C22 . C23 . 120.9(3) yes
C21 . C22 . H221 . 119.3 no
C23 . C22 . H221 . 119.8 no
C22 . C23 . C24 . 120.1(3) yes
C22 . C23 . H231 . 120.8 no
C24 . C23 . H231 . 119.0 no
C23 . C24 . C25 . 120.3(3) yes
C23 . C24 . H241 . 120.4 no
C25 . C24 . H241 . 119.3 no
C24 . C25 . C26 . 119.5(3) yes
C24 . C25 . H251 . 120.4 no
C26 . C25 . H251 . 120.1 no
C21 . C26 . C25 . 121.0(3) yes
C21 . C26 . H261 . 120.7 no
C25 . C26 . H261 . 118.3 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 20/09/11 at 14:14:43
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
CONT ENANTIO 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) H   (  13,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) H   (  43,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 20/09/11 at 14:14:44
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;




####################################################################### 
# 
# 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_jas138
_database_code_depnum_ccdc_archive 'CCDC 1530816'
_audit_update_record             
;
2017-02-03 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_audit_creation_date             14-02-10
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 'jas138 At 9:40 on 10/ 2'
_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                   11.03020(10)
_cell_length_b                   16.4541(2)
_cell_length_c                   35.0725(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.3927(5)
_cell_angle_gamma                90
_cell_volume                     6354.22(13)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
As 0.0499 2.0058 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972
2.5310 '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'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 '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'


_cell_formula_units_Z            12

# Given Formula = C16 H24 As1 B1 F6 P2 
# Dc =      1.50 Fooo =   2904.00 Mu =     18.04 M =   1434.11
# Found Formula = C16 H24 As1 B1 F6 P2 
# Dc =      1.50 FOOO =   2904.00 Mu =     18.04 M =   1434.10

_chemical_formula_sum            'C16 H24 As1 B1 F6 P2'
_chemical_formula_moiety         'C16 H24 B1 P2, As1 F6'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         478.03


_cell_measurement_reflns_used    96362
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27
_cell_measurement_temperature    200

_exptl_crystal_description       lath
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.070
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_max          0.420

_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2904
_exptl_absorpt_coefficient_mu    1.804

# Absorption correction 

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

# 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    '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            77060
_reflns_number_total             14566
_diffrn_reflns_av_R_equivalents  0.070
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 14566 
# Theoretical number of reflections is about 29127 


_diffrn_reflns_theta_min         2.562
_diffrn_reflns_theta_max         27.477
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.477
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              21
_reflns_limit_l_min              0
_reflns_limit_l_max              45

_oxford_diffrn_Wilson_B_factor   2.84
_oxford_diffrn_Wilson_scale      56.53

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

_refine_diff_density_min         -1.28
_refine_diff_density_max         1.80


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         14557
_refine_ls_number_restraints     36
_refine_ls_number_parameters     703
_oxford_refine_ls_R_factor_ref   0.0894
_refine_ls_wR_factor_ref         0.1606
_refine_ls_goodness_of_fit_ref   0.9629
_refine_ls_shift/su_max          0.0008437
_refine_ls_shift/su_mean         0.0000261


# The values computed from all data 
_oxford_reflns_number_all        14557
_refine_ls_R_factor_all          0.0894
_refine_ls_wR_factor_all         0.1606

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10395
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_gt          0.1419

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref # 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: 
 19.8 28.6 13.9 3.40 
;

# 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
As1 As 0.16715(5) 0.84448(3) 0.559354(15) 0.0374 1.0000 Uani . . . . . .
As2 As 0.34634(5) 0.34492(3) 0.565764(15) 0.0377 1.0000 Uani . . . . . .
As3 As 0.78972(5) 0.28853(4) 0.749662(18) 0.0462 1.0000 Uani . . . . . .
B1 B 0.9291(5) 0.5457(4) 0.62832(18) 0.0419 1.0000 Uani . . . . . .
B2 B 0.6166(5) 0.0413(4) 0.63018(16) 0.0355 1.0000 Uani . . . . . .
B3 B 0.2455(6) 0.1045(4) 0.68330(17) 0.0444 1.0000 Uani . . . . . .
F1 F 0.2652(4) 0.8672(2) 0.59731(11) 0.0717 1.0000 Uani . . . . . .
F2 F 0.2878(3) 0.8437(3) 0.53096(11) 0.0694 1.0000 Uani . . . . . .
F3 F 0.1899(3) 0.7431(2) 0.56855(11) 0.0556 1.0000 Uani . . . . . .
F4 F 0.1440(4) 0.9458(2) 0.55058(12) 0.0684 1.0000 Uani . . . . . .
F5 F 0.0478(4) 0.8440(3) 0.58796(14) 0.0848 1.0000 Uani . . . . . .
F6 F 0.0721(4) 0.8201(3) 0.52087(13) 0.0827 1.0000 Uani . . . . . .
F11 F 0.3631(4) 0.4457(2) 0.55625(14) 0.0763 1.0000 Uani . . . . . .
F12 F 0.2141(3) 0.3429(3) 0.53784(12) 0.0696 1.0000 Uani . . . . . .
F13 F 0.3288(4) 0.2452(2) 0.57609(16) 0.0862 1.0000 Uani . . . . . .
F14 F 0.2624(5) 0.3694(3) 0.60327(12) 0.0871 1.0000 Uani . . . . . .
F15 F 0.4761(4) 0.3472(3) 0.59462(15) 0.0866 1.0000 Uani . . . . . .
F16 F 0.4260(4) 0.3205(3) 0.52765(15) 0.1011 1.0000 Uani . . . . . .
F21 F 0.6926(5) 0.3653(4) 0.7397(2) 0.1255 1.0000 Uani . U . . . .
F22 F 0.8851(5) 0.2112(3) 0.7608(2) 0.1220 1.0000 Uani . U . . . .
F23 F 0.6947(5) 0.2566(5) 0.7817(2) 0.1419 1.0000 Uani . U . . . .
F24 F 0.8638(6) 0.3423(5) 0.7840(2) 0.1607 1.0000 Uani . U . . . .
F25 F 0.7131(6) 0.2353(5) 0.7169(2) 0.1703 1.0000 Uani . U . . . .
F26 F 0.8861(6) 0.3262(6) 0.7195(2) 0.1655 1.0000 Uani . U . . . .
P1 P 0.94041(12) 0.55890(8) 0.57419(4) 0.0357 1.0000 Uani . . . . . .
P2 P 0.76803(11) 0.52646(8) 0.64457(4) 0.0355 1.0000 Uani . . . . . .
P3 P 0.78370(11) 0.01980(8) 0.64493(4) 0.0344 1.0000 Uani . . . . . .
P4 P 0.57869(11) 0.05490(8) 0.57600(4) 0.0334 1.0000 Uani . . . . . .
P5 P 0.28473(12) 0.21225(8) 0.70173(4) 0.0388 1.0000 Uani . . . . . .
P6 P 0.32239(13) 0.01987(8) 0.71368(4) 0.0395 1.0000 Uani . . . . . .
C1 C 0.8860(6) 0.6555(3) 0.55650(17) 0.0490 1.0000 Uani . . . . . .
C2 C 1.0983(5) 0.5521(4) 0.56322(19) 0.0513 1.0000 Uani . . . . . .
C3 C 0.7170(5) 0.4238(3) 0.63529(17) 0.0462 1.0000 Uani . . . . . .
C4 C 0.7718(6) 0.5391(4) 0.69573(15) 0.0494 1.0000 Uani . . . . . .
C11 C 0.8588(4) 0.4801(3) 0.54763(14) 0.0360 1.0000 Uani . . . . . .
C12 C 0.7424(5) 0.4943(3) 0.53114(15) 0.0413 1.0000 Uani . . . . . .
C13 C 0.6755(5) 0.4304(4) 0.51490(16) 0.0470 1.0000 Uani . . . . . .
C14 C 0.7243(6) 0.3533(4) 0.51423(16) 0.0510 1.0000 Uani . . . . . .
C15 C 0.8404(6) 0.3390(3) 0.52942(17) 0.0516 1.0000 Uani . . . . . .
C16 C 0.9074(5) 0.4021(3) 0.54648(16) 0.0454 1.0000 Uani . . . . . .
C21 C 0.6540(4) 0.5957(3) 0.62514(13) 0.0353 1.0000 Uani . . . . . .
C22 C 0.6633(5) 0.6776(4) 0.63515(17) 0.0462 1.0000 Uani . . . . . .
C23 C 0.5777(6) 0.7327(4) 0.6209(2) 0.0574 1.0000 Uani . . . . . .
C24 C 0.4828(6) 0.7068(4) 0.59617(19) 0.0557 1.0000 Uani . . . . . .
C25 C 0.4725(5) 0.6262(4) 0.58666(17) 0.0517 1.0000 Uani . . . . . .
C26 C 0.5578(5) 0.5699(3) 0.60078(15) 0.0421 1.0000 Uani . . . . . .
C31 C 0.8062(5) 0.0320(4) 0.69625(16) 0.0513 1.0000 Uani . . . . . .
C32 C 0.8294(5) -0.0826(4) 0.63495(18) 0.0501 1.0000 Uani . . . . . .
C33 C 0.6249(6) 0.1516(3) 0.55759(16) 0.0464 1.0000 Uani . . . . . .
C34 C 0.4164(5) 0.0496(4) 0.56733(17) 0.0469 1.0000 Uani . . . . . .
C41 C 0.8857(4) 0.0896(3) 0.62375(15) 0.0370 1.0000 Uani . . . . . .
C42 C 0.9769(5) 0.0634(3) 0.60091(15) 0.0408 1.0000 Uani . . . . . .
C43 C 1.0513(5) 0.1201(4) 0.58421(17) 0.0494 1.0000 Uani . . . . . .
C44 C 1.0346(5) 0.2014(4) 0.59082(19) 0.0552 1.0000 Uani . . . . . .
C45 C 0.9462(6) 0.2279(4) 0.6137(2) 0.0539 1.0000 Uani . . . . . .
C46 C 0.8706(5) 0.1721(3) 0.63025(17) 0.0444 1.0000 Uani . . . . . .
C51 C 0.6464(4) -0.0238(3) 0.54861(13) 0.0356 1.0000 Uani . . . . . .
C52 C 0.5944(5) -0.1009(3) 0.54656(15) 0.0439 1.0000 Uani . . . . . .
C53 C 0.6527(6) -0.1640(3) 0.52893(18) 0.0545 1.0000 Uani . . . . . .
C54 C 0.7645(6) -0.1514(4) 0.51421(17) 0.0506 1.0000 Uani . . . . . .
C55 C 0.8170(5) -0.0751(4) 0.51613(15) 0.0457 1.0000 Uani . . . . . .
C56 C 0.7579(5) -0.0117(3) 0.53297(14) 0.0400 1.0000 Uani . . . . . .
C61 C 0.4292(6) 0.2452(4) 0.68563(19) 0.0571 1.0000 Uani . . . . . .
C62 C 0.1740(6) 0.2843(4) 0.68349(18) 0.0545 1.0000 Uani . . . . . .
C63 C 0.4796(5) 0.0354(4) 0.72684(16) 0.0492 1.0000 Uani . . . . . .
C64 C 0.3150(7) -0.0732(4) 0.68691(19) 0.0651 1.0000 Uani . . . . . .
C71 C 0.2873(5) 0.2203(3) 0.75306(14) 0.0377 1.0000 Uani . . . . . .
C72 C 0.3913(6) 0.2392(4) 0.77558(18) 0.0537 1.0000 Uani . . . . . .
C73 C 0.3876(9) 0.2413(4) 0.8150(2) 0.0743 1.0000 Uani . . . . . .
C74 C 0.2804(10) 0.2244(4) 0.8319(2) 0.0800 1.0000 Uani . . . . . .
C75 C 0.1778(8) 0.2065(4) 0.8101(2) 0.0664 1.0000 Uani . . . . . .
C76 C 0.1804(6) 0.2042(4) 0.77022(17) 0.0495 1.0000 Uani . . . . . .
C81 C 0.2472(5) 0.0012(3) 0.75721(15) 0.0388 1.0000 Uani . . . . . .
C82 C 0.3025(5) 0.0157(3) 0.79297(15) 0.0426 1.0000 Uani . . . . . .
C83 C 0.2390(6) 0.0036(4) 0.82575(17) 0.0529 1.0000 Uani . . . . . .
C84 C 0.1215(6) -0.0230(4) 0.82254(19) 0.0567 1.0000 Uani . . . . . .
C85 C 0.0652(5) -0.0377(4) 0.7874(2) 0.0613 1.0000 Uani . . . . . .
C86 C 0.1278(5) -0.0263(4) 0.75448(18) 0.0499 1.0000 Uani . . . . . .
H1 H 0.9641 0.6014 0.6425 0.0500 1.0000 Uiso . . . . . .
H2 H 0.9865 0.4938 0.6376 0.0500 1.0000 Uiso . . . . . .
H3 H 0.5900 0.0973 0.6446 0.0424 1.0000 Uiso . . . . . .
H4 H 0.5623 -0.0099 0.6400 0.0424 1.0000 Uiso . . . . . .
H5 H 0.1466 0.0963 0.6833 0.0533 1.0000 Uiso . . . . . .
H6 H 0.2746 0.0991 0.6540 0.0533 1.0000 Uiso . . . . . .
H11 H 0.8029 0.6616 0.5617 0.0585 1.0000 Uiso . . . . . .
H12 H 0.9321 0.6979 0.5688 0.0585 1.0000 Uiso . . . . . .
H13 H 0.8941 0.6582 0.5297 0.0585 1.0000 Uiso . . . . . .
H21 H 1.1308 0.5017 0.5722 0.0613 1.0000 Uiso . . . . . .
H22 H 1.1425 0.5954 0.5754 0.0613 1.0000 Uiso . . . . . .
H23 H 1.1045 0.5558 0.5364 0.0613 1.0000 Uiso . . . . . .
H31 H 0.7134 0.4140 0.6085 0.0552 1.0000 Uiso . . . . . .
H32 H 0.6386 0.4168 0.6446 0.0552 1.0000 Uiso . . . . . .
H33 H 0.7722 0.3868 0.6477 0.0552 1.0000 Uiso . . . . . .
H41 H 0.7983 0.5925 0.7022 0.0589 1.0000 Uiso . . . . . .
H42 H 0.6927 0.5307 0.7044 0.0589 1.0000 Uiso . . . . . .
H43 H 0.8263 0.5007 0.7075 0.0589 1.0000 Uiso . . . . . .
H121 H 0.7091 0.5475 0.5310 0.0492 1.0000 Uiso . . . . . .
H131 H 0.5957 0.4398 0.5042 0.0561 1.0000 Uiso . . . . . .
H141 H 0.6777 0.3098 0.5033 0.0609 1.0000 Uiso . . . . . .
H151 H 0.8748 0.2863 0.5282 0.0613 1.0000 Uiso . . . . . .
H161 H 0.9868 0.3919 0.5575 0.0540 1.0000 Uiso . . . . . .
H221 H 0.7288 0.6956 0.6518 0.0554 1.0000 Uiso . . . . . .
H231 H 0.5840 0.7883 0.6280 0.0684 1.0000 Uiso . . . . . .
H241 H 0.4249 0.7449 0.5858 0.0661 1.0000 Uiso . . . . . .
H251 H 0.4063 0.6086 0.5702 0.0616 1.0000 Uiso . . . . . .
H261 H 0.5501 0.5142 0.5939 0.0501 1.0000 Uiso . . . . . .
H311 H 0.7832 0.0854 0.7032 0.0613 1.0000 Uiso . . . . . .
H312 H 0.8893 0.0234 0.7038 0.0613 1.0000 Uiso . . . . . .
H313 H 0.7577 -0.0064 0.7087 0.0613 1.0000 Uiso . . . . . .
H321 H 0.8195 -0.0923 0.6083 0.0599 1.0000 Uiso . . . . . .
H322 H 0.9123 -0.0897 0.6432 0.0599 1.0000 Uiso . . . . . .
H323 H 0.7807 -0.1196 0.6481 0.0599 1.0000 Uiso . . . . . .
H331 H 0.7102 0.1573 0.5616 0.0554 1.0000 Uiso . . . . . .
H332 H 0.5856 0.1940 0.5705 0.0554 1.0000 Uiso . . . . . .
H333 H 0.6025 0.1545 0.5311 0.0554 1.0000 Uiso . . . . . .
H341 H 0.3877 -0.0006 0.5766 0.0562 1.0000 Uiso . . . . . .
H342 H 0.3795 0.0932 0.5801 0.0562 1.0000 Uiso . . . . . .
H343 H 0.3965 0.0536 0.5407 0.0562 1.0000 Uiso . . . . . .
H421 H 0.9886 0.0071 0.5967 0.0486 1.0000 Uiso . . . . . .
H431 H 1.1132 0.1026 0.5684 0.0588 1.0000 Uiso . . . . . .
H441 H 1.0851 0.2400 0.5793 0.0659 1.0000 Uiso . . . . . .
H451 H 0.9365 0.2843 0.6184 0.0646 1.0000 Uiso . . . . . .
H461 H 0.8087 0.1903 0.6459 0.0531 1.0000 Uiso . . . . . .
H521 H 0.5186 -0.1104 0.5573 0.0523 1.0000 Uiso . . . . . .
H531 H 0.6155 -0.2161 0.5269 0.0647 1.0000 Uiso . . . . . .
H541 H 0.8055 -0.1952 0.5028 0.0603 1.0000 Uiso . . . . . .
H551 H 0.8937 -0.0663 0.5059 0.0545 1.0000 Uiso . . . . . .
H561 H 0.7940 0.0408 0.5339 0.0475 1.0000 Uiso . . . . . .
H611 H 0.4908 0.2086 0.6947 0.0680 1.0000 Uiso . . . . . .
H612 H 0.4470 0.2981 0.6952 0.0680 1.0000 Uiso . . . . . .
H613 H 0.4254 0.2464 0.6585 0.0680 1.0000 Uiso . . . . . .
H621 H 0.0961 0.2693 0.6913 0.0650 1.0000 Uiso . . . . . .
H622 H 0.1944 0.3369 0.6932 0.0650 1.0000 Uiso . . . . . .
H623 H 0.1729 0.2851 0.6564 0.0650 1.0000 Uiso . . . . . .
H631 H 0.4891 0.0841 0.7411 0.0588 1.0000 Uiso . . . . . .
H632 H 0.5094 -0.0092 0.7418 0.0588 1.0000 Uiso . . . . . .
H633 H 0.5236 0.0393 0.7044 0.0588 1.0000 Uiso . . . . . .
H641 H 0.2330 -0.0848 0.6791 0.0779 1.0000 Uiso . . . . . .
H642 H 0.3472 -0.1163 0.7025 0.0779 1.0000 Uiso . . . . . .
H643 H 0.3614 -0.0679 0.6651 0.0779 1.0000 Uiso . . . . . .
H721 H 0.4652 0.2508 0.7639 0.0642 1.0000 Uiso . . . . . .
H731 H 0.4587 0.2542 0.8304 0.0889 1.0000 Uiso . . . . . .
H741 H 0.2785 0.2252 0.8589 0.0954 1.0000 Uiso . . . . . .
H751 H 0.1042 0.1958 0.8218 0.0791 1.0000 Uiso . . . . . .
H761 H 0.1088 0.1917 0.7551 0.0590 1.0000 Uiso . . . . . .
H821 H 0.3843 0.0340 0.7953 0.0508 1.0000 Uiso . . . . . .
H831 H 0.2774 0.0139 0.8502 0.0629 1.0000 Uiso . . . . . .
H841 H 0.0786 -0.0313 0.8449 0.0679 1.0000 Uiso . . . . . .
H851 H -0.0168 -0.0558 0.7854 0.0732 1.0000 Uiso . . . . . .
H861 H 0.0889 -0.0372 0.7301 0.0596 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.16026(7)
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
As1 . F1 . 1.707(4) yes
As1 . F2 . 1.708(3) yes
As1 . F3 . 1.714(3) yes
As1 . F4 . 1.711(3) yes
As1 . F5 . 1.702(4) yes
As1 . F6 . 1.707(4) yes
As2 . F11 . 1.704(4) yes
As2 . F12 . 1.708(3) yes
As2 . F13 . 1.694(4) yes
As2 . F14 . 1.701(4) yes
As2 . F15 . 1.704(4) yes
As2 . F16 . 1.691(4) yes
As3 . F21 . 1.680(5) yes
As3 . F22 . 1.682(5) yes
As3 . F23 . 1.665(6) yes
As3 . F24 . 1.669(6) yes
As3 . F25 . 1.638(6) yes
As3 . F26 . 1.663(7) yes
B1 . P1 . 1.922(6) yes
B1 . P2 . 1.924(6) yes
B1 . H1 . 1.101 no
B1 . H2 . 1.100 no
B2 . P3 . 1.917(5) yes
B2 . P4 . 1.935(6) yes
B2 . H3 . 1.099 no
B2 . H4 . 1.101 no
B3 . P5 . 1.927(7) yes
B3 . P6 . 1.920(7) yes
B3 . H5 . 1.100 no
B3 . H6 . 1.100 no
P1 . C1 . 1.797(6) yes
P1 . C2 . 1.809(6) yes
P1 . C11 . 1.805(5) yes
P2 . C3 . 1.804(6) yes
P2 . C4 . 1.804(6) yes
P2 . C21 . 1.801(5) yes
P3 . C31 . 1.813(6) yes
P3 . C32 . 1.799(6) yes
P3 . C41 . 1.798(5) yes
P4 . C33 . 1.802(6) yes
P4 . C34 . 1.800(5) yes
P4 . C51 . 1.801(5) yes
P5 . C61 . 1.805(6) yes
P5 . C62 . 1.793(6) yes
P5 . C71 . 1.804(5) yes
P6 . C63 . 1.786(6) yes
P6 . C64 . 1.796(6) yes
P6 . C81 . 1.806(5) yes
C1 . H11 . 0.951 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . H21 . 0.950 no
C2 . H22 . 0.951 no
C2 . H23 . 0.949 no
C3 . H31 . 0.951 no
C3 . H32 . 0.949 no
C3 . H33 . 0.949 no
C4 . H41 . 0.950 no
C4 . H42 . 0.950 no
C4 . H43 . 0.950 no
C11 . C12 . 1.396(7) yes
C11 . C16 . 1.393(7) yes
C12 . C13 . 1.388(8) yes
C12 . H121 . 0.949 no
C13 . C14 . 1.379(9) yes
C13 . H131 . 0.949 no
C14 . C15 . 1.378(9) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.388(8) yes
C15 . H151 . 0.950 no
C16 . H161 . 0.950 no
C21 . C22 . 1.396(8) yes
C21 . C26 . 1.389(7) yes
C22 . C23 . 1.380(8) yes
C22 . H221 . 0.949 no
C23 . C24 . 1.385(9) yes
C23 . H231 . 0.951 no
C24 . C25 . 1.371(9) yes
C24 . H241 . 0.951 no
C25 . C26 . 1.391(8) yes
C25 . H251 . 0.950 no
C26 . H261 . 0.950 no
C31 . H311 . 0.951 no
C31 . H312 . 0.949 no
C31 . H313 . 0.950 no
C32 . H321 . 0.950 no
C32 . H322 . 0.950 no
C32 . H323 . 0.949 no
C33 . H331 . 0.948 no
C33 . H332 . 0.951 no
C33 . H333 . 0.949 no
C34 . H341 . 0.950 no
C34 . H342 . 0.950 no
C34 . H343 . 0.950 no
C41 . C42 . 1.391(7) yes
C41 . C46 . 1.388(7) yes
C42 . C43 . 1.394(8) yes
C42 . H421 . 0.949 no
C43 . C44 . 1.372(9) yes
C43 . H431 . 0.950 no
C44 . C45 . 1.370(9) yes
C44 . H441 . 0.951 no
C45 . C46 . 1.390(8) yes
C45 . H451 . 0.950 no
C46 . H461 . 0.950 no
C51 . C52 . 1.393(7) yes
C51 . C56 . 1.390(7) yes
C52 . C53 . 1.387(8) yes
C52 . H521 . 0.951 no
C53 . C54 . 1.380(9) yes
C53 . H531 . 0.950 no
C54 . C55 . 1.383(8) yes
C54 . H541 . 0.950 no
C55 . C56 . 1.381(8) yes
C55 . H551 . 0.949 no
C56 . H561 . 0.951 no
C61 . H611 . 0.949 no
C61 . H612 . 0.950 no
C61 . H613 . 0.950 no
C62 . H621 . 0.950 no
C62 . H622 . 0.951 no
C62 . H623 . 0.949 no
C63 . H631 . 0.949 no
C63 . H632 . 0.950 no
C63 . H633 . 0.951 no
C64 . H641 . 0.949 no
C64 . H642 . 0.952 no
C64 . H643 . 0.950 no
C71 . C72 . 1.388(7) yes
C71 . C76 . 1.381(8) yes
C72 . C73 . 1.387(10) yes
C72 . H721 . 0.952 no
C73 . C74 . 1.381(12) yes
C73 . H731 . 0.950 no
C74 . C75 . 1.361(12) yes
C74 . H741 . 0.949 no
C75 . C76 . 1.400(9) yes
C75 . H751 . 0.949 no
C76 . H761 . 0.948 no
C81 . C82 . 1.383(7) yes
C81 . C86 . 1.390(8) yes
C82 . C83 . 1.395(8) yes
C82 . H821 . 0.950 no
C83 . C84 . 1.366(9) yes
C83 . H831 . 0.950 no
C84 . C85 . 1.370(10) yes
C84 . H841 . 0.950 no
C85 . C86 . 1.392(9) yes
C85 . H851 . 0.951 no
C86 . H861 . 0.951 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
F1 . As1 . F2 . 88.7(2) yes
F1 . As1 . F3 . 89.30(19) yes
F2 . As1 . F3 . 89.56(18) yes
F1 . As1 . F4 . 90.4(2) yes
F2 . As1 . F4 . 90.88(19) yes
F3 . As1 . F4 . 179.48(19) yes
F1 . As1 . F5 . 91.0(2) yes
F2 . As1 . F5 . 179.2(2) yes
F3 . As1 . F5 . 89.68(19) yes
F4 . As1 . F5 . 89.9(2) yes
F1 . As1 . F6 . 178.4(2) yes
F2 . As1 . F6 . 90.0(2) yes
F3 . As1 . F6 . 89.8(2) yes
F4 . As1 . F6 . 90.5(2) yes
F5 . As1 . F6 . 90.3(3) yes
F11 . As2 . F12 . 90.3(2) yes
F11 . As2 . F13 . 178.9(3) yes
F12 . As2 . F13 . 90.0(2) yes
F11 . As2 . F14 . 89.5(2) yes
F12 . As2 . F14 . 87.9(2) yes
F13 . As2 . F14 . 89.4(3) yes
F11 . As2 . F15 . 89.9(2) yes
F12 . As2 . F15 . 178.6(2) yes
F13 . As2 . F15 . 89.8(2) yes
F14 . As2 . F15 . 90.7(3) yes
F11 . As2 . F16 . 90.5(3) yes
F12 . As2 . F16 . 90.5(2) yes
F13 . As2 . F16 . 90.6(3) yes
F14 . As2 . F16 . 178.3(3) yes
F15 . As2 . F16 . 91.0(3) yes
F21 . As3 . F22 . 178.4(3) yes
F21 . As3 . F23 . 87.6(3) yes
F22 . As3 . F23 . 90.8(3) yes
F21 . As3 . F24 . 91.7(4) yes
F22 . As3 . F24 . 87.7(4) yes
F23 . As3 . F24 . 89.0(4) yes
F21 . As3 . F25 . 87.8(4) yes
F22 . As3 . F25 . 92.7(4) yes
F23 . As3 . F25 . 89.1(5) yes
F24 . As3 . F25 . 178.0(4) yes
F21 . As3 . F26 . 90.7(4) yes
F22 . As3 . F26 . 90.9(4) yes
F23 . As3 . F26 . 176.0(5) yes
F24 . As3 . F26 . 87.5(5) yes
F25 . As3 . F26 . 94.4(5) yes
P1 . B1 . P2 . 115.2(3) yes
P1 . B1 . H1 . 108.0 no
P2 . B1 . H1 . 108.0 no
P1 . B1 . H2 . 108.1 no
P2 . B1 . H2 . 108.0 no
H1 . B1 . H2 . 109.4 no
P3 . B2 . P4 . 115.8(3) yes
P3 . B2 . H3 . 108.0 no
P4 . B2 . H3 . 107.9 no
P3 . B2 . H4 . 107.9 no
P4 . B2 . H4 . 107.8 no
H3 . B2 . H4 . 109.4 no
P5 . B3 . P6 . 113.5(3) yes
P5 . B3 . H5 . 108.5 no
P6 . B3 . H5 . 108.4 no
P5 . B3 . H6 . 108.5 no
P6 . B3 . H6 . 108.5 no
H5 . B3 . H6 . 109.5 no
B1 . P1 . C1 . 113.6(3) yes
B1 . P1 . C2 . 108.8(3) yes
C1 . P1 . C2 . 106.7(3) yes
B1 . P1 . C11 . 111.7(2) yes
C1 . P1 . C11 . 108.1(3) yes
C2 . P1 . C11 . 107.6(3) yes
B1 . P2 . C3 . 112.6(3) yes
B1 . P2 . C4 . 108.0(3) yes
C3 . P2 . C4 . 106.0(3) yes
B1 . P2 . C21 . 114.9(3) yes
C3 . P2 . C21 . 108.7(3) yes
C4 . P2 . C21 . 106.1(3) yes
B2 . P3 . C31 . 108.7(3) yes
B2 . P3 . C32 . 113.3(3) yes
C31 . P3 . C32 . 105.9(3) yes
B2 . P3 . C41 . 112.7(2) yes
C31 . P3 . C41 . 106.7(3) yes
C32 . P3 . C41 . 109.1(3) yes
B2 . P4 . C33 . 113.9(3) yes
B2 . P4 . C34 . 108.4(3) yes
C33 . P4 . C34 . 106.4(3) yes
B2 . P4 . C51 . 111.6(2) yes
C33 . P4 . C51 . 108.0(3) yes
C34 . P4 . C51 . 108.4(3) yes
B3 . P5 . C61 . 110.9(3) yes
B3 . P5 . C62 . 110.8(3) yes
C61 . P5 . C62 . 106.5(3) yes
B3 . P5 . C71 . 113.1(3) yes
C61 . P5 . C71 . 109.1(3) yes
C62 . P5 . C71 . 106.1(3) yes
B3 . P6 . C63 . 115.4(3) yes
B3 . P6 . C64 . 108.9(3) yes
C63 . P6 . C64 . 105.7(3) yes
B3 . P6 . C81 . 112.5(3) yes
C63 . P6 . C81 . 107.0(3) yes
C64 . P6 . C81 . 106.7(3) yes
P1 . C1 . H11 . 109.5 no
P1 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.4 no
P1 . C1 . H13 . 109.5 no
H11 . C1 . H13 . 109.4 no
H12 . C1 . H13 . 109.5 no
P1 . C2 . H21 . 109.4 no
P1 . C2 . H22 . 109.4 no
H21 . C2 . H22 . 109.4 no
P1 . C2 . H23 . 109.5 no
H21 . C2 . H23 . 109.6 no
H22 . C2 . H23 . 109.5 no
P2 . C3 . H31 . 109.3 no
P2 . C3 . H32 . 109.4 no
H31 . C3 . H32 . 109.5 no
P2 . C3 . H33 . 109.5 no
H31 . C3 . H33 . 109.5 no
H32 . C3 . H33 . 109.7 no
P2 . C4 . H41 . 109.4 no
P2 . C4 . H42 . 109.5 no
H41 . C4 . H42 . 109.5 no
P2 . C4 . H43 . 109.5 no
H41 . C4 . H43 . 109.5 no
H42 . C4 . H43 . 109.5 no
P1 . C11 . C12 . 120.8(4) yes
P1 . C11 . C16 . 119.7(4) yes
C12 . C11 . C16 . 119.3(5) yes
C11 . C12 . C13 . 119.8(5) yes
C11 . C12 . H121 . 120.2 no
C13 . C12 . H121 . 120.1 no
C12 . C13 . C14 . 120.4(5) yes
C12 . C13 . H131 . 119.8 no
C14 . C13 . H131 . 119.8 no
C13 . C14 . C15 . 120.3(5) yes
C13 . C14 . H141 . 119.9 no
C15 . C14 . H141 . 119.8 no
C14 . C15 . C16 . 119.9(5) yes
C14 . C15 . H151 . 120.2 no
C16 . C15 . H151 . 119.9 no
C11 . C16 . C15 . 120.3(5) yes
C11 . C16 . H161 . 119.8 no
C15 . C16 . H161 . 119.8 no
P2 . C21 . C22 . 118.5(4) yes
P2 . C21 . C26 . 122.0(4) yes
C22 . C21 . C26 . 119.5(5) yes
C21 . C22 . C23 . 120.3(5) yes
C21 . C22 . H221 . 119.8 no
C23 . C22 . H221 . 119.9 no
C22 . C23 . C24 . 120.0(6) yes
C22 . C23 . H231 . 119.9 no
C24 . C23 . H231 . 120.0 no
C23 . C24 . C25 . 119.9(6) yes
C23 . C24 . H241 . 120.1 no
C25 . C24 . H241 . 120.0 no
C24 . C25 . C26 . 120.9(5) yes
C24 . C25 . H251 . 119.6 no
C26 . C25 . H251 . 119.5 no
C25 . C26 . C21 . 119.4(5) yes
C25 . C26 . H261 . 120.3 no
C21 . C26 . H261 . 120.3 no
P3 . C31 . H311 . 109.4 no
P3 . C31 . H312 . 109.5 no
H311 . C31 . H312 . 109.5 no
P3 . C31 . H313 . 109.5 no
H311 . C31 . H313 . 109.4 no
H312 . C31 . H313 . 109.6 no
P3 . C32 . H321 . 109.4 no
P3 . C32 . H322 . 109.4 no
H321 . C32 . H322 . 109.5 no
P3 . C32 . H323 . 109.5 no
H321 . C32 . H323 . 109.6 no
H322 . C32 . H323 . 109.5 no
P4 . C33 . H331 . 109.5 no
P4 . C33 . H332 . 109.3 no
H331 . C33 . H332 . 109.5 no
P4 . C33 . H333 . 109.4 no
H331 . C33 . H333 . 109.7 no
H332 . C33 . H333 . 109.4 no
P4 . C34 . H341 . 109.5 no
P4 . C34 . H342 . 109.4 no
H341 . C34 . H342 . 109.5 no
P4 . C34 . H343 . 109.4 no
H341 . C34 . H343 . 109.5 no
H342 . C34 . H343 . 109.5 no
P3 . C41 . C42 . 122.2(4) yes
P3 . C41 . C46 . 118.2(4) yes
C42 . C41 . C46 . 119.7(5) yes
C41 . C42 . C43 . 119.9(5) yes
C41 . C42 . H421 . 120.1 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 119.5(5) yes
C42 . C43 . H431 . 120.2 no
C44 . C43 . H431 . 120.2 no
C43 . C44 . C45 . 121.0(5) yes
C43 . C44 . H441 . 119.4 no
C45 . C44 . H441 . 119.5 no
C44 . C45 . C46 . 120.0(6) yes
C44 . C45 . H451 . 120.1 no
C46 . C45 . H451 . 119.9 no
C45 . C46 . C41 . 119.7(5) yes
C45 . C46 . H461 . 120.1 no
C41 . C46 . H461 . 120.1 no
P4 . C51 . C52 . 120.0(4) yes
P4 . C51 . C56 . 120.8(4) yes
C52 . C51 . C56 . 118.8(5) yes
C51 . C52 . C53 . 120.4(5) yes
C51 . C52 . H521 . 119.9 no
C53 . C52 . H521 . 119.8 no
C52 . C53 . C54 . 120.2(5) yes
C52 . C53 . H531 . 119.9 no
C54 . C53 . H531 . 120.0 no
C53 . C54 . C55 . 119.9(5) yes
C53 . C54 . H541 . 120.1 no
C55 . C54 . H541 . 120.0 no
C54 . C55 . C56 . 120.0(5) yes
C54 . C55 . H551 . 120.0 no
C56 . C55 . H551 . 120.0 no
C51 . C56 . C55 . 120.7(5) yes
C51 . C56 . H561 . 119.7 no
C55 . C56 . H561 . 119.6 no
P5 . C61 . H611 . 109.5 no
P5 . C61 . H612 . 109.4 no
H611 . C61 . H612 . 109.6 no
P5 . C61 . H613 . 109.4 no
H611 . C61 . H613 . 109.5 no
H612 . C61 . H613 . 109.5 no
P5 . C62 . H621 . 109.4 no
P5 . C62 . H622 . 109.4 no
H621 . C62 . H622 . 109.4 no
P5 . C62 . H623 . 109.5 no
H621 . C62 . H623 . 109.6 no
H622 . C62 . H623 . 109.5 no
P6 . C63 . H631 . 109.5 no
P6 . C63 . H632 . 109.4 no
H631 . C63 . H632 . 109.6 no
P6 . C63 . H633 . 109.4 no
H631 . C63 . H633 . 109.5 no
H632 . C63 . H633 . 109.4 no
P6 . C64 . H641 . 109.6 no
P6 . C64 . H642 . 109.4 no
H641 . C64 . H642 . 109.4 no
P6 . C64 . H643 . 109.5 no
H641 . C64 . H643 . 109.6 no
H642 . C64 . H643 . 109.3 no
P5 . C71 . C72 . 123.2(4) yes
P5 . C71 . C76 . 117.2(4) yes
C72 . C71 . C76 . 119.5(5) yes
C71 . C72 . C73 . 120.0(7) yes
C71 . C72 . H721 . 120.0 no
C73 . C72 . H721 . 120.0 no
C72 . C73 . C74 . 120.0(7) yes
C72 . C73 . H731 . 120.0 no
C74 . C73 . H731 . 120.0 no
C73 . C74 . C75 . 120.4(7) yes
C73 . C74 . H741 . 119.7 no
C75 . C74 . H741 . 119.9 no
C74 . C75 . C76 . 120.2(7) yes
C74 . C75 . H751 . 120.0 no
C76 . C75 . H751 . 119.9 no
C75 . C76 . C71 . 119.9(6) yes
C75 . C76 . H761 . 120.0 no
C71 . C76 . H761 . 120.1 no
P6 . C81 . C82 . 122.5(4) yes
P6 . C81 . C86 . 118.5(4) yes
C82 . C81 . C86 . 118.9(5) yes
C81 . C82 . C83 . 120.4(5) yes
C81 . C82 . H821 . 119.8 no
C83 . C82 . H821 . 119.7 no
C82 . C83 . C84 . 119.8(6) yes
C82 . C83 . H831 . 120.1 no
C84 . C83 . H831 . 120.1 no
C83 . C84 . C85 . 120.6(6) yes
C83 . C84 . H841 . 119.7 no
C85 . C84 . H841 . 119.8 no
C84 . C85 . C86 . 120.1(6) yes
C84 . C85 . H851 . 119.9 no
C86 . C85 . H851 . 120.0 no
C85 . C86 . C81 . 120.1(6) yes
C85 . C86 . H861 . 120.0 no
C81 . C86 . H861 . 119.9 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 10/02/14 at 10:38:09
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 10/02/14 at 10:38:09
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.01 = F(21) TO F(22) 
U(IJ) 0.0, 0.01 = F(22) TO F(23) 
U(IJ) 0.0, 0.01 = F(23) TO F(24) 
U(IJ) 0.0, 0.01 = F(24) TO F(25) 
U(IJ) 0.0, 0.01 = F(25) TO F(26) 
U(IJ) 0.0, 0.01 = F(26) TO F(21) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-1 2 2 x .
3 1 15 x .
-8 1 1 x .
3 5 10 x .
3 1 12 x .
3 3 17 x .
1 0 3 x .
0 2 2 x .
1 1 3 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 943353'
_audit_update_record             
;
2013-06-07 deposited with the CCDC.
2017-05-12 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                   18.4285(7)
_cell_length_b                   8.5936(3)
_cell_length_c                   20.9657(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.666(2)
_cell_angle_gamma                90
_cell_volume                     3309.3(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 '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'


_cell_formula_units_Z            4

# Given Formula = C26 H50 B2 Br4 P2 
# Dc =      1.54 Fooo =   1544.00 Mu =     49.76 M =    382.93
# Found Formula = C26 H50 B2 Br4 P2 
# Dc =      1.54 FOOO =   1544.00 Mu =     49.76 M =    382.93

_chemical_formula_sum            'C26 H50 B2 Br4 P2'
_chemical_formula_moiety         'C26 H50 B2 Br4 P2'
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_weight         765.87


_cell_measurement_reflns_used    14946
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25
_cell_measurement_temperature    273

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.040
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_max          0.160

_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1544
_exptl_absorpt_coefficient_mu    4.976

# 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 0.040
-1 0 0 0.030
0 1 0 0.050
0 0 1 0.020
0 0 -1 0.020
7 -6 -4 0.077


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_T_max  0.827
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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      273
_diffrn_reflns_number            22553
_reflns_number_total             2903
_diffrn_reflns_av_R_equivalents  0.073
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 2903 
# Theoretical number of reflections is about 5825 


_diffrn_reflns_theta_min         2.617
_diffrn_reflns_theta_max         24.994
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        24.994
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -21
_reflns_limit_h_max              21
_reflns_limit_k_min              0
_reflns_limit_k_max              10
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   5.53
_oxford_diffrn_Wilson_scale      79.73

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

_refine_diff_density_min         -1.03
_refine_diff_density_max         1.58


# 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         2903
_refine_ls_number_restraints     119
_refine_ls_number_parameters     155
_oxford_refine_ls_R_factor_ref   0.0899
_refine_ls_wR_factor_ref         0.1817
_refine_ls_goodness_of_fit_ref   0.9337
_refine_ls_shift/su_max          0.0006748
_refine_ls_shift/su_mean         0.0000337


# The values computed from all data 
_oxford_reflns_number_all        2903
_refine_ls_R_factor_all          0.0899
_refine_ls_wR_factor_all         0.1817

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2052
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_gt          0.1672

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.10P)² +24.01P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
B1 B 0.2857(6) 0.1545(12) 0.3556(5) 0.0624 1.0000 Uani . . . . . .
Br1 Br 0.19845(8) 0.01813(14) 0.35748(6) 0.0959 1.0000 Uani . . . . . .
Br2 Br 0.37517(9) 0.05262(18) 0.39844(7) 0.1091 1.0000 Uani . . . . . .
P1 P 0.27195(10) 0.3457(2) 0.40369(8) 0.0396 1.0000 Uani D . . . . .
C1 C 0.2778(4) 0.3093(9) 0.4893(3) 0.0421 1.0000 Uani D . . . . .
C11 C 0.3426(4) 0.4875(12) 0.3896(3) 0.0674 1.0000 Uani D U . . . .
C12 C 0.4020(5) 0.5112(13) 0.4405(4) 0.0888 1.0000 Uani D U . . . .
C13 C 0.4595(4) 0.6240(11) 0.4256(4) 0.0890 1.0000 Uani D U . . . .
C14 C 0.4736(4) 0.6467(11) 0.3597(4) 0.1103 1.0000 Uani D U . . . .
C15 C 0.4194(4) 0.6108(10) 0.3124(3) 0.0982 1.0000 Uani D U . . . .
C16 C 0.3668(4) 0.4895(10) 0.3230(3) 0.0678 1.0000 Uani D U . . . .
C21 C 0.1828(4) 0.4321(9) 0.3824(3) 0.0446 1.0000 Uani D . . . . .
C22 C 0.1690(5) 0.4600(11) 0.3098(4) 0.0568 1.0000 Uani D . . . . .
C23 C 0.0921(5) 0.5152(12) 0.2934(5) 0.0651 1.0000 Uani D . . . . .
C24 C 0.0740(5) 0.6571(12) 0.3303(5) 0.0740 1.0000 Uani D . . . . .
C25 C 0.0885(6) 0.6343(14) 0.4018(5) 0.0896 1.0000 Uani D . . . . .
C26 C 0.1666(5) 0.5791(12) 0.4196(4) 0.0671 1.0000 Uani D . . . . .
H1 H 0.2950 0.1837 0.3048 0.0753 1.0000 Uiso R . . . . .
H11 H 0.2703 0.4051 0.5105 0.0508 1.0000 Uiso DR . . . . .
H12 H 0.3253 0.2715 0.5019 0.0508 1.0000 Uiso DR . . . . .
H111 H 0.3167 0.5829 0.3909 0.0811 1.0000 Uiso R . . . . .
H121 H 0.3809 0.5470 0.4776 0.1065 1.0000 Uiso DR . . . . .
H122 H 0.4248 0.4134 0.4492 0.1065 1.0000 Uiso DR . . . . .
H131 H 0.5039 0.5898 0.4475 0.1075 1.0000 Uiso DR . . . . .
H132 H 0.4464 0.7221 0.4422 0.1075 1.0000 Uiso DR . . . . .
H141 H 0.4847 0.7538 0.3548 0.1325 1.0000 Uiso DR . . . . .
H142 H 0.5149 0.5856 0.3519 0.1325 1.0000 Uiso R . . . . .
H151 H 0.3923 0.7035 0.3036 0.1180 1.0000 Uiso DR . . . . .
H152 H 0.4431 0.5816 0.2757 0.1180 1.0000 Uiso R . . . . .
H161 H 0.3883 0.3918 0.3148 0.0815 1.0000 Uiso DR . . . . .
H162 H 0.3253 0.5050 0.2938 0.0815 1.0000 Uiso DR . . . . .
H211 H 0.1480 0.3569 0.3931 0.0536 1.0000 Uiso DR . . . . .
H221 H 0.2020 0.5368 0.2970 0.0683 1.0000 Uiso DR . . . . .
H222 H 0.1765 0.3656 0.2877 0.0683 1.0000 Uiso DR . . . . .
H231 H 0.0595 0.4341 0.3027 0.0784 1.0000 Uiso DR . . . . .
H232 H 0.0861 0.5385 0.2490 0.0784 1.0000 Uiso DR . . . . .
H241 H 0.1027 0.7414 0.3174 0.0888 1.0000 Uiso DR . . . . .
H242 H 0.0239 0.6807 0.3210 0.0888 1.0000 Uiso DR . . . . .
H251 H 0.0812 0.7304 0.4227 0.1076 1.0000 Uiso DR . . . . .
H252 H 0.0556 0.5589 0.4157 0.1076 1.0000 Uiso DR . . . . .
H261 H 0.1724 0.5573 0.4642 0.0807 1.0000 Uiso DR . . . . .
H262 H 0.1996 0.6587 0.4097 0.0807 1.0000 Uiso DR . . . . .

_refine_ls_extinction_coef       110(30)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.12927(18)
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 . Br1 . 1.992(12) yes
B1 . Br2 . 2.013(11) yes
B1 . P1 . 1.956(10) yes
B1 . H1 . 1.120 no
P1 . C1 . 1.817(7) yes
P1 . C11 . 1.825(7) yes
P1 . C21 . 1.825(8) yes
C1 . C1 4_556 1.538(14) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C11 . C12 . 1.479(7) yes
C11 . C16 . 1.500(7) yes
C11 . H111 . 0.950 no
C12 . C13 . 1.488(7) yes
C12 . H121 . 0.950 no
C12 . H122 . 0.950 no
C13 . C14 . 1.441(7) yes
C13 . H131 . 0.950 no
C13 . H132 . 0.950 no
C14 . C15 . 1.383(8) yes
C14 . H141 . 0.950 no
C14 . H142 . 0.950 no
C15 . C16 . 1.453(7) yes
C15 . H151 . 0.950 no
C15 . H152 . 0.950 no
C16 . H161 . 0.950 no
C16 . H162 . 0.950 no
C21 . C22 . 1.542(10) yes
C21 . C26 . 1.527(12) yes
C21 . H211 . 0.950 no
C22 . C23 . 1.508(12) yes
C22 . H221 . 0.950 no
C22 . H222 . 0.950 no
C23 . C24 . 1.497(14) yes
C23 . H231 . 0.950 no
C23 . H232 . 0.950 no
C24 . C25 . 1.514(14) yes
C24 . H241 . 0.950 no
C24 . H242 . 0.950 no
C25 . C26 . 1.531(13) yes
C25 . H251 . 0.950 no
C25 . H252 . 0.950 no
C26 . H261 . 0.950 no
C26 . H262 . 0.950 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
Br1 . B1 . Br2 . 111.6(5) yes
Br1 . B1 . P1 . 110.2(5) yes
Br2 . B1 . P1 . 105.7(5) yes
Br1 . B1 . H1 . 109.8 no
Br2 . B1 . H1 . 109.8 no
P1 . B1 . H1 . 109.8 no
B1 . P1 . C1 . 111.5(4) yes
B1 . P1 . C11 . 110.7(5) yes
C1 . P1 . C11 . 106.8(3) yes
B1 . P1 . C21 . 111.6(4) yes
C1 . P1 . C21 . 107.0(3) yes
C11 . P1 . C21 . 109.2(4) yes
C1 4_556 C1 . P1 . 114.4(6) yes
C1 4_556 C1 . H11 . 108.2 no
P1 . C1 . H11 . 108.2 no
C1 4_556 C1 . H12 . 108.2 no
P1 . C1 . H12 . 108.2 no
H11 . C1 . H12 . 109.5 no
P1 . C11 . C12 . 118.1(5) yes
P1 . C11 . C16 . 115.4(5) yes
C12 . C11 . C16 . 114.3(5) yes
P1 . C11 . H111 . 101.8 no
C12 . C11 . H111 . 101.7 no
C16 . C11 . H111 . 101.9 no
C11 . C12 . C13 . 115.9(5) yes
C11 . C12 . H121 . 107.9 no
C13 . C12 . H121 . 107.9 no
C11 . C12 . H122 . 107.8 no
C13 . C12 . H122 . 107.8 no
H121 . C12 . H122 . 109.5 no
C12 . C13 . C14 . 118.4(6) yes
C12 . C13 . H131 . 107.2 no
C14 . C13 . H131 . 106.8 no
C12 . C13 . H132 . 107.2 no
C14 . C13 . H132 . 107.5 no
H131 . C13 . H132 . 109.5 no
C13 . C14 . C15 . 118.8(5) yes
C13 . C14 . H141 . 106.9 no
C15 . C14 . H141 . 106.8 no
C13 . C14 . H142 . 107.5 no
C15 . C14 . H142 . 107.2 no
H141 . C14 . H142 . 109.5 no
C14 . C15 . C16 . 120.2(6) yes
C14 . C15 . H151 . 106.8 no
C16 . C15 . H151 . 106.6 no
C14 . C15 . H152 . 106.7 no
C16 . C15 . H152 . 106.9 no
H151 . C15 . H152 . 109.5 no
C11 . C16 . C15 . 113.7(5) yes
C11 . C16 . H161 . 108.5 no
C15 . C16 . H161 . 108.3 no
C11 . C16 . H162 . 108.5 no
C15 . C16 . H162 . 108.3 no
H161 . C16 . H162 . 109.5 no
P1 . C21 . C22 . 112.2(5) yes
P1 . C21 . C26 . 114.9(6) yes
C22 . C21 . C26 . 110.6(7) yes
P1 . C21 . H211 . 106.1 no
C22 . C21 . H211 . 106.1 no
C26 . C21 . H211 . 106.1 no
C21 . C22 . C23 . 110.5(7) yes
C21 . C22 . H221 . 109.2 no
C23 . C22 . H221 . 109.2 no
C21 . C22 . H222 . 109.2 no
C23 . C22 . H222 . 109.2 no
H221 . C22 . H222 . 109.5 no
C22 . C23 . C24 . 112.5(8) yes
C22 . C23 . H231 . 108.7 no
C24 . C23 . H231 . 108.6 no
C22 . C23 . H232 . 108.7 no
C24 . C23 . H232 . 108.8 no
H231 . C23 . H232 . 109.5 no
C23 . C24 . C25 . 112.2(8) yes
C23 . C24 . H241 . 108.7 no
C25 . C24 . H241 . 108.9 no
C23 . C24 . H242 . 108.8 no
C25 . C24 . H242 . 108.8 no
H241 . C24 . H242 . 109.5 no
C24 . C25 . C26 . 111.6(8) yes
C24 . C25 . H251 . 108.9 no
C26 . C25 . H251 . 108.9 no
C24 . C25 . H252 . 109.0 no
C26 . C25 . H252 . 109.0 no
H251 . C25 . H252 . 109.5 no
C25 . C26 . C21 . 110.5(8) yes
C25 . C26 . H261 . 109.2 no
C21 . C26 . H261 . 109.2 no
C25 . C26 . H262 . 109.3 no
C21 . C26 . H262 . 109.2 no
H261 . C26 . H262 . 109.5 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 07/08/12 at 11:20:11
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE B   (   1,X'S) H   (   1,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 07/08/12 at 11:20:11
#
#LIST     16                                                                    
U(IJ) 0.0, 0.01 = C(11) TO C(12) 
U(IJ) 0.0, 0.01 = C(12) TO C(13) 
U(IJ) 0.0, 0.01 = C(13) TO C(14) 
U(IJ) 0.0, 0.01 = C(14) TO C(15) 
U(IJ) 0.0, 0.01 = C(15) TO C(16) 
U(IJ) 0.0, 0.01 = C(16) TO C(11) 
REM 
DIST 0.0, 0.01 = MEAN C(11) TO C(12), C(12) TO C(13) 
DIST 0.0, 0.01 = MEAN C(12) TO C(13), C(13) TO C(14) 
DIST 0.0, 0.01 = MEAN C(13) TO C(14), C(14) TO C(15) 
DIST 0.0, 0.01 = MEAN C(14) TO C(15), C(15) TO C(16) 
DIST 0.0, 0.01 = MEAN C(15) TO C(16), C(16) TO C(11) 
DIST 0.0, 0.01 = MEAN C(16) TO C(11), C(11) TO C(12) 
REM 
ANGLE 0.0, 1. = MEAN C(11) TO C(12) TO C(13), C(12) TO C(13) TO C(14) 
ANGLE 0.0, 1. = MEAN C(12) TO C(13) TO C(14), C(13) TO C(14) TO C(15) 
ANGLE 0.0, 1. = MEAN C(13) TO C(14) TO C(15), C(14) TO C(15) TO C(16) 
ANGLE 0.0, 1. = MEAN C(14) TO C(15) TO C(16), C(15) TO C(16) TO C(11) 
ANGLE 0.0, 1. = MEAN C(15) TO C(16) TO C(11), C(16) TO C(11) TO C(12) 
ANGLE 0.0, 1. = MEAN C(16) TO C(11) TO C(12), C(11) TO C(12) TO C(13) 
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            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 1) TO H(11) 
CONT C ( 1) TO H(12) 
REST 0.054, 0.002 = H(11,U[ISO]) 
REST 0.054, 0.002 = H(12,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(11) TO C ( 1) TO C(1,-1,2,0,0,1) 
CONT H(11) TO C ( 1) TO P(1) 
CONT H(12) TO C ( 1) TO C(1,-1,2,0,0,1) 
CONT H(12) TO C ( 1) TO P(1) 
ANGLE 109.54, 2.0 = 
CONT H(11) TO C ( 1) TO H(12) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 12) TO H(121) 
CONT C ( 12) TO H(122) 
REST 0.128, 0.002 = H(121,U[ISO]) 
REST 0.128, 0.002 = H(122,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) 
CONT H(122) TO C ( 12) TO C(11) 
CONT H(122) TO C ( 12) TO C(13) 
ANGLE 109.54, 2.0 = 
CONT H(121) TO C ( 12) TO H(122) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 13) TO H(131) 
CONT C ( 13) TO H(132) 
REST 0.102, 0.002 = H(131,U[ISO]) 
REST 0.102, 0.002 = H(132,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(131) TO C ( 13) TO C(12) 
CONT H(131) TO C ( 13) TO C(14) 
CONT H(132) TO C ( 13) TO C(12) 
CONT H(132) TO C ( 13) TO C(14) 
ANGLE 109.54, 2.0 = 
CONT H(131) TO C ( 13) TO H(132) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 14) TO H(141) 
REST 0.138, 0.002 = H(141,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(141) TO C ( 14) TO C(13) 
CONT H(141) TO C ( 14) TO C(15) 
PLANAR C ( 14) C(13) C(15) H(141) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 15) TO H(151) 
REST 0.139, 0.002 = H(151,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(151) TO C ( 15) TO C(14) 
CONT H(151) TO C ( 15) TO C(16) 
PLANAR C ( 15) C(14) C(16) H(151) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 16) TO H(161) 
CONT C ( 16) TO H(162) 
REST 0.084, 0.002 = H(161,U[ISO]) 
REST 0.084, 0.002 = H(162,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(161) TO C ( 16) TO C(15) 
CONT H(161) TO C ( 16) TO C(11) 
CONT H(162) TO C ( 16) TO C(15) 
CONT H(162) TO C ( 16) TO C(11) 
ANGLE 109.54, 2.0 = 
CONT H(161) TO C ( 16) TO H(162) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 21) TO H(211) 
REST 0.056, 0.002 = H(211,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(211) TO C ( 21) TO P(1) 
CONT H(211) TO C ( 21) TO C(22) 
CONT H(211) TO C ( 21) TO C(26) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 22) TO H(221) 
CONT C ( 22) TO H(222) 
REST 0.071, 0.002 = H(221,U[ISO]) 
REST 0.071, 0.002 = H(222,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) 
CONT H(222) TO C ( 22) TO C(21) 
CONT H(222) TO C ( 22) TO C(23) 
ANGLE 109.54, 2.0 = 
CONT H(221) TO C ( 22) TO H(222) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 23) TO H(231) 
CONT C ( 23) TO H(232) 
REST 0.079, 0.002 = H(231,U[ISO]) 
REST 0.079, 0.002 = H(232,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(231) TO C ( 23) TO C(22) 
CONT H(231) TO C ( 23) TO C(24) 
CONT H(232) TO C ( 23) TO C(22) 
CONT H(232) TO C ( 23) TO C(24) 
ANGLE 109.54, 2.0 = 
CONT H(231) TO C ( 23) TO H(232) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 24) TO H(241) 
CONT C ( 24) TO H(242) 
REST 0.092, 0.002 = H(241,U[ISO]) 
REST 0.092, 0.002 = H(242,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(241) TO C ( 24) TO C(23) 
CONT H(241) TO C ( 24) TO C(25) 
CONT H(242) TO C ( 24) TO C(23) 
CONT H(242) TO C ( 24) TO C(25) 
ANGLE 109.54, 2.0 = 
CONT H(241) TO C ( 24) TO H(242) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 25) TO H(251) 
CONT C ( 25) TO H(252) 
REST 0.109, 0.002 = H(251,U[ISO]) 
REST 0.109, 0.002 = H(252,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(251) TO C ( 25) TO C(24) 
CONT H(251) TO C ( 25) TO C(26) 
CONT H(252) TO C ( 25) TO C(24) 
CONT H(252) TO C ( 25) TO C(26) 
ANGLE 109.54, 2.0 = 
CONT H(251) TO C ( 25) TO H(252) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 26) TO H(261) 
CONT C ( 26) TO H(262) 
REST 0.086, 0.002 = H(261,U[ISO]) 
REST 0.086, 0.002 = H(262,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(261) TO C ( 26) TO C(21) 
CONT H(261) TO C ( 26) TO C(25) 
CONT H(262) TO C ( 26) TO C(21) 
CONT H(262) TO C ( 26) TO C(25) 
ANGLE 109.54, 2.0 = 
CONT H(261) TO C ( 26) TO H(262) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


