# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
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data_107nprt13
_audit_creation_date             13-09-23
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title '107nprt13 in C 2/c'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   35.4499(3)
_cell_length_b                   11.14380(10)
_cell_length_c                   25.1650(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.2861(3)
_cell_angle_gamma                90
_cell_volume                     9633.92(14)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc'
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'
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'
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'


_cell_formula_units_Z            8

# Given Formula = C41.25 H55 B1.38 F20.62 N2.75 
# Dc =      1.37 Fooo =   4160.00 Mu =      1.36 M =    996.11
# Found Formula = C53 H48 B1 F15 N2 
# Dc =      1.39 FOOO =   4160.00 Mu =      1.21 M =   1008.76

_chemical_formula_sum            'C53 H48 B1 F15 N2'
_chemical_formula_moiety         'C53 H48 B1 F15 N2'
_chemical_compound_source        .
_chemical_formula_weight         1008.76


_cell_measurement_reflns_used    11382
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.090
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.210

_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             4160
_exptl_absorpt_coefficient_mu    0.121

# Sheldrick geometric approximatio 0.99 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_T_max  0.99
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            134500
_reflns_number_total             10963
_diffrn_reflns_av_R_equivalents  0.027
# Number of reflections without Friedels Law is 21331 
# Number of reflections with Friedels Law is 10963 
# Theoretical number of reflections is about 11036 


_diffrn_reflns_theta_min         5.106
_diffrn_reflns_theta_max         27.473
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        26.923
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_reflns_limit_h_min              -46
_reflns_limit_h_max              44
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              32

_oxford_diffrn_Wilson_B_factor   3.13
_oxford_diffrn_Wilson_scale      45.71

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

_refine_diff_density_min         -0.52
_refine_diff_density_max         0.89


# 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>0.0\s(I)
_refine_ls_number_reflns         10962
_refine_ls_number_restraints     0
_refine_ls_number_parameters     640
_oxford_refine_ls_R_factor_ref   0.0875
_refine_ls_wR_factor_ref         0.1603
_refine_ls_goodness_of_fit_ref   0.9296
_refine_ls_shift/su_max          0.0006195
_refine_ls_shift/su_mean         0.0000308


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10963
_refine_ls_R_factor_all          0.0875
_refine_ls_wR_factor_all         0.1603

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7870
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_gt          0.1340

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #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: 
 23.0 34.1 16.0 3.82 
;

# 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
F1 F 0.47512(4) 0.18460(13) 0.49430(6) 0.0359 1.0000 Uani . . . . . .
C2 C 0.47691(7) 0.1356(2) 0.54392(10) 0.0304 1.0000 Uani . . . . . .
C3 C 0.44579(6) 0.1531(2) 0.56814(9) 0.0286 1.0000 Uani . . . . . .
C4 C 0.45129(7) 0.0964(2) 0.61854(10) 0.0313 1.0000 Uani . . . . . .
F5 F 0.42414(4) 0.10369(13) 0.64841(6) 0.0389 1.0000 Uani . . . . . .
C6 C 0.48391(8) 0.0295(2) 0.64305(10) 0.0360 1.0000 Uani . . . . . .
F7 F 0.48734(5) -0.02016(15) 0.69278(6) 0.0483 1.0000 Uani . . . . . .
C8 C 0.51354(7) 0.0171(2) 0.61716(11) 0.0372 1.0000 Uani . . . . . .
C9 C 0.51011(7) 0.0712(2) 0.56709(11) 0.0342 1.0000 Uani . . . . . .
F10 F 0.53906(4) 0.06083(13) 0.54150(7) 0.0432 1.0000 Uani . . . . . .
F11 F 0.54565(5) -0.04599(15) 0.64078(7) 0.0516 1.0000 Uani . . . . . .
B12 B 0.40648(7) 0.2238(2) 0.53281(10) 0.0279 1.0000 Uani . . . . . .
C13 C 0.37221(6) 0.2505(2) 0.56611(9) 0.0291 1.0000 Uani . . . . . .
C14 C 0.37492(6) 0.3689(2) 0.59703(9) 0.0296 1.0000 Uani . . . . . .
N15 N 0.34217(5) 0.38841(18) 0.62474(8) 0.0295 1.0000 Uani . . . . . .
C16 C 0.35568(6) 0.4434(2) 0.67164(9) 0.0299 1.0000 Uani . . . . . .
N17 N 0.39355(5) 0.45629(17) 0.68502(8) 0.0288 1.0000 Uani . . . . . .
C18 C 0.41020(7) 0.3876(2) 0.64554(10) 0.0332 1.0000 Uani . . . . . .
C19 C 0.41505(7) 0.5145(2) 0.73447(10) 0.0337 1.0000 Uani . . . . . .
C20 C 0.42688(7) 0.4470(3) 0.78213(10) 0.0384 1.0000 Uani . . . . . .
C21 C 0.42039(9) 0.3126(3) 0.78266(12) 0.0461 1.0000 Uani . . . . . .
C22 C 0.40738(14) 0.2692(4) 0.83307(18) 0.0835 1.0000 Uani . . . . . .
C23 C 0.45719(10) 0.2460(3) 0.77888(14) 0.0628 1.0000 Uani . . . . . .
C24 C 0.44628(9) 0.5087(4) 0.82961(12) 0.0570 1.0000 Uani . . . . . .
C25 C 0.45302(11) 0.6308(4) 0.82804(16) 0.0707 1.0000 Uani . . . . . .
C26 C 0.44162(10) 0.6935(3) 0.78017(17) 0.0674 1.0000 Uani . . . . . .
C27 C 0.42205(8) 0.6377(3) 0.73178(13) 0.0477 1.0000 Uani . . . . . .
C28 C 0.40961(11) 0.7079(3) 0.67853(17) 0.0667 1.0000 Uani . . . . . .
C29 C 0.44236(16) 0.7151(4) 0.64878(19) 0.0855 1.0000 Uani . . . . . .
C30 C 0.39585(14) 0.8355(4) 0.6874(2) 0.0963 1.0000 Uani . . . . . .
C31 C 0.30145(6) 0.3611(2) 0.60276(10) 0.0304 1.0000 Uani . . . . . .
C32 C 0.27868(7) 0.4414(2) 0.56562(11) 0.0392 1.0000 Uani . . . . . .
C33 C 0.23898(8) 0.4151(3) 0.54785(13) 0.0483 1.0000 Uani . . . . . .
C34 C 0.22332(8) 0.3160(3) 0.56659(13) 0.0484 1.0000 Uani . . . . . .
C35 C 0.24675(8) 0.2372(3) 0.60233(13) 0.0449 1.0000 Uani . . . . . .
C36 C 0.28667(7) 0.2565(2) 0.62099(11) 0.0365 1.0000 Uani . . . . . .
C37 C 0.31230(8) 0.1687(3) 0.65981(12) 0.0456 1.0000 Uani . . . . . .
C38 C 0.30817(10) 0.1835(4) 0.71866(14) 0.0657 1.0000 Uani . . . . . .
C39 C 0.30459(11) 0.0398(3) 0.64026(18) 0.0702 1.0000 Uani . . . . . .
C40 C 0.29533(8) 0.5530(3) 0.54477(15) 0.0553 1.0000 Uani . . . . . .
C41 C 0.28272(16) 0.6672(3) 0.56833(17) 0.0856 1.0000 Uani . . . . . .
C42 C 0.28497(15) 0.5599(3) 0.48302(17) 0.0791 1.0000 Uani . . . . . .
C43 C 0.41658(6) 0.3574(2) 0.51075(9) 0.0290 1.0000 Uani . . . . . .
C44 C 0.38808(7) 0.4219(2) 0.47361(10) 0.0329 1.0000 Uani . . . . . .
F45 F 0.35355(4) 0.36877(13) 0.45034(6) 0.0396 1.0000 Uani . . . . . .
C46 C 0.39144(8) 0.5405(2) 0.45954(11) 0.0425 1.0000 Uani . . . . . .
F47 F 0.36199(6) 0.59624(16) 0.42410(8) 0.0582 1.0000 Uani . . . . . .
C48 C 0.42501(9) 0.6024(2) 0.48307(12) 0.0459 1.0000 Uani . . . . . .
F49 F 0.42852(7) 0.71861(15) 0.47062(8) 0.0671 1.0000 Uani . . . . . .
C50 C 0.45436(8) 0.5441(2) 0.51937(11) 0.0404 1.0000 Uani . . . . . .
C51 C 0.44959(7) 0.4252(2) 0.53261(10) 0.0331 1.0000 Uani . . . . . .
F52 F 0.47983(4) 0.37909(13) 0.57116(6) 0.0407 1.0000 Uani . . . . . .
F53 F 0.48751(5) 0.60254(15) 0.54297(7) 0.0540 1.0000 Uani . . . . . .
C54 C 0.38790(6) 0.1272(2) 0.48287(9) 0.0290 1.0000 Uani . . . . . .
C55 C 0.38701(7) 0.1361(2) 0.42744(10) 0.0330 1.0000 Uani . . . . . .
F56 F 0.40358(4) 0.23041(14) 0.40829(6) 0.0401 1.0000 Uani . . . . . .
C57 C 0.36967(7) 0.0522(3) 0.38836(10) 0.0387 1.0000 Uani . . . . . .
F58 F 0.36924(5) 0.06811(17) 0.33505(6) 0.0529 1.0000 Uani . . . . . .
C59 C 0.35236(8) -0.0481(3) 0.40353(12) 0.0437 1.0000 Uani . . . . . .
F60 F 0.33461(5) -0.12867(17) 0.36592(8) 0.0622 1.0000 Uani . . . . . .
C61 C 0.35362(8) -0.0644(2) 0.45794(12) 0.0416 1.0000 Uani . . . . . .
C62 C 0.37111(7) 0.0211(2) 0.49557(10) 0.0341 1.0000 Uani . . . . . .
F63 F 0.37131(5) -0.00361(13) 0.54841(6) 0.0442 1.0000 Uani . . . . . .
F64 F 0.33719(6) -0.16282(15) 0.47407(8) 0.0595 1.0000 Uani . . . . . .
C65 C 0.27590(15) 0.3961(5) 0.2130(2) 0.0871 1.0000 Uani . . . . . .
C66 C 0.27004(14) 0.4922(5) 0.2392(3) 0.0946 1.0000 Uani . . . . . .
C67 C 0.23946(19) 0.5718(6) 0.2232(3) 0.1420 1.0000 Uani . . . . . .
C68 C 0.29778(16) 0.5147(5) 0.2927(2) 0.0880 1.0000 Uani . . . . . .
C69 C 0.3276(2) 0.4302(6) 0.3051(3) 0.1194 1.0000 Uani . . . . . .
C70 C 0.33277(16) 0.3362(5) 0.2780(3) 0.1012 1.0000 Uani . . . . . .
C71 C 0.30398(17) 0.3185(6) 0.2264(3) 0.1038 1.0000 Uani . . . . . .
H132 H 0.3715 0.1860 0.5917 0.0349 1.0000 Uiso R . . . . .
H131 H 0.3472 0.2531 0.5379 0.0354 1.0000 Uiso R . . . . .
H141 H 0.3735 0.4371 0.5709 0.0356 1.0000 Uiso R . . . . .
H161 H 0.3395 0.4734 0.6941 0.0367 1.0000 Uiso R . . . . .
H182 H 0.4307 0.4340 0.6355 0.0402 1.0000 Uiso R . . . . .
H181 H 0.4200 0.3110 0.6619 0.0404 1.0000 Uiso R . . . . .
H211 H 0.3998 0.2923 0.7501 0.0543 1.0000 Uiso R . . . . .
H222 H 0.4013 0.1826 0.8295 0.1268 1.0000 Uiso R . . . . .
H221 H 0.4278 0.2822 0.8660 0.1271 1.0000 Uiso R . . . . .
H223 H 0.3841 0.3140 0.8361 0.1266 1.0000 Uiso R . . . . .
H232 H 0.4522 0.1585 0.7760 0.0949 1.0000 Uiso R . . . . .
H231 H 0.4779 0.2593 0.8119 0.0944 1.0000 Uiso R . . . . .
H233 H 0.4663 0.2736 0.7470 0.0946 1.0000 Uiso R . . . . .
H241 H 0.4547 0.4651 0.8622 0.0678 1.0000 Uiso R . . . . .
H251 H 0.4661 0.6711 0.8608 0.0842 1.0000 Uiso R . . . . .
H261 H 0.4472 0.7772 0.7799 0.0822 1.0000 Uiso R . . . . .
H281 H 0.3877 0.6646 0.6548 0.0794 1.0000 Uiso R . . . . .
H291 H 0.4337 0.7623 0.6152 0.1292 1.0000 Uiso R . . . . .
H293 H 0.4646 0.7546 0.6737 0.1288 1.0000 Uiso R . . . . .
H292 H 0.4499 0.6340 0.6395 0.1287 1.0000 Uiso R . . . . .
H301 H 0.3858 0.8726 0.6513 0.1460 1.0000 Uiso R . . . . .
H303 H 0.4181 0.8819 0.7082 0.1461 1.0000 Uiso R . . . . .
H302 H 0.3755 0.8291 0.7071 0.1459 1.0000 Uiso R . . . . .
H331 H 0.2227 0.4684 0.5232 0.0579 1.0000 Uiso R . . . . .
H341 H 0.1955 0.3025 0.5551 0.0583 1.0000 Uiso R . . . . .
H351 H 0.2362 0.1696 0.6145 0.0544 1.0000 Uiso R . . . . .
H371 H 0.3395 0.1895 0.6601 0.0541 1.0000 Uiso R . . . . .
H383 H 0.3253 0.1265 0.7433 0.0985 1.0000 Uiso R . . . . .
H382 H 0.3147 0.2656 0.7304 0.0992 1.0000 Uiso R . . . . .
H381 H 0.2813 0.1665 0.7187 0.0983 1.0000 Uiso R . . . . .
H393 H 0.3229 -0.0137 0.6641 0.1056 1.0000 Uiso R . . . . .
H392 H 0.2784 0.0165 0.6408 0.1056 1.0000 Uiso R . . . . .
H391 H 0.3070 0.0323 0.6026 0.1055 1.0000 Uiso R . . . . .
H401 H 0.3238 0.5475 0.5566 0.0682 1.0000 Uiso R . . . . .
H412 H 0.2937 0.7359 0.5545 0.1285 1.0000 Uiso R . . . . .
H411 H 0.2911 0.6646 0.6080 0.1288 1.0000 Uiso R . . . . .
H413 H 0.2545 0.6711 0.5571 0.1293 1.0000 Uiso R . . . . .
H422 H 0.2984 0.6287 0.4724 0.1204 1.0000 Uiso R . . . . .
H421 H 0.2932 0.4860 0.4688 0.1211 1.0000 Uiso R . . . . .
H423 H 0.2569 0.5705 0.4705 0.1208 1.0000 Uiso R . . . . .
H672 H 0.2459 0.6370 0.2520 0.2213 1.0000 Uiso R . . . . .
H671 H 0.2390 0.6035 0.1860 0.2208 1.0000 Uiso R . . . . .
H673 H 0.2139 0.5315 0.2235 0.2205 1.0000 Uiso R . . . . .
H651 H 0.2554 0.3883 0.1787 0.1134 1.0000 Uiso R . . . . .
H681 H 0.2925 0.5873 0.3164 0.1124 1.0000 Uiso R . . . . .
H691 H 0.3467 0.4422 0.3389 0.1462 1.0000 Uiso R . . . . .
H701 H 0.3537 0.2804 0.2909 0.1258 1.0000 Uiso R . . . . .
H711 H 0.3061 0.2475 0.2024 0.1330 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.16409(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
F1 . C2 . 1.350(3) yes
C2 . C3 . 1.400(3) yes
C2 . C9 . 1.379(3) yes
C3 . C4 . 1.387(3) yes
C3 . B12 . 1.656(3) yes
C4 . F5 . 1.362(3) yes
C4 . C6 . 1.387(3) yes
C6 . F7 . 1.346(3) yes
C6 . C8 . 1.373(4) yes
C8 . C9 . 1.375(4) yes
C8 . F11 . 1.345(3) yes
C9 . F10 . 1.344(3) yes
B12 . C13 . 1.664(3) yes
B12 . C43 . 1.659(3) yes
B12 . C54 . 1.662(3) yes
C13 . C14 . 1.522(3) yes
C13 . H132 . 0.971 no
C13 . H131 . 0.989 no
C14 . N15 . 1.510(3) yes
C14 . C18 . 1.531(3) yes
C14 . H141 . 0.999 no
N15 . C16 . 1.311(3) yes
N15 . C31 . 1.445(3) yes
C16 . N17 . 1.309(3) yes
C16 . H161 . 0.961 no
N17 . C18 . 1.487(3) yes
N17 . C19 . 1.443(3) yes
C18 . H182 . 0.974 no
C18 . H181 . 0.973 no
C19 . C20 . 1.390(4) yes
C19 . C27 . 1.399(4) yes
C20 . C21 . 1.516(4) yes
C20 . C24 . 1.403(4) yes
C21 . C22 . 1.531(4) yes
C21 . C23 . 1.524(4) yes
C21 . H211 . 0.981 no
C22 . H222 . 0.988 no
C22 . H221 . 0.967 no
C22 . H223 . 0.984 no
C23 . H232 . 0.991 no
C23 . H231 . 0.974 no
C23 . H233 . 0.986 no
C24 . C25 . 1.384(5) yes
C24 . H241 . 0.936 no
C25 . C26 . 1.364(6) yes
C25 . H251 . 0.953 no
C26 . C27 . 1.391(4) yes
C26 . H261 . 0.954 no
C27 . C28 . 1.520(5) yes
C28 . C29 . 1.531(6) yes
C28 . C30 . 1.538(5) yes
C28 . H281 . 0.983 no
C29 . H291 . 0.978 no
C29 . H293 . 0.983 no
C29 . H292 . 0.987 no
C30 . H301 . 0.981 no
C30 . H303 . 0.980 no
C30 . H302 . 0.974 no
C31 . C32 . 1.398(3) yes
C31 . C36 . 1.401(3) yes
C32 . C33 . 1.398(4) yes
C32 . C40 . 1.524(4) yes
C33 . C34 . 1.371(4) yes
C33 . H331 . 0.946 no
C34 . C35 . 1.379(4) yes
C34 . H341 . 0.967 no
C35 . C36 . 1.393(3) yes
C35 . H351 . 0.926 no
C36 . C37 . 1.516(4) yes
C37 . C38 . 1.532(4) yes
C37 . C39 . 1.521(5) yes
C37 . H371 . 0.990 no
C38 . H383 . 0.985 no
C38 . H382 . 0.972 no
C38 . H381 . 0.973 no
C39 . H393 . 0.971 no
C39 . H392 . 0.967 no
C39 . H391 . 0.975 no
C40 . C41 . 1.517(5) yes
C40 . C42 . 1.508(5) yes
C40 . H401 . 0.983 no
C41 . H412 . 0.962 no
C41 . H411 . 0.970 no
C41 . H413 . 0.971 no
C42 . H422 . 0.974 no
C42 . H421 . 0.972 no
C42 . H423 . 0.973 no
C43 . C44 . 1.395(3) yes
C43 . C51 . 1.387(3) yes
C44 . F45 . 1.356(3) yes
C44 . C46 . 1.382(3) yes
C46 . F47 . 1.346(3) yes
C46 . C48 . 1.376(4) yes
C48 . F49 . 1.345(3) yes
C48 . C50 . 1.367(4) yes
C50 . C51 . 1.387(3) yes
C50 . F53 . 1.347(3) yes
C51 . F52 . 1.357(3) yes
C54 . C55 . 1.391(3) yes
C54 . C62 . 1.396(3) yes
C55 . F56 . 1.350(3) yes
C55 . C57 . 1.386(3) yes
C57 . F58 . 1.349(3) yes
C57 . C59 . 1.373(4) yes
C59 . F60 . 1.343(3) yes
C59 . C61 . 1.371(4) yes
C61 . C62 . 1.379(3) yes
C61 . F64 . 1.350(3) yes
C62 . F63 . 1.356(3) yes
C65 . C66 . 1.301(7) yes
C65 . C71 . 1.298(7) yes
C65 . H651 . 0.986 no
C66 . C67 . 1.381(7) yes
C66 . C68 . 1.480(7) yes
C67 . H672 . 1.013 no
C67 . H671 . 0.996 no
C67 . H673 . 1.012 no
C68 . C69 . 1.393(8) yes
C68 . H681 . 1.049 no
C69 . C70 . 1.288(8) yes
C69 . H691 . 0.956 no
C70 . C71 . 1.454(8) yes
C70 . H701 . 0.961 no
C71 . H711 . 1.009 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F1 . C2 . C3 . 119.0(2) yes
F1 . C2 . C9 . 116.2(2) yes
C3 . C2 . C9 . 124.8(2) yes
C2 . C3 . C4 . 112.7(2) yes
C2 . C3 . B12 . 118.8(2) yes
C4 . C3 . B12 . 128.1(2) yes
C3 . C4 . F5 . 121.2(2) yes
C3 . C4 . C6 . 124.5(2) yes
F5 . C4 . C6 . 114.3(2) yes
C4 . C6 . F7 . 120.6(2) yes
C4 . C6 . C8 . 119.6(2) yes
F7 . C6 . C8 . 119.7(2) yes
C6 . C8 . C9 . 119.1(2) yes
C6 . C8 . F11 . 120.4(2) yes
C9 . C8 . F11 . 120.5(2) yes
C2 . C9 . C8 . 119.3(2) yes
C2 . C9 . F10 . 121.0(2) yes
C8 . C9 . F10 . 119.7(2) yes
C3 . B12 . C13 . 115.92(18) yes
C3 . B12 . C43 . 112.57(18) yes
C13 . B12 . C43 . 104.64(18) yes
C3 . B12 . C54 . 102.85(17) yes
C13 . B12 . C54 . 107.12(17) yes
C43 . B12 . C54 . 113.95(18) yes
B12 . C13 . C14 . 116.79(18) yes
B12 . C13 . H132 . 110.2 no
C14 . C13 . H132 . 108.1 no
B12 . C13 . H131 . 106.2 no
C14 . C13 . H131 . 105.9 no
H132 . C13 . H131 . 109.4 no
C13 . C14 . N15 . 113.72(18) yes
C13 . C14 . C18 . 117.50(19) yes
N15 . C14 . C18 . 100.49(17) yes
C13 . C14 . H141 . 109.6 no
N15 . C14 . H141 . 106.0 no
C18 . C14 . H141 . 108.6 no
C14 . N15 . C16 . 109.34(18) yes
C14 . N15 . C31 . 127.01(18) yes
C16 . N15 . C31 . 123.48(19) yes
N15 . C16 . N17 . 114.0(2) yes
N15 . C16 . H161 . 123.6 no
N17 . C16 . H161 . 122.3 no
C16 . N17 . C18 . 108.83(18) yes
C16 . N17 . C19 . 124.13(19) yes
C18 . N17 . C19 . 126.55(18) yes
C14 . C18 . N17 . 102.82(17) yes
C14 . C18 . H182 . 112.4 no
N17 . C18 . H182 . 110.1 no
C14 . C18 . H181 . 110.6 no
N17 . C18 . H181 . 109.2 no
H182 . C18 . H181 . 111.4 no
N17 . C19 . C20 . 118.9(2) yes
N17 . C19 . C27 . 117.5(2) yes
C20 . C19 . C27 . 123.6(2) yes
C19 . C20 . C21 . 121.9(2) yes
C19 . C20 . C24 . 116.8(3) yes
C21 . C20 . C24 . 121.3(3) yes
C20 . C21 . C22 . 113.4(3) yes
C20 . C21 . C23 . 110.3(3) yes
C22 . C21 . C23 . 109.6(3) yes
C20 . C21 . H211 . 107.7 no
C22 . C21 . H211 . 107.8 no
C23 . C21 . H211 . 107.9 no
C21 . C22 . H222 . 109.7 no
C21 . C22 . H221 . 110.4 no
H222 . C22 . H221 . 109.0 no
C21 . C22 . H223 . 109.5 no
H222 . C22 . H223 . 109.4 no
H221 . C22 . H223 . 108.7 no
C21 . C23 . H232 . 110.1 no
C21 . C23 . H231 . 110.3 no
H232 . C23 . H231 . 107.2 no
C21 . C23 . H233 . 110.8 no
H232 . C23 . H233 . 109.6 no
H231 . C23 . H233 . 108.7 no
C20 . C24 . C25 . 120.6(3) yes
C20 . C24 . H241 . 118.3 no
C25 . C24 . H241 . 121.1 no
C24 . C25 . C26 . 120.9(3) yes
C24 . C25 . H251 . 119.3 no
C26 . C25 . H251 . 119.9 no
C25 . C26 . C27 . 121.3(3) yes
C25 . C26 . H261 . 119.3 no
C27 . C26 . H261 . 119.4 no
C19 . C27 . C26 . 116.9(3) yes
C19 . C27 . C28 . 122.1(3) yes
C26 . C27 . C28 . 121.0(3) yes
C27 . C28 . C29 . 111.6(3) yes
C27 . C28 . C30 . 112.4(4) yes
C29 . C28 . C30 . 109.2(3) yes
C27 . C28 . H281 . 107.2 no
C29 . C28 . H281 . 108.1 no
C30 . C28 . H281 . 108.1 no
C28 . C29 . H291 . 109.6 no
C28 . C29 . H293 . 107.3 no
H291 . C29 . H293 . 110.0 no
C28 . C29 . H292 . 110.5 no
H291 . C29 . H292 . 109.5 no
H293 . C29 . H292 . 109.9 no
C28 . C30 . H301 . 108.1 no
C28 . C30 . H303 . 108.8 no
H301 . C30 . H303 . 109.5 no
C28 . C30 . H302 . 107.9 no
H301 . C30 . H302 . 110.9 no
H303 . C30 . H302 . 111.5 no
N15 . C31 . C32 . 118.6(2) yes
N15 . C31 . C36 . 118.0(2) yes
C32 . C31 . C36 . 123.4(2) yes
C31 . C32 . C33 . 116.7(2) yes
C31 . C32 . C40 . 122.9(2) yes
C33 . C32 . C40 . 120.4(2) yes
C32 . C33 . C34 . 121.3(3) yes
C32 . C33 . H331 . 118.8 no
C34 . C33 . H331 . 119.8 no
C33 . C34 . C35 . 120.5(2) yes
C33 . C34 . H341 . 119.5 no
C35 . C34 . H341 . 120.1 no
C34 . C35 . C36 . 121.3(3) yes
C34 . C35 . H351 . 120.4 no
C36 . C35 . H351 . 118.2 no
C31 . C36 . C35 . 116.7(2) yes
C31 . C36 . C37 . 122.3(2) yes
C35 . C36 . C37 . 121.0(2) yes
C36 . C37 . C38 . 111.6(2) yes
C36 . C37 . C39 . 111.7(3) yes
C38 . C37 . C39 . 111.2(3) yes
C36 . C37 . H371 . 106.4 no
C38 . C37 . H371 . 107.0 no
C39 . C37 . H371 . 108.6 no
C37 . C38 . H383 . 110.4 no
C37 . C38 . H382 . 108.9 no
H383 . C38 . H382 . 110.6 no
C37 . C38 . H381 . 108.0 no
H383 . C38 . H381 . 108.9 no
H382 . C38 . H381 . 110.1 no
C37 . C39 . H393 . 109.9 no
C37 . C39 . H392 . 110.2 no
H393 . C39 . H392 . 108.8 no
C37 . C39 . H391 . 110.1 no
H393 . C39 . H391 . 110.1 no
H392 . C39 . H391 . 107.7 no
C32 . C40 . C41 . 111.9(3) yes
C32 . C40 . C42 . 112.3(3) yes
C41 . C40 . C42 . 109.9(3) yes
C32 . C40 . H401 . 107.6 no
C41 . C40 . H401 . 108.3 no
C42 . C40 . H401 . 106.6 no
C40 . C41 . H412 . 109.9 no
C40 . C41 . H411 . 109.4 no
H412 . C41 . H411 . 110.3 no
C40 . C41 . H413 . 107.8 no
H412 . C41 . H413 . 109.9 no
H411 . C41 . H413 . 109.4 no
C40 . C42 . H422 . 108.2 no
C40 . C42 . H421 . 108.5 no
H422 . C42 . H421 . 110.7 no
C40 . C42 . H423 . 108.1 no
H422 . C42 . H423 . 110.2 no
H421 . C42 . H423 . 111.1 no
B12 . C43 . C44 . 120.4(2) yes
B12 . C43 . C51 . 125.9(2) yes
C44 . C43 . C51 . 112.7(2) yes
C43 . C44 . F45 . 119.5(2) yes
C43 . C44 . C46 . 124.8(2) yes
F45 . C44 . C46 . 115.7(2) yes
C44 . C46 . F47 . 120.6(3) yes
C44 . C46 . C48 . 119.3(3) yes
F47 . C46 . C48 . 120.0(2) yes
C46 . C48 . F49 . 120.1(3) yes
C46 . C48 . C50 . 118.9(2) yes
F49 . C48 . C50 . 120.9(3) yes
C48 . C50 . C51 . 119.8(2) yes
C48 . C50 . F53 . 120.1(2) yes
C51 . C50 . F53 . 120.1(2) yes
C43 . C51 . C50 . 124.5(2) yes
C43 . C51 . F52 . 121.2(2) yes
C50 . C51 . F52 . 114.3(2) yes
B12 . C54 . C55 . 128.3(2) yes
B12 . C54 . C62 . 119.1(2) yes
C55 . C54 . C62 . 112.6(2) yes
C54 . C55 . F56 . 120.6(2) yes
C54 . C55 . C57 . 124.1(2) yes
F56 . C55 . C57 . 115.3(2) yes
C55 . C57 . F58 . 120.8(2) yes
C55 . C57 . C59 . 120.1(2) yes
F58 . C57 . C59 . 119.1(2) yes
C57 . C59 . F60 . 120.8(3) yes
C57 . C59 . C61 . 118.6(2) yes
F60 . C59 . C61 . 120.6(3) yes
C59 . C61 . C62 . 119.5(2) yes
C59 . C61 . F64 . 119.9(2) yes
C62 . C61 . F64 . 120.6(2) yes
C54 . C62 . C61 . 125.0(2) yes
C54 . C62 . F63 . 119.8(2) yes
C61 . C62 . F63 . 115.2(2) yes
C66 . C65 . C71 . 128.7(6) yes
C66 . C65 . H651 . 109.9 no
C71 . C65 . H651 . 121.4 no
C65 . C66 . C67 . 126.4(7) yes
C65 . C66 . C68 . 116.5(5) yes
C67 . C66 . C68 . 117.0(6) yes
C66 . C67 . H672 . 103.2 no
C66 . C67 . H671 . 109.3 no
H672 . C67 . H671 . 111.5 no
C66 . C67 . H673 . 110.6 no
H672 . C67 . H673 . 111.0 no
H671 . C67 . H673 . 111.0 no
C66 . C68 . C69 . 112.8(5) yes
C66 . C68 . H681 . 118.5 no
C69 . C68 . H681 . 128.7 no
C68 . C69 . C70 . 129.0(7) yes
C68 . C69 . H691 . 116.0 no
C70 . C69 . H691 . 115.0 no
C69 . C70 . C71 . 115.1(6) yes
C69 . C70 . H701 . 123.0 no
C71 . C70 . H701 . 121.8 no
C70 . C71 . C65 . 117.7(6) yes
C70 . C71 . H711 . 120.1 no
C65 . C71 . H711 . 122.2 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 23/09/13 at 15:48:56
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 231,X'S) H   ( 233,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   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 293,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 303,X'S) H   ( 302,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   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 383,X'S) H   ( 382,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 393,X'S) H   ( 392,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 412,X'S) H   ( 411,X'S) H   ( 413,X'S) 
RIDE C   (  42,X'S) H   ( 422,X'S) H   ( 421,X'S) H   ( 423,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) H   ( 673,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 23/09/13 at 15:48:56
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_database_code_depnum_ccdc_archive 'CCDC 1006573'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_186NPRT14
_audit_creation_date             2014-03-30
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '186NPRT14 in P 21/n'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   10.44290(10)
_cell_length_b                   32.1025(5)
_cell_length_c                   12.9291(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.0078(12)
_cell_angle_gamma                90
_cell_volume                     4268.44(10)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn'
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'
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'
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'
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'


_cell_formula_units_Z            4

# Given Formula = C40 H40 B0.25 F3 N2 
# Dc =      0.95 Fooo =   1912.00 Mu =      5.13 M =    608.47
# Found Formula = C47 H42 B1 F15 N2 
# Dc =      1.45 FOOO =   1912.00 Mu =     11.35 M =    930.64

_chemical_formula_sum            'C47 H42 B1 F15 N2'
_chemical_formula_moiety         'C47 H42 B1 F15 N2'
_chemical_compound_source        .
_chemical_formula_weight         930.64


_cell_measurement_reflns_used    12863
_cell_measurement_theta_min      3
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_max          0.220

_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    1.135

# Sheldrick geometric approximatio 0.79 0.84 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.84
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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            25214
_reflns_number_total             8853
_diffrn_reflns_av_R_equivalents  0.049
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8853 
# Theoretical number of reflections is about 17890 


_diffrn_reflns_theta_min         3.735
_diffrn_reflns_theta_max         76.281
_diffrn_measured_fraction_theta_max 0.989

_diffrn_reflns_theta_full        73.992
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              -13
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              40
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.67
_oxford_diffrn_Wilson_scale      0.02

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

_refine_diff_density_min         -0.29
_refine_diff_density_max         0.40


# 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>-3.0\s(I)
_refine_ls_number_reflns         8821
_refine_ls_number_restraints     0
_refine_ls_number_parameters     587
_oxford_refine_ls_R_factor_ref   0.0492
_refine_ls_wR_factor_ref         0.1281
_refine_ls_goodness_of_fit_ref   1.0077
_refine_ls_shift/su_max          0.0008770
_refine_ls_shift/su_mean         0.0000719


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8821
_refine_ls_R_factor_all          0.0492
_refine_ls_wR_factor_all         0.1281

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8278
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_gt          0.1258

# 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= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 2.02P] 
 ,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
F1 F 1.07596(10) 0.60187(3) 1.56552(7) 0.0346 1.0000 Uani . . . . . .
C2 C 1.00775(15) 0.61118(5) 1.47027(11) 0.0249 1.0000 Uani . . . . . .
C3 C 1.04852(14) 0.59775(5) 1.38065(12) 0.0249 1.0000 Uani . . . . . .
F4 F 1.15798(9) 0.57533(4) 1.38770(8) 0.0360 1.0000 Uani . . . . . .
C5 C 0.97524(14) 0.60724(5) 1.28288(11) 0.0220 1.0000 Uani . . . . . .
F6 F 1.02350(9) 0.59233(3) 1.19996(7) 0.0314 1.0000 Uani . . . . . .
C7 C 0.86037(13) 0.62978(4) 1.26875(10) 0.0185 1.0000 Uani . . . . . .
C8 C 0.82423(14) 0.64189(4) 1.36301(11) 0.0208 1.0000 Uani . . . . . .
C9 C 0.89462(15) 0.63379(5) 1.46172(11) 0.0237 1.0000 Uani . . . . . .
F10 F 0.85352(10) 0.64776(3) 1.54828(7) 0.0331 1.0000 Uani . . . . . .
F11 F 0.71330(9) 0.66349(3) 1.36171(7) 0.0283 1.0000 Uani . . . . . .
B12 B 0.76401(14) 0.64045(5) 1.15503(11) 0.0165 1.0000 Uani . . . . . .
C13 C 0.64383(13) 0.60661(5) 1.16078(10) 0.0202 1.0000 Uani . . . . . .
C14 C 0.53254(14) 0.61410(5) 1.20349(11) 0.0234 1.0000 Uani . . . . . .
F15 F 0.49943(9) 0.65299(3) 1.22825(7) 0.0298 1.0000 Uani . . . . . .
C16 C 0.44756(15) 0.58356(6) 1.22640(13) 0.0316 1.0000 Uani . . . . . .
F17 F 0.34498(10) 0.59352(4) 1.27002(9) 0.0442 1.0000 Uani . . . . . .
C18 C 0.47021(17) 0.54247(6) 1.20435(15) 0.0383 1.0000 Uani . . . . . .
F19 F 0.39023(13) 0.51232(4) 1.22649(13) 0.0617 1.0000 Uani . . . . . .
C20 C 0.57683(18) 0.53288(5) 1.16029(15) 0.0352 1.0000 Uani . . . . . .
C21 C 0.66060(15) 0.56427(5) 1.14073(12) 0.0258 1.0000 Uani . . . . . .
F22 F 0.76591(10) 0.55092(3) 1.10280(8) 0.0334 1.0000 Uani . . . . . .
F23 F 0.60073(13) 0.49291(3) 1.13756(12) 0.0541 1.0000 Uani . . . . . .
C24 C 0.84056(13) 0.63491(4) 1.05351(10) 0.0176 1.0000 Uani . . . . . .
C25 C 0.76719(12) 0.65149(4) 0.94909(10) 0.0169 1.0000 Uani . . . . . .
N26 N 0.85221(11) 0.65347(4) 0.86629(9) 0.0170 1.0000 Uani . . . . . .
C27 C 0.83721(12) 0.62838(4) 0.78480(10) 0.0170 1.0000 Uani . . . . . .
N28 N 0.75626(11) 0.59642(4) 0.77051(9) 0.0182 1.0000 Uani . . . . . .
C29 C 0.74033(14) 0.57279(4) 0.67333(10) 0.0199 1.0000 Uani . . . . . .
C30 C 0.83695(15) 0.54404(5) 0.65823(12) 0.0246 1.0000 Uani . . . . . .
C31 C 0.95589(16) 0.53553(5) 0.74172(13) 0.0308 1.0000 Uani . . . . . .
C32 C 0.9208(2) 0.50809(7) 0.82989(15) 0.0477 1.0000 Uani . . . . . .
C33 C 1.06928(17) 0.51553(6) 0.69922(16) 0.0369 1.0000 Uani . . . . . .
C34 C 0.81763(18) 0.52269(5) 0.56263(13) 0.0335 1.0000 Uani . . . . . .
C35 C 0.70760(19) 0.52909(6) 0.48760(14) 0.0382 1.0000 Uani . . . . . .
C36 C 0.61330(17) 0.55702(6) 0.50577(13) 0.0340 1.0000 Uani . . . . . .
C37 C 0.62812(14) 0.57994(5) 0.59896(11) 0.0239 1.0000 Uani . . . . . .
C38 C 0.52397(15) 0.61109(5) 0.61500(12) 0.0278 1.0000 Uani . . . . . .
C39 C 0.39575(18) 0.58889(8) 0.62264(17) 0.0483 1.0000 Uani . . . . . .
C40 C 0.5037(2) 0.64442(7) 0.52929(15) 0.0446 1.0000 Uani . . . . . .
C41 C 0.67625(13) 0.58725(5) 0.85110(11) 0.0209 1.0000 Uani . . . . . .
C42 C 0.64404(13) 0.62762(5) 0.90214(11) 0.0201 1.0000 Uani . . . . . .
C43 C 0.95409(13) 0.68476(4) 0.87679(10) 0.0184 1.0000 Uani . . . . . .
C44 C 1.08360(13) 0.67243(5) 0.91105(10) 0.0203 1.0000 Uani . . . . . .
C45 C 1.12679(14) 0.62738(5) 0.93045(12) 0.0247 1.0000 Uani . . . . . .
C46 C 1.20782(17) 0.62149(6) 1.03976(14) 0.0369 1.0000 Uani . . . . . .
C47 C 1.20489(18) 0.61332(6) 0.84630(15) 0.0366 1.0000 Uani . . . . . .
C48 C 1.17832(14) 0.70359(5) 0.92520(12) 0.0255 1.0000 Uani . . . . . .
C49 C 1.14572(15) 0.74493(5) 0.90596(12) 0.0281 1.0000 Uani . . . . . .
C50 C 1.01756(15) 0.75614(5) 0.86945(12) 0.0263 1.0000 Uani . . . . . .
C51 C 0.91857(14) 0.72642(5) 0.85410(11) 0.0211 1.0000 Uani . . . . . .
C52 C 0.77966(14) 0.73984(5) 0.81036(11) 0.0239 1.0000 Uani . . . . . .
C53 C 0.73981(18) 0.77781(7) 0.86788(17) 0.0442 1.0000 Uani . . . . . .
C54 C 0.7637(2) 0.74876(8) 0.69288(14) 0.0460 1.0000 Uani . . . . . .
C55 C 0.72161(13) 0.69033(4) 1.15180(10) 0.0186 1.0000 Uani . . . . . .
C56 C 0.60692(14) 0.70672(5) 1.09548(11) 0.0211 1.0000 Uani . . . . . .
F57 F 0.51581(8) 0.68105(3) 1.04155(7) 0.0265 1.0000 Uani . . . . . .
C58 C 0.57748(15) 0.74876(5) 1.08553(12) 0.0273 1.0000 Uani . . . . . .
F59 F 0.46597(10) 0.76169(3) 1.02630(9) 0.0386 1.0000 Uani . . . . . .
C60 C 0.66577(18) 0.77746(5) 1.13374(13) 0.0314 1.0000 Uani . . . . . .
F61 F 0.63965(13) 0.81833(3) 1.12503(10) 0.0491 1.0000 Uani . . . . . .
C62 C 0.78277(17) 0.76358(5) 1.18802(13) 0.0294 1.0000 Uani . . . . . .
C63 C 0.80843(14) 0.72122(5) 1.19491(11) 0.0232 1.0000 Uani . . . . . .
F64 F 0.92742(9) 0.71089(3) 1.24729(8) 0.0343 1.0000 Uani . . . . . .
F65 F 0.87187(12) 0.79119(3) 1.23408(9) 0.0448 1.0000 Uani . . . . . .
H241 H 0.9234 0.6498 1.0685 0.0214 1.0000 Uiso R . . . . .
H242 H 0.8623 0.6054 1.0434 0.0208 1.0000 Uiso R . . . . .
H251 H 0.7435 0.6807 0.9597 0.0190 1.0000 Uiso R . . . . .
H271 H 0.8922 0.6335 0.7332 0.0191 1.0000 Uiso R . . . . .
H311 H 0.9876 0.5623 0.7713 0.0374 1.0000 Uiso R . . . . .
H321 H 0.9986 0.5033 0.8813 0.0711 1.0000 Uiso R . . . . .
H323 H 0.8578 0.5208 0.8646 0.0715 1.0000 Uiso R . . . . .
H322 H 0.8859 0.4823 0.8024 0.0720 1.0000 Uiso R . . . . .
H332 H 1.1462 0.5144 0.7537 0.0554 1.0000 Uiso R . . . . .
H331 H 1.0901 0.5318 0.6417 0.0553 1.0000 Uiso R . . . . .
H333 H 1.0470 0.4878 0.6740 0.0547 1.0000 Uiso R . . . . .
H341 H 0.8808 0.5040 0.5489 0.0400 1.0000 Uiso R . . . . .
H351 H 0.6972 0.5141 0.4223 0.0472 1.0000 Uiso R . . . . .
H361 H 0.5371 0.5610 0.4554 0.0412 1.0000 Uiso R . . . . .
H381 H 0.5507 0.6250 0.6820 0.0332 1.0000 Uiso R . . . . .
H391 H 0.3317 0.6086 0.6390 0.0736 1.0000 Uiso R . . . . .
H393 H 0.4101 0.5680 0.6781 0.0737 1.0000 Uiso R . . . . .
H392 H 0.3640 0.5754 0.5565 0.0738 1.0000 Uiso R . . . . .
H402 H 0.4389 0.6637 0.5449 0.0681 1.0000 Uiso R . . . . .
H401 H 0.5887 0.6580 0.5248 0.0674 1.0000 Uiso R . . . . .
H403 H 0.4709 0.6316 0.4602 0.0689 1.0000 Uiso R . . . . .
H411 H 0.7234 0.5684 0.9025 0.0255 1.0000 Uiso R . . . . .
H412 H 0.5951 0.5743 0.8194 0.0247 1.0000 Uiso R . . . . .
H421 H 0.5931 0.6452 0.8501 0.0244 1.0000 Uiso R . . . . .
H422 H 0.5949 0.6218 0.9565 0.0230 1.0000 Uiso R . . . . .
H451 H 1.0469 0.6113 0.9265 0.0297 1.0000 Uiso R . . . . .
H461 H 1.2217 0.5921 1.0526 0.0553 1.0000 Uiso R . . . . .
H463 H 1.2920 0.6353 1.0427 0.0540 1.0000 Uiso R . . . . .
H462 H 1.1602 0.6317 1.0934 0.0551 1.0000 Uiso R . . . . .
H472 H 1.2309 0.5846 0.8568 0.0542 1.0000 Uiso R . . . . .
H471 H 1.2835 0.6291 0.8489 0.0541 1.0000 Uiso R . . . . .
H473 H 1.1563 0.6159 0.7752 0.0552 1.0000 Uiso R . . . . .
H481 H 1.2694 0.6964 0.9481 0.0306 1.0000 Uiso R . . . . .
H491 H 1.2111 0.7653 0.9183 0.0343 1.0000 Uiso R . . . . .
H501 H 0.9963 0.7841 0.8537 0.0311 1.0000 Uiso R . . . . .
H521 H 0.7203 0.7177 0.8199 0.0291 1.0000 Uiso R . . . . .
H531 H 0.6453 0.7815 0.8507 0.0646 1.0000 Uiso R . . . . .
H533 H 0.7845 0.8023 0.8534 0.0668 1.0000 Uiso R . . . . .
H532 H 0.7577 0.7726 0.9446 0.0664 1.0000 Uiso R . . . . .
H542 H 0.6721 0.7551 0.6671 0.0698 1.0000 Uiso R . . . . .
H541 H 0.8183 0.7718 0.6809 0.0715 1.0000 Uiso R . . . . .
H543 H 0.7923 0.7251 0.6562 0.0702 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       75(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          4.03(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
F1 . C2 . 1.3448(16) yes
C2 . C3 . 1.371(2) yes
C2 . C9 . 1.375(2) yes
C3 . F4 . 1.3406(18) yes
C3 . C5 . 1.393(2) yes
C5 . F6 . 1.3491(17) yes
C5 . C7 . 1.386(2) yes
C7 . C8 . 1.3923(19) yes
C7 . B12 . 1.6666(19) yes
C8 . C9 . 1.382(2) yes
C8 . F11 . 1.3478(17) yes
C9 . F10 . 1.3434(17) yes
B12 . C13 . 1.671(2) yes
B12 . C24 . 1.6608(19) yes
B12 . C55 . 1.660(2) yes
C13 . C14 . 1.392(2) yes
C13 . C21 . 1.400(2) yes
C14 . F15 . 1.3487(19) yes
C14 . C16 . 1.389(2) yes
C16 . F17 . 1.333(2) yes
C16 . C18 . 1.378(3) yes
C18 . F19 . 1.3415(19) yes
C18 . C20 . 1.371(3) yes
C20 . C21 . 1.386(2) yes
C20 . F23 . 1.349(2) yes
C21 . F22 . 1.3495(19) yes
C24 . C25 . 1.5275(17) yes
C24 . H241 . 0.978 no
C24 . H242 . 0.990 no
C25 . N26 . 1.5062(16) yes
C25 . C42 . 1.5291(18) yes
C25 . H251 . 0.987 no
N26 . C27 . 1.3138(18) yes
N26 . C43 . 1.4523(17) yes
C27 . N28 . 1.3217(18) yes
C27 . H271 . 0.967 no
N28 . C29 . 1.4524(17) yes
N28 . C41 . 1.4741(17) yes
C29 . C30 . 1.406(2) yes
C29 . C37 . 1.3997(19) yes
C30 . C31 . 1.522(2) yes
C30 . C34 . 1.397(2) yes
C31 . C32 . 1.535(3) yes
C31 . C33 . 1.531(2) yes
C31 . H311 . 0.975 no
C32 . H321 . 0.969 no
C32 . H323 . 0.950 no
C32 . H322 . 0.948 no
C33 . H332 . 0.973 no
C33 . H331 . 0.965 no
C33 . H333 . 0.962 no
C34 . C35 . 1.384(3) yes
C34 . H341 . 0.931 no
C35 . C36 . 1.382(3) yes
C35 . H351 . 0.961 no
C36 . C37 . 1.397(2) yes
C36 . H361 . 0.946 no
C37 . C38 . 1.518(2) yes
C38 . C39 . 1.535(2) yes
C38 . C40 . 1.529(2) yes
C38 . H381 . 0.971 no
C39 . H391 . 0.970 no
C39 . H393 . 0.975 no
C39 . H392 . 0.964 no
C40 . H402 . 0.963 no
C40 . H401 . 0.999 no
C40 . H403 . 0.989 no
C41 . C42 . 1.518(2) yes
C41 . H411 . 0.968 no
C41 . H412 . 0.968 no
C42 . H421 . 0.964 no
C42 . H422 . 0.958 no
C43 . C44 . 1.4050(19) yes
C43 . C51 . 1.405(2) yes
C44 . C45 . 1.522(2) yes
C44 . C48 . 1.396(2) yes
C45 . C46 . 1.528(2) yes
C45 . C47 . 1.537(2) yes
C45 . H451 . 0.974 no
C46 . H461 . 0.965 no
C46 . H463 . 0.979 no
C46 . H462 . 0.978 no
C47 . H472 . 0.963 no
C47 . H471 . 0.960 no
C47 . H473 . 0.973 no
C48 . C49 . 1.382(2) yes
C48 . H481 . 0.974 no
C49 . C50 . 1.387(2) yes
C49 . H491 . 0.940 no
C50 . C51 . 1.395(2) yes
C50 . H501 . 0.938 no
C51 . C52 . 1.5247(19) yes
C52 . C53 . 1.523(2) yes
C52 . C54 . 1.526(2) yes
C52 . H521 . 0.966 no
C53 . H531 . 0.980 no
C53 . H533 . 0.949 no
C53 . H532 . 0.992 no
C54 . H542 . 0.978 no
C54 . H541 . 0.962 no
C54 . H543 . 0.970 no
C55 . C56 . 1.3923(19) yes
C55 . C63 . 1.393(2) yes
C56 . F57 . 1.3566(17) yes
C56 . C58 . 1.385(2) yes
C58 . F59 . 1.3435(18) yes
C58 . C60 . 1.374(2) yes
C60 . F61 . 1.3410(19) yes
C60 . C62 . 1.373(2) yes
C62 . C63 . 1.386(2) yes
C62 . F65 . 1.3466(19) yes
C63 . F64 . 1.3491(17) yes
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 . C2 . C3 . 120.73(14) yes
F1 . C2 . C9 . 120.14(14) yes
C3 . C2 . C9 . 119.12(13) yes
C2 . C3 . F4 . 119.84(13) yes
C2 . C3 . C5 . 119.72(14) yes
F4 . C3 . C5 . 120.44(14) yes
C3 . C5 . F6 . 114.93(13) yes
C3 . C5 . C7 . 124.08(14) yes
F6 . C5 . C7 . 120.99(12) yes
C5 . C7 . C8 . 112.98(12) yes
C5 . C7 . B12 . 126.86(12) yes
C8 . C7 . B12 . 120.06(12) yes
C7 . C8 . C9 . 125.04(14) yes
C7 . C8 . F11 . 119.73(12) yes
C9 . C8 . F11 . 115.23(13) yes
C8 . C9 . C2 . 119.03(14) yes
C8 . C9 . F10 . 120.72(14) yes
C2 . C9 . F10 . 120.25(13) yes
C7 . B12 . C13 . 99.80(10) yes
C7 . B12 . C24 . 112.05(10) yes
C13 . B12 . C24 . 115.72(11) yes
C7 . B12 . C55 . 109.75(11) yes
C13 . B12 . C55 . 115.41(11) yes
C24 . B12 . C55 . 104.26(10) yes
B12 . C13 . C14 . 126.20(13) yes
B12 . C13 . C21 . 120.24(12) yes
C14 . C13 . C21 . 112.41(13) yes
C13 . C14 . F15 . 121.37(13) yes
C13 . C14 . C16 . 124.84(15) yes
F15 . C14 . C16 . 113.79(14) yes
C14 . C16 . F17 . 120.72(17) yes
C14 . C16 . C18 . 119.51(16) yes
F17 . C16 . C18 . 119.76(15) yes
C16 . C18 . F19 . 120.71(18) yes
C16 . C18 . C20 . 118.80(15) yes
F19 . C18 . C20 . 120.49(18) yes
C18 . C20 . C21 . 119.76(17) yes
C18 . C20 . F23 . 119.89(16) yes
C21 . C20 . F23 . 120.34(17) yes
C13 . C21 . C20 . 124.66(15) yes
C13 . C21 . F22 . 120.77(13) yes
C20 . C21 . F22 . 114.53(15) yes
B12 . C24 . C25 . 115.14(10) yes
B12 . C24 . H241 . 108.7 no
C25 . C24 . H241 . 107.2 no
B12 . C24 . H242 . 111.1 no
C25 . C24 . H242 . 108.0 no
H241 . C24 . H242 . 106.3 no
C24 . C25 . N26 . 112.08(10) yes
C24 . C25 . C42 . 115.75(11) yes
N26 . C25 . C42 . 107.34(10) yes
C24 . C25 . H251 . 108.0 no
N26 . C25 . H251 . 104.5 no
C42 . C25 . H251 . 108.6 no
C25 . N26 . C27 . 122.76(11) yes
C25 . N26 . C43 . 118.40(10) yes
C27 . N26 . C43 . 118.84(11) yes
N26 . C27 . N28 . 124.90(12) yes
N26 . C27 . H271 . 116.6 no
N28 . C27 . H271 . 118.5 no
C27 . N28 . C29 . 120.05(11) yes
C27 . N28 . C41 . 118.92(11) yes
C29 . N28 . C41 . 120.89(11) yes
N28 . C29 . C30 . 119.08(12) yes
N28 . C29 . C37 . 117.71(13) yes
C30 . C29 . C37 . 123.21(13) yes
C29 . C30 . C31 . 122.42(13) yes
C29 . C30 . C34 . 116.63(14) yes
C31 . C30 . C34 . 120.94(14) yes
C30 . C31 . C32 . 111.03(15) yes
C30 . C31 . C33 . 114.05(14) yes
C32 . C31 . C33 . 108.99(14) yes
C30 . C31 . H311 . 107.4 no
C32 . C31 . H311 . 108.9 no
C33 . C31 . H311 . 106.2 no
C31 . C32 . H321 . 108.7 no
C31 . C32 . H323 . 112.3 no
H321 . C32 . H323 . 108.1 no
C31 . C32 . H322 . 110.4 no
H321 . C32 . H322 . 110.0 no
H323 . C32 . H322 . 107.3 no
C31 . C33 . H332 . 110.4 no
C31 . C33 . H331 . 110.0 no
H332 . C33 . H331 . 108.0 no
C31 . C33 . H333 . 110.7 no
H332 . C33 . H333 . 109.4 no
H331 . C33 . H333 . 108.3 no
C30 . C34 . C35 . 121.46(16) yes
C30 . C34 . H341 . 119.1 no
C35 . C34 . H341 . 119.4 no
C34 . C35 . C36 . 120.43(15) yes
C34 . C35 . H351 . 119.7 no
C36 . C35 . H351 . 119.9 no
C35 . C36 . C37 . 120.85(15) yes
C35 . C36 . H361 . 120.7 no
C37 . C36 . H361 . 118.4 no
C29 . C37 . C36 . 117.40(14) yes
C29 . C37 . C38 . 123.25(13) yes
C36 . C37 . C38 . 119.34(14) yes
C37 . C38 . C39 . 110.90(15) yes
C37 . C38 . C40 . 112.00(13) yes
C39 . C38 . C40 . 111.03(15) yes
C37 . C38 . H381 . 108.8 no
C39 . C38 . H381 . 105.9 no
C40 . C38 . H381 . 107.9 no
C38 . C39 . H391 . 110.7 no
C38 . C39 . H393 . 110.0 no
H391 . C39 . H393 . 108.2 no
C38 . C39 . H392 . 108.7 no
H391 . C39 . H392 . 110.0 no
H393 . C39 . H392 . 109.2 no
C38 . C40 . H402 . 108.2 no
C38 . C40 . H401 . 109.5 no
H402 . C40 . H401 . 113.4 no
C38 . C40 . H403 . 110.2 no
H402 . C40 . H403 . 108.1 no
H401 . C40 . H403 . 107.5 no
N28 . C41 . C42 . 109.41(11) yes
N28 . C41 . H411 . 109.1 no
C42 . C41 . H411 . 111.1 no
N28 . C41 . H412 . 110.4 no
C42 . C41 . H412 . 107.9 no
H411 . C41 . H412 . 109.0 no
C25 . C42 . C41 . 111.45(11) yes
C25 . C42 . H421 . 107.9 no
C41 . C42 . H421 . 109.4 no
C25 . C42 . H422 . 109.1 no
C41 . C42 . H422 . 109.9 no
H421 . C42 . H422 . 109.0 no
N26 . C43 . C44 . 118.94(12) yes
N26 . C43 . C51 . 118.44(12) yes
C44 . C43 . C51 . 122.60(13) yes
C43 . C44 . C45 . 124.13(13) yes
C43 . C44 . C48 . 117.42(13) yes
C45 . C44 . C48 . 118.42(13) yes
C44 . C45 . C46 . 111.76(13) yes
C44 . C45 . C47 . 109.93(13) yes
C46 . C45 . C47 . 109.99(13) yes
C44 . C45 . H451 . 105.5 no
C46 . C45 . H451 . 108.3 no
C47 . C45 . H451 . 111.2 no
C45 . C46 . H461 . 108.9 no
C45 . C46 . H463 . 109.2 no
H461 . C46 . H463 . 109.2 no
C45 . C46 . H462 . 110.3 no
H461 . C46 . H462 . 106.5 no
H463 . C46 . H462 . 112.6 no
C45 . C47 . H472 . 110.7 no
C45 . C47 . H471 . 112.1 no
H472 . C47 . H471 . 106.3 no
C45 . C47 . H473 . 113.0 no
H472 . C47 . H473 . 107.5 no
H471 . C47 . H473 . 106.9 no
C44 . C48 . C49 . 121.18(14) yes
C44 . C48 . H481 . 120.2 no
C49 . C48 . H481 . 118.6 no
C48 . C49 . C50 . 120.22(14) yes
C48 . C49 . H491 . 119.3 no
C50 . C49 . H491 . 120.4 no
C49 . C50 . C51 . 121.21(15) yes
C49 . C50 . H501 . 120.0 no
C51 . C50 . H501 . 118.8 no
C43 . C51 . C50 . 117.32(13) yes
C43 . C51 . C52 . 123.09(13) yes
C50 . C51 . C52 . 119.55(13) yes
C51 . C52 . C53 . 111.60(13) yes
C51 . C52 . C54 . 110.77(13) yes
C53 . C52 . C54 . 110.13(15) yes
C51 . C52 . H521 . 109.6 no
C53 . C52 . H521 . 106.9 no
C54 . C52 . H521 . 107.7 no
C52 . C53 . H531 . 109.6 no
C52 . C53 . H533 . 112.4 no
H531 . C53 . H533 . 111.4 no
C52 . C53 . H532 . 109.5 no
H531 . C53 . H532 . 104.8 no
H533 . C53 . H532 . 108.9 no
C52 . C54 . H542 . 108.1 no
C52 . C54 . H541 . 109.8 no
H542 . C54 . H541 . 110.8 no
C52 . C54 . H543 . 110.5 no
H542 . C54 . H543 . 111.3 no
H541 . C54 . H543 . 106.3 no
B12 . C55 . C56 . 125.40(12) yes
B12 . C55 . C63 . 121.63(12) yes
C56 . C55 . C63 . 112.40(13) yes
C55 . C56 . F57 . 120.13(13) yes
C55 . C56 . C58 . 125.01(14) yes
F57 . C56 . C58 . 114.81(13) yes
C56 . C58 . F59 . 120.69(15) yes
C56 . C58 . C60 . 119.38(14) yes
F59 . C58 . C60 . 119.88(14) yes
C58 . C60 . F61 . 120.49(16) yes
C58 . C60 . C62 . 118.79(15) yes
F61 . C60 . C62 . 120.68(16) yes
C60 . C62 . C63 . 119.74(15) yes
C60 . C62 . F65 . 119.84(15) yes
C63 . C62 . F65 . 120.42(15) yes
C55 . C63 . C62 . 124.59(14) yes
C55 . C63 . F64 . 120.30(13) yes
C62 . C63 . F64 . 115.12(13) yes
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 . C56 . 125.60 0.987 2.586 3.260(2) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 30/03/14 at 11:38:35
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 323,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) H   ( 333,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   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 393,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 401,X'S) H   ( 403,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 463,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 472,X'S) H   ( 471,X'S) H   ( 473,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 533,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) H   ( 543,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 30/03/14 at 11:38:35
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_database_code_depnum_ccdc_archive 'CCDC 1006574'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_224NPRT14
_audit_creation_date             2014-05-18
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '224NPRT14 in P -1'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   12.3124(4)
_cell_length_b                   15.5237(5)
_cell_length_c                   15.6860(4)
_cell_angle_alpha                66.407(3)
_cell_angle_beta                 80.487(2)
_cell_angle_gamma                89.507(3)
_cell_volume                     2704.24(16)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 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'
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'
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'


_cell_formula_units_Z            2

# Given Formula = C150 H160 B2 F30 N4 O1 
# Dc =      3.23 Fooo =   1140.00 Mu =     21.90 M =   2626.51
# Found Formula = C56 H64 B1 F15 N2 O2 
# Dc =      1.34 FOOO =   1140.00 Mu =     10.02 M =   1092.92

_chemical_formula_sum            'C56 H64 B1 F15 N2 O2'
_chemical_formula_moiety         'C56 H64 B1 F15 N2 O2'
_chemical_compound_source        .
_chemical_formula_weight         1092.92


_cell_measurement_reflns_used    14230
_cell_measurement_theta_min      4
_cell_measurement_theta_max      77
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.180
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_max          0.250

_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    1.002

# Sheldrick geometric approximatio 0.81 0.84 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  0.84
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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            28501
_reflns_number_total             11217
_diffrn_reflns_av_R_equivalents  0.019
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 11217 
# Theoretical number of reflections is about 22777 


_diffrn_reflns_theta_min         3.113
_diffrn_reflns_theta_max         76.660
_diffrn_measured_fraction_theta_max 0.985

_diffrn_reflns_theta_full        74.361
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              -17
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   2.50
_oxford_diffrn_Wilson_scale      0.07

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

_refine_diff_density_min         -0.26
_refine_diff_density_max         0.31


# 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>-3.0\s(I)
_refine_ls_number_reflns         11175
_refine_ls_number_restraints     0
_refine_ls_number_parameters     686
_oxford_refine_ls_R_factor_ref   0.0372
_refine_ls_wR_factor_ref         0.0893
_refine_ls_goodness_of_fit_ref   1.0011
_refine_ls_shift/su_max          0.0005864
_refine_ls_shift/su_mean         0.0000361


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11176
_refine_ls_R_factor_all          0.0372
_refine_ls_wR_factor_all         0.0893

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10306
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_gt          0.0873

# 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= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 0.92P] 
 ,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
F1 F -0.04228(6) 0.13912(5) 0.82710(4) 0.0283 1.0000 Uani . . . . . .
C2 C -0.08297(9) 0.22372(7) 0.78266(8) 0.0218 1.0000 Uani . . . . . .
C3 C -0.05938(8) 0.26826(7) 0.68427(7) 0.0199 1.0000 Uani . . . . . .
C4 C -0.10359(9) 0.35563(7) 0.64944(7) 0.0210 1.0000 Uani . . . . . .
F5 F -0.08608(6) 0.41066(4) 0.55556(4) 0.0273 1.0000 Uani . . . . . .
C6 C -0.16692(9) 0.39471(8) 0.70498(8) 0.0242 1.0000 Uani . . . . . .
F7 F -0.20749(6) 0.47921(5) 0.66442(5) 0.0332 1.0000 Uani . . . . . .
C8 C -0.18812(9) 0.34631(8) 0.80159(8) 0.0259 1.0000 Uani . . . . . .
C9 C -0.14577(9) 0.25928(8) 0.84083(8) 0.0242 1.0000 Uani . . . . . .
F10 F -0.16734(6) 0.20956(5) 0.93492(5) 0.0335 1.0000 Uani . . . . . .
F11 F -0.24920(6) 0.38202(6) 0.85722(5) 0.0372 1.0000 Uani . . . . . .
B12 B 0.02375(10) 0.22103(8) 0.62290(8) 0.0187 1.0000 Uani . . . . . .
C13 C 0.14671(9) 0.21854(7) 0.65469(7) 0.0198 1.0000 Uani . . . . . .
C14 C 0.17572(8) 0.29716(7) 0.68351(7) 0.0182 1.0000 Uani . . . . . .
N15 N 0.27293(7) 0.27538(6) 0.73625(6) 0.0175 1.0000 Uani . . . . . .
C16 C 0.28555(8) 0.31416(7) 0.79528(7) 0.0183 1.0000 Uani . . . . . .
N17 N 0.23515(7) 0.38700(6) 0.80287(6) 0.0193 1.0000 Uani . . . . . .
C18 C 0.17699(9) 0.45692(8) 0.73117(8) 0.0232 1.0000 Uani . . . . . .
C19 C 0.22645(10) 0.47219(7) 0.63042(7) 0.0237 1.0000 Uani . . . . . .
C20 C 0.19449(9) 0.39373(7) 0.60169(7) 0.0214 1.0000 Uani . . . . . .
C21 C 0.24713(9) 0.40934(8) 0.88290(7) 0.0214 1.0000 Uani . . . . . .
C22 C 0.33793(9) 0.46770(8) 0.87428(8) 0.0238 1.0000 Uani . . . . . .
C23 C 0.34614(10) 0.48904(9) 0.95158(9) 0.0310 1.0000 Uani . . . . . .
C24 C 0.26749(11) 0.45440(10) 1.03284(9) 0.0362 1.0000 Uani . . . . . .
C25 C 0.17763(11) 0.39817(10) 1.03865(9) 0.0340 1.0000 Uani . . . . . .
C26 C 0.16463(10) 0.37499(8) 0.96341(8) 0.0262 1.0000 Uani . . . . . .
C27 C 0.06167(10) 0.31697(9) 0.97216(8) 0.0299 1.0000 Uani . . . . . .
C28 C 0.05234(13) 0.22153(10) 1.05603(11) 0.0460 1.0000 Uani . . . . . .
C29 C -0.04020(11) 0.37206(11) 0.98028(11) 0.0413 1.0000 Uani . . . . . .
C30 C 0.42593(9) 0.50905(8) 0.78623(8) 0.0264 1.0000 Uani . . . . . .
C31 C 0.42961(13) 0.61650(10) 0.74473(10) 0.0400 1.0000 Uani . . . . . .
C32 C 0.53860(11) 0.47392(11) 0.80729(11) 0.0409 1.0000 Uani . . . . . .
C33 C 0.34542(9) 0.20139(7) 0.73352(7) 0.0206 1.0000 Uani . . . . . .
C34 C 0.44185(9) 0.22607(8) 0.66558(8) 0.0259 1.0000 Uani . . . . . .
C35 C 0.47787(10) 0.32735(9) 0.59826(8) 0.0293 1.0000 Uani . . . . . .
C36 C 0.58280(12) 0.36082(11) 0.61948(11) 0.0426 1.0000 Uani . . . . . .
C37 C 0.49319(13) 0.34018(12) 0.49505(10) 0.0455 1.0000 Uani . . . . . .
C38 C 0.50805(11) 0.15361(10) 0.66193(10) 0.0352 1.0000 Uani . . . . . .
C39 C 0.47885(12) 0.06116(10) 0.72331(11) 0.0392 1.0000 Uani . . . . . .
C40 C 0.38404(11) 0.03894(9) 0.79087(10) 0.0338 1.0000 Uani . . . . . .
C41 C 0.31483(9) 0.10817(8) 0.79840(8) 0.0247 1.0000 Uani . . . . . .
C42 C 0.21412(10) 0.08106(8) 0.87680(8) 0.0270 1.0000 Uani . . . . . .
C43 C 0.14365(11) -0.00256(9) 0.88234(10) 0.0359 1.0000 Uani . . . . . .
C44 C 0.25030(12) 0.05807(10) 0.97214(9) 0.0386 1.0000 Uani . . . . . .
C45 C -0.01855(9) 0.11021(7) 0.64813(7) 0.0218 1.0000 Uani . . . . . .
C46 C -0.11971(10) 0.06378(8) 0.69838(9) 0.0286 1.0000 Uani . . . . . .
F47 F -0.19848(6) 0.10645(5) 0.73494(6) 0.0362 1.0000 Uani . . . . . .
C48 C -0.14910(12) -0.02809(10) 0.71461(11) 0.0413 1.0000 Uani . . . . . .
F49 F -0.24784(9) -0.06844(7) 0.76590(8) 0.0667 1.0000 Uani . . . . . .
C50 C -0.07764(14) -0.07792(9) 0.67808(12) 0.0445 1.0000 Uani . . . . . .
F51 F -0.10582(10) -0.16696(6) 0.69365(9) 0.0707 1.0000 Uani . . . . . .
C52 C 0.02231(12) -0.03495(9) 0.62495(11) 0.0372 1.0000 Uani . . . . . .
C53 C 0.04953(10) 0.05628(8) 0.61192(8) 0.0270 1.0000 Uani . . . . . .
F54 F 0.14871(6) 0.09393(5) 0.55766(6) 0.0362 1.0000 Uani . . . . . .
F55 F 0.09246(8) -0.08152(6) 0.58599(8) 0.0546 1.0000 Uani . . . . . .
C56 C 0.01890(9) 0.27263(7) 0.50828(7) 0.0207 1.0000 Uani . . . . . .
C57 C -0.08286(9) 0.27387(8) 0.47997(8) 0.0228 1.0000 Uani . . . . . .
F58 F -0.17555(5) 0.24122(5) 0.54609(5) 0.0291 1.0000 Uani . . . . . .
C59 C -0.09842(10) 0.30716(8) 0.38762(8) 0.0267 1.0000 Uani . . . . . .
F60 F -0.20012(6) 0.30594(5) 0.36679(5) 0.0364 1.0000 Uani . . . . . .
C61 C -0.00866(11) 0.34216(8) 0.31600(8) 0.0298 1.0000 Uani . . . . . .
F62 F -0.02228(7) 0.37447(6) 0.22505(5) 0.0431 1.0000 Uani . . . . . .
C63 C 0.09426(10) 0.34246(8) 0.33854(8) 0.0279 1.0000 Uani . . . . . .
C64 C 0.10616(9) 0.30790(8) 0.43281(8) 0.0234 1.0000 Uani . . . . . .
F65 F 0.21125(5) 0.31049(5) 0.44676(5) 0.0301 1.0000 Uani . . . . . .
F66 F 0.18310(7) 0.37364(6) 0.26925(5) 0.0397 1.0000 Uani . . . . . .
O67 O 0.45755(8) 0.22554(7) 0.95768(7) 0.0384 1.0000 Uani . . . . . .
C68 C 0.40653(15) 0.22639(13) 1.04556(11) 0.0516 1.0000 Uani . . . . . .
C69 C 0.4788(2) 0.27157(18) 1.08679(17) 0.0850 1.0000 Uani . . . . . .
C70 C 0.54151(13) 0.16013(12) 0.96737(11) 0.0458 1.0000 Uani . . . . . .
C71 C 0.58434(13) 0.16013(12) 0.87295(11) 0.0487 1.0000 Uani . . . . . .
O72 O 0.42553(10) 0.84553(8) 0.69687(8) 0.0510 1.0000 Uani . . . . . .
C73 C 0.31321(17) 0.86510(15) 0.69059(17) 0.0698 1.0000 Uani . . . . . .
C74 C 0.24244(18) 0.81000(18) 0.7820(2) 0.0832 1.0000 Uani . . . . . .
C75 C 0.4964(2) 0.88675(17) 0.60934(15) 0.0777 1.0000 Uani . . . . . .
C76 C 0.6110(2) 0.8616(2) 0.6210(2) 0.1040 1.0000 Uani . . . . . .
H132 H 0.1443 0.1596 0.7095 0.0228 1.0000 Uiso R . . . . .
H131 H 0.2062 0.2168 0.6050 0.0233 1.0000 Uiso R . . . . .
H141 H 0.1148 0.2996 0.7326 0.0184 1.0000 Uiso R . . . . .
H161 H 0.3359 0.2860 0.8378 0.0215 1.0000 Uiso R . . . . .
H182 H 0.1858 0.5160 0.7385 0.0261 1.0000 Uiso R . . . . .
H181 H 0.0973 0.4368 0.7471 0.0260 1.0000 Uiso R . . . . .
H192 H 0.3072 0.4796 0.6222 0.0272 1.0000 Uiso R . . . . .
H191 H 0.2041 0.5333 0.5875 0.0273 1.0000 Uiso R . . . . .
H202 H 0.1262 0.4073 0.5771 0.0241 1.0000 Uiso R . . . . .
H201 H 0.2511 0.3928 0.5499 0.0247 1.0000 Uiso R . . . . .
H231 H 0.4090 0.5281 0.9468 0.0356 1.0000 Uiso R . . . . .
H241 H 0.2743 0.4688 1.0856 0.0421 1.0000 Uiso R . . . . .
H251 H 0.1235 0.3740 1.0952 0.0387 1.0000 Uiso R . . . . .
H271 H 0.0666 0.3056 0.9132 0.0343 1.0000 Uiso R . . . . .
H282 H -0.0112 0.1824 1.0594 0.0670 1.0000 Uiso R . . . . .
H281 H 0.0421 0.2300 1.1175 0.0686 1.0000 Uiso R . . . . .
H283 H 0.1187 0.1867 1.0524 0.0683 1.0000 Uiso R . . . . .
H292 H -0.1070 0.3339 0.9873 0.0587 1.0000 Uiso R . . . . .
H293 H -0.0470 0.3870 1.0367 0.0600 1.0000 Uiso R . . . . .
H291 H -0.0357 0.4329 0.9231 0.0600 1.0000 Uiso R . . . . .
H301 H 0.4076 0.4879 0.7386 0.0307 1.0000 Uiso R . . . . .
H312 H 0.4879 0.6434 0.6900 0.0581 1.0000 Uiso R . . . . .
H313 H 0.4443 0.6410 0.7914 0.0574 1.0000 Uiso R . . . . .
H311 H 0.3590 0.6400 0.7263 0.0598 1.0000 Uiso R . . . . .
H323 H 0.5934 0.4997 0.7494 0.0588 1.0000 Uiso R . . . . .
H321 H 0.5621 0.4963 0.8529 0.0595 1.0000 Uiso R . . . . .
H322 H 0.5352 0.4039 0.8353 0.0600 1.0000 Uiso R . . . . .
H351 H 0.4189 0.3672 0.6083 0.0331 1.0000 Uiso R . . . . .
H363 H 0.6037 0.4278 0.5751 0.0619 1.0000 Uiso R . . . . .
H361 H 0.5704 0.3555 0.6849 0.0621 1.0000 Uiso R . . . . .
H362 H 0.6439 0.3223 0.6107 0.0631 1.0000 Uiso R . . . . .
H371 H 0.5085 0.4080 0.4539 0.0657 1.0000 Uiso R . . . . .
H373 H 0.5552 0.3047 0.4815 0.0657 1.0000 Uiso R . . . . .
H372 H 0.4265 0.3161 0.4832 0.0666 1.0000 Uiso R . . . . .
H381 H 0.5748 0.1691 0.6167 0.0410 1.0000 Uiso R . . . . .
H391 H 0.5243 0.0117 0.7204 0.0462 1.0000 Uiso R . . . . .
H401 H 0.3652 -0.0256 0.8347 0.0386 1.0000 Uiso R . . . . .
H421 H 0.1685 0.1366 0.8633 0.0291 1.0000 Uiso R . . . . .
H432 H 0.0770 -0.0140 0.9288 0.0527 1.0000 Uiso R . . . . .
H431 H 0.1837 -0.0603 0.9008 0.0520 1.0000 Uiso R . . . . .
H433 H 0.1225 0.0094 0.8210 0.0518 1.0000 Uiso R . . . . .
H442 H 0.1851 0.0413 1.0238 0.0559 1.0000 Uiso R . . . . .
H443 H 0.2915 0.1127 0.9704 0.0557 1.0000 Uiso R . . . . .
H441 H 0.2971 0.0039 0.9872 0.0568 1.0000 Uiso R . . . . .
H682 H 0.3836 0.1594 1.0922 0.0613 1.0000 Uiso R . . . . .
H681 H 0.3387 0.2632 1.0349 0.0617 1.0000 Uiso R . . . . .
H692 H 0.4319 0.2779 1.1407 0.1261 1.0000 Uiso R . . . . .
H691 H 0.5366 0.2304 1.1106 0.1255 1.0000 Uiso R . . . . .
H693 H 0.5088 0.3343 1.0374 0.1257 1.0000 Uiso R . . . . .
H701 H 0.6023 0.1776 0.9935 0.0552 1.0000 Uiso R . . . . .
H702 H 0.5072 0.0957 1.0133 0.0545 1.0000 Uiso R . . . . .
H711 H 0.6407 0.1161 0.8763 0.0729 1.0000 Uiso R . . . . .
H713 H 0.6156 0.2229 0.8272 0.0720 1.0000 Uiso R . . . . .
H712 H 0.5228 0.1416 0.8496 0.0718 1.0000 Uiso R . . . . .
H732 H 0.3055 0.9352 0.6707 0.0833 1.0000 Uiso R . . . . .
H731 H 0.2941 0.8455 0.6391 0.0837 1.0000 Uiso R . . . . .
H743 H 0.1630 0.8255 0.7795 0.1254 1.0000 Uiso R . . . . .
H741 H 0.2665 0.8219 0.8354 0.1244 1.0000 Uiso R . . . . .
H742 H 0.2455 0.7401 0.7968 0.1245 1.0000 Uiso R . . . . .
H751 H 0.4911 0.9585 0.5837 0.0929 1.0000 Uiso R . . . . .
H752 H 0.4721 0.8619 0.5640 0.0932 1.0000 Uiso R . . . . .
H762 H 0.6590 0.8925 0.5612 0.1550 1.0000 Uiso R . . . . .
H763 H 0.6354 0.8837 0.6668 0.1548 1.0000 Uiso R . . . . .
H761 H 0.6168 0.7928 0.6436 0.1548 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       69(6)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          5.96(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
F1 . C2 . 1.3539(12) yes
C2 . C3 . 1.3948(15) yes
C2 . C9 . 1.3777(16) yes
C3 . C4 . 1.3882(15) yes
C3 . B12 . 1.6547(15) yes
C4 . F5 . 1.3550(12) yes
C4 . C6 . 1.3875(15) yes
C6 . F7 . 1.3419(13) yes
C6 . C8 . 1.3750(17) yes
C8 . C9 . 1.3799(16) yes
C8 . F11 . 1.3407(13) yes
C9 . F10 . 1.3442(13) yes
B12 . C13 . 1.6659(15) yes
B12 . C45 . 1.6702(15) yes
B12 . C56 . 1.6612(15) yes
C13 . C14 . 1.5246(14) yes
C13 . H132 . 0.969 no
C13 . H131 . 0.985 no
C14 . N15 . 1.5256(12) yes
C14 . C20 . 1.5217(14) yes
C14 . H141 . 0.995 no
N15 . C16 . 1.3188(13) yes
N15 . C33 . 1.4584(13) yes
C16 . N17 . 1.3226(14) yes
C16 . H161 . 0.959 no
N17 . C18 . 1.4938(13) yes
N17 . C21 . 1.4590(13) yes
C18 . C19 . 1.5196(15) yes
C18 . H182 . 0.977 no
C18 . H181 . 0.992 no
C19 . C20 . 1.5322(14) yes
C19 . H192 . 0.983 no
C19 . H191 . 0.987 no
C20 . H202 . 0.969 no
C20 . H201 . 0.985 no
C21 . C22 . 1.3994(15) yes
C21 . C26 . 1.3990(15) yes
C22 . C23 . 1.3975(16) yes
C22 . C30 . 1.5170(15) yes
C23 . C24 . 1.3798(18) yes
C23 . H231 . 0.961 no
C24 . C25 . 1.3834(18) yes
C24 . H241 . 0.956 no
C25 . C26 . 1.3969(16) yes
C25 . H251 . 0.955 no
C26 . C27 . 1.5166(16) yes
C27 . C28 . 1.5271(19) yes
C27 . C29 . 1.5286(19) yes
C27 . H271 . 1.001 no
C28 . H282 . 0.976 no
C28 . H281 . 1.012 no
C28 . H283 . 0.982 no
C29 . H292 . 0.983 no
C29 . H293 . 0.992 no
C29 . H291 . 1.003 no
C30 . C31 . 1.5266(18) yes
C30 . C32 . 1.5248(17) yes
C30 . H301 . 0.986 no
C31 . H312 . 0.970 no
C31 . H313 . 0.992 no
C31 . H311 . 0.982 no
C32 . H323 . 0.975 no
C32 . H321 . 0.993 no
C32 . H322 . 0.994 no
C33 . C34 . 1.3982(15) yes
C33 . C41 . 1.4055(15) yes
C34 . C35 . 1.5206(16) yes
C34 . C38 . 1.3976(17) yes
C35 . C36 . 1.5305(18) yes
C35 . C37 . 1.5290(18) yes
C35 . H351 . 0.984 no
C36 . H363 . 0.998 no
C36 . H361 . 0.982 no
C36 . H362 . 0.984 no
C37 . H371 . 0.989 no
C37 . H373 . 0.982 no
C37 . H372 . 0.979 no
C38 . C39 . 1.380(2) yes
C38 . H381 . 0.954 no
C39 . C40 . 1.382(2) yes
C39 . H391 . 0.958 no
C40 . C41 . 1.3954(16) yes
C40 . H401 . 0.964 no
C41 . C42 . 1.5224(16) yes
C42 . C43 . 1.5329(16) yes
C42 . C44 . 1.5339(17) yes
C42 . H421 . 0.994 no
C43 . H432 . 0.969 no
C43 . H431 . 0.981 no
C43 . H433 . 0.983 no
C44 . H442 . 0.995 no
C44 . H443 . 0.981 no
C44 . H441 . 0.986 no
C45 . C46 . 1.3887(16) yes
C45 . C53 . 1.3919(16) yes
C46 . F47 . 1.3480(14) yes
C46 . C48 . 1.3848(17) yes
C48 . F49 . 1.3432(16) yes
C48 . C50 . 1.370(2) yes
C50 . F51 . 1.3418(15) yes
C50 . C52 . 1.373(2) yes
C52 . C53 . 1.3834(17) yes
C52 . F55 . 1.3457(16) yes
C53 . F54 . 1.3519(14) yes
C56 . C57 . 1.3944(15) yes
C56 . C64 . 1.3879(15) yes
C57 . F58 . 1.3538(13) yes
C57 . C59 . 1.3759(16) yes
C59 . F60 . 1.3474(14) yes
C59 . C61 . 1.3748(18) yes
C61 . F62 . 1.3490(13) yes
C61 . C63 . 1.3713(18) yes
C63 . C64 . 1.3897(16) yes
C63 . F66 . 1.3443(14) yes
C64 . F65 . 1.3510(13) yes
O67 . C68 . 1.4223(19) yes
O67 . C70 . 1.4258(18) yes
C68 . C69 . 1.505(3) yes
C68 . H682 . 1.012 no
C68 . H681 . 1.006 no
C69 . H692 . 0.980 no
C69 . H691 . 0.972 no
C69 . H693 . 0.996 no
C70 . C71 . 1.488(2) yes
C70 . H701 . 0.998 no
C70 . H702 . 1.014 no
C71 . H711 . 0.962 no
C71 . H713 . 0.984 no
C71 . H712 . 0.986 no
O72 . C73 . 1.424(2) yes
O72 . C75 . 1.402(2) yes
C73 . C74 . 1.471(3) yes
C73 . H732 . 1.013 no
C73 . H731 . 1.030 no
C74 . H743 . 1.009 no
C74 . H741 . 1.016 no
C74 . H742 . 1.016 no
C75 . C76 . 1.482(4) yes
C75 . H751 . 1.028 no
C75 . H752 . 1.018 no
C76 . H762 . 0.960 no
C76 . H763 . 0.997 no
C76 . H761 . 0.987 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 . C2 . C3 . 119.47(9) yes
F1 . C2 . C9 . 115.55(9) yes
C3 . C2 . C9 . 124.99(10) yes
C2 . C3 . C4 . 112.68(10) yes
C2 . C3 . B12 . 120.16(9) yes
C4 . C3 . B12 . 126.88(9) yes
C3 . C4 . F5 . 121.08(9) yes
C3 . C4 . C6 . 124.53(10) yes
F5 . C4 . C6 . 114.38(9) yes
C4 . C6 . F7 . 120.06(10) yes
C4 . C6 . C8 . 119.68(10) yes
F7 . C6 . C8 . 120.26(10) yes
C6 . C8 . C9 . 118.69(10) yes
C6 . C8 . F11 . 121.15(10) yes
C9 . C8 . F11 . 120.16(10) yes
C8 . C9 . C2 . 119.41(10) yes
C8 . C9 . F10 . 119.89(10) yes
C2 . C9 . F10 . 120.70(10) yes
C3 . B12 . C13 . 106.87(8) yes
C3 . B12 . C45 . 111.92(8) yes
C13 . B12 . C45 . 107.58(8) yes
C3 . B12 . C56 . 111.65(8) yes
C13 . B12 . C56 . 117.43(9) yes
C45 . B12 . C56 . 101.34(8) yes
B12 . C13 . C14 . 116.01(8) yes
B12 . C13 . H132 . 105.2 no
C14 . C13 . H132 . 107.3 no
B12 . C13 . H131 . 111.1 no
C14 . C13 . H131 . 109.1 no
H132 . C13 . H131 . 107.6 no
C13 . C14 . N15 . 112.27(8) yes
C13 . C14 . C20 . 113.49(8) yes
N15 . C14 . C20 . 110.93(8) yes
C13 . C14 . H141 . 108.9 no
N15 . C14 . H141 . 101.9 no
C20 . C14 . H141 . 108.6 no
C14 . N15 . C16 . 120.88(8) yes
C14 . N15 . C33 . 121.00(8) yes
C16 . N15 . C33 . 117.56(8) yes
N15 . C16 . N17 . 126.95(9) yes
N15 . C16 . H161 . 116.5 no
N17 . C16 . H161 . 116.5 no
C16 . N17 . C18 . 126.28(9) yes
C16 . N17 . C21 . 118.09(9) yes
C18 . N17 . C21 . 115.21(8) yes
N17 . C18 . C19 . 112.91(9) yes
N17 . C18 . H182 . 105.4 no
C19 . C18 . H182 . 108.8 no
N17 . C18 . H181 . 108.8 no
C19 . C18 . H181 . 112.1 no
H182 . C18 . H181 . 108.6 no
C18 . C19 . C20 . 114.40(9) yes
C18 . C19 . H192 . 108.7 no
C20 . C19 . H192 . 109.8 no
C18 . C19 . H191 . 108.1 no
C20 . C19 . H191 . 110.2 no
H192 . C19 . H191 . 105.2 no
C19 . C20 . C14 . 113.36(8) yes
C19 . C20 . H202 . 109.4 no
C14 . C20 . H202 . 107.0 no
C19 . C20 . H201 . 109.4 no
C14 . C20 . H201 . 110.8 no
H202 . C20 . H201 . 106.6 no
N17 . C21 . C22 . 118.66(9) yes
N17 . C21 . C26 . 118.51(9) yes
C22 . C21 . C26 . 122.76(10) yes
C21 . C22 . C23 . 117.30(10) yes
C21 . C22 . C30 . 123.75(10) yes
C23 . C22 . C30 . 118.95(10) yes
C22 . C23 . C24 . 121.29(11) yes
C22 . C23 . H231 . 117.9 no
C24 . C23 . H231 . 120.8 no
C23 . C24 . C25 . 120.09(11) yes
C23 . C24 . H241 . 120.7 no
C25 . C24 . H241 . 119.3 no
C24 . C25 . C26 . 121.19(11) yes
C24 . C25 . H251 . 119.8 no
C26 . C25 . H251 . 119.0 no
C21 . C26 . C25 . 117.34(11) yes
C21 . C26 . C27 . 123.88(10) yes
C25 . C26 . C27 . 118.76(10) yes
C26 . C27 . C28 . 111.37(11) yes
C26 . C27 . C29 . 109.76(11) yes
C28 . C27 . C29 . 111.11(11) yes
C26 . C27 . H271 . 108.2 no
C28 . C27 . H271 . 108.2 no
C29 . C27 . H271 . 108.1 no
C27 . C28 . H282 . 111.5 no
C27 . C28 . H281 . 110.5 no
H282 . C28 . H281 . 107.0 no
C27 . C28 . H283 . 111.5 no
H282 . C28 . H283 . 108.1 no
H281 . C28 . H283 . 108.0 no
C27 . C29 . H292 . 109.7 no
C27 . C29 . H293 . 110.9 no
H292 . C29 . H293 . 107.5 no
C27 . C29 . H291 . 110.7 no
H292 . C29 . H291 . 109.8 no
H293 . C29 . H291 . 108.1 no
C22 . C30 . C31 . 110.70(10) yes
C22 . C30 . C32 . 110.98(10) yes
C31 . C30 . C32 . 110.79(11) yes
C22 . C30 . H301 . 108.7 no
C31 . C30 . H301 . 108.2 no
C32 . C30 . H301 . 107.3 no
C30 . C31 . H312 . 111.1 no
C30 . C31 . H313 . 111.1 no
H312 . C31 . H313 . 107.2 no
C30 . C31 . H311 . 111.5 no
H312 . C31 . H311 . 108.9 no
H313 . C31 . H311 . 106.9 no
C30 . C32 . H323 . 109.6 no
C30 . C32 . H321 . 110.1 no
H323 . C32 . H321 . 107.2 no
C30 . C32 . H322 . 110.3 no
H323 . C32 . H322 . 111.0 no
H321 . C32 . H322 . 108.5 no
N15 . C33 . C34 . 118.54(9) yes
N15 . C33 . C41 . 118.72(9) yes
C34 . C33 . C41 . 122.74(10) yes
C33 . C34 . C35 . 122.87(10) yes
C33 . C34 . C38 . 117.60(11) yes
C35 . C34 . C38 . 119.52(11) yes
C34 . C35 . C36 . 111.34(10) yes
C34 . C35 . C37 . 111.58(11) yes
C36 . C35 . C37 . 110.88(11) yes
C34 . C35 . H351 . 107.6 no
C36 . C35 . H351 . 107.5 no
C37 . C35 . H351 . 107.7 no
C35 . C36 . H363 . 109.6 no
C35 . C36 . H361 . 110.0 no
H363 . C36 . H361 . 109.6 no
C35 . C36 . H362 . 110.1 no
H363 . C36 . H362 . 108.4 no
H361 . C36 . H362 . 109.1 no
C35 . C37 . H371 . 108.8 no
C35 . C37 . H373 . 109.8 no
H371 . C37 . H373 . 109.7 no
C35 . C37 . H372 . 109.9 no
H371 . C37 . H372 . 110.3 no
H373 . C37 . H372 . 108.2 no
C34 . C38 . C39 . 120.96(12) yes
C34 . C38 . H381 . 118.9 no
C39 . C38 . H381 . 120.2 no
C38 . C39 . C40 . 120.22(12) yes
C38 . C39 . H391 . 120.7 no
C40 . C39 . H391 . 119.1 no
C39 . C40 . C41 . 121.53(12) yes
C39 . C40 . H401 . 119.8 no
C41 . C40 . H401 . 118.7 no
C33 . C41 . C40 . 116.93(11) yes
C33 . C41 . C42 . 123.32(10) yes
C40 . C41 . C42 . 119.71(10) yes
C41 . C42 . C43 . 112.64(10) yes
C41 . C42 . C44 . 109.92(10) yes
C43 . C42 . C44 . 109.72(10) yes
C41 . C42 . H421 . 107.5 no
C43 . C42 . H421 . 108.7 no
C44 . C42 . H421 . 108.2 no
C42 . C43 . H432 . 110.3 no
C42 . C43 . H431 . 111.3 no
H432 . C43 . H431 . 107.9 no
C42 . C43 . H433 . 111.1 no
H432 . C43 . H433 . 108.3 no
H431 . C43 . H433 . 107.7 no
C42 . C44 . H442 . 110.7 no
C42 . C44 . H443 . 110.2 no
H442 . C44 . H443 . 108.4 no
C42 . C44 . H441 . 110.4 no
H442 . C44 . H441 . 107.8 no
H443 . C44 . H441 . 109.3 no
B12 . C45 . C46 . 127.63(10) yes
B12 . C45 . C53 . 119.15(10) yes
C46 . C45 . C53 . 113.11(10) yes
C45 . C46 . F47 . 121.59(10) yes
C45 . C46 . C48 . 123.95(12) yes
F47 . C46 . C48 . 114.46(11) yes
C46 . C48 . F49 . 120.09(13) yes
C46 . C48 . C50 . 120.06(13) yes
F49 . C48 . C50 . 119.85(12) yes
C48 . C50 . F51 . 120.23(14) yes
C48 . C50 . C52 . 118.88(12) yes
F51 . C50 . C52 . 120.89(14) yes
C50 . C52 . C53 . 119.32(12) yes
C50 . C52 . F55 . 119.94(12) yes
C53 . C52 . F55 . 120.74(13) yes
C45 . C53 . C52 . 124.63(12) yes
C45 . C53 . F54 . 119.72(10) yes
C52 . C53 . F54 . 115.62(11) yes
B12 . C56 . C57 . 118.37(9) yes
B12 . C56 . C64 . 128.30(10) yes
C57 . C56 . C64 . 112.98(10) yes
C56 . C57 . F58 . 119.58(9) yes
C56 . C57 . C59 . 124.94(11) yes
F58 . C57 . C59 . 115.47(10) yes
C57 . C59 . F60 . 120.88(11) yes
C57 . C59 . C61 . 119.25(11) yes
F60 . C59 . C61 . 119.88(10) yes
C59 . C61 . F62 . 120.05(11) yes
C59 . C61 . C63 . 119.06(10) yes
F62 . C61 . C63 . 120.88(11) yes
C61 . C63 . C64 . 119.74(11) yes
C61 . C63 . F66 . 119.66(10) yes
C64 . C63 . F66 . 120.57(11) yes
C63 . C64 . C56 . 124.02(11) yes
C63 . C64 . F65 . 114.68(10) yes
C56 . C64 . F65 . 121.30(10) yes
C68 . O67 . C70 . 112.84(11) yes
O67 . C68 . C69 . 113.81(17) yes
O67 . C68 . H682 . 109.0 no
C69 . C68 . H682 . 109.3 no
O67 . C68 . H681 . 107.8 no
C69 . C68 . H681 . 107.9 no
H682 . C68 . H681 . 108.9 no
C68 . C69 . H692 . 106.8 no
C68 . C69 . H691 . 109.9 no
H692 . C69 . H691 . 107.8 no
C68 . C69 . H693 . 108.7 no
H692 . C69 . H693 . 111.2 no
H691 . C69 . H693 . 112.4 no
O67 . C70 . C71 . 108.63(11) yes
O67 . C70 . H701 . 110.4 no
C71 . C70 . H701 . 110.5 no
O67 . C70 . H702 . 107.8 no
C71 . C70 . H702 . 110.8 no
H701 . C70 . H702 . 108.7 no
C70 . C71 . H711 . 111.5 no
C70 . C71 . H713 . 111.5 no
H711 . C71 . H713 . 108.1 no
C70 . C71 . H712 . 108.5 no
H711 . C71 . H712 . 108.4 no
H713 . C71 . H712 . 108.7 no
C73 . O72 . C75 . 112.84(18) yes
O72 . C73 . C74 . 109.71(18) yes
O72 . C73 . H732 . 109.1 no
C74 . C73 . H732 . 111.6 no
O72 . C73 . H731 . 106.5 no
C74 . C73 . H731 . 110.3 no
H732 . C73 . H731 . 109.5 no
C73 . C74 . H743 . 110.6 no
C73 . C74 . H741 . 111.6 no
H743 . C74 . H741 . 109.3 no
C73 . C74 . H742 . 109.9 no
H743 . C74 . H742 . 106.8 no
H741 . C74 . H742 . 108.5 no
O72 . C75 . C76 . 109.7(2) yes
O72 . C75 . H751 . 108.5 no
C76 . C75 . H751 . 110.7 no
O72 . C75 . H752 . 108.8 no
C76 . C75 . H752 . 109.2 no
H751 . C75 . H752 . 109.9 no
C75 . C76 . H762 . 108.8 no
C75 . C76 . H763 . 110.3 no
H762 . C76 . H763 . 108.0 no
C75 . C76 . H761 . 110.8 no
H762 . C76 . H761 . 109.4 no
H763 . C76 . H761 . 109.4 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C14 . H141 . C2 . 129.75 0.995 2.571 3.297(2) yes
C16 . H161 . O67 . 173.11 0.959 2.481 3.434(2) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 18/05/14 at 18:07:48
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,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   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 281,X'S) H   ( 283,X'S) 
RIDE C   (  29,X'S) H   ( 292,X'S) H   ( 293,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 312,X'S) H   ( 313,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 323,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 363,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 373,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) H   ( 433,X'S) 
RIDE C   (  44,X'S) H   ( 442,X'S) H   ( 443,X'S) H   ( 441,X'S) 
RIDE C   (  68,X'S) H   ( 682,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 692,X'S) H   ( 691,X'S) H   ( 693,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 702,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) H   ( 713,X'S) H   ( 712,X'S) 
RIDE C   (  73,X'S) H   ( 732,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 743,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   ( 762,X'S) H   ( 763,X'S) H   ( 761,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 18/05/14 at 18:07:48
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_database_code_depnum_ccdc_archive 'CCDC 1006575'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_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                   10.5956(2)
_cell_length_b                   22.6260(3)
_cell_length_c                   24.4132(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.9391(6)
_cell_angle_gamma                90
_cell_volume                     5781.64(16)

_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'
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'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 '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'


_cell_formula_units_Z            4

# Given Formula = C58 H63 B1 F15 K1 N1 O6 
# Dc =      1.38 Fooo =   2528.00 Mu =      1.90 M =   1205.02
# Found Formula = C58 H63 B1 F15 K1 N2 O6 
# Dc =      1.40 FOOO =   2528.00 Mu =      1.92 M =   1219.03

_chemical_formula_sum            'C58 H63 B1 F15 K1 N2 O6'
_chemical_formula_moiety         'C58 H63 B1 F15 K1 N2 O6'
_chemical_compound_source        ?
_chemical_formula_weight         1219.03


_cell_measurement_reflns_used    12567
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.140
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.400

_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    0.192

# Sheldrick geometric approximatio 0.96 0.97 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.97
# 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    '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            70863
_reflns_number_total             13012
_diffrn_reflns_av_R_equivalents  0.037
# Number of reflections without Friedels Law is 24262 
# Number of reflections with Friedels Law is 13012 
# Theoretical number of reflections is about 13290 


_diffrn_reflns_theta_min         5.116
_diffrn_reflns_theta_max         27.506
_diffrn_measured_fraction_theta_max 0.979

_diffrn_reflns_theta_full        25.030
_diffrn_measured_fraction_theta_full 0.982


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      13.68

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

_refine_diff_density_min         -0.69
_refine_diff_density_max         1.01


# 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>-3.0\s(I)
_refine_ls_number_reflns         13012
_refine_ls_number_restraints     108
_refine_ls_number_parameters     776
_oxford_refine_ls_R_factor_ref   0.1062
_refine_ls_wR_factor_ref         0.1453
_refine_ls_goodness_of_fit_ref   0.9348
_refine_ls_shift/su_max          0.0205665
_refine_ls_shift/su_mean         0.0005101


# The values computed from all data 
_oxford_reflns_number_all        13012
_refine_ls_R_factor_all          0.1062
_refine_ls_wR_factor_all         0.1453

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9113
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_gt          0.1251

# 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: 
 24.9 35.3 16.8 3.87 
;

# 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
K1 K 0.93543(7) 0.54134(3) 0.20768(3) 0.0373 1.0000 Uani . . . . . .
F2 F 0.59080(16) 0.80871(8) 0.42284(8) 0.0392 1.0000 Uani . . . . . .
C3 C 0.6689(3) 0.85177(13) 0.44706(11) 0.0305 1.0000 Uani . . . . . .
C4 C 0.7958(3) 0.83884(13) 0.46761(11) 0.0278 1.0000 Uani . . . . . .
C5 C 0.8620(3) 0.88717(13) 0.49259(11) 0.0304 1.0000 Uani . . . . . .
F6 F 0.98637(17) 0.88244(8) 0.51566(7) 0.0396 1.0000 Uani . . . . . .
C7 C 0.8097(3) 0.94259(13) 0.49645(12) 0.0331 1.0000 Uani . . . . . .
F8 F 0.87982(19) 0.98728(8) 0.52213(8) 0.0454 1.0000 Uani . . . . . .
C9 C 0.6841(3) 0.95268(13) 0.47472(13) 0.0361 1.0000 Uani . . . . . .
C10 C 0.6133(3) 0.90663(14) 0.44965(12) 0.0349 1.0000 Uani . . . . . .
F11 F 0.48991(18) 0.91531(9) 0.42777(9) 0.0496 1.0000 Uani . . . . . .
F12 F 0.6328(2) 1.00672(8) 0.47742(9) 0.0519 1.0000 Uani . . . . . .
B13 B 0.8518(3) 0.77032(14) 0.46281(12) 0.0263 1.0000 Uani . . . . . .
C14 C 0.7837(3) 0.73309(13) 0.50903(11) 0.0280 1.0000 Uani . . . . . .
C15 C 0.6883(3) 0.69007(14) 0.49966(11) 0.0311 1.0000 Uani . . . . . .
F16 F 0.63999(17) 0.67249(9) 0.44771(7) 0.0416 1.0000 Uani . . . . . .
C17 C 0.6345(3) 0.66215(14) 0.54099(13) 0.0352 1.0000 Uani . . . . . .
F18 F 0.54479(19) 0.62027(9) 0.52801(8) 0.0499 1.0000 Uani . . . . . .
C19 C 0.6745(3) 0.67635(15) 0.59544(12) 0.0368 1.0000 Uani . . . . . .
F20 F 0.6247(2) 0.64874(10) 0.63588(8) 0.0532 1.0000 Uani . . . . . .
C21 C 0.7668(3) 0.71902(15) 0.60785(11) 0.0346 1.0000 Uani . . . . . .
C22 C 0.8172(3) 0.74615(13) 0.56563(12) 0.0297 1.0000 Uani . . . . . .
F23 F 0.90655(16) 0.78812(8) 0.58124(7) 0.0361 1.0000 Uani . . . . . .
F24 F 0.80787(19) 0.73357(10) 0.66113(7) 0.0484 1.0000 Uani . . . . . .
C25 C 0.8125(3) 0.74641(12) 0.39774(11) 0.0276 1.0000 Uani . . . . . .
C26 C 0.8984(3) 0.69897(13) 0.37946(11) 0.0289 1.0000 Uani . . . . . .
N27 N 0.8568(2) 0.67542(10) 0.32146(9) 0.0256 1.0000 Uani . . . . . .
C28 C 0.8078(3) 0.71400(12) 0.27647(10) 0.0259 1.0000 Uani . . . . . .
C29 C 0.8936(3) 0.74788(14) 0.25119(11) 0.0332 1.0000 Uani . . . . . .
C30 C 1.0368(3) 0.74363(16) 0.26939(14) 0.0420 1.0000 Uani . . . . . .
C31 C 1.0972(4) 0.7070(2) 0.22747(19) 0.0608 1.0000 Uani . . . . . .
C32 C 1.1010(4) 0.80406(19) 0.27797(17) 0.0602 1.0000 Uani . . . . . .
C33 C 0.8441(3) 0.78415(15) 0.20700(13) 0.0414 1.0000 Uani . . . . . .
C34 C 0.7152(4) 0.78645(15) 0.18806(13) 0.0430 1.0000 Uani . . . . . .
C35 C 0.6320(3) 0.75324(14) 0.21382(12) 0.0373 1.0000 Uani . . . . . .
C36 C 0.6759(3) 0.71680(13) 0.25871(11) 0.0310 1.0000 Uani . . . . . .
C37 C 0.5815(3) 0.68092(15) 0.28599(13) 0.0380 1.0000 Uani . . . . . .
C38 C 0.4771(3) 0.71967(18) 0.30389(15) 0.0504 1.0000 Uani . . . . . .
C39 C 0.5242(4) 0.63190(19) 0.24678(18) 0.0627 1.0000 Uani . . . . . .
C40 C 0.8924(3) 0.61881(12) 0.31458(11) 0.0276 1.0000 Uani . . . . . .
N41 N 0.9354(2) 0.59922(11) 0.36649(9) 0.0305 1.0000 Uani . . . . . .
C42 C 0.9122(3) 0.64081(13) 0.41049(11) 0.0343 1.0000 Uani . . . . . .
C43 C 0.9768(3) 0.54051(13) 0.38210(11) 0.0301 1.0000 Uani . . . . . .
C44 C 0.8867(3) 0.49761(13) 0.39067(12) 0.0339 1.0000 Uani . . . . . .
C45 C 0.9320(3) 0.44289(14) 0.41160(14) 0.0409 1.0000 Uani . . . . . .
C46 C 1.0613(3) 0.43179(15) 0.42402(14) 0.0437 1.0000 Uani . . . . . .
C47 C 1.1484(3) 0.47405(15) 0.41431(14) 0.0412 1.0000 Uani . . . . . .
C48 C 1.1090(3) 0.52939(13) 0.39356(11) 0.0344 1.0000 Uani D . . . . .
C52 C 0.7437(3) 0.50958(15) 0.37826(14) 0.0408 1.0000 Uani . . . . . .
C53 C 0.6803(4) 0.5016(3) 0.4291(2) 0.0776 1.0000 Uani . . . . . .
C54 C 0.6811(4) 0.4725(2) 0.3299(2) 0.0816 1.0000 Uani . . . . . .
C55 C 1.0105(3) 0.76848(12) 0.47548(11) 0.0281 1.0000 Uani . . . . . .
C56 C 1.0870(3) 0.72947(13) 0.50974(11) 0.0292 1.0000 Uani . . . . . .
F57 F 1.03546(16) 0.69146(8) 0.54289(7) 0.0362 1.0000 Uani . . . . . .
C58 C 1.2180(3) 0.72463(14) 0.51255(13) 0.0365 1.0000 Uani . . . . . .
F59 F 1.28434(18) 0.68589(9) 0.54794(8) 0.0491 1.0000 Uani . . . . . .
C60 C 1.2804(3) 0.75943(16) 0.47981(13) 0.0409 1.0000 Uani . . . . . .
F61 F 1.40812(18) 0.75570(11) 0.48258(9) 0.0611 1.0000 Uani . . . . . .
C62 C 1.2116(3) 0.79991(15) 0.44534(13) 0.0396 1.0000 Uani . . . . . .
C63 C 1.0813(3) 0.80325(13) 0.44431(11) 0.0318 1.0000 Uani . . . . . .
F64 F 1.01975(17) 0.84379(8) 0.40831(7) 0.0406 1.0000 Uani . . . . . .
F65 F 1.27055(19) 0.83530(10) 0.41291(9) 0.0559 1.0000 Uani . . . . . .
O66 O 0.7097(2) 0.58289(10) 0.15402(10) 0.0454 1.0000 Uani . . . . . .
C67 C 0.7250(4) 0.64099(17) 0.13429(16) 0.0565 1.0000 Uani . . . . . .
C68 C 0.8143(5) 0.64396(18) 0.09396(16) 0.0644 1.0000 Uani . . . . . .
O69 O 0.9375(3) 0.62480(12) 0.12052(11) 0.0564 1.0000 Uani . . . . . .
C70 C 1.0293(5) 0.6264(2) 0.08404(18) 0.0706 1.0000 Uani . . . . . .
C71 C 1.1560(5) 0.6085(2) 0.1156(2) 0.0700 1.0000 Uani . . . . . .
O72 O 1.1447(3) 0.55115(13) 0.13603(13) 0.0629 1.0000 Uani . . . . . .
C73 C 1.2617(4) 0.5289(3) 0.1654(2) 0.0803 1.0000 Uani . . . . . .
C74 C 1.2452(4) 0.4672(2) 0.1837(2) 0.0708 1.0000 Uani . . . . . .
O75 O 1.1536(3) 0.46586(13) 0.21999(12) 0.0613 1.0000 Uani . . . . . .
C76 C 1.1409(5) 0.4079(2) 0.2420(2) 0.0704 1.0000 Uani . . . . . .
C77 C 1.0348(4) 0.4079(2) 0.27499(17) 0.0655 1.0000 Uani . . . . . .
O78 O 0.9168(2) 0.42594(11) 0.24478(10) 0.0494 1.0000 Uani . . . . . .
C79 C 0.8628(4) 0.38687(16) 0.20185(14) 0.0493 1.0000 Uani . . . . . .
C80 C 0.7295(4) 0.40659(15) 0.18233(15) 0.0477 1.0000 Uani . . . . . .
O81 O 0.7341(2) 0.46319(10) 0.15784(9) 0.0415 1.0000 Uani . . . . . .
C82 C 0.6118(3) 0.48950(17) 0.14583(15) 0.0470 1.0000 Uani . . . . . .
C83 C 0.6243(4) 0.54708(17) 0.11766(14) 0.0475 1.0000 Uani . . . . . .
C300 C 1.2104(4) 0.57433(14) 0.38274(15) 0.0448 0.702(12) Uani D . P 1 1 .
C301 C 1.2937(7) 0.5499(3) 0.3429(3) 0.0651 0.702(12) Uani D . P 1 1 .
C302 C 1.2899(6) 0.5947(3) 0.4365(2) 0.0599 0.702(12) Uani D . P 1 1 .
C310 C 1.1989(7) 0.5793(3) 0.3841(3) 0.0464 0.298(12) Uani D . P 1 2 .
C311 C 1.2281(14) 0.5785(7) 0.3255(4) 0.0572 0.298(12) Uani D . P 1 2 .
C312 C 1.3207(11) 0.5775(7) 0.4265(6) 0.0591 0.298(12) Uani D . P 1 2 .
H251 H 0.8195 0.7800 0.3737 0.0330 1.0000 Uiso R . . . . .
H252 H 0.7257 0.7319 0.3923 0.0333 1.0000 Uiso R . . . . .
H261 H 0.9853 0.7162 0.3804 0.0343 1.0000 Uiso R . . . . .
H301 H 1.0521 0.7220 0.3043 0.0503 1.0000 Uiso R . . . . .
H311 H 1.1882 0.7060 0.2395 0.0907 1.0000 Uiso R . . . . .
H313 H 1.0789 0.7268 0.1920 0.0909 1.0000 Uiso R . . . . .
H312 H 1.0622 0.6674 0.2253 0.0910 1.0000 Uiso R . . . . .
H322 H 1.1877 0.7997 0.2954 0.0899 1.0000 Uiso R . . . . .
H321 H 1.0562 0.8279 0.3008 0.0895 1.0000 Uiso R . . . . .
H323 H 1.0995 0.8235 0.2431 0.0896 1.0000 Uiso R . . . . .
H331 H 0.8988 0.8072 0.1896 0.0500 1.0000 Uiso R . . . . .
H341 H 0.6834 0.8104 0.1578 0.0518 1.0000 Uiso R . . . . .
H351 H 0.5446 0.7552 0.2012 0.0448 1.0000 Uiso R . . . . .
H371 H 0.6275 0.6621 0.3189 0.0458 1.0000 Uiso R . . . . .
H382 H 0.4243 0.6949 0.3229 0.0756 1.0000 Uiso R . . . . .
H383 H 0.5146 0.7503 0.3290 0.0757 1.0000 Uiso R . . . . .
H381 H 0.4258 0.7371 0.2719 0.0757 1.0000 Uiso R . . . . .
H391 H 0.4661 0.6088 0.2645 0.0936 1.0000 Uiso R . . . . .
H393 H 0.4780 0.6487 0.2135 0.0938 1.0000 Uiso R . . . . .
H392 H 0.5911 0.6067 0.2373 0.0937 1.0000 Uiso R . . . . .
H422 H 0.9809 0.6403 0.4408 0.0407 1.0000 Uiso R . . . . .
H421 H 0.8332 0.6305 0.4244 0.0411 1.0000 Uiso R . . . . .
H451 H 0.8742 0.4139 0.4167 0.0489 1.0000 Uiso R . . . . .
H461 H 1.0896 0.3947 0.4382 0.0531 1.0000 Uiso R . . . . .
H471 H 1.2362 0.4659 0.4209 0.0500 1.0000 Uiso R . . . . .
H521 H 0.7314 0.5507 0.3668 0.0488 1.0000 Uiso R . . . . .
H533 H 0.5923 0.5139 0.4206 0.1166 1.0000 Uiso R . . . . .
H531 H 0.7235 0.5247 0.4600 0.1172 1.0000 Uiso R . . . . .
H532 H 0.6836 0.4606 0.4393 0.1169 1.0000 Uiso R . . . . .
H541 H 0.5920 0.4828 0.3203 0.1223 1.0000 Uiso R . . . . .
H543 H 0.7235 0.4788 0.2985 0.1233 1.0000 Uiso R . . . . .
H542 H 0.6871 0.4315 0.3405 0.1229 1.0000 Uiso R . . . . .
H672 H 0.7600 0.6654 0.1668 0.0680 1.0000 Uiso R . . . . .
H671 H 0.6402 0.6567 0.1171 0.0679 1.0000 Uiso R . . . . .
H681 H 0.8194 0.6854 0.0830 0.0771 1.0000 Uiso R . . . . .
H682 H 0.7823 0.6199 0.0617 0.0769 1.0000 Uiso R . . . . .
H702 H 1.0341 0.6660 0.0689 0.0848 1.0000 Uiso R . . . . .
H701 H 1.0054 0.5991 0.0533 0.0848 1.0000 Uiso R . . . . .
H712 H 1.1833 0.6352 0.1467 0.0833 1.0000 Uiso R . . . . .
H711 H 1.2206 0.6088 0.0917 0.0836 1.0000 Uiso R . . . . .
H732 H 1.2890 0.5538 0.1970 0.0959 1.0000 Uiso R . . . . .
H731 H 1.3256 0.5295 0.1415 0.0958 1.0000 Uiso R . . . . .
H742 H 1.3264 0.4530 0.2036 0.0849 1.0000 Uiso R . . . . .
H741 H 1.2189 0.4419 0.1515 0.0851 1.0000 Uiso R . . . . .
H762 H 1.2200 0.3981 0.2663 0.0845 1.0000 Uiso R . . . . .
H761 H 1.1220 0.3788 0.2121 0.0840 1.0000 Uiso R . . . . .
H772 H 1.0603 0.4359 0.3065 0.0779 1.0000 Uiso R . . . . .
H771 H 1.0262 0.3674 0.2890 0.0781 1.0000 Uiso R . . . . .
H792 H 0.9123 0.3887 0.1717 0.0587 1.0000 Uiso R . . . . .
H791 H 0.8643 0.3469 0.2154 0.0594 1.0000 Uiso R . . . . .
H802 H 0.6846 0.4093 0.2147 0.0570 1.0000 Uiso R . . . . .
H801 H 0.6848 0.3781 0.1557 0.0571 1.0000 Uiso R . . . . .
H821 H 0.5772 0.4959 0.1799 0.0572 1.0000 Uiso R . . . . .
H822 H 0.5547 0.4636 0.1212 0.0566 1.0000 Uiso R . . . . .
H831 H 0.5414 0.5666 0.1102 0.0572 1.0000 Uiso R . . . . .
H832 H 0.6565 0.5414 0.0832 0.0568 1.0000 Uiso R . . . . .
H3001 H 1.1659 0.6089 0.3650 0.0544 0.702(12) Uiso R . P 1 1 .
H3013 H 1.3547 0.5791 0.3360 0.0959 0.702(12) Uiso R . P 1 1 .
H3011 H 1.3386 0.5159 0.3596 0.0957 0.702(12) Uiso R . P 1 1 .
H3012 H 1.2399 0.5387 0.3086 0.0962 0.702(12) Uiso R . P 1 1 .
H3021 H 1.3410 0.6286 0.4287 0.0899 0.702(12) Uiso R . P 1 1 .
H3023 H 1.2348 0.6059 0.4635 0.0901 0.702(12) Uiso R . P 1 1 .
H3022 H 1.3464 0.5628 0.4514 0.0901 0.702(12) Uiso R . P 1 1 .
H3101 H 1.1557 0.6170 0.3893 0.0559 0.298(12) Uiso R . P 1 2 .
H3111 H 1.2956 0.6061 0.3221 0.0870 0.298(12) Uiso R . P 1 2 .
H3113 H 1.2553 0.5391 0.3173 0.0872 0.298(12) Uiso R . P 1 2 .
H3112 H 1.1530 0.5886 0.3002 0.0869 0.298(12) Uiso R . P 1 2 .
H3122 H 1.3693 0.6131 0.4241 0.0869 0.298(12) Uiso R . P 1 2 .
H3121 H 1.2976 0.5744 0.4636 0.0871 0.298(12) Uiso R . P 1 2 .
H3123 H 1.3714 0.5439 0.4199 0.0869 0.298(12) Uiso R . P 1 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.29095(19)
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
F2 . C3 . 1.353(3) yes
C3 . C4 . 1.391(4) yes
C3 . C10 . 1.379(4) yes
C4 . C5 . 1.388(4) yes
C4 . B13 . 1.671(4) yes
C5 . F6 . 1.355(3) yes
C5 . C7 . 1.380(4) yes
C7 . F8 . 1.350(3) yes
C7 . C9 . 1.373(4) yes
C9 . C10 . 1.371(4) yes
C9 . F12 . 1.344(3) yes
C10 . F11 . 1.348(3) yes
B13 . C14 . 1.660(4) yes
B13 . C25 . 1.668(4) yes
B13 . C55 . 1.662(4) yes
C14 . C15 . 1.397(4) yes
C14 . C22 . 1.404(4) yes
C15 . F16 . 1.352(3) yes
C15 . C17 . 1.386(4) yes
C17 . F18 . 1.345(3) yes
C17 . C19 . 1.369(4) yes
C19 . F20 . 1.344(3) yes
C19 . C21 . 1.374(5) yes
C21 . C22 . 1.377(4) yes
C21 . F24 . 1.347(3) yes
C22 . F23 . 1.354(3) yes
C25 . C26 . 1.519(4) yes
C25 . H251 . 0.970 no
C25 . H252 . 0.965 no
C26 . N27 . 1.513(3) yes
C26 . C42 . 1.514(4) yes
C26 . H261 . 0.997 no
N27 . C28 . 1.435(3) yes
N27 . C40 . 1.353(4) yes
C28 . C29 . 1.403(4) yes
C28 . C36 . 1.399(4) yes
C29 . C30 . 1.516(4) yes
C29 . C33 . 1.391(4) yes
C30 . C31 . 1.532(5) yes
C30 . C32 . 1.527(5) yes
C30 . H301 . 0.975 no
C31 . H311 . 0.964 no
C31 . H313 . 0.968 no
C31 . H312 . 0.969 no
C32 . H322 . 0.957 no
C32 . H321 . 0.953 no
C32 . H323 . 0.957 no
C33 . C34 . 1.373(5) yes
C33 . H331 . 0.930 no
C34 . C35 . 1.382(5) yes
C34 . H341 . 0.935 no
C35 . C36 . 1.393(4) yes
C35 . H351 . 0.930 no
C36 . C37 . 1.520(4) yes
C37 . C38 . 1.527(5) yes
C37 . C39 . 1.528(5) yes
C37 . H371 . 0.971 no
C38 . H382 . 0.961 no
C38 . H383 . 0.968 no
C38 . H381 . 0.964 no
C39 . H391 . 0.960 no
C39 . H393 . 0.959 no
C39 . H392 . 0.966 no
C40 . N41 . 1.353(3) yes
N41 . C42 . 1.477(3) yes
N41 . C43 . 1.432(4) yes
C42 . H422 . 0.955 no
C42 . H421 . 0.979 no
C43 . C44 . 1.400(4) yes
C43 . C48 . 1.408(4) yes
C44 . C45 . 1.396(4) yes
C44 . C52 . 1.522(4) yes
C45 . C46 . 1.380(5) yes
C45 . H451 . 0.919 no
C46 . C47 . 1.375(5) yes
C46 . H461 . 0.938 no
C47 . C48 . 1.390(4) yes
C47 . H471 . 0.937 no
C48 . C300 . 1.531(4) yes
C48 . C310 . 1.517(6) yes
C52 . C53 . 1.510(5) yes
C52 . C54 . 1.513(5) yes
C52 . H521 . 0.976 no
C53 . H533 . 0.964 no
C53 . H531 . 0.973 no
C53 . H532 . 0.960 no
C54 . H541 . 0.966 no
C54 . H543 . 0.959 no
C54 . H542 . 0.962 no
C55 . C56 . 1.387(4) yes
C55 . C63 . 1.392(4) yes
C56 . F57 . 1.353(3) yes
C56 . C58 . 1.384(4) yes
C58 . F59 . 1.349(4) yes
C58 . C60 . 1.364(5) yes
C60 . F61 . 1.347(3) yes
C60 . C62 . 1.374(5) yes
C62 . C63 . 1.379(4) yes
C62 . F65 . 1.346(4) yes
C63 . F64 . 1.364(3) yes
O66 . C67 . 1.418(4) yes
O66 . C83 . 1.419(4) yes
C67 . C68 . 1.469(6) yes
C67 . H672 . 0.990 no
C67 . H671 . 0.996 no
C68 . O69 . 1.432(5) yes
C68 . H681 . 0.979 no
C68 . H682 . 0.974 no
O69 . C70 . 1.418(5) yes
C70 . C71 . 1.495(7) yes
C70 . H702 . 0.973 no
C70 . H701 . 0.975 no
C71 . O72 . 1.402(5) yes
C71 . H712 . 0.979 no
C71 . H711 . 0.966 no
O72 . C73 . 1.423(6) yes
C73 . C74 . 1.484(7) yes
C73 . H732 . 0.964 no
C73 . H731 . 0.960 no
C74 . O75 . 1.413(5) yes
C74 . H742 . 0.974 no
C74 . H741 . 0.976 no
O75 . C76 . 1.431(5) yes
C76 . C77 . 1.481(6) yes
C76 . H762 . 0.975 no
C76 . H761 . 0.980 no
C77 . O78 . 1.410(5) yes
C77 . H772 . 1.001 no
C77 . H771 . 0.988 no
O78 . C79 . 1.422(4) yes
C79 . C80 . 1.488(5) yes
C79 . H792 . 0.968 no
C79 . H791 . 0.963 no
C80 . O81 . 1.417(4) yes
C80 . H802 . 0.986 no
C80 . H801 . 0.983 no
O81 . C82 . 1.415(4) yes
C82 . C83 . 1.489(5) yes
C82 . H821 . 0.970 no
C82 . H822 . 0.978 no
C83 . H831 . 0.974 no
C83 . H832 . 0.964 no
C300 . C301 . 1.517(5) yes
C300 . C302 . 1.517(5) yes
C300 . H3001 . 0.979 no
C301 . H3013 . 0.957 no
C301 . H3011 . 0.961 no
C301 . H3012 . 0.971 no
C302 . H3021 . 0.973 no
C302 . H3023 . 0.979 no
C302 . H3022 . 0.972 no
C310 . C311 . 1.509(6) yes
C310 . C312 . 1.524(7) yes
C310 . H3101 . 0.985 no
C311 . H3111 . 0.963 no
C311 . H3113 . 0.967 no
C311 . H3112 . 0.957 no
C312 . H3122 . 0.963 no
C312 . H3121 . 0.977 no
C312 . H3123 . 0.960 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
F2 . C3 . C4 . 119.8(3) yes
F2 . C3 . C10 . 115.6(3) yes
C4 . C3 . C10 . 124.6(3) yes
C3 . C4 . C5 . 112.8(3) yes
C3 . C4 . B13 . 120.3(2) yes
C5 . C4 . B13 . 126.9(2) yes
C4 . C5 . F6 . 120.9(3) yes
C4 . C5 . C7 . 124.4(3) yes
F6 . C5 . C7 . 114.7(3) yes
C5 . C7 . F8 . 121.0(3) yes
C5 . C7 . C9 . 120.0(3) yes
F8 . C7 . C9 . 119.0(3) yes
C7 . C9 . C10 . 118.4(3) yes
C7 . C9 . F12 . 120.5(3) yes
C10 . C9 . F12 . 121.1(3) yes
C3 . C10 . C9 . 119.8(3) yes
C3 . C10 . F11 . 120.5(3) yes
C9 . C10 . F11 . 119.7(3) yes
C4 . B13 . C14 . 103.1(2) yes
C4 . B13 . C25 . 109.2(2) yes
C14 . B13 . C25 . 114.3(2) yes
C4 . B13 . C55 . 111.7(2) yes
C14 . B13 . C55 . 113.3(2) yes
C25 . B13 . C55 . 105.4(2) yes
B13 . C14 . C15 . 128.5(2) yes
B13 . C14 . C22 . 119.5(2) yes
C15 . C14 . C22 . 111.9(2) yes
C14 . C15 . F16 . 121.2(2) yes
C14 . C15 . C17 . 124.6(3) yes
F16 . C15 . C17 . 114.2(3) yes
C15 . C17 . F18 . 120.3(3) yes
C15 . C17 . C19 . 120.0(3) yes
F18 . C17 . C19 . 119.7(3) yes
C17 . C19 . F20 . 120.4(3) yes
C17 . C19 . C21 . 118.8(3) yes
F20 . C19 . C21 . 120.8(3) yes
C19 . C21 . C22 . 119.6(3) yes
C19 . C21 . F24 . 119.8(3) yes
C22 . C21 . F24 . 120.6(3) yes
C14 . C22 . C21 . 125.1(3) yes
C14 . C22 . F23 . 118.9(3) yes
C21 . C22 . F23 . 116.0(2) yes
B13 . C25 . C26 . 115.9(2) yes
B13 . C25 . H251 . 106.9 no
C26 . C25 . H251 . 105.7 no
B13 . C25 . H252 . 109.5 no
C26 . C25 . H252 . 108.7 no
H251 . C25 . H252 . 110.1 no
C25 . C26 . N27 . 115.0(2) yes
C25 . C26 . C42 . 118.9(2) yes
N27 . C26 . C42 . 98.8(2) yes
C25 . C26 . H261 . 108.1 no
N27 . C26 . H261 . 107.0 no
C42 . C26 . H261 . 108.1 no
C26 . N27 . C28 . 121.3(2) yes
C26 . N27 . C40 . 113.8(2) yes
C28 . N27 . C40 . 123.7(2) yes
N27 . C28 . C29 . 119.2(2) yes
N27 . C28 . C36 . 119.3(2) yes
C29 . C28 . C36 . 121.5(3) yes
C28 . C29 . C30 . 121.5(3) yes
C28 . C29 . C33 . 118.1(3) yes
C30 . C29 . C33 . 120.3(3) yes
C29 . C30 . C31 . 110.0(3) yes
C29 . C30 . C32 . 112.8(3) yes
C31 . C30 . C32 . 110.6(3) yes
C29 . C30 . H301 . 108.1 no
C31 . C30 . H301 . 106.4 no
C32 . C30 . H301 . 108.7 no
C30 . C31 . H311 . 108.1 no
C30 . C31 . H313 . 107.6 no
H311 . C31 . H313 . 109.6 no
C30 . C31 . H312 . 109.9 no
H311 . C31 . H312 . 110.5 no
H313 . C31 . H312 . 111.0 no
C30 . C32 . H322 . 110.2 no
C30 . C32 . H321 . 109.6 no
H322 . C32 . H321 . 109.2 no
C30 . C32 . H323 . 110.2 no
H322 . C32 . H323 . 109.0 no
H321 . C32 . H323 . 108.6 no
C29 . C33 . C34 . 121.3(3) yes
C29 . C33 . H331 . 119.8 no
C34 . C33 . H331 . 118.9 no
C33 . C34 . C35 . 119.8(3) yes
C33 . C34 . H341 . 120.4 no
C35 . C34 . H341 . 119.8 no
C34 . C35 . C36 . 121.4(3) yes
C34 . C35 . H351 . 119.8 no
C36 . C35 . H351 . 118.8 no
C28 . C36 . C35 . 117.8(3) yes
C28 . C36 . C37 . 122.3(3) yes
C35 . C36 . C37 . 119.9(3) yes
C36 . C37 . C38 . 112.0(3) yes
C36 . C37 . C39 . 109.7(3) yes
C38 . C37 . C39 . 111.2(3) yes
C36 . C37 . H371 . 108.5 no
C38 . C37 . H371 . 108.0 no
C39 . C37 . H371 . 107.4 no
C37 . C38 . H382 . 107.8 no
C37 . C38 . H383 . 110.3 no
H382 . C38 . H383 . 109.0 no
C37 . C38 . H381 . 110.3 no
H382 . C38 . H381 . 109.4 no
H383 . C38 . H381 . 110.0 no
C37 . C39 . H391 . 109.4 no
C37 . C39 . H393 . 110.0 no
H391 . C39 . H393 . 108.6 no
C37 . C39 . H392 . 110.1 no
H391 . C39 . H392 . 109.5 no
H393 . C39 . H392 . 109.2 no
N27 . C40 . N41 . 104.7(2) yes
C40 . N41 . C42 . 113.7(2) yes
C40 . N41 . C43 . 126.7(2) yes
C42 . N41 . C43 . 118.4(2) yes
C26 . C42 . N41 . 101.8(2) yes
C26 . C42 . H422 . 113.7 no
N41 . C42 . H422 . 111.3 no
C26 . C42 . H421 . 111.1 no
N41 . C42 . H421 . 110.4 no
H422 . C42 . H421 . 108.5 no
N41 . C43 . C44 . 119.6(3) yes
N41 . C43 . C48 . 118.3(3) yes
C44 . C43 . C48 . 121.8(3) yes
C43 . C44 . C45 . 117.7(3) yes
C43 . C44 . C52 . 121.9(3) yes
C45 . C44 . C52 . 120.4(3) yes
C44 . C45 . C46 . 121.0(3) yes
C44 . C45 . H451 . 118.9 no
C46 . C45 . H451 . 120.0 no
C45 . C46 . C47 . 120.4(3) yes
C45 . C46 . H461 . 119.5 no
C47 . C46 . H461 . 120.1 no
C46 . C47 . C48 . 121.2(3) yes
C46 . C47 . H471 . 120.5 no
C48 . C47 . H471 . 118.3 no
C43 . C48 . C47 . 117.8(3) yes
C43 . C48 . C300 . 123.3(3) yes
C47 . C48 . C300 . 118.8(3) yes
C43 . C48 . C47 . 117.8(3) yes
C43 . C48 . C310 . 117.7(4) yes
C47 . C48 . C310 . 124.4(4) yes
C44 . C52 . C53 . 111.8(3) yes
C44 . C52 . C54 . 111.0(3) yes
C53 . C52 . C54 . 112.1(4) yes
C44 . C52 . H521 . 108.1 no
C53 . C52 . H521 . 107.1 no
C54 . C52 . H521 . 106.4 no
C52 . C53 . H533 . 109.1 no
C52 . C53 . H531 . 111.0 no
H533 . C53 . H531 . 109.5 no
C52 . C53 . H532 . 109.1 no
H533 . C53 . H532 . 109.3 no
H531 . C53 . H532 . 108.8 no
C52 . C54 . H541 . 110.4 no
C52 . C54 . H543 . 109.8 no
H541 . C54 . H543 . 109.4 no
C52 . C54 . H542 . 108.9 no
H541 . C54 . H542 . 108.6 no
H543 . C54 . H542 . 109.8 no
B13 . C55 . C56 . 127.4(3) yes
B13 . C55 . C63 . 120.0(2) yes
C56 . C55 . C63 . 112.1(3) yes
C55 . C56 . F57 . 120.9(2) yes
C55 . C56 . C58 . 124.6(3) yes
F57 . C56 . C58 . 114.5(3) yes
C56 . C58 . F59 . 120.1(3) yes
C56 . C58 . C60 . 119.9(3) yes
F59 . C58 . C60 . 119.9(3) yes
C58 . C60 . F61 . 120.6(3) yes
C58 . C60 . C62 . 119.0(3) yes
F61 . C60 . C62 . 120.4(3) yes
C60 . C62 . C63 . 118.8(3) yes
C60 . C62 . F65 . 120.4(3) yes
C63 . C62 . F65 . 120.8(3) yes
C55 . C63 . C62 . 125.6(3) yes
C55 . C63 . F64 . 119.2(3) yes
C62 . C63 . F64 . 115.2(3) yes
C67 . O66 . C83 . 114.3(3) yes
O66 . C67 . C68 . 112.9(3) yes
O66 . C67 . H672 . 107.0 no
C68 . C67 . H672 . 108.1 no
O66 . C67 . H671 . 109.4 no
C68 . C67 . H671 . 109.4 no
H672 . C67 . H671 . 109.9 no
C67 . C68 . O69 . 108.6(3) yes
C67 . C68 . H681 . 107.3 no
O69 . C68 . H681 . 109.2 no
C67 . C68 . H682 . 109.8 no
O69 . C68 . H682 . 112.0 no
H681 . C68 . H682 . 109.8 no
C68 . O69 . C70 . 112.0(3) yes
O69 . C70 . C71 . 108.6(4) yes
O69 . C70 . H702 . 110.0 no
C71 . C70 . H702 . 110.5 no
O69 . C70 . H701 . 110.2 no
C71 . C70 . H701 . 109.3 no
H702 . C70 . H701 . 108.3 no
C70 . C71 . O72 . 108.4(3) yes
C70 . C71 . H712 . 111.4 no
O72 . C71 . H712 . 109.0 no
C70 . C71 . H711 . 110.5 no
O72 . C71 . H711 . 109.2 no
H712 . C71 . H711 . 108.2 no
C71 . O72 . C73 . 113.0(4) yes
O72 . C73 . C74 . 110.5(4) yes
O72 . C73 . H732 . 109.0 no
C74 . C73 . H732 . 110.1 no
O72 . C73 . H731 . 109.3 no
C74 . C73 . H731 . 108.9 no
H732 . C73 . H731 . 108.9 no
C73 . C74 . O75 . 109.5(4) yes
C73 . C74 . H742 . 108.9 no
O75 . C74 . H742 . 108.6 no
C73 . C74 . H741 . 110.0 no
O75 . C74 . H741 . 110.7 no
H742 . C74 . H741 . 109.2 no
C74 . O75 . C76 . 111.6(3) yes
O75 . C76 . C77 . 109.1(3) yes
O75 . C76 . H762 . 108.3 no
C77 . C76 . H762 . 108.8 no
O75 . C76 . H761 . 110.8 no
C77 . C76 . H761 . 108.7 no
H762 . C76 . H761 . 111.1 no
C76 . C77 . O78 . 113.7(3) yes
C76 . C77 . H772 . 106.4 no
O78 . C77 . H772 . 109.3 no
C76 . C77 . H771 . 107.9 no
O78 . C77 . H771 . 109.1 no
H772 . C77 . H771 . 110.4 no
C77 . O78 . C79 . 115.3(3) yes
O78 . C79 . C80 . 107.6(3) yes
O78 . C79 . H792 . 109.3 no
C80 . C79 . H792 . 110.1 no
O78 . C79 . H791 . 110.3 no
C80 . C79 . H791 . 110.8 no
H792 . C79 . H791 . 108.7 no
C79 . C80 . O81 . 108.2(3) yes
C79 . C80 . H802 . 108.4 no
O81 . C80 . H802 . 109.5 no
C79 . C80 . H801 . 110.5 no
O81 . C80 . H801 . 111.1 no
H802 . C80 . H801 . 109.1 no
C80 . O81 . C82 . 112.1(3) yes
O81 . C82 . C83 . 108.6(3) yes
O81 . C82 . H821 . 109.9 no
C83 . C82 . H821 . 109.8 no
O81 . C82 . H822 . 109.5 no
C83 . C82 . H822 . 109.3 no
H821 . C82 . H822 . 109.7 no
C82 . C83 . O66 . 107.7(3) yes
C82 . C83 . H831 . 109.9 no
O66 . C83 . H831 . 109.0 no
C82 . C83 . H832 . 110.9 no
O66 . C83 . H832 . 110.1 no
H831 . C83 . H832 . 109.1 no
C48 . C300 . C301 . 111.27(7) yes
C48 . C300 . C302 . 111.27(7) yes
C301 . C300 . C302 . 111.43(7) yes
C48 . C300 . H3001 . 107.7 no
C301 . C300 . H3001 . 107.2 no
C302 . C300 . H3001 . 107.7 no
C300 . C301 . H3013 . 109.7 no
C300 . C301 . H3011 . 108.5 no
H3013 . C301 . H3011 . 109.0 no
C300 . C301 . H3012 . 109.0 no
H3013 . C301 . H3012 . 110.5 no
H3011 . C301 . H3012 . 110.1 no
C300 . C302 . H3021 . 108.7 no
C300 . C302 . H3023 . 110.6 no
H3021 . C302 . H3023 . 109.6 no
C300 . C302 . H3022 . 108.9 no
H3021 . C302 . H3022 . 109.3 no
H3023 . C302 . H3022 . 109.7 no
C48 . C310 . C311 . 111.24(7) yes
C48 . C310 . C312 . 111.27(7) yes
C311 . C310 . C312 . 111.46(7) yes
C48 . C310 . H3101 . 108.0 no
C311 . C310 . H3101 . 107.4 no
C312 . C310 . H3101 . 107.2 no
C310 . C311 . H3111 . 109.8 no
C310 . C311 . H3113 . 108.5 no
H3111 . C311 . H3113 . 109.3 no
C310 . C311 . H3112 . 109.7 no
H3111 . C311 . H3112 . 110.2 no
H3113 . C311 . H3112 . 109.3 no
C310 . C312 . H3122 . 110.0 no
C310 . C312 . H3121 . 108.9 no
H3122 . C312 . H3121 . 109.1 no
C310 . C312 . H3123 . 110.1 no
H3122 . C312 . H3123 . 109.5 no
H3121 . C312 . H3123 . 109.1 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 23/10/13 at 09:52:39
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 313,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) H   ( 323,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   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 382,X'S) H   ( 383,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 393,X'S) H   ( 392,X'S) 
RIDE C   (  42,X'S) H   ( 422,X'S) H   ( 421,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 533,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 543,X'S) H   ( 542,X'S) 
RIDE C   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 682,X'S) 
RIDE C   (  70,X'S) H   ( 702,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 712,X'S) H   ( 711,X'S) 
RIDE C   (  73,X'S) H   ( 732,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 742,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 762,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 772,X'S) H   ( 771,X'S) 
RIDE C   (  79,X'S) H   ( 792,X'S) H   ( 791,X'S) 
RIDE C   (  80,X'S) H   ( 802,X'S) H   ( 801,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   ( 300,X'S) H   (3001,X'S) 
RIDE C   ( 301,X'S) H   (3013,X'S) H   (3011,X'S) H   (3012,X'S) 
RIDE C   ( 302,X'S) H   (3021,X'S) H   (3023,X'S) H   (3022,X'S) 
RIDE C   ( 310,X'S) H   (3101,X'S) 
RIDE C   ( 311,X'S) H   (3111,X'S) H   (3113,X'S) H   (3112,X'S) 
RIDE C   ( 312,X'S) H   (3122,X'S) H   (3121,X'S) H   (3123,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 23/10/13 at 09:52:39
#
#LIST     16                                                                    
SAME C(48) C(300) C(301) C(302) AND 
CONT C(48) C(300) C(302) C(301) AND 
CONT C(48) C(310) C(311) C(312) AND 
CONT C(48) C(310) C(312) C(311) 
SIMU 0.01 C(48) C(300) C(301) C(302) AND 
CONT C(48) C(300) C(302) C(301) AND 
CONT C(48) C(310) C(311) C(312) AND 
CONT C(48) C(310) C(312) C(311) 
DELU 0.01 C(48) C(300) C(301) C(302) AND 
CONT C(48) C(300) C(302) C(301) AND 
CONT C(48) C(310) C(311) C(312) AND 
CONT C(48) C(310) C(312) C(311) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_database_code_depnum_ccdc_archive 'CCDC 1006576'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_211NPRT14
_audit_creation_date             2014-05-04
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '211NPRT14 in P 21/n'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   10.32040(10)
_cell_length_b                   23.3192(2)
_cell_length_c                   23.4928(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.6503(8)
_cell_angle_gamma                90
_cell_volume                     5589.54(9)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn'
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'
Rh 0.0927 3.6045 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062
5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
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'


_cell_formula_units_Z            4

# Given Formula = C50 H50 B1 F15 N2 Rh1 
# Dc =      1.28 Fooo =   2496.00 Mu =     31.98 M =   1077.65
# Found Formula = C60 H65 B1 F15 N2 Rh1 
# Dc =      1.44 FOOO =   2496.00 Mu =     32.63 M =   1212.87

_chemical_formula_sum            'C60 H65 B1 F15 N2 Rh1'
_chemical_formula_moiety         'C60 H65 B1 F15 N2 Rh1'
_chemical_compound_source        .
_chemical_formula_weight         1212.87


_cell_measurement_reflns_used    28299
_cell_measurement_theta_min      4
_cell_measurement_theta_max      77
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.180
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_max          0.250

_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2496
_exptl_absorpt_coefficient_mu    3.263

# Sheldrick geometric approximatio 0.50 0.56 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.56
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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            57957
_reflns_number_total             11714
_diffrn_reflns_av_R_equivalents  0.031
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 11714 
# Theoretical number of reflections is about 23548 


_diffrn_reflns_theta_min         4.243
_diffrn_reflns_theta_max         76.688
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        75.155
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -13
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              29

_oxford_diffrn_Wilson_B_factor   1.70
_oxford_diffrn_Wilson_scale      0.20

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

_refine_diff_density_min         -0.62
_refine_diff_density_max         0.74


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         11673
_refine_ls_number_restraints     0
_refine_ls_number_parameters     713
_oxford_refine_ls_R_factor_ref   0.0312
_refine_ls_wR_factor_ref         0.0784
_refine_ls_goodness_of_fit_ref   1.0058
_refine_ls_shift/su_max          0.0009233
_refine_ls_shift/su_mean         0.0000303


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11673
_refine_ls_R_factor_all          0.0312
_refine_ls_wR_factor_all         0.0784

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                11045
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_gt          0.0773

# 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= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 4.40P] 
 ,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
Rh1 Rh 0.176230(12) 0.336639(5) 0.091566(5) 0.0204 1.0000 Uani . . . . . .
C2 C 0.19767(15) 0.34737(7) 0.17716(7) 0.0175 1.0000 Uani . . . . . .
N3 N 0.17611(13) 0.29554(6) 0.19798(6) 0.0184 1.0000 Uani . . . . . .
C4 C 0.13486(17) 0.25356(7) 0.15425(7) 0.0202 1.0000 Uani . . . . . .
C5 C 0.00902(17) 0.26095(8) 0.12158(7) 0.0242 1.0000 Uani . . . . . .
C6 C -0.09387(17) 0.30097(8) 0.14002(8) 0.0269 1.0000 Uani . . . . . .
C7 C -0.2003(2) 0.26498(11) 0.16180(11) 0.0425 1.0000 Uani . . . . . .
C8 C -0.1534(2) 0.34179(10) 0.09238(9) 0.0377 1.0000 Uani . . . . . .
C9 C -0.0282(2) 0.22253(9) 0.07599(8) 0.0314 1.0000 Uani . . . . . .
C10 C 0.0519(2) 0.17793(9) 0.06544(8) 0.0341 1.0000 Uani . . . . . .
C11 C 0.1725(2) 0.16982(8) 0.09979(8) 0.0315 1.0000 Uani . . . . . .
C12 C 0.21787(18) 0.20708(8) 0.14455(7) 0.0245 1.0000 Uani . . . . . .
C13 C 0.34922(19) 0.19850(8) 0.18257(8) 0.0291 1.0000 Uani . . . . . .
C14 C 0.4076(2) 0.13874(10) 0.17708(11) 0.0432 1.0000 Uani . . . . . .
C15 C 0.4497(2) 0.24381(9) 0.17196(10) 0.0379 1.0000 Uani . . . . . .
C16 C 0.21197(16) 0.29130(7) 0.26167(7) 0.0196 1.0000 Uani . . . . . .
C17 C 0.21432(18) 0.35534(7) 0.27636(7) 0.0235 1.0000 Uani . . . . . .
N18 N 0.23114(13) 0.38309(6) 0.22103(6) 0.0183 1.0000 Uani . . . . . .
C19 C 0.26354(16) 0.44271(7) 0.21820(7) 0.0196 1.0000 Uani . . . . . .
C20 C 0.39676(17) 0.45791(8) 0.22594(7) 0.0235 1.0000 Uani . . . . . .
C21 C 0.42707(19) 0.51613(8) 0.22602(8) 0.0298 1.0000 Uani . . . . . .
C22 C 0.3293(2) 0.55722(8) 0.21845(9) 0.0331 1.0000 Uani . . . . . .
C23 C 0.19899(19) 0.54116(8) 0.21061(8) 0.0295 1.0000 Uani . . . . . .
C24 C 0.16306(17) 0.48345(7) 0.21073(7) 0.0235 1.0000 Uani . . . . . .
C25 C 0.01864(18) 0.46754(8) 0.20524(8) 0.0288 1.0000 Uani . . . . . .
C26 C -0.0635(2) 0.49573(11) 0.15323(10) 0.0439 1.0000 Uani . . . . . .
C27 C -0.0340(2) 0.48271(11) 0.26081(10) 0.0421 1.0000 Uani . . . . . .
C28 C 0.50536(18) 0.41333(9) 0.23574(9) 0.0321 1.0000 Uani . . . . . .
C29 C 0.5677(3) 0.41196(13) 0.29910(11) 0.0529 1.0000 Uani . . . . . .
C30 C 0.6124(2) 0.42363(12) 0.19858(11) 0.0483 1.0000 Uani . . . . . .
C31 C 0.12102(16) 0.25265(7) 0.28962(6) 0.0184 1.0000 Uani . . . . . .
B32 B 0.15301(18) 0.24642(8) 0.36095(7) 0.0177 1.0000 Uani . . . . . .
C33 C 0.10216(17) 0.18191(7) 0.37874(7) 0.0207 1.0000 Uani . . . . . .
C34 C 0.17135(19) 0.14287(8) 0.41645(7) 0.0260 1.0000 Uani . . . . . .
F35 F 0.29307(12) 0.15502(5) 0.44370(5) 0.0330 1.0000 Uani . . . . . .
C36 C 0.1245(2) 0.08936(8) 0.42890(8) 0.0335 1.0000 Uani . . . . . .
F37 F 0.19832(16) 0.05415(6) 0.46577(6) 0.0508 1.0000 Uani . . . . . .
C38 C 0.0024(2) 0.07222(8) 0.40320(9) 0.0355 1.0000 Uani . . . . . .
F39 F -0.04440(16) 0.02036(5) 0.41461(7) 0.0530 1.0000 Uani . . . . . .
C40 C -0.07172(19) 0.10918(8) 0.36623(9) 0.0320 1.0000 Uani . . . . . .
C41 C -0.02197(18) 0.16255(7) 0.35533(8) 0.0248 1.0000 Uani . . . . . .
F42 F -0.10262(10) 0.19661(5) 0.31936(5) 0.0321 1.0000 Uani . . . . . .
F43 F -0.19138(12) 0.09285(6) 0.34021(7) 0.0471 1.0000 Uani . . . . . .
C44 C 0.31497(16) 0.25313(7) 0.37713(7) 0.0196 1.0000 Uani . . . . . .
C45 C 0.39534(17) 0.21336(7) 0.35539(7) 0.0225 1.0000 Uani . . . . . .
F46 F 0.34106(11) 0.16635(4) 0.32766(5) 0.0283 1.0000 Uani . . . . . .
C47 C 0.52942(18) 0.21803(8) 0.35803(8) 0.0284 1.0000 Uani . . . . . .
F48 F 0.59801(12) 0.17720(6) 0.33538(6) 0.0417 1.0000 Uani . . . . . .
C49 C 0.59250(17) 0.26506(9) 0.38457(8) 0.0308 1.0000 Uani . . . . . .
F50 F 0.72277(11) 0.27042(6) 0.38858(6) 0.0457 1.0000 Uani . . . . . .
C51 C 0.51983(18) 0.30608(8) 0.40736(7) 0.0272 1.0000 Uani . . . . . .
C52 C 0.38467(17) 0.29931(7) 0.40340(7) 0.0224 1.0000 Uani . . . . . .
F53 F 0.32290(11) 0.34296(5) 0.42598(5) 0.0302 1.0000 Uani . . . . . .
F54 F 0.57944(12) 0.35249(6) 0.43292(5) 0.0376 1.0000 Uani . . . . . .
C55 C 0.07383(16) 0.29191(7) 0.39783(7) 0.0196 1.0000 Uani . . . . . .
C56 C -0.01997(17) 0.33252(7) 0.37747(8) 0.0229 1.0000 Uani . . . . . .
F57 F -0.05877(11) 0.34057(5) 0.32038(5) 0.0320 1.0000 Uani . . . . . .
C58 C -0.08298(17) 0.36771(8) 0.41236(8) 0.0286 1.0000 Uani . . . . . .
F59 F -0.17065(12) 0.40669(6) 0.38893(6) 0.0437 1.0000 Uani . . . . . .
C60 C -0.0577(2) 0.36188(9) 0.47100(9) 0.0319 1.0000 Uani . . . . . .
F61 F -0.11932(14) 0.39473(6) 0.50553(6) 0.0484 1.0000 Uani . . . . . .
C62 C 0.0323(2) 0.32167(9) 0.49399(8) 0.0295 1.0000 Uani . . . . . .
C63 C 0.09493(17) 0.28877(7) 0.45773(7) 0.0235 1.0000 Uani . . . . . .
F64 F 0.18409(11) 0.25099(5) 0.48400(4) 0.0310 1.0000 Uani . . . . . .
F65 F 0.05936(15) 0.31490(6) 0.55138(5) 0.0450 1.0000 Uani . . . . . .
C66 C 0.1167(2) 0.32684(9) -0.00419(8) 0.0328 1.0000 Uani . . . . . .
C67 C 0.2303(2) 0.29751(9) 0.01323(8) 0.0362 1.0000 Uani . . . . . .
C68 C 0.3679(3) 0.31838(11) 0.00856(10) 0.0471 1.0000 Uani . . . . . .
C69 C 0.3947(2) 0.37991(12) 0.02894(10) 0.0457 1.0000 Uani . . . . . .
C70 C 0.31914(19) 0.39700(9) 0.07690(8) 0.0317 1.0000 Uani . . . . . .
C71 C 0.1954(2) 0.42251(8) 0.06728(8) 0.0288 1.0000 Uani . . . . . .
C72 C 0.1135(2) 0.43410(9) 0.00920(9) 0.0396 1.0000 Uani . . . . . .
C73 C 0.1118(2) 0.38490(9) -0.03325(8) 0.0369 1.0000 Uani . . . . . .
C74 C 0.1969(7) 0.9975(2) 1.1209(3) 0.1280 1.0000 Uani . . . . . .
C76 C 0.2728(5) 0.9835(2) 1.0812(3) 0.1116 1.0000 Uani . . . . . .
C78 C 0.1928(4) 0.98437(19) 1.0261(3) 0.1119 1.0000 Uani . . . . . .
C80 C 0.2675(4) 0.95900(19) 0.9814(3) 0.1281 1.0000 Uani . . . . . .
C82 C 0.1896(5) 0.9559(2) 0.9206(3) 0.1332 1.0000 Uani . . . . . .
C83 C 0.2453(8) 0.9279(3) 0.8654(4) 0.2276 1.0000 Uani . . . . . .
H61 H -0.0505 0.3237 0.1720 0.0315 1.0000 Uiso R . . . . .
H73 H -0.2596 0.2898 0.1782 0.0619 1.0000 Uiso R . . . . .
H72 H -0.1632 0.2388 0.1911 0.0614 1.0000 Uiso R . . . . .
H71 H -0.2483 0.2431 0.1316 0.0616 1.0000 Uiso R . . . . .
H81 H -0.2179 0.3665 0.1063 0.0561 1.0000 Uiso R . . . . .
H82 H -0.0850 0.3661 0.0802 0.0561 1.0000 Uiso R . . . . .
H83 H -0.1947 0.3201 0.0599 0.0560 1.0000 Uiso R . . . . .
H91 H -0.1111 0.2277 0.0528 0.0377 1.0000 Uiso R . . . . .
H101 H 0.0250 0.1520 0.0345 0.0400 1.0000 Uiso R . . . . .
H111 H 0.2270 0.1389 0.0925 0.0372 1.0000 Uiso R . . . . .
H131 H 0.3365 0.2023 0.2227 0.0332 1.0000 Uiso R . . . . .
H141 H 0.4835 0.1347 0.2062 0.0641 1.0000 Uiso R . . . . .
H142 H 0.4302 0.1332 0.1387 0.0637 1.0000 Uiso R . . . . .
H143 H 0.3433 0.1093 0.1830 0.0636 1.0000 Uiso R . . . . .
H151 H 0.5277 0.2402 0.1994 0.0558 1.0000 Uiso R . . . . .
H152 H 0.4133 0.2820 0.1746 0.0556 1.0000 Uiso R . . . . .
H153 H 0.4701 0.2402 0.1331 0.0554 1.0000 Uiso R . . . . .
H161 H 0.3030 0.2767 0.2700 0.0230 1.0000 Uiso R . . . . .
H171 H 0.2883 0.3658 0.3064 0.0281 1.0000 Uiso R . . . . .
H172 H 0.1320 0.3672 0.2873 0.0279 1.0000 Uiso R . . . . .
H211 H 0.5143 0.5276 0.2312 0.0353 1.0000 Uiso R . . . . .
H221 H 0.3510 0.5962 0.2184 0.0388 1.0000 Uiso R . . . . .
H231 H 0.1349 0.5690 0.2060 0.0351 1.0000 Uiso R . . . . .
H251 H 0.0106 0.4260 0.2005 0.0336 1.0000 Uiso R . . . . .
H261 H -0.1560 0.4817 0.1499 0.0655 1.0000 Uiso R . . . . .
H262 H -0.0618 0.5373 0.1584 0.0661 1.0000 Uiso R . . . . .
H263 H -0.0265 0.4861 0.1184 0.0658 1.0000 Uiso R . . . . .
H271 H -0.1227 0.4692 0.2589 0.0629 1.0000 Uiso R . . . . .
H272 H -0.0332 0.5239 0.2644 0.0625 1.0000 Uiso R . . . . .
H273 H 0.0217 0.4664 0.2945 0.0626 1.0000 Uiso R . . . . .
H281 H 0.4651 0.3760 0.2253 0.0380 1.0000 Uiso R . . . . .
H291 H 0.6315 0.3814 0.3059 0.0773 1.0000 Uiso R . . . . .
H292 H 0.6117 0.4480 0.3093 0.0778 1.0000 Uiso R . . . . .
H293 H 0.5009 0.4068 0.3233 0.0777 1.0000 Uiso R . . . . .
H303 H 0.6797 0.3943 0.2061 0.0714 1.0000 Uiso R . . . . .
H302 H 0.6544 0.4606 0.2072 0.0716 1.0000 Uiso R . . . . .
H301 H 0.5756 0.4226 0.1580 0.0719 1.0000 Uiso R . . . . .
H311 H 0.0328 0.2653 0.2780 0.0205 1.0000 Uiso R . . . . .
H312 H 0.1274 0.2150 0.2736 0.0214 1.0000 Uiso R . . . . .
H661 H 0.0342 0.3058 -0.0086 0.0386 1.0000 Uiso R . . . . .
H671 H 0.2237 0.2554 0.0188 0.0430 1.0000 Uiso R . . . . .
H681 H 0.3844 0.3146 -0.0312 0.0557 1.0000 Uiso R . . . . .
H682 H 0.4284 0.2942 0.0342 0.0571 1.0000 Uiso R . . . . .
H691 H 0.4877 0.3834 0.0432 0.0552 1.0000 Uiso R . . . . .
H692 H 0.3700 0.4069 -0.0043 0.0554 1.0000 Uiso R . . . . .
H701 H 0.3732 0.4065 0.1141 0.0368 1.0000 Uiso R . . . . .
H711 H 0.1736 0.4457 0.0987 0.0341 1.0000 Uiso R . . . . .
H721 H 0.1497 0.4676 -0.0060 0.0482 1.0000 Uiso R . . . . .
H722 H 0.0208 0.4410 0.0158 0.0486 1.0000 Uiso R . . . . .
H731 H 0.1901 0.3891 -0.0533 0.0449 1.0000 Uiso R . . . . .
H732 H 0.0330 0.3875 -0.0612 0.0445 1.0000 Uiso R . . . . .
H761 H 0.3460 1.0123 1.0833 0.1438 1.0000 Uiso R . . . . .
H762 H 0.3142 0.9450 1.0916 0.1445 1.0000 Uiso R . . . . .
H781 H 0.1653 1.0243 1.0180 0.1369 1.0000 Uiso R . . . . .
H782 H 0.1122 0.9615 1.0289 0.1369 1.0000 Uiso R . . . . .
H801 H 0.3469 0.9821 0.9817 0.1499 1.0000 Uiso R . . . . .
H802 H 0.2901 0.9195 0.9942 0.1502 1.0000 Uiso R . . . . .
H821 H 0.1647 0.9964 0.9101 0.1635 1.0000 Uiso R . . . . .
H822 H 0.1104 0.9329 0.9242 0.1636 1.0000 Uiso R . . . . .
H831 H 0.1803 0.9305 0.8322 0.2612 1.0000 Uiso R . . . . .
H832 H 0.3211 0.9485 0.8589 0.2612 1.0000 Uiso R . . . . .
H833 H 0.2674 0.8888 0.8728 0.2612 1.0000 Uiso R . . . . .
H741 H 0.2479 0.9973 1.1581 0.1491 1.0000 Uiso R . . . . .
H742 H 0.1609 1.0346 1.1128 0.1491 1.0000 Uiso R . . . . .
H743 H 0.1279 0.9703 1.1197 0.1491 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       50(6)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          2.246(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
Rh1 . C2 . 2.0053(16) yes
Rh1 . N3 . 2.6777(13) yes
Rh1 . C4 . 2.5085(16) yes
Rh1 . C5 . 2.6374(18) yes
Rh1 . C66 . 2.2528(18) yes
Rh1 . C67 . 2.2000(18) yes
Rh1 . C70 . 2.1043(18) yes
Rh1 . C71 . 2.0996(17) yes
C2 . N3 . 1.335(2) yes
C2 . N18 . 1.330(2) yes
N3 . C4 . 1.436(2) yes
N3 . C16 . 1.4895(19) yes
C4 . C5 . 1.416(2) yes
C4 . C12 . 1.421(2) yes
C5 . C6 . 1.525(2) yes
C5 . C9 . 1.405(2) yes
C6 . C7 . 1.531(3) yes
C6 . C8 . 1.526(3) yes
C6 . H61 . 0.972 no
C7 . H73 . 0.963 no
C7 . H72 . 0.955 no
C7 . H71 . 0.950 no
C8 . H81 . 0.973 no
C8 . H82 . 0.981 no
C8 . H83 . 0.961 no
C9 . C10 . 1.375(3) yes
C9 . H91 . 0.950 no
C10 . C11 . 1.390(3) yes
C10 . H101 . 0.954 no
C11 . C12 . 1.390(3) yes
C11 . H111 . 0.946 no
C12 . C13 . 1.520(3) yes
C13 . C14 . 1.531(3) yes
C13 . C15 . 1.527(3) yes
C13 . H131 . 0.975 no
C14 . H141 . 0.965 no
C14 . H142 . 0.973 no
C14 . H143 . 0.979 no
C15 . H151 . 0.957 no
C15 . H152 . 0.971 no
C15 . H153 . 0.971 no
C16 . C17 . 1.532(2) yes
C16 . C31 . 1.520(2) yes
C16 . H161 . 0.991 no
C17 . N18 . 1.485(2) yes
C17 . H171 . 0.990 no
C17 . H172 . 0.964 no
N18 . C19 . 1.434(2) yes
C19 . C20 . 1.405(2) yes
C19 . C24 . 1.398(2) yes
C20 . C21 . 1.393(2) yes
C20 . C28 . 1.521(3) yes
C21 . C22 . 1.383(3) yes
C21 . H211 . 0.930 no
C22 . C23 . 1.381(3) yes
C22 . H221 . 0.936 no
C23 . C24 . 1.396(2) yes
C23 . H231 . 0.922 no
C24 . C25 . 1.523(2) yes
C25 . C26 . 1.527(3) yes
C25 . C27 . 1.529(3) yes
C25 . H251 . 0.978 no
C26 . H261 . 1.000 no
C26 . H262 . 0.977 no
C26 . H263 . 0.979 no
C27 . H271 . 0.963 no
C27 . H272 . 0.965 no
C27 . H273 . 0.982 no
C28 . C29 . 1.530(3) yes
C28 . C30 . 1.527(3) yes
C28 . H281 . 0.980 no
C29 . H291 . 0.967 no
C29 . H292 . 0.968 no
C29 . H293 . 0.965 no
C30 . H303 . 0.972 no
C30 . H302 . 0.972 no
C30 . H301 . 0.972 no
C31 . B32 . 1.665(2) yes
C31 . H311 . 0.957 no
C31 . H312 . 0.960 no
B32 . C33 . 1.667(2) yes
B32 . C44 . 1.665(2) yes
B32 . C55 . 1.660(2) yes
C33 . C34 . 1.390(2) yes
C33 . C41 . 1.391(3) yes
C34 . F35 . 1.351(2) yes
C34 . C36 . 1.385(3) yes
C36 . F37 . 1.344(2) yes
C36 . C38 . 1.372(3) yes
C38 . F39 . 1.344(2) yes
C38 . C40 . 1.372(3) yes
C40 . C41 . 1.385(2) yes
C40 . F43 . 1.348(2) yes
C41 . F42 . 1.351(2) yes
C44 . C45 . 1.392(2) yes
C44 . C52 . 1.387(2) yes
C45 . F46 . 1.353(2) yes
C45 . C47 . 1.380(2) yes
C47 . F48 . 1.343(2) yes
C47 . C49 . 1.376(3) yes
C49 . F50 . 1.339(2) yes
C49 . C51 . 1.373(3) yes
C51 . C52 . 1.393(2) yes
C51 . F54 . 1.341(2) yes
C52 . F53 . 1.351(2) yes
C55 . C56 . 1.387(2) yes
C55 . C63 . 1.393(2) yes
C56 . F57 . 1.354(2) yes
C56 . C58 . 1.389(3) yes
C58 . F59 . 1.341(2) yes
C58 . C60 . 1.370(3) yes
C60 . F61 . 1.343(2) yes
C60 . C62 . 1.372(3) yes
C62 . C63 . 1.378(2) yes
C62 . F65 . 1.344(2) yes
C63 . F64 . 1.354(2) yes
C66 . C67 . 1.366(3) yes
C66 . C73 . 1.514(3) yes
C66 . H661 . 0.975 no
C67 . C68 . 1.521(3) yes
C67 . H671 . 0.995 no
C68 . C69 . 1.525(4) yes
C68 . H681 . 0.978 no
C68 . H682 . 0.978 no
C69 . C70 . 1.517(3) yes
C69 . H691 . 0.971 no
C69 . H692 . 1.004 no
C70 . C71 . 1.396(3) yes
C70 . H701 . 0.989 no
C71 . C72 . 1.518(3) yes
C71 . H711 . 0.969 no
C72 . C73 . 1.519(3) yes
C72 . H721 . 0.959 no
C72 . H722 . 1.005 no
C73 . H731 . 0.999 no
C73 . H732 . 0.967 no
C74 . C76 . 1.345(7) yes
C74 . H741 . 0.950 no
C74 . H742 . 0.950 no
C74 . H743 . 0.950 no
C76 . C78 . 1.425(7) yes
C76 . H761 . 1.006 no
C76 . H762 . 1.009 no
C78 . C80 . 1.514(8) yes
C78 . H781 . 0.983 no
C78 . H782 . 0.998 no
C80 . C82 . 1.533(8) yes
C80 . H801 . 0.980 no
C80 . H802 . 0.987 no
C82 . C83 . 1.631(9) yes
C82 . H821 . 1.000 no
C82 . H822 . 0.992 no
C83 . H831 . 0.950 no
C83 . H832 . 0.950 no
C83 . H833 . 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
C2 . Rh1 . N3 . 28.82(5) yes
C2 . Rh1 . C4 . 60.69(6) yes
N3 . Rh1 . C4 . 31.95(5) yes
C2 . Rh1 . C5 . 78.08(6) yes
N3 . Rh1 . C5 . 54.46(5) yes
C4 . Rh1 . C5 . 31.82(5) yes
C2 . Rh1 . C66 . 170.54(7) yes
N3 . Rh1 . C66 . 149.06(6) yes
C4 . Rh1 . C66 . 117.57(6) yes
C5 . Rh1 . C66 . 96.19(6) yes
C2 . Rh1 . C67 . 152.49(7) yes
N3 . Rh1 . C67 . 131.94(6) yes
C4 . Rh1 . C67 . 104.93(6) yes
C5 . Rh1 . C67 . 101.80(7) yes
C66 . Rh1 . C67 . 35.71(8) yes
C2 . Rh1 . C70 . 96.11(7) yes
N3 . Rh1 . C70 . 119.41(6) yes
C4 . Rh1 . C70 . 142.94(7) yes
C5 . Rh1 . C70 . 173.87(6) yes
C66 . Rh1 . C70 . 89.83(7) yes
C2 . Rh1 . C71 . 98.79(7) yes
N3 . Rh1 . C71 . 127.47(6) yes
C4 . Rh1 . C71 . 158.03(6) yes
C5 . Rh1 . C71 . 143.43(7) yes
C66 . Rh1 . C71 . 81.27(7) yes
C67 . Rh1 . C70 . 82.43(8) yes
C67 . Rh1 . C71 . 97.02(7) yes
C70 . Rh1 . C71 . 38.78(8) yes
Rh1 . C2 . N3 . 104.78(11) yes
Rh1 . C2 . N18 . 146.29(12) yes
N3 . C2 . N18 . 108.75(13) yes
C2 . N3 . Rh1 . 46.40(8) yes
C2 . N3 . C4 . 113.74(13) yes
Rh1 . N3 . C4 . 67.53(8) yes
C2 . N3 . C16 . 113.46(13) yes
Rh1 . N3 . C16 . 157.91(10) yes
C4 . N3 . C16 . 132.49(13) yes
N3 . C4 . Rh1 . 80.53(9) yes
N3 . C4 . C5 . 116.98(15) yes
Rh1 . C4 . C5 . 79.11(10) yes
N3 . C4 . C12 . 120.90(15) yes
Rh1 . C4 . C12 . 109.57(11) yes
C5 . C4 . C12 . 122.12(15) yes
C4 . C5 . Rh1 . 69.07(9) yes
C4 . C5 . C6 . 122.79(15) yes
Rh1 . C5 . C6 . 100.26(11) yes
C4 . C5 . C9 . 117.33(17) yes
Rh1 . C5 . C9 . 109.76(12) yes
C6 . C5 . C9 . 118.98(16) yes
C5 . C6 . C7 . 108.97(16) yes
C5 . C6 . C8 . 113.19(15) yes
C7 . C6 . C8 . 110.93(17) yes
C5 . C6 . H61 . 107.1 no
C7 . C6 . H61 . 108.1 no
C8 . C6 . H61 . 108.3 no
C6 . C7 . H73 . 109.6 no
C6 . C7 . H72 . 111.1 no
H73 . C7 . H72 . 107.8 no
C6 . C7 . H71 . 111.4 no
H73 . C7 . H71 . 109.2 no
H72 . C7 . H71 . 107.6 no
C6 . C8 . H81 . 110.0 no
C6 . C8 . H82 . 110.3 no
H81 . C8 . H82 . 108.4 no
C6 . C8 . H83 . 109.6 no
H81 . C8 . H83 . 109.5 no
H82 . C8 . H83 . 109.0 no
C5 . C9 . C10 . 121.12(18) yes
C5 . C9 . H91 . 118.3 no
C10 . C9 . H91 . 120.5 no
C9 . C10 . C11 . 120.57(17) yes
C9 . C10 . H101 . 120.2 no
C11 . C10 . H101 . 119.3 no
C10 . C11 . C12 . 121.64(18) yes
C10 . C11 . H111 . 120.3 no
C12 . C11 . H111 . 118.1 no
C4 . C12 . C11 . 117.08(17) yes
C4 . C12 . C13 . 120.79(16) yes
C11 . C12 . C13 . 122.11(17) yes
C12 . C13 . C14 . 113.43(17) yes
C12 . C13 . C15 . 112.35(16) yes
C14 . C13 . C15 . 109.31(17) yes
C12 . C13 . H131 . 108.5 no
C14 . C13 . H131 . 106.1 no
C15 . C13 . H131 . 106.7 no
C13 . C14 . H141 . 108.5 no
C13 . C14 . H142 . 110.5 no
H141 . C14 . H142 . 111.3 no
C13 . C14 . H143 . 110.0 no
H141 . C14 . H143 . 109.0 no
H142 . C14 . H143 . 107.6 no
C13 . C15 . H151 . 110.6 no
C13 . C15 . H152 . 110.2 no
H151 . C15 . H152 . 109.4 no
C13 . C15 . H153 . 110.0 no
H151 . C15 . H153 . 110.3 no
H152 . C15 . H153 . 106.3 no
N3 . C16 . C17 . 98.90(12) yes
N3 . C16 . C31 . 113.39(13) yes
C17 . C16 . C31 . 118.08(14) yes
N3 . C16 . H161 . 107.8 no
C17 . C16 . H161 . 108.0 no
C31 . C16 . H161 . 109.9 no
C16 . C17 . N18 . 103.15(12) yes
C16 . C17 . H171 . 112.7 no
N18 . C17 . H171 . 109.7 no
C16 . C17 . H172 . 110.8 no
N18 . C17 . H172 . 109.5 no
H171 . C17 . H172 . 110.8 no
C17 . N18 . C2 . 110.75(13) yes
C17 . N18 . C19 . 121.44(13) yes
C2 . N18 . C19 . 127.36(13) yes
N18 . C19 . C20 . 117.97(15) yes
N18 . C19 . C24 . 119.41(15) yes
C20 . C19 . C24 . 122.54(15) yes
C19 . C20 . C21 . 117.46(16) yes
C19 . C20 . C28 . 122.13(16) yes
C21 . C20 . C28 . 120.39(16) yes
C20 . C21 . C22 . 121.03(17) yes
C20 . C21 . H211 . 119.6 no
C22 . C21 . H211 . 119.4 no
C21 . C22 . C23 . 120.40(17) yes
C21 . C22 . H221 . 120.1 no
C23 . C22 . H221 . 119.5 no
C22 . C23 . C24 . 120.96(18) yes
C22 . C23 . H231 . 119.4 no
C24 . C23 . H231 . 119.6 no
C19 . C24 . C23 . 117.59(16) yes
C19 . C24 . C25 . 122.91(15) yes
C23 . C24 . C25 . 119.45(16) yes
C24 . C25 . C26 . 112.43(16) yes
C24 . C25 . C27 . 109.89(16) yes
C26 . C25 . C27 . 110.96(17) yes
C24 . C25 . H251 . 108.4 no
C26 . C25 . H251 . 107.9 no
C27 . C25 . H251 . 107.0 no
C25 . C26 . H261 . 109.3 no
C25 . C26 . H262 . 109.3 no
H261 . C26 . H262 . 109.4 no
C25 . C26 . H263 . 109.2 no
H261 . C26 . H263 . 110.3 no
H262 . C26 . H263 . 109.2 no
C25 . C27 . H271 . 110.0 no
C25 . C27 . H272 . 107.8 no
H271 . C27 . H272 . 109.0 no
C25 . C27 . H273 . 111.0 no
H271 . C27 . H273 . 110.3 no
H272 . C27 . H273 . 108.6 no
C20 . C28 . C29 . 110.73(18) yes
C20 . C28 . C30 . 112.72(17) yes
C29 . C28 . C30 . 108.96(18) yes
C20 . C28 . H281 . 107.1 no
C29 . C28 . H281 . 109.0 no
C30 . C28 . H281 . 108.2 no
C28 . C29 . H291 . 110.6 no
C28 . C29 . H292 . 109.7 no
H291 . C29 . H292 . 108.4 no
C28 . C29 . H293 . 110.1 no
H291 . C29 . H293 . 109.9 no
H292 . C29 . H293 . 108.2 no
C28 . C30 . H303 . 110.1 no
C28 . C30 . H302 . 111.1 no
H303 . C30 . H302 . 107.5 no
C28 . C30 . H301 . 110.3 no
H303 . C30 . H301 . 108.9 no
H302 . C30 . H301 . 108.8 no
C16 . C31 . B32 . 116.40(13) yes
C16 . C31 . H311 . 108.4 no
B32 . C31 . H311 . 110.5 no
C16 . C31 . H312 . 106.8 no
B32 . C31 . H312 . 107.4 no
H311 . C31 . H312 . 106.8 no
C31 . B32 . C33 . 107.99(12) yes
C31 . B32 . C44 . 105.19(12) yes
C33 . B32 . C44 . 111.77(13) yes
C31 . B32 . C55 . 115.52(13) yes
C33 . B32 . C55 . 104.33(12) yes
C44 . B32 . C55 . 112.13(13) yes
B32 . C33 . C34 . 126.85(15) yes
B32 . C33 . C41 . 119.98(15) yes
C34 . C33 . C41 . 113.17(16) yes
C33 . C34 . F35 . 121.08(16) yes
C33 . C34 . C36 . 124.20(18) yes
F35 . C34 . C36 . 114.72(17) yes
C34 . C36 . F37 . 120.3(2) yes
C34 . C36 . C38 . 119.74(19) yes
F37 . C36 . C38 . 119.99(18) yes
C36 . C38 . F39 . 120.5(2) yes
C36 . C38 . C40 . 118.88(17) yes
F39 . C38 . C40 . 120.6(2) yes
C38 . C40 . C41 . 119.66(19) yes
C38 . C40 . F43 . 119.67(17) yes
C41 . C40 . F43 . 120.66(19) yes
C33 . C41 . C40 . 124.30(18) yes
C33 . C41 . F42 . 120.02(15) yes
C40 . C41 . F42 . 115.67(17) yes
B32 . C44 . C45 . 119.13(14) yes
B32 . C44 . C52 . 127.61(15) yes
C45 . C44 . C52 . 112.51(15) yes
C44 . C45 . F46 . 119.36(15) yes
C44 . C45 . C47 . 125.44(17) yes
F46 . C45 . C47 . 115.17(16) yes
C45 . C47 . F48 . 120.72(18) yes
C45 . C47 . C49 . 119.09(17) yes
F48 . C47 . C49 . 120.19(17) yes
C47 . C49 . F50 . 120.52(19) yes
C47 . C49 . C51 . 118.89(16) yes
F50 . C49 . C51 . 120.59(18) yes
C49 . C51 . C52 . 119.68(17) yes
C49 . C51 . F54 . 119.74(16) yes
C52 . C51 . F54 . 120.58(17) yes
C51 . C52 . C44 . 124.39(17) yes
C51 . C52 . F53 . 114.53(15) yes
C44 . C52 . F53 . 121.05(15) yes
B32 . C55 . C56 . 128.98(15) yes
B32 . C55 . C63 . 118.62(14) yes
C56 . C55 . C63 . 112.29(15) yes
C55 . C56 . F57 . 121.57(15) yes
C55 . C56 . C58 . 124.37(17) yes
F57 . C56 . C58 . 114.06(15) yes
C56 . C58 . F59 . 120.36(17) yes
C56 . C58 . C60 . 119.96(17) yes
F59 . C58 . C60 . 119.66(17) yes
C58 . C60 . F61 . 120.97(19) yes
C58 . C60 . C62 . 118.63(17) yes
F61 . C60 . C62 . 120.40(18) yes
C60 . C62 . C63 . 119.34(17) yes
C60 . C62 . F65 . 120.10(17) yes
C63 . C62 . F65 . 120.56(18) yes
C55 . C63 . C62 . 125.35(17) yes
C55 . C63 . F64 . 119.14(15) yes
C62 . C63 . F64 . 115.51(15) yes
Rh1 . C66 . C67 . 70.04(11) yes
Rh1 . C66 . C73 . 110.19(12) yes
C67 . C66 . C73 . 123.5(2) yes
Rh1 . C66 . H661 . 105.0 no
C67 . C66 . H661 . 118.5 no
C73 . C66 . H661 . 115.7 no
Rh1 . C67 . C66 . 74.25(11) yes
Rh1 . C67 . C68 . 106.54(14) yes
C66 . C67 . C68 . 125.94(19) yes
Rh1 . C67 . H671 . 105.6 no
C66 . C67 . H671 . 117.4 no
C68 . C67 . H671 . 114.2 no
C67 . C68 . C69 . 113.95(18) yes
C67 . C68 . H681 . 109.8 no
C69 . C68 . H681 . 109.6 no
C67 . C68 . H682 . 106.7 no
C69 . C68 . H682 . 106.3 no
H681 . C68 . H682 . 110.4 no
C68 . C69 . C70 . 113.03(18) yes
C68 . C69 . H691 . 108.0 no
C70 . C69 . H691 . 108.3 no
C68 . C69 . H692 . 109.4 no
C70 . C69 . H692 . 108.3 no
H691 . C69 . H692 . 109.8 no
C69 . C70 . Rh1 . 113.41(15) yes
C69 . C70 . C71 . 123.49(18) yes
Rh1 . C70 . C71 . 70.42(10) yes
C69 . C70 . H701 . 115.5 no
Rh1 . C70 . H701 . 108.8 no
C71 . C70 . H701 . 115.4 no
C70 . C71 . Rh1 . 70.79(11) yes
C70 . C71 . C72 . 126.44(18) yes
Rh1 . C71 . C72 . 110.58(13) yes
C70 . C71 . H711 . 115.3 no
Rh1 . C71 . H711 . 106.5 no
C72 . C71 . H711 . 115.0 no
C71 . C72 . C73 . 113.93(17) yes
C71 . C72 . H721 . 106.5 no
C73 . C72 . H721 . 109.7 no
C71 . C72 . H722 . 107.7 no
C73 . C72 . H722 . 107.8 no
H721 . C72 . H722 . 111.2 no
C72 . C73 . C66 . 112.54(16) yes
C72 . C73 . H731 . 107.8 no
C66 . C73 . H731 . 109.0 no
C72 . C73 . H732 . 109.0 no
C66 . C73 . H732 . 109.2 no
H731 . C73 . H732 . 109.3 no
C76 . C74 . H741 . 109.7 no
C76 . C74 . H742 . 109.5 no
H741 . C74 . H742 . 109.5 no
C76 . C74 . H743 . 109.2 no
H741 . C74 . H743 . 109.5 no
H742 . C74 . H743 . 109.5 no
C74 . C76 . C78 . 107.9(5) yes
C74 . C76 . H761 . 108.4 no
C78 . C76 . H761 . 111.3 no
C74 . C76 . H762 . 108.4 no
C78 . C76 . H762 . 113.5 no
H761 . C76 . H762 . 107.1 no
C76 . C78 . C80 . 109.7(4) yes
C76 . C78 . H781 . 107.5 no
C80 . C78 . H781 . 113.4 no
C76 . C78 . H782 . 108.0 no
C80 . C78 . H782 . 110.6 no
H781 . C78 . H782 . 107.5 no
C78 . C80 . C82 . 114.5(4) yes
C78 . C80 . H801 . 107.1 no
C82 . C80 . H801 . 110.7 no
C78 . C80 . H802 . 106.0 no
C82 . C80 . H802 . 107.8 no
H801 . C80 . H802 . 110.7 no
C80 . C82 . C83 . 124.2(5) yes
C80 . C82 . H821 . 105.4 no
C83 . C82 . H821 . 106.9 no
C80 . C82 . H822 . 105.5 no
C83 . C82 . H822 . 104.2 no
H821 . C82 . H822 . 110.3 no
C82 . C83 . H831 . 109.6 no
C82 . C83 . H832 . 108.8 no
H831 . C83 . H832 . 109.5 no
C82 . C83 . H833 . 110.0 no
H831 . C83 . H833 . 109.5 no
H832 . C83 . H833 . 109.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C16 . H161 . C45 . 125.66 0.991 2.558 3.237(3) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 04/05/14 at 11:00:57
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  73,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 303,X'S) H   ( 302,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 682,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) H   ( 692,X'S) 
RIDE C   (  70,X'S) H   ( 701,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) H   ( 743,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) H   ( 802,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) H   ( 833,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 04/05/14 at 11:00:57
#
#LIST     16                                                                    
REM 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_database_code_depnum_ccdc_archive 'CCDC 1006577'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_204NPRT14
_audit_creation_date             2014-04-23
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '204NPRT14 in P -1'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   10.8473(3)
_cell_length_b                   16.4395(4)
_cell_length_c                   19.8987(4)
_cell_angle_alpha                69.270(2)
_cell_angle_beta                 87.964(2)
_cell_angle_gamma                88.679(2)
_cell_volume                     3316.39(15)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 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'
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'
Au -4.4197 7.2980 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956
12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
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'
Li 0.0008 0.0003 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610
0.0377 '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'


_cell_formula_units_Z            2

# Given Formula = C90 H100 Au1 B1 Cl1 F15 Li1 N1 O4 
# Dc =      1.80 Fooo =   1472.00 Mu =     54.40 M =   1794.93
# Found Formula = C63 H73 Au1 B1 Cl1 F15 Li1 N2 O4 
# Dc =      1.46 FOOO =   1472.00 Mu =     53.03 M =   1457.42

_chemical_formula_sum            'C63 H73 Au1 B1 Cl1 F15 Li1 N2 O4'
_chemical_formula_moiety         'C63 H73 Au1 B1 Cl1 F15 Li1 N2 O4'
_chemical_compound_source        .
_chemical_formula_weight         1457.42


_cell_measurement_reflns_used    18372
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.010
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_max          0.090

_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    5.303

# Sheldrick geometric approximatio 0.77 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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            89243
_reflns_number_total             13788
_diffrn_reflns_av_R_equivalents  0.139
# Number of reflections without Friedels Law is 13863 
# Number of reflections with Friedels Law is 13788 
# Theoretical number of reflections is about 14115 


_diffrn_reflns_theta_min         3.013
_diffrn_reflns_theta_max         77.543
_diffrn_measured_fraction_theta_max 0.977

_diffrn_reflns_theta_full        67.462
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              -19
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   4.50
_oxford_diffrn_Wilson_scale      0.15

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

_refine_diff_density_min         -2.64
_refine_diff_density_max         3.25


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         13735
_refine_ls_number_restraints     416
_refine_ls_number_parameters     903
_oxford_refine_ls_R_factor_ref   0.1159
_refine_ls_wR_factor_ref         0.2188
_refine_ls_goodness_of_fit_ref   1.0183
_refine_ls_shift/su_max          0.0017059
_refine_ls_shift/su_mean         0.0000981


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        13735
_refine_ls_R_factor_all          0.1159
_refine_ls_wR_factor_all         0.2188

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9287
_refine_ls_R_factor_gt           0.0839
_refine_ls_wR_factor_gt          0.2025

# 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 #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 +28.17P] 
 ,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
Au1 Au 0.66113(4) 1.18802(3) 0.20611(3) 0.0617 1.0000 Uani . . . . . .
Cl2 Cl 0.6303(4) 1.3315(2) 0.1410(2) 0.1029 1.0000 Uani . . . . . .
C3 C 0.6844(6) 1.0636(6) 0.2690(4) 0.0424 1.0000 Uani . . . . . .
C5 C 0.7493(7) 1.0208(6) 0.1699(4) 0.0451 1.0000 Uani . . . . . .
C6 C 0.8694(8) 1.0443(6) 0.1406(5) 0.0556 1.0000 Uani . . . . . .
C7 C 0.9680(8) 1.0730(7) 0.1803(6) 0.0627 1.0000 Uani . . . . . .
C8 C 0.9845(11) 1.1728(7) 0.1499(7) 0.0851 1.0000 Uani . . . . . .
C9 C 1.0919(8) 1.0274(8) 0.1804(7) 0.0747 1.0000 Uani . . . . . .
C10 C 0.8935(10) 1.0478(7) 0.0710(6) 0.0677 1.0000 Uani . . . . . .
C11 C 0.8067(11) 1.0278(8) 0.0317(6) 0.0726 1.0000 Uani . . . . . .
C12 C 0.6881(10) 1.0066(7) 0.0602(5) 0.0657 1.0000 Uani . . . . . .
C13 C 0.6574(8) 1.0036(7) 0.1290(5) 0.0565 1.0000 Uani . . . . . .
C14 C 0.5247(8) 0.9883(7) 0.1564(5) 0.0599 1.0000 Uani . . . . . .
C15 C 0.4482(9) 1.0696(8) 0.1184(7) 0.0820 1.0000 Uani . . . . . .
C16 C 0.4687(10) 0.9082(8) 0.1484(7) 0.0786 1.0000 Uani . . . . . .
C17 C 0.7330(6) 0.9067(5) 0.2915(4) 0.0426 1.0000 Uani . . . . . .
C18 C 0.8664(6) 0.8802(6) 0.3094(5) 0.0450 1.0000 Uani . . . . . .
C20 C 1.0620(7) 0.7697(6) 0.3291(5) 0.0531 1.0000 Uani . . . . . .
C21 C 1.1366(8) 0.8184(7) 0.3547(6) 0.0624 1.0000 Uani . . . . . .
C23 C 1.2634(8) 0.8124(8) 0.3552(6) 0.0688 1.0000 Uani . . . . . .
C25 C 1.3235(7) 0.7548(7) 0.3290(6) 0.0656 1.0000 Uani . . . . . .
C27 C 1.2543(8) 0.7036(7) 0.3055(6) 0.0655 1.0000 Uani . . . . . .
C28 C 1.1291(8) 0.7107(7) 0.3060(6) 0.0601 1.0000 Uani . . . . . .
C31 C 0.8505(8) 0.7558(6) 0.2611(6) 0.0597 1.0000 Uani . . . . . .
C32 C 0.9004(10) 0.7906(7) 0.1914(6) 0.0695 1.0000 Uani . . . . . .
C34 C 0.8435(13) 0.7874(9) 0.1290(9) 0.0893 1.0000 Uani . . . . . .
C36 C 0.7328(15) 0.7495(11) 0.1380(10) 0.1008 1.0000 Uani . . . . . .
C38 C 0.6790(11) 0.7121(10) 0.2041(10) 0.0948 1.0000 Uani . . . . . .
C39 C 0.7381(9) 0.7181(7) 0.2632(7) 0.0723 1.0000 Uani . . . . . .
C42 C 0.8720(8) 0.7058(7) 0.4091(6) 0.0657 1.0000 Uani . . . . . .
C43 C 0.8580(9) 0.7282(8) 0.4713(7) 0.0766 1.0000 Uani . . . . . .
C45 C 0.8411(10) 0.6660(11) 0.5399(7) 0.0906 1.0000 Uani . . . . . .
C47 C 0.8385(13) 0.5805(11) 0.5491(9) 0.1054 1.0000 Uani . . . . . .
C49 C 0.8515(13) 0.5550(9) 0.4923(11) 0.1095 1.0000 Uani . . . . . .
C50 C 0.8706(10) 0.6177(8) 0.4254(7) 0.0816 1.0000 Uani . . . . . .
C53 C 0.6441(7) 0.8895(6) 0.3550(5) 0.0487 1.0000 Uani . . . . . .
C54 C 0.6634(8) 0.9539(6) 0.3923(5) 0.0531 1.0000 Uani . . . . . .
C56 C 0.6258(8) 1.1078(6) 0.3712(5) 0.0540 1.0000 Uani . . . . . .
C57 C 0.5005(8) 1.1211(7) 0.3848(5) 0.0534 1.0000 Uani . . . . . .
C58 C 0.4736(10) 1.1775(8) 0.4224(6) 0.0735 1.0000 Uani . . . . . .
C59 C 0.5656(12) 1.2191(9) 0.4424(7) 0.0871 1.0000 Uani . . . . . .
C60 C 0.6879(11) 1.2064(8) 0.4256(6) 0.0803 1.0000 Uani . . . . . .
C61 C 0.7210(9) 1.1514(7) 0.3892(5) 0.0611 1.0000 Uani . . . . . .
C62 C 0.8557(9) 1.1387(8) 0.3720(6) 0.0695 1.0000 Uani . . . . . .
C63 C 0.9119(13) 1.2249(9) 0.3239(8) 0.0980 1.0000 Uani . . . . . .
C64 C 0.9283(10) 1.0957(10) 0.4392(7) 0.0987 1.0000 Uani . . . . . .
C65 C 0.3967(8) 1.0785(7) 0.3618(5) 0.0614 1.0000 Uani . . . . . .
C66 C 0.3057(10) 1.0324(9) 0.4230(6) 0.0790 1.0000 Uani . . . . . .
C67 C 0.3287(10) 1.1460(9) 0.2997(6) 0.0814 1.0000 Uani . . . . . .
C69 C 0.806(3) 0.3211(15) 0.9880(9) 0.1306 0.69(2) Uani D . P 1 1 .
C70 C 0.714(2) 0.2551(15) 0.9858(11) 0.1298 0.69(2) Uani D . P 1 1 .
C71 C 0.728(2) 0.2549(15) 0.9124(11) 0.1343 0.69(2) Uani D . P 1 1 .
C72 C 0.8241(17) 0.3226(10) 0.8776(8) 0.1407 1.0000 Uani D . . . . .
C74 C 0.6648(14) 0.5465(7) 0.9773(8) 0.1091 1.0000 Uani D . . . . .
C75 C 0.647(10) 0.630(2) 0.991(4) 0.1088 0.21(2) Uani D . P 1 2 .
C76 C 0.629(2) 0.6304(10) 0.9875(14) 0.1117 0.79(2) Uani D . P 1 1 .
C77 C 0.695(8) 0.6963(12) 0.924(5) 0.1081 0.21(2) Uani D . P 1 2 .
C78 C 0.715(2) 0.6938(7) 0.9391(14) 0.1166 0.79(2) Uani D . P 1 1 .
C79 C 0.804(8) 0.652(6) 0.902(4) 0.1064 0.21(2) Uani D . P 1 2 .
C80 C 0.8261(18) 0.6400(15) 0.9335(13) 0.1167 0.79(2) Uani D . P 1 1 .
C82 C 0.9954(11) 0.5319(11) 0.7553(8) 0.1138 1.0000 Uani D . . . . .
C83 C 1.105(5) 0.472(5) 0.778(3) 0.1126 0.21(2) Uani D . P 1 2 .
C84 C 1.1320(12) 0.5137(17) 0.7551(8) 0.1180 0.79(2) Uani D . P 1 1 .
C85 C 1.120(7) 0.463(4) 0.853(3) 0.1131 0.21(2) Uani D . P 1 2 .
C86 C 1.1626(16) 0.4850(16) 0.8313(10) 0.1205 0.79(2) Uani D . P 1 1 .
C87 C 1.069(3) 0.5311(17) 0.8630(9) 0.1197 0.79(2) Uani D . P 1 1 .
C88 C 1.081(11) 0.551(5) 0.855(3) 0.1124 0.21(2) Uani D . P 1 2 .
C90 C 0.5664(16) 0.4874(10) 0.8104(8) 0.1315 1.0000 Uani D . . . . .
C91 C 0.497(2) 0.5336(15) 0.7433(10) 0.1322 0.79(2) Uani D . P 1 1 .
C92 C 0.519(6) 0.521(6) 0.7353(18) 0.1309 0.21(2) Uani D . P 1 2 .
C93 C 0.562(2) 0.6155(13) 0.7100(10) 0.1312 0.79(2) Uani D . P 1 1 .
C94 C 0.617(9) 0.578(5) 0.6931(18) 0.1310 0.21(2) Uani D . P 1 2 .
C95 C 0.677(9) 0.609(7) 0.746(5) 0.1312 0.21(2) Uani D . P 1 2 .
C96 C 0.658(2) 0.6132(16) 0.7636(12) 0.1285 0.79(2) Uani D . P 1 1 .
C97 C 0.713(7) 0.317(4) 0.979(3) 0.1443 0.31(2) Uani D . P 1 2 .
C98 C 0.663(4) 0.248(3) 0.954(3) 0.1427 0.31(2) Uani D . P 1 2 .
C99 C 0.760(5) 0.237(2) 0.905(3) 0.1409 0.31(2) Uani D . P 1 2 .
N4 N 0.7230(5) 1.0013(4) 0.2461(4) 0.0420 1.0000 Uani . . . . . .
N55 N 0.6554(6) 1.0432(5) 0.3397(4) 0.0465 1.0000 Uani . . . . . .
B19 B 0.9085(8) 0.7780(7) 0.3291(6) 0.0514 1.0000 Uani . . . . . .
F22 F 1.0881(5) 0.8749(5) 0.3834(4) 0.0912 1.0000 Uani . . . . . .
F24 F 1.3299(5) 0.8630(6) 0.3809(4) 0.1000 1.0000 Uani . . . . . .
F26 F 1.4475(4) 0.7497(5) 0.3292(4) 0.0893 1.0000 Uani . . . . . .
F29 F 1.0703(5) 0.6574(4) 0.2796(4) 0.0821 1.0000 Uani . . . . . .
F30 F 1.3126(5) 0.6453(5) 0.2811(5) 0.1006 1.0000 Uani . . . . . .
F33 F 1.0094(6) 0.8305(4) 0.1799(3) 0.0759 1.0000 Uani . . . . . .
F35 F 0.9000(9) 0.8231(6) 0.0649(4) 0.1163 1.0000 Uani . . . . . .
F37 F 0.6735(9) 0.7486(8) 0.0801(6) 0.1519 1.0000 Uani . . . . . .
F40 F 0.6756(5) 0.6834(4) 0.3278(4) 0.0890 1.0000 Uani . . . . . .
F41 F 0.5677(6) 0.6759(6) 0.2125(6) 0.1282 1.0000 Uani . . . . . .
F44 F 0.8592(6) 0.8108(5) 0.4683(3) 0.0810 1.0000 Uani . . . . . .
F46 F 0.8269(7) 0.6947(6) 0.5964(4) 0.1173 1.0000 Uani . . . . . .
F48 F 0.8211(8) 0.5196(6) 0.6171(5) 0.1467 1.0000 Uani . . . . . .
F51 F 0.8843(7) 0.5853(4) 0.3713(5) 0.1074 1.0000 Uani . . . . . .
F52 F 0.8488(9) 0.4695(5) 0.5009(6) 0.1446 1.0000 Uani . . . . . .
O68 O 0.8120(11) 0.3770(6) 0.9161(5) 0.1152 1.0000 Uani . . . . . .
O73 O 0.7804(8) 0.5568(6) 0.9415(6) 0.0980 1.0000 Uani . . . . . .
O81 O 0.9630(8) 0.5390(7) 0.8234(5) 0.1001 1.0000 Uani . . . . . .
O89 O 0.6770(9) 0.5332(7) 0.8078(5) 0.0979 1.0000 Uani . . . . . .
Li97 Li 0.807(2) 0.5015(16) 0.8735(13) 0.0934 1.0000 Uani . . . . . .
H71 H 0.9391 1.0578 0.2304 0.0748 1.0000 Uiso R . . . . .
H83 H 1.0461 1.1893 0.1762 0.1279 1.0000 Uiso R . . . . .
H82 H 0.9085 1.2012 0.1542 0.1280 1.0000 Uiso R . . . . .
H81 H 1.0101 1.1905 0.1003 0.1280 1.0000 Uiso R . . . . .
H91 H 1.1475 1.0428 0.2103 0.1118 1.0000 Uiso R . . . . .
H92 H 1.1260 1.0454 0.1322 0.1120 1.0000 Uiso R . . . . .
H93 H 1.0806 0.9655 0.1987 0.1120 1.0000 Uiso R . . . . .
H101 H 0.9714 1.0641 0.0506 0.0809 1.0000 Uiso R . . . . .
H111 H 0.8272 1.0279 -0.0141 0.0870 1.0000 Uiso R . . . . .
H121 H 0.6291 0.9945 0.0325 0.0790 1.0000 Uiso R . . . . .
H141 H 0.5224 0.9806 0.2077 0.0722 1.0000 Uiso R . . . . .
H151 H 0.3657 1.0627 0.1387 0.1229 1.0000 Uiso R . . . . .
H152 H 0.4844 1.1197 0.1240 0.1230 1.0000 Uiso R . . . . .
H153 H 0.4458 1.0782 0.0682 0.1229 1.0000 Uiso R . . . . .
H163 H 0.3846 0.9029 0.1660 0.1180 1.0000 Uiso R . . . . .
H162 H 0.5149 0.8573 0.1761 0.1180 1.0000 Uiso R . . . . .
H161 H 0.4719 0.9136 0.0988 0.1180 1.0000 Uiso R . . . . .
H171 H 0.7044 0.8740 0.2627 0.0510 1.0000 Uiso R . . . . .
H181 H 0.8846 0.8966 0.3499 0.0539 1.0000 Uiso R . . . . .
H182 H 0.9168 0.9140 0.2681 0.0540 1.0000 Uiso R . . . . .
H531 H 0.6577 0.8309 0.3886 0.0579 1.0000 Uiso R . . . . .
H532 H 0.5604 0.8953 0.3385 0.0579 1.0000 Uiso R . . . . .
H541 H 0.7439 0.9447 0.4135 0.0639 1.0000 Uiso R . . . . .
H542 H 0.6007 0.9461 0.4299 0.0640 1.0000 Uiso R . . . . .
H581 H 0.3922 1.1867 0.4342 0.0878 1.0000 Uiso R . . . . .
H591 H 0.5457 1.2560 0.4673 0.1049 1.0000 Uiso R . . . . .
H601 H 0.7489 1.2357 0.4392 0.0960 1.0000 Uiso R . . . . .
H621 H 0.8592 1.0998 0.3443 0.0830 1.0000 Uiso R . . . . .
H633 H 0.9951 1.2146 0.3105 0.1470 1.0000 Uiso R . . . . .
H632 H 0.9117 1.2647 0.3495 0.1469 1.0000 Uiso R . . . . .
H631 H 0.8642 1.2490 0.2816 0.1470 1.0000 Uiso R . . . . .
H641 H 1.0122 1.0880 0.4258 0.1479 1.0000 Uiso R . . . . .
H642 H 0.9257 1.1317 0.4679 0.1479 1.0000 Uiso R . . . . .
H643 H 0.8931 1.0401 0.4662 0.1479 1.0000 Uiso R . . . . .
H651 H 0.4331 1.0347 0.3437 0.0740 1.0000 Uiso R . . . . .
H663 H 0.2446 1.0041 0.4057 0.1179 1.0000 Uiso R . . . . .
H662 H 0.2661 1.0740 0.4403 0.1179 1.0000 Uiso R . . . . .
H661 H 0.3487 0.9902 0.4612 0.1180 1.0000 Uiso R . . . . .
H671 H 0.2632 1.1185 0.2852 0.1219 1.0000 Uiso R . . . . .
H672 H 0.2952 1.1915 0.3152 0.1219 1.0000 Uiso R . . . . .
H673 H 0.3858 1.1702 0.2598 0.1219 1.0000 Uiso R . . . . .
H691 H 0.7783 0.3518 1.0194 0.1570 0.69(2) Uiso R . P 1 1 .
H692 H 0.8863 0.2940 1.0027 0.1570 0.69(2) Uiso R . P 1 1 .
H701 H 0.6313 0.2719 0.9956 0.1561 0.69(2) Uiso R . P 1 1 .
H702 H 0.7340 0.1982 1.0205 0.1560 0.69(2) Uiso R . P 1 1 .
H711 H 0.6501 0.2715 0.8880 0.1610 0.69(2) Uiso R . P 1 1 .
H712 H 0.7544 0.1984 0.9122 0.1610 0.69(2) Uiso R . P 1 1 .
H751 H 0.6934 0.6292 1.0320 0.1310 0.21(2) Uiso R . P 1 2 .
H752 H 0.5604 0.6401 0.9989 0.1310 0.21(2) Uiso R . P 1 2 .
H761 H 0.6391 0.6260 1.0370 0.1340 0.79(2) Uiso R . P 1 1 .
H762 H 0.5449 0.6469 0.9735 0.1341 0.79(2) Uiso R . P 1 1 .
H771 H 0.7205 0.7470 0.9344 0.1300 0.21(2) Uiso R . P 1 2 .
H772 H 0.6329 0.7133 0.8879 0.1300 0.21(2) Uiso R . P 1 2 .
H781 H 0.7377 0.7372 0.9591 0.1400 0.79(2) Uiso R . P 1 1 .
H782 H 0.6805 0.7220 0.8921 0.1401 0.79(2) Uiso R . P 1 1 .
H791 H 0.8803 0.6696 0.9172 0.1280 0.21(2) Uiso R . P 1 2 .
H792 H 0.8061 0.6671 0.8508 0.1280 0.21(2) Uiso R . P 1 2 .
H801 H 0.8817 0.6349 0.9719 0.1400 0.79(2) Uiso R . P 1 1 .
H802 H 0.8691 0.6651 0.8873 0.1400 0.79(2) Uiso R . P 1 1 .
H831 H 1.1774 0.4979 0.7493 0.1350 0.21(2) Uiso R . P 1 2 .
H832 H 1.0899 0.4161 0.7741 0.1350 0.21(2) Uiso R . P 1 2 .
H841 H 1.1760 0.5662 0.7279 0.1410 0.79(2) Uiso R . P 1 1 .
H842 H 1.1507 0.4685 0.7358 0.1410 0.79(2) Uiso R . P 1 1 .
H851 H 1.2054 0.4509 0.8668 0.1350 0.21(2) Uiso R . P 1 2 .
H852 H 1.0677 0.4177 0.8850 0.1350 0.21(2) Uiso R . P 1 2 .
H861 H 1.2456 0.5019 0.8371 0.1440 0.79(2) Uiso R . P 1 1 .
H862 H 1.1545 0.4225 0.8534 0.1441 0.79(2) Uiso R . P 1 1 .
H871 H 1.0981 0.5880 0.8588 0.1430 0.79(2) Uiso R . P 1 1 .
H872 H 1.0517 0.4968 0.9132 0.1429 0.79(2) Uiso R . P 1 1 .
H881 H 1.1309 0.5993 0.8249 0.1350 0.21(2) Uiso R . P 1 2 .
H882 H 1.0728 0.5533 0.9032 0.1350 0.21(2) Uiso R . P 1 2 .
H911 H 0.4123 0.5447 0.7553 0.1581 0.79(2) Uiso R . P 1 1 .
H912 H 0.4978 0.5005 0.7116 0.1581 0.79(2) Uiso R . P 1 1 .
H921 H 0.4419 0.5521 0.7331 0.1570 0.21(2) Uiso R . P 1 2 .
H922 H 0.5081 0.4731 0.7180 0.1570 0.21(2) Uiso R . P 1 2 .
H931 H 0.5063 0.6646 0.7034 0.1570 0.79(2) Uiso R . P 1 1 .
H932 H 0.5999 0.6189 0.6642 0.1571 0.79(2) Uiso R . P 1 1 .
H941 H 0.5822 0.6260 0.6542 0.1570 0.21(2) Uiso R . P 1 2 .
H942 H 0.6766 0.5466 0.6738 0.1570 0.21(2) Uiso R . P 1 2 .
H951 H 0.6272 0.6538 0.7556 0.1570 0.21(2) Uiso R . P 1 2 .
H952 H 0.7597 0.6303 0.7309 0.1570 0.21(2) Uiso R . P 1 2 .
H961 H 0.6294 0.6486 0.7913 0.1551 0.79(2) Uiso R . P 1 1 .
H962 H 0.7348 0.6362 0.7384 0.1550 0.79(2) Uiso R . P 1 1 .
H971 H 0.6535 0.3514 0.9911 0.1730 0.31(2) Uiso . . P 1 2 .
H972 H 0.7648 0.2865 1.0237 0.1730 0.31(2) Uiso . . P 1 2 .
H981 H 0.5873 0.2706 0.9307 0.1710 0.31(2) Uiso . . P 1 2 .
H982 H 0.6492 0.1948 0.9944 0.1710 0.31(2) Uiso . . P 1 2 .
H991 H 0.8163 0.1890 0.9294 0.1690 0.31(2) Uiso R . P 1 2 .
H992 H 0.7225 0.2257 0.8660 0.1690 0.31(2) Uiso R . P 1 2 .
H901 H 0.5062 0.4992 0.8432 0.1580 0.21(2) Uiso R . P 1 2 .
H902 H 0.5831 0.4253 0.8258 0.1580 0.21(2) Uiso R . P 1 2 .
H903 H 0.5162 0.4862 0.8522 0.1581 0.79(2) Uiso R . P 1 1 .
H904 H 0.5863 0.4283 0.8132 0.1581 0.79(2) Uiso R . P 1 1 .
H721 H 0.8085 0.3533 0.8271 0.1690 0.69(2) Uiso R . P 1 1 .
H722 H 0.9059 0.2961 0.8827 0.1691 0.69(2) Uiso R . P 1 1 .
H723 H 0.9114 0.3091 0.8754 0.1690 0.31(2) Uiso R . P 1 2 .
H724 H 0.7959 0.3547 0.8296 0.1690 0.31(2) Uiso R . P 1 2 .
H821 H 0.9759 0.5859 0.7168 0.1360 0.79(2) Uiso R . P 1 1 .
H822 H 0.9508 0.4847 0.7492 0.1360 0.79(2) Uiso R . P 1 1 .
H823 H 1.0168 0.5877 0.7192 0.1360 0.21(2) Uiso R . P 1 2 .
H824 H 0.9303 0.5058 0.7378 0.1360 0.21(2) Uiso R . P 1 2 .
H741 H 0.6657 0.4968 1.0218 0.1310 0.21(2) Uiso R . P 1 2 .
H742 H 0.6009 0.5393 0.9470 0.1310 0.21(2) Uiso R . P 1 2 .
H743 H 0.6697 0.5005 1.0239 0.1310 0.79(2) Uiso R . P 1 1 .
H744 H 0.6039 0.5320 0.9489 0.1309 0.79(2) Uiso R . P 1 1 .

_refine_ls_extinction_coef       61(7)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          3.04(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
Au1 . Cl2 . 2.277(3) yes
Au1 . C3 . 2.000(9) yes
C3 . N4 . 1.316(10) yes
C3 . N55 . 1.352(10) yes
C5 . C6 . 1.412(11) yes
C5 . C13 . 1.403(12) yes
C5 . N4 . 1.453(10) yes
C6 . C7 . 1.530(14) yes
C6 . C10 . 1.381(14) yes
C7 . C8 . 1.547(14) yes
C7 . C9 . 1.523(13) yes
C7 . H71 . 0.978 no
C8 . H83 . 0.963 no
C8 . H82 . 0.955 no
C8 . H81 . 0.957 no
C9 . H91 . 0.960 no
C9 . H92 . 0.962 no
C9 . H93 . 0.962 no
C10 . C11 . 1.362(15) yes
C10 . H101 . 0.927 no
C11 . C12 . 1.388(15) yes
C11 . H111 . 0.929 no
C12 . C13 . 1.382(13) yes
C12 . H121 . 0.928 no
C13 . C14 . 1.515(12) yes
C14 . C15 . 1.525(15) yes
C14 . C16 . 1.525(15) yes
C14 . H141 . 0.982 no
C15 . H151 . 0.960 no
C15 . H152 . 0.963 no
C15 . H153 . 0.959 no
C16 . H163 . 0.960 no
C16 . H162 . 0.962 no
C16 . H161 . 0.958 no
C17 . C18 . 1.519(10) yes
C17 . C53 . 1.510(11) yes
C17 . N4 . 1.500(10) yes
C17 . H171 . 0.975 no
C18 . B19 . 1.642(13) yes
C18 . H181 . 0.964 no
C18 . H182 . 0.971 no
C20 . C21 . 1.380(13) yes
C20 . C28 . 1.394(13) yes
C20 . B19 . 1.667(11) yes
C21 . C23 . 1.376(12) yes
C21 . F22 . 1.340(11) yes
C23 . C25 . 1.376(14) yes
C23 . F24 . 1.352(12) yes
C25 . C27 . 1.351(14) yes
C25 . F26 . 1.346(9) yes
C27 . C28 . 1.361(12) yes
C27 . F30 . 1.354(11) yes
C28 . F29 . 1.350(11) yes
C31 . C32 . 1.394(15) yes
C31 . C39 . 1.373(13) yes
C31 . B19 . 1.669(15) yes
C32 . C34 . 1.424(17) yes
C32 . F33 . 1.339(12) yes
C34 . C36 . 1.34(2) yes
C34 . F35 . 1.332(16) yes
C36 . C38 . 1.36(2) yes
C36 . F37 . 1.342(16) yes
C38 . C39 . 1.393(18) yes
C38 . F41 . 1.338(14) yes
C39 . F40 . 1.370(14) yes
C42 . C43 . 1.415(17) yes
C42 . C50 . 1.367(16) yes
C42 . B19 . 1.655(15) yes
C43 . C45 . 1.394(16) yes
C43 . F44 . 1.338(14) yes
C45 . C47 . 1.35(2) yes
C45 . F46 . 1.367(17) yes
C47 . C49 . 1.34(2) yes
C47 . F48 . 1.378(15) yes
C49 . C50 . 1.378(19) yes
C49 . F52 . 1.355(17) yes
C50 . F51 . 1.361(16) yes
C53 . C54 . 1.513(13) yes
C53 . H531 . 0.971 no
C53 . H532 . 0.968 no
C54 . N55 . 1.473(11) yes
C54 . H541 . 0.969 no
C54 . H542 . 0.969 no
C56 . C57 . 1.403(12) yes
C56 . C61 . 1.397(13) yes
C56 . N55 . 1.438(11) yes
C57 . C58 . 1.405(13) yes
C57 . C65 . 1.505(13) yes
C58 . C59 . 1.368(16) yes
C58 . H581 . 0.928 no
C59 . C60 . 1.386(16) yes
C59 . H591 . 0.928 no
C60 . C61 . 1.379(14) yes
C60 . H601 . 0.929 no
C61 . C62 . 1.516(14) yes
C62 . C63 . 1.527(16) yes
C62 . C64 . 1.512(15) yes
C62 . H621 . 0.982 no
C63 . H633 . 0.961 no
C63 . H632 . 0.961 no
C63 . H631 . 0.959 no
C64 . H641 . 0.958 no
C64 . H642 . 0.956 no
C64 . H643 . 0.961 no
C65 . C66 . 1.526(14) yes
C65 . C67 . 1.535(14) yes
C65 . H651 . 0.982 no
C66 . H663 . 0.958 no
C66 . H662 . 0.957 no
C66 . H661 . 0.957 no
C67 . H671 . 0.956 no
C67 . H672 . 0.965 no
C67 . H673 . 0.961 no
C69 . C70 . 1.503(7) yes
C69 . O68 . 1.40(2) yes
C69 . H691 . 0.970 no
C69 . H692 . 0.970 no
C70 . C71 . 1.464(7) yes
C70 . H701 . 0.969 no
C70 . H702 . 0.971 no
C71 . C72 . 1.506(7) yes
C71 . H711 . 0.970 no
C71 . H712 . 0.969 no
C72 . O68 . 1.369(16) yes
C72 . H721 . 0.972 no
C72 . H722 . 0.971 no
C72 . C99 . 1.500(7) yes
C72 . O68 . 1.369(16) yes
C72 . H723 . 0.971 no
C72 . H724 . 0.971 no
C74 . C76 . 1.502(7) yes
C74 . O73 . 1.403(15) yes
C74 . H743 . 0.969 no
C74 . H744 . 0.970 no
C74 . C75 . 1.502(7) yes
C74 . O73 . 1.403(15) yes
C74 . H741 . 0.970 no
C74 . H742 . 0.970 no
C75 . C77 . 1.464(7) yes
C75 . H751 . 0.971 no
C75 . H752 . 0.970 no
C76 . C78 . 1.466(7) yes
C76 . H761 . 0.972 no
C76 . H762 . 0.972 no
C77 . C79 . 1.503(7) yes
C77 . H771 . 0.971 no
C77 . H772 . 0.970 no
C78 . C80 . 1.501(7) yes
C78 . H781 . 0.970 no
C78 . H782 . 0.969 no
C79 . O73 . 1.51(8) yes
C79 . H791 . 0.969 no
C79 . H792 . 0.970 no
C80 . O73 . 1.42(2) yes
C80 . H801 . 0.970 no
C80 . H802 . 0.970 no
C82 . C84 . 1.505(7) yes
C82 . O81 . 1.433(16) yes
C82 . H821 . 0.969 no
C82 . H822 . 0.970 no
C82 . C83 . 1.503(7) yes
C82 . O81 . 1.433(16) yes
C82 . H823 . 0.970 no
C82 . H824 . 0.970 no
C83 . C85 . 1.465(7) yes
C83 . H831 . 0.969 no
C83 . H832 . 0.969 no
C84 . C86 . 1.467(7) yes
C84 . H841 . 0.968 no
C84 . H842 . 0.966 no
C85 . C88 . 1.503(7) yes
C85 . H851 . 0.970 no
C85 . H852 . 0.971 no
C86 . C87 . 1.504(7) yes
C86 . H861 . 0.970 no
C86 . H862 . 0.969 no
C87 . O81 . 1.39(3) yes
C87 . H871 . 0.969 no
C87 . H872 . 0.971 no
C88 . O81 . 1.50(11) yes
C88 . H881 . 0.970 no
C88 . H882 . 0.969 no
C90 . C91 . 1.503(7) yes
C90 . O89 . 1.421(16) yes
C90 . H903 . 0.974 no
C90 . H904 . 0.972 no
C90 . C92 . 1.501(7) yes
C90 . O89 . 1.421(16) yes
C90 . H901 . 0.971 no
C90 . H902 . 0.971 no
C91 . C93 . 1.463(7) yes
C91 . H911 . 0.967 no
C91 . H912 . 0.967 no
C92 . C94 . 1.461(7) yes
C92 . H921 . 0.970 no
C92 . H922 . 0.970 no
C93 . C96 . 1.504(7) yes
C93 . H931 . 0.972 no
C93 . H932 . 0.969 no
C94 . C95 . 1.503(7) yes
C94 . H941 . 0.970 no
C94 . H942 . 0.969 no
C95 . O89 . 1.40(10) yes
C95 . H951 . 0.970 no
C95 . H952 . 0.970 no
C96 . O89 . 1.31(2) yes
C96 . H961 . 0.971 no
C96 . H962 . 0.971 no
C97 . C98 . 1.504(7) yes
C97 . O68 . 1.67(6) yes
C97 . H971 . 0.928 no
C97 . H972 . 1.029 no
C98 . C99 . 1.461(7) yes
C98 . H981 . 0.958 no
C98 . H982 . 0.972 no
C99 . H991 . 0.970 no
C99 . H992 . 0.970 no
O68 . Li97 . 1.92(3) yes
O68 . Li97 . 1.92(3) yes
O73 . Li97 . 1.89(2) yes
O73 . Li97 . 1.89(2) yes
O81 . Li97 . 1.93(2) yes
O81 . Li97 . 1.93(2) yes
O89 . Li97 . 1.90(3) yes
O89 . Li97 . 1.90(3) yes
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
Cl2 . Au1 . C3 . 176.2(3) yes
Au1 . C3 . N4 . 124.6(6) yes
Au1 . C3 . N55 . 116.7(6) yes
N4 . C3 . N55 . 118.7(8) yes
C6 . C5 . C13 . 120.9(8) yes
C6 . C5 . N4 . 120.5(8) yes
C13 . C5 . N4 . 117.9(7) yes
C5 . C6 . C7 . 122.5(8) yes
C5 . C6 . C10 . 117.6(9) yes
C7 . C6 . C10 . 119.6(8) yes
C6 . C7 . C8 . 111.5(9) yes
C6 . C7 . C9 . 113.0(9) yes
C8 . C7 . C9 . 110.1(8) yes
C6 . C7 . H71 . 107.5 no
C8 . C7 . H71 . 106.8 no
C9 . C7 . H71 . 107.6 no
C7 . C8 . H83 . 109.9 no
C7 . C8 . H82 . 110.0 no
H83 . C8 . H82 . 108.8 no
C7 . C8 . H81 . 109.4 no
H83 . C8 . H81 . 109.3 no
H82 . C8 . H81 . 109.4 no
C7 . C9 . H91 . 109.6 no
C7 . C9 . H92 . 109.4 no
H91 . C9 . H92 . 109.2 no
C7 . C9 . H93 . 109.5 no
H91 . C9 . H93 . 109.4 no
H92 . C9 . H93 . 109.7 no
C6 . C10 . C11 . 122.1(9) yes
C6 . C10 . H101 . 118.7 no
C11 . C10 . H101 . 119.2 no
C10 . C11 . C12 . 120.1(10) yes
C10 . C11 . H111 . 119.9 no
C12 . C11 . H111 . 120.0 no
C11 . C12 . C13 . 120.7(10) yes
C11 . C12 . H121 . 119.4 no
C13 . C12 . H121 . 119.9 no
C5 . C13 . C12 . 118.6(8) yes
C5 . C13 . C14 . 121.7(8) yes
C12 . C13 . C14 . 119.6(9) yes
C13 . C14 . C15 . 109.1(9) yes
C13 . C14 . C16 . 113.5(9) yes
C15 . C14 . C16 . 111.0(8) yes
C13 . C14 . H141 . 108.1 no
C15 . C14 . H141 . 106.8 no
C16 . C14 . H141 . 108.1 no
C14 . C15 . H151 . 109.7 no
C14 . C15 . H152 . 110.1 no
H151 . C15 . H152 . 109.2 no
C14 . C15 . H153 . 109.2 no
H151 . C15 . H153 . 109.4 no
H152 . C15 . H153 . 109.2 no
C14 . C16 . H163 . 109.2 no
C14 . C16 . H162 . 109.2 no
H163 . C16 . H162 . 109.4 no
C14 . C16 . H161 . 109.7 no
H163 . C16 . H161 . 109.8 no
H162 . C16 . H161 . 109.6 no
C18 . C17 . C53 . 115.8(7) yes
C18 . C17 . N4 . 111.0(6) yes
C53 . C17 . N4 . 108.0(6) yes
C18 . C17 . H171 . 107.5 no
C53 . C17 . H171 . 107.2 no
N4 . C17 . H171 . 107.0 no
C17 . C18 . B19 . 119.5(7) yes
C17 . C18 . H181 . 106.5 no
B19 . C18 . H181 . 107.5 no
C17 . C18 . H182 . 107.0 no
B19 . C18 . H182 . 106.8 no
H181 . C18 . H182 . 109.3 no
C21 . C20 . C28 . 112.4(8) yes
C21 . C20 . B19 . 123.6(8) yes
C28 . C20 . B19 . 124.0(8) yes
C20 . C21 . C23 . 124.4(9) yes
C20 . C21 . F22 . 121.0(7) yes
C23 . C21 . F22 . 114.6(9) yes
C21 . C23 . C25 . 119.9(9) yes
C21 . C23 . F24 . 120.7(9) yes
C25 . C23 . F24 . 119.4(8) yes
C23 . C25 . C27 . 118.0(8) yes
C23 . C25 . F26 . 119.5(9) yes
C27 . C25 . F26 . 122.5(9) yes
C25 . C27 . C28 . 120.8(9) yes
C25 . C27 . F30 . 118.4(8) yes
C28 . C27 . F30 . 120.8(10) yes
C20 . C28 . C27 . 124.5(10) yes
C20 . C28 . F29 . 120.2(8) yes
C27 . C28 . F29 . 115.3(9) yes
C32 . C31 . C39 . 112.2(10) yes
C32 . C31 . B19 . 121.8(9) yes
C39 . C31 . B19 . 124.7(10) yes
C31 . C32 . C34 . 124.7(12) yes
C31 . C32 . F33 . 119.7(9) yes
C34 . C32 . F33 . 115.6(11) yes
C32 . C34 . C36 . 117.4(15) yes
C32 . C34 . F35 . 119.4(13) yes
C36 . C34 . F35 . 123.2(15) yes
C34 . C36 . C38 . 121.6(14) yes
C34 . C36 . F37 . 119.3(18) yes
C38 . C36 . F37 . 119.1(15) yes
C36 . C38 . C39 . 118.4(12) yes
C36 . C38 . F41 . 121.3(14) yes
C39 . C38 . F41 . 120.1(16) yes
C38 . C39 . C31 . 125.5(13) yes
C38 . C39 . F40 . 115.5(11) yes
C31 . C39 . F40 . 119.0(11) yes
C43 . C42 . C50 . 111.8(11) yes
C43 . C42 . B19 . 122.4(10) yes
C50 . C42 . B19 . 125.0(11) yes
C42 . C43 . C45 . 122.4(13) yes
C42 . C43 . F44 . 122.2(10) yes
C45 . C43 . F44 . 115.4(13) yes
C43 . C45 . C47 . 120.3(15) yes
C43 . C45 . F46 . 117.7(15) yes
C47 . C45 . F46 . 122.0(14) yes
C45 . C47 . C49 . 120.2(14) yes
C45 . C47 . F48 . 119.8(18) yes
C49 . C47 . F48 . 120.0(17) yes
C47 . C49 . C50 . 118.3(15) yes
C47 . C49 . F52 . 120.7(16) yes
C50 . C49 . F52 . 121.0(18) yes
C49 . C50 . C42 . 126.9(15) yes
C49 . C50 . F51 . 113.9(13) yes
C42 . C50 . F51 . 119.2(11) yes
C17 . C53 . C54 . 110.3(7) yes
C17 . C53 . H531 . 109.1 no
C54 . C53 . H531 . 109.4 no
C17 . C53 . H532 . 109.3 no
C54 . C53 . H532 . 109.2 no
H531 . C53 . H532 . 109.5 no
C53 . C54 . N55 . 109.6(7) yes
C53 . C54 . H541 . 110.0 no
N55 . C54 . H541 . 109.1 no
C53 . C54 . H542 . 109.7 no
N55 . C54 . H542 . 109.4 no
H541 . C54 . H542 . 108.9 no
C57 . C56 . C61 . 123.4(9) yes
C57 . C56 . N55 . 117.1(8) yes
C61 . C56 . N55 . 119.5(8) yes
C56 . C57 . C58 . 116.4(9) yes
C56 . C57 . C65 . 124.0(8) yes
C58 . C57 . C65 . 119.6(8) yes
C57 . C58 . C59 . 121.0(10) yes
C57 . C58 . H581 . 119.5 no
C59 . C58 . H581 . 119.4 no
C58 . C59 . C60 . 120.5(11) yes
C58 . C59 . H591 . 119.5 no
C60 . C59 . H591 . 120.0 no
C59 . C60 . C61 . 121.5(11) yes
C59 . C60 . H601 . 119.1 no
C61 . C60 . H601 . 119.4 no
C56 . C61 . C60 . 117.0(9) yes
C56 . C61 . C62 . 122.9(9) yes
C60 . C61 . C62 . 120.1(10) yes
C61 . C62 . C63 . 110.5(10) yes
C61 . C62 . C64 . 112.0(9) yes
C63 . C62 . C64 . 112.2(10) yes
C61 . C62 . H621 . 107.4 no
C63 . C62 . H621 . 106.9 no
C64 . C62 . H621 . 107.5 no
C62 . C63 . H633 . 109.2 no
C62 . C63 . H632 . 109.6 no
H633 . C63 . H632 . 109.7 no
C62 . C63 . H631 . 109.3 no
H633 . C63 . H631 . 109.5 no
H632 . C63 . H631 . 109.5 no
C62 . C64 . H641 . 109.1 no
C62 . C64 . H642 . 109.6 no
H641 . C64 . H642 . 109.4 no
C62 . C64 . H643 . 109.4 no
H641 . C64 . H643 . 109.6 no
H642 . C64 . H643 . 109.7 no
C57 . C65 . C66 . 113.3(8) yes
C57 . C65 . C67 . 110.0(9) yes
C66 . C65 . C67 . 110.2(8) yes
C57 . C65 . H651 . 107.7 no
C66 . C65 . H651 . 107.7 no
C67 . C65 . H651 . 107.7 no
C65 . C66 . H663 . 109.4 no
C65 . C66 . H662 . 109.6 no
H663 . C66 . H662 . 109.2 no
C65 . C66 . H661 . 109.6 no
H663 . C66 . H661 . 109.6 no
H662 . C66 . H661 . 109.4 no
C65 . C67 . H671 . 109.6 no
C65 . C67 . H672 . 109.6 no
H671 . C67 . H672 . 109.4 no
C65 . C67 . H673 . 109.0 no
H671 . C67 . H673 . 109.4 no
H672 . C67 . H673 . 109.8 no
C70 . C69 . O68 . 101.9(12) yes
C70 . C69 . H691 . 111.8 no
O68 . C69 . H691 . 111.1 no
C70 . C69 . H692 . 111.0 no
O68 . C69 . H692 . 110.7 no
H691 . C69 . H692 . 110.1 no
C69 . C70 . C71 . 103.92(7) yes
C69 . C70 . H701 . 111.1 no
C71 . C70 . H701 . 111.0 no
C69 . C70 . H702 . 110.6 no
C71 . C70 . H702 . 110.7 no
H701 . C70 . H702 . 109.4 no
C70 . C71 . C72 . 103.92(7) yes
C70 . C71 . H711 . 110.1 no
C72 . C71 . H711 . 110.5 no
C70 . C71 . H712 . 111.3 no
C72 . C71 . H712 . 111.0 no
H711 . C71 . H712 . 109.9 no
C71 . C72 . O68 . 102.8(10) yes
C71 . C72 . H721 . 111.4 no
O68 . C72 . H721 . 111.3 no
C71 . C72 . H722 . 110.6 no
O68 . C72 . H722 . 110.8 no
H721 . C72 . H722 . 109.8 no
C99 . C72 . O68 . 118.8(19) yes
C99 . C72 . H723 . 105.7 no
O68 . C72 . H723 . 106.9 no
C99 . C72 . H724 . 108.5 no
O68 . C72 . H724 . 107.1 no
H723 . C72 . H724 . 109.6 no
C76 . C74 . O73 . 108.5(9) yes
C76 . C74 . H743 . 109.2 no
O73 . C74 . H743 . 109.7 no
C76 . C74 . H744 . 110.0 no
O73 . C74 . H744 . 109.7 no
H743 . C74 . H744 . 109.6 no
C75 . C74 . O73 . 103(3) yes
C75 . C74 . H741 . 111.8 no
O73 . C74 . H741 . 110.8 no
C75 . C74 . H742 . 111.0 no
O73 . C74 . H742 . 110.8 no
H741 . C74 . H742 . 109.6 no
C74 . C75 . C77 . 103.92(7) yes
C74 . C75 . H751 . 110.5 no
C77 . C75 . H751 . 111.5 no
C74 . C75 . H752 . 109.9 no
C77 . C75 . H752 . 111.3 no
H751 . C75 . H752 . 109.6 no
C74 . C76 . C78 . 103.93(7) yes
C74 . C76 . H761 . 111.2 no
C78 . C76 . H761 . 110.9 no
C74 . C76 . H762 . 110.8 no
C78 . C76 . H762 . 110.2 no
H761 . C76 . H762 . 109.7 no
C75 . C77 . C79 . 103.92(7) yes
C75 . C77 . H771 . 109.7 no
C79 . C77 . H771 . 110.8 no
C75 . C77 . H772 . 111.1 no
C79 . C77 . H772 . 111.7 no
H771 . C77 . H772 . 109.6 no
C76 . C78 . C80 . 103.93(7) yes
C76 . C78 . H781 . 111.3 no
C80 . C78 . H781 . 110.3 no
C76 . C78 . H782 . 111.1 no
C80 . C78 . H782 . 110.2 no
H781 . C78 . H782 . 109.9 no
C77 . C79 . O73 . 104(4) yes
C77 . C79 . H791 . 111.0 no
O73 . C79 . H791 . 111.0 no
C77 . C79 . H792 . 109.7 no
O73 . C79 . H792 . 111.6 no
H791 . C79 . H792 . 109.6 no
C78 . C80 . O73 . 105.8(12) yes
C78 . C80 . H801 . 109.7 no
O73 . C80 . H801 . 109.8 no
C78 . C80 . H802 . 111.3 no
O73 . C80 . H802 . 110.3 no
H801 . C80 . H802 . 109.8 no
C84 . C82 . O81 . 106.8(8) yes
C84 . C82 . H821 . 110.3 no
O81 . C82 . H821 . 110.0 no
C84 . C82 . H822 . 110.0 no
O81 . C82 . H822 . 110.2 no
H821 . C82 . H822 . 109.6 no
C83 . C82 . O81 . 98.1(20) yes
C83 . C82 . H823 . 112.7 no
O81 . C82 . H823 . 112.1 no
C83 . C82 . H824 . 111.9 no
O81 . C82 . H824 . 112.1 no
H823 . C82 . H824 . 109.5 no
C82 . C83 . C85 . 103.93(7) yes
C82 . C83 . H831 . 110.2 no
C85 . C83 . H831 . 110.7 no
C82 . C83 . H832 . 111.2 no
C85 . C83 . H832 . 111.1 no
H831 . C83 . H832 . 109.6 no
C82 . C84 . C86 . 103.93(7) yes
C82 . C84 . H841 . 110.3 no
C86 . C84 . H841 . 110.5 no
C82 . C84 . H842 . 110.9 no
C86 . C84 . H842 . 110.8 no
H841 . C84 . H842 . 110.3 no
C83 . C85 . C88 . 103.93(7) yes
C83 . C85 . H851 . 110.8 no
C88 . C85 . H851 . 110.4 no
C83 . C85 . H852 . 110.6 no
C88 . C85 . H852 . 111.3 no
H851 . C85 . H852 . 109.7 no
C84 . C86 . C87 . 103.93(7) yes
C84 . C86 . H861 . 111.2 no
C87 . C86 . H861 . 110.7 no
C84 . C86 . H862 . 110.3 no
C87 . C86 . H862 . 110.8 no
H861 . C86 . H862 . 109.9 no
C86 . C87 . O81 . 105.7(13) yes
C86 . C87 . H871 . 110.7 no
O81 . C87 . H871 . 110.4 no
C86 . C87 . H872 . 110.2 no
O81 . C87 . H872 . 110.0 no
H871 . C87 . H872 . 109.8 no
C85 . C88 . O81 . 87(5) yes
C85 . C88 . H881 . 115.2 no
O81 . C88 . H881 . 114.8 no
C85 . C88 . H882 . 114.4 no
O81 . C88 . H882 . 114.7 no
H881 . C88 . H882 . 109.6 no
C91 . C90 . O89 . 108.7(8) yes
C91 . C90 . H903 . 109.5 no
O89 . C90 . H903 . 109.5 no
C91 . C90 . H904 . 109.8 no
O89 . C90 . H904 . 109.6 no
H903 . C90 . H904 . 109.8 no
C92 . C90 . O89 . 106(2) yes
C92 . C90 . H901 . 110.0 no
O89 . C90 . H901 . 110.2 no
C92 . C90 . H902 . 110.5 no
O89 . C90 . H902 . 110.4 no
H901 . C90 . H902 . 109.6 no
C90 . C91 . C93 . 103.93(7) yes
C90 . C91 . H911 . 110.4 no
C93 . C91 . H911 . 110.3 no
C90 . C91 . H912 . 111.5 no
C93 . C91 . H912 . 110.8 no
H911 . C91 . H912 . 109.8 no
C90 . C92 . C94 . 103.92(7) yes
C90 . C92 . H921 . 111.1 no
C94 . C92 . H921 . 111.2 no
C90 . C92 . H922 . 110.8 no
C94 . C92 . H922 . 110.2 no
H921 . C92 . H922 . 109.6 no
C91 . C93 . C96 . 103.93(7) yes
C91 . C93 . H931 . 110.4 no
C96 . C93 . H931 . 110.0 no
C91 . C93 . H932 . 110.7 no
C96 . C93 . H932 . 111.6 no
H931 . C93 . H932 . 110.0 no
C92 . C94 . C95 . 103.92(7) yes
C92 . C94 . H941 . 110.6 no
C95 . C94 . H941 . 111.4 no
C92 . C94 . H942 . 111.4 no
C95 . C94 . H942 . 109.8 no
H941 . C94 . H942 . 109.6 no
C94 . C95 . O89 . 102(5) yes
C94 . C95 . H951 . 110.7 no
O89 . C95 . H951 . 110.1 no
C94 . C95 . H952 . 112.4 no
O89 . C95 . H952 . 112.3 no
H951 . C95 . H952 . 109.5 no
C93 . C96 . O89 . 110.8(10) yes
C93 . C96 . H961 . 109.3 no
O89 . C96 . H961 . 108.9 no
C93 . C96 . H962 . 109.5 no
O89 . C96 . H962 . 108.9 no
H961 . C96 . H962 . 109.4 no
C98 . C97 . O68 . 108(3) yes
C98 . C97 . H971 . 114.7 no
O68 . C97 . H971 . 111.5 no
C98 . C97 . H972 . 108.2 no
O68 . C97 . H972 . 105.7 no
H971 . C97 . H972 . 108.3 no
C97 . C98 . C99 . 103.92(7) yes
C97 . C98 . H981 . 107.3 no
C99 . C98 . H981 . 113.6 no
C97 . C98 . H982 . 110.4 no
C99 . C98 . H982 . 110.8 no
H981 . C98 . H982 . 110.5 no
C72 . C99 . C98 . 103.92(7) yes
C72 . C99 . H991 . 112.2 no
C98 . C99 . H991 . 112.4 no
C72 . C99 . H992 . 109.6 no
C98 . C99 . H992 . 108.8 no
H991 . C99 . H992 . 109.7 no
C17 . N4 . C5 . 114.6(6) yes
C17 . N4 . C3 . 125.4(7) yes
C5 . N4 . C3 . 119.8(7) yes
C54 . N55 . C56 . 114.0(7) yes
C54 . N55 . C3 . 123.0(7) yes
C56 . N55 . C3 . 122.7(8) yes
C31 . B19 . C20 . 111.6(8) yes
C31 . B19 . C42 . 113.5(8) yes
C20 . B19 . C42 . 101.0(7) yes
C31 . B19 . C18 . 101.4(7) yes
C20 . B19 . C18 . 109.8(7) yes
C42 . B19 . C18 . 119.8(8) yes
C69 . O68 . C72 . 104.4(11) yes
C69 . O68 . Li97 . 131.5(12) yes
C72 . O68 . Li97 . 124.0(11) yes
C97 . O68 . C72 . 97.4(17) yes
C97 . O68 . Li97 . 125(2) yes
C72 . O68 . Li97 . 124.0(11) yes
C80 . O73 . C74 . 108.6(10) yes
C80 . O73 . Li97 . 124.4(13) yes
C74 . O73 . Li97 . 117.7(10) yes
C79 . O73 . C74 . 109(3) yes
C79 . O73 . Li97 . 107(3) yes
C74 . O73 . Li97 . 117.7(10) yes
C82 . O81 . C87 . 109.6(10) yes
C82 . O81 . Li97 . 123.4(11) yes
C87 . O81 . Li97 . 119.2(13) yes
C88 . O81 . C82 . 106(3) yes
C88 . O81 . Li97 . 127(3) yes
C82 . O81 . Li97 . 123.4(11) yes
C90 . O89 . C96 . 106.3(12) yes
C90 . O89 . Li97 . 127.9(11) yes
C96 . O89 . Li97 . 123.3(12) yes
C90 . O89 . C95 . 109(3) yes
C90 . O89 . Li97 . 127.9(11) yes
C95 . O89 . Li97 . 123(3) yes
O68 . Li97 . O81 . 108.0(13) yes
O68 . Li97 . O73 . 113.2(13) yes
O81 . Li97 . O73 . 108.9(12) yes
O68 . Li97 . O89 . 108.0(12) yes
O81 . Li97 . O89 . 110.2(12) yes
O73 . Li97 . O89 . 108.5(13) yes
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
C17 . H171 . C39 . 135.2 0.975 2.578 3.34(3) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 23/04/14 at 15:32:32
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
CONT EXTPARAM 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  83,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,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   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 633,X'S) H   ( 632,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) H   ( 642,X'S) H   ( 643,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 663,X'S) H   ( 662,X'S) H   ( 661,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) H   ( 672,X'S) H   ( 673,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) H   ( 692,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 702,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) H   ( 723,X'S) H   ( 724,X'S) 
RIDE C   (  74,X'S) H   ( 743,X'S) H   ( 744,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   (  77,X'S) H   ( 771,X'S) H   ( 772,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) H   ( 792,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) H   ( 802,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) H   ( 822,X'S) H   ( 823,X'S) H   ( 824,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   (  87,X'S) H   ( 871,X'S) H   ( 872,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) H   ( 882,X'S) 
RIDE C   (  90,X'S) H   ( 903,X'S) H   ( 904,X'S) H   ( 901,X'S) H   ( 902,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) H   ( 912,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) H   ( 922,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) H   ( 932,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) H   ( 942,X'S) 
RIDE C   (  95,X'S) H   ( 951,X'S) H   ( 952,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) H   ( 962,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) H   ( 992,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 23/04/14 at 15:32:32
#
#LIST     16                                                                    
SAME  C(96)  C(93)  C(91)  C(90) AND 
CONT  C(90)  C(91)  C(93)  C(96) AND 
CONT  C(95)  C(94)  C(92)  C(90) AND 
CONT  C(90)  C(92)  C(94)  C(95) AND 
CONT  C(82)  C(84)  C(86)  C(87) AND 
CONT  C(87)  C(86)  C(84)  C(82) AND 
CONT  C(82)  C(83)  C(85)  C(88) AND 
CONT  C(88)  C(85)  C(83)  C(82) AND 
CONT  C(74)  C(75)  C(77)  C(79) AND 
CONT  C(79)  C(77)  C(75)  C(74) AND 
CONT  C(74)  C(76)  C(78)  C(80) AND 
CONT  C(80)  C(78)  C(76)  C(74) AND 
CONT  C(69)  C(70)  C(71)  C(72) AND 
CONT  C(72)  C(71)  C(70)  C(69) AND 
CONT  C(97)  C(98)  C(99)  C(72) AND 
CONT  C(72)  C(99)  C(98)  C(97) 
DELU 0.01 C(96)  C(93)  C(91)  C(90) AND 
CONT  C(90)  C(91)  C(93)  C(96) AND 
CONT  C(95)  C(94)  C(92)  C(90) AND 
CONT  C(90)  C(92)  C(94)  C(95) AND 
CONT  C(82)  C(84)  C(86)  C(87) AND 
CONT  C(87)  C(86)  C(84)  C(82) AND 
CONT  C(82)  C(83)  C(85)  C(88) AND 
CONT  C(88)  C(85)  C(83)  C(82) AND 
CONT  C(74)  C(75)  C(77)  C(79) AND 
CONT  C(79)  C(77)  C(75)  C(74) AND 
CONT  C(74)  C(76)  C(78)  C(80) AND 
CONT  C(80)  C(78)  C(76)  C(74) AND 
CONT  C(69)  C(70)  C(71)  C(72) AND 
CONT  C(72)  C(71)  C(70)  C(69) AND 
CONT  C(97)  C(98)  C(99)  C(72) AND 
CONT  C(72)  C(99)  C(98)  C(97) 
SIMU 0.01 C(96)  C(93)  C(91)  C(90) AND 
CONT  C(90)  C(91)  C(93)  C(96) AND 
CONT  C(95)  C(94)  C(92)  C(90) AND 
CONT  C(90)  C(92)  C(94)  C(95) AND 
CONT  C(82)  C(84)  C(86)  C(87) AND 
CONT  C(87)  C(86)  C(84)  C(82) AND 
CONT  C(82)  C(83)  C(85)  C(88) AND 
CONT  C(88)  C(85)  C(83)  C(82) AND 
CONT  C(74)  C(75)  C(77)  C(79) AND 
CONT  C(79)  C(77)  C(75)  C(74) AND 
CONT  C(74)  C(76)  C(78)  C(80) AND 
CONT  C(80)  C(78)  C(76)  C(74) AND 
CONT  C(69)  C(70)  C(71)  C(72) AND 
CONT  C(72)  C(71)  C(70)  C(69) AND 
CONT  C(97)  C(98)  C(99)  C(72) AND 
CONT  C(72)  C(99)  C(98)  C(97) 
END                                                                             
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 192 44 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 1006578'
