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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
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# Crystallographic Data Centre (CCDC).
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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data_cx0580
_database_code_depnum_ccdc_archive 'CCDC 1469900'
_audit_update_record             
;
2016-03-21 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_audit_creation_date             2016-02-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H18 O3 P S2, Na, 1.5(H2 O)'
_chemical_formula_sum            'C16 H21 Na O4.50 P S2'
_chemical_formula_weight         403.41
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   29.3940(10)
_cell_length_b                   5.6190(2)
_cell_length_c                   25.1528(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.918(2)
_cell_angle_gamma                90
_cell_volume                     4014.3(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.103
_cell_measurement_theta_min      3.568
_shelx_estimated_absorpt_T_max   0.917
_shelx_estimated_absorpt_T_min   0.374
_exptl_absorpt_coefficient_mu    3.543
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0949 before and 0.0519 after correction.
The Ratio of minimum to maximum transmission is 0.7757.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1688
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.025
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27769
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.207
_diffrn_reflns_theta_min         1.555
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   microsource
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6102
_reflns_number_total             6828
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.746
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0532
_refine_ls_restrained_S_all      6.255
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0730P)²+8.0227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1449
_refine_special_details          
'Distance restraints were imposed on the disordered oxygen atoms and refined hydrogen atoms. Rigid bond restraints were imposed on the displacement parameters as well as restraints on similar amplitudes separated by less than 1.7 Ang. on the disordered oxygen atoms.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1S-H1SB = O1S-H1SA
 0.87 with sigma of 0.01
 O2S-H2SA \\sim O2S-H2SB
 with sigma of 0.01
 H2SA-H2SB \\sim H1SA-H1SB \\sim H3SA-H3SB
 with sigma of 0.001
 O2S-H2SA \\sim O2S-H2SB \\sim O1S-H1SA \\sim O1S-H1SB \\sim O3S-H3SA \\sim
O3S-H3SB
 with sigma of 0.01
 S2A-O2A \\sim S2A-O2B \\sim S2A-O1A \\sim S2A-O1B \\sim S2A-O3A \\sim S2A-O3B
 with sigma of 0.01
3. Rigid bond restraints
 O3B, O3A, O1B, O1A, O2B, O2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3B \\sim O3A \\sim O1B \\sim O1A \\sim O2B \\sim O2A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O1B)=Sof(O3B)=Sof(O2B)=1-FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=FVAR(1)
6.a Free rotating group:
 H1SA(H1SB), H3SA(H3SB)
6.b Secondary CH2 refined with riding coordinates:
 C12(H12C,H12D), C14(H14C,H14D), C15(H15C,H15D), C16(H16A,H16B), C12A(H12A,
 H12B), C13A(H13A,H13B), C14A(H14A,H14B), C15A(H15A,H15B)
6.c Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C13(H13), C2A(H2A), C3A(H3A), C4(H4), C4A(H4A), C5A(H5A), C6A(H6A),
 C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.27848(2) 0.41055(13) 0.31571(3) 0.02201(19) Uani 1 1 d . . . . .
S2 S 0.39645(3) 0.85221(14) 0.29415(3) 0.0255(2) Uani 1 1 d . . . . .
P1 P 0.14672(2) 0.81135(13) 0.29721(3) 0.01555(18) Uani 1 1 d . . . . .
O1 O 0.37374(10) 0.9771(6) 0.24434(13) 0.0547(8) Uani 1 1 d . . . . .
O2 O 0.42346(8) 0.6484(4) 0.28434(9) 0.0261(5) Uani 1 1 d . . . . .
O3 O 0.42485(8) 1.0107(4) 0.33744(11) 0.0357(6) Uani 1 1 d . . . . .
C00R C 0.14448(11) 0.9318(6) 0.18899(12) 0.0219(6) Uani 1 1 d . . . . .
H00R H 0.1609 1.0703 0.2051 0.026 Uiso 1 1 calc R . . . .
C1 C 0.09382(10) 0.6862(5) 0.31239(11) 0.0153(6) Uani 1 1 d . . . . .
C2 C 0.05354(10) 0.8282(5) 0.29677(11) 0.0182(6) Uani 1 1 d . . . . .
H2 H 0.0552 0.9779 0.2798 0.022 Uiso 1 1 calc R . . . .
C3 C 0.01122(10) 0.7537(6) 0.30561(12) 0.0212(6) Uani 1 1 d . . . . .
H3 H -0.0159 0.8518 0.2947 0.025 Uiso 1 1 calc R . . . .
C5 C 0.04804(11) 0.3941(5) 0.34664(12) 0.0208(6) Uani 1 1 d . . . . .
H5 H 0.0462 0.2459 0.3641 0.025 Uiso 1 1 calc R . . . .
C6 C 0.09070(10) 0.4675(5) 0.33746(11) 0.0184(6) Uani 1 1 d . . . . .
H6 H 0.1177 0.3683 0.3483 0.022 Uiso 1 1 calc R . . . .
C7 C 0.13158(9) 0.7621(5) 0.22227(11) 0.0158(6) Uani 1 1 d . . . . .
C8 C 0.10782(10) 0.5588(5) 0.19778(12) 0.0202(6) Uani 1 1 d . . . . .
H8 H 0.0994 0.4392 0.2202 0.024 Uiso 1 1 calc R . . . .
C9 C 0.00834(10) 0.5363(6) 0.33041(12) 0.0220(6) Uani 1 1 d . . . . .
H9 H -0.0208 0.4846 0.3363 0.026 Uiso 1 1 calc R . . . .
C10 C 0.10930(11) 0.7013(6) 0.10830(12) 0.0240(7) Uani 1 1 d . . . . .
H10 H 0.1014 0.6812 0.0695 0.029 Uiso 1 1 calc R . . . .
C11 C 0.13352(12) 0.9013(6) 0.13177(13) 0.0277(7) Uani 1 1 d . . . . .
H11 H 0.1428 1.0180 0.1093 0.033 Uiso 1 1 calc R . . . .
C12 C 0.19149(10) 0.5751(5) 0.31941(12) 0.0190(6) Uani 1 1 d . . . . .
H12C H 0.1986 0.5534 0.3598 0.023 Uiso 1 1 calc R . . . .
H12D H 0.1796 0.4224 0.3015 0.023 Uiso 1 1 calc R . . . .
C13 C 0.09640(10) 0.5294(6) 0.14125(12) 0.0224(6) Uani 1 1 d . . . . .
H13 H 0.0797 0.3917 0.1250 0.027 Uiso 1 1 calc R . . . .
C14 C 0.32354(10) 0.5375(6) 0.28668(13) 0.0232(6) Uani 1 1 d . . . . .
H14C H 0.3459 0.4106 0.2829 0.028 Uiso 1 1 calc R . . . .
H14D H 0.3086 0.5989 0.2494 0.028 Uiso 1 1 calc R . . . .
C15 C 0.35080(10) 0.7387(6) 0.32152(12) 0.0212(6) Uani 1 1 d . . . . .
H15C H 0.3646 0.6795 0.3593 0.025 Uiso 1 1 calc R . . . .
H15D H 0.3288 0.8692 0.3238 0.025 Uiso 1 1 calc R . . . .
C16 C 0.23594(10) 0.6510(5) 0.30281(12) 0.0204(6) Uani 1 1 d . . . . .
H16A H 0.2498 0.7932 0.3242 0.024 Uiso 1 1 calc R . . . .
H16B H 0.2277 0.6932 0.2633 0.024 Uiso 1 1 calc R . . . .
S1A S 0.30867(3) -0.08659(14) 0.44750(4) 0.0273(2) Uani 1 1 d . . . . .
S2A S 0.43300(2) 0.36481(13) 0.46107(3) 0.02290(19) Uani 1 1 d D . . . .
P1A P 0.19142(3) 0.33592(13) 0.47768(3) 0.01697(18) Uani 1 1 d . . . . .
O1A O 0.42762(11) 0.5040(6) 0.50973(11) 0.0375(10) Uani 0.842(7) 1 d D U P A 1
O2A O 0.4418(3) 0.5188(8) 0.4189(2) 0.0237(13) Uani 0.842(7) 1 d D U P A 1
O3A O 0.46601(10) 0.1750(5) 0.47845(16) 0.0325(9) Uani 0.842(7) 1 d D U P A 1
C1A C 0.13401(10) 0.1973(5) 0.47304(11) 0.0166(6) Uani 1 1 d . . . . .
C2A C 0.11989(10) -0.0220(5) 0.44820(11) 0.0180(6) Uani 1 1 d . . . . .
H2A H 0.1416 -0.1158 0.4351 0.022 Uiso 1 1 calc R . . . .
C3A C 0.07434(10) -0.1039(5) 0.44259(11) 0.0195(6) Uani 1 1 d . . . . .
H3A H 0.0649 -0.2521 0.4250 0.023 Uiso 1 1 calc R . . . .
C4 C 0.20893(11) 0.1451(6) 0.58594(13) 0.0231(6) Uani 1 1 d . . . . .
H4 H 0.1893 0.0156 0.5700 0.028 Uiso 1 1 calc R . . . .
C4A C 0.04255(10) 0.0292(6) 0.46243(12) 0.0222(6) Uani 1 1 d . . . . .
H4A H 0.0114 -0.0273 0.4585 0.027 Uiso 1 1 calc R . . . .
C5A C 0.05657(10) 0.2463(6) 0.48820(12) 0.0225(6) Uani 1 1 d . . . . .
H5A H 0.0351 0.3370 0.5025 0.027 Uiso 1 1 calc R . . . .
C6A C 0.10171(11) 0.3298(5) 0.49299(12) 0.0194(6) Uani 1 1 d . . . . .
H6A H 0.1109 0.4792 0.5101 0.023 Uiso 1 1 calc R . . . .
C7A C 0.21707(10) 0.3280(5) 0.55265(12) 0.0180(6) Uani 1 1 d . . . . .
C8A C 0.24606(11) 0.5157(6) 0.57661(13) 0.0261(7) Uani 1 1 d . . . . .
H8A H 0.2517 0.6429 0.5543 0.031 Uiso 1 1 calc R . . . .
C9A C 0.26682(12) 0.5190(6) 0.63290(14) 0.0312(8) Uani 1 1 d . . . . .
H9A H 0.2869 0.6469 0.6488 0.037 Uiso 1 1 calc R . . . .
C10A C 0.25827(12) 0.3367(7) 0.66565(13) 0.0310(8) Uani 1 1 d . . . . .
H10A H 0.2723 0.3397 0.7041 0.037 Uiso 1 1 calc R . . . .
C11A C 0.22915(12) 0.1485(6) 0.64260(13) 0.0280(7) Uani 1 1 d . . . . .
H11A H 0.2231 0.0233 0.6652 0.034 Uiso 1 1 calc R . . . .
C12A C 0.22413(10) 0.0892(5) 0.45552(12) 0.0196(6) Uani 1 1 d . . . . .
H12A H 0.2216 -0.0563 0.4768 0.023 Uiso 1 1 calc R . . . .
H12B H 0.2104 0.0548 0.4160 0.023 Uiso 1 1 calc R . . . .
C13A C 0.27549(11) 0.1593(6) 0.46494(13) 0.0242(7) Uani 1 1 d . . . . .
H13A H 0.2886 0.2036 0.5040 0.029 Uiso 1 1 calc R . . . .
H13B H 0.2781 0.2990 0.4419 0.029 Uiso 1 1 calc R . . . .
C14A C 0.36748(10) 0.0346(6) 0.47073(14) 0.0258(7) Uani 1 1 d . . . . .
H14A H 0.3723 0.0939 0.5088 0.031 Uiso 1 1 calc R . . . .
H14B H 0.3906 -0.0940 0.4713 0.031 Uiso 1 1 calc R . . . .
C15A C 0.37674(10) 0.2361(5) 0.43464(12) 0.0196(6) Uani 1 1 d . . . . .
H15A H 0.3523 0.3601 0.4318 0.023 Uiso 1 1 calc R . . . .
H15B H 0.3744 0.1744 0.3972 0.023 Uiso 1 1 calc R . . . .
Na1 Na 0.49050(5) 0.8642(3) 0.42643(6) 0.0382(4) Uani 1 1 d . . . . .
Na2 Na 0.47004(4) 0.3620(2) 0.34114(5) 0.0268(3) Uani 1 1 d . . . . .
O1S O 0.53506(10) 0.1904(6) 0.40749(14) 0.0521(8) Uani 1 1 d D . . . .
H1SA H 0.5345 0.2812 0.4381 0.078 Uiso 1 1 d D . . . .
H1SB H 0.5535 0.1391 0.3848 0.078 Uiso 1 1 d DG . . . .
O2S O 0.52239(12) 0.7063(7) 0.3552(3) 0.0964(16) Uani 1 1 d D . . . .
H2SA H 0.5235(16) 0.595(8) 0.3842(15) 0.145 Uiso 1 1 d DR . . . .
H2SB H 0.5455(12) 0.751(10) 0.3366(16) 0.145 Uiso 1 1 d DR . . . .
O3S O 0.50726(18) 0.1709(11) 0.2805(2) 0.118(2) Uani 1 1 d D . . . .
H3SA H 0.4932 0.3093 0.2622 0.177 Uiso 1 1 d D . . . .
H3SB H 0.5347 0.1720 0.2677 0.177 Uiso 1 1 d DG . . . .
O1B O 0.4518(5) 0.364(3) 0.5191(3) 0.030(4) Uani 0.158(7) 1 d D U P A 2
O3B O 0.4609(5) 0.183(3) 0.4407(10) 0.046(5) Uani 0.158(7) 1 d D U P A 2
O2B O 0.4363(15) 0.576(3) 0.4290(13) 0.021(6) Uani 0.158(7) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C14 1.815(3) . ?
S1 C16 1.813(3) . ?
S2 O1 1.441(3) . ?
S2 O2 1.450(2) . ?
S2 O3 1.486(3) . ?
S2 C15 1.777(3) . ?
P1 C1 1.834(3) . ?
P1 C7 1.843(3) . ?
P1 C12 1.851(3) . ?
C00R H00R 0.9500 . ?
C00R C7 1.384(4) . ?
C00R C11 1.402(4) . ?
C1 C2 1.398(4) . ?
C1 C6 1.395(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(4) . ?
C3 H3 0.9500 . ?
C3 C9 1.384(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(4) . ?
C5 C9 1.386(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(4) . ?
C8 H8 0.9500 . ?
C8 C13 1.384(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.379(5) . ?
C10 C13 1.388(4) . ?
C11 H11 0.9500 . ?
C12 H12C 0.9900 . ?
C12 H12D 0.9900 . ?
C12 C16 1.531(4) . ?
C13 H13 0.9500 . ?
C14 H14C 0.9900 . ?
C14 H14D 0.9900 . ?
C14 C15 1.525(4) . ?
C15 H15C 0.9900 . ?
C15 H15D 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
S1A C13A 1.809(3) . ?
S1A C14A 1.809(3) . ?
S2A O1A 1.495(3) . ?
S2A O2A 1.443(3) . ?
S2A O3A 1.432(3) . ?
S2A C15A 1.770(3) . ?
S2A O1B 1.422(7) . ?
S2A O3B 1.480(8) . ?
S2A O2B 1.451(8) . ?
P1A C1A 1.835(3) . ?
P1A C7A 1.842(3) . ?
P1A C12A 1.853(3) . ?
C1A C2A 1.395(4) . ?
C1A C6A 1.398(4) . ?
C2A H2A 0.9500 . ?
C2A C3A 1.388(4) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.386(4) . ?
C4 H4 0.9500 . ?
C4 C7A 1.385(4) . ?
C4 C11A 1.396(5) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.393(5) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.383(4) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.392(4) . ?
C8A H8A 0.9500 . ?
C8A C9A 1.390(5) . ?
C9A H9A 0.9500 . ?
C9A C10A 1.377(5) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.390(5) . ?
C11A H11A 0.9500 . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C12A C13A 1.519(4) . ?
C13A H13A 0.9900 . ?
C13A H13B 0.9900 . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C14A C15A 1.519(4) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
Na1 H2SA 2.21(5) . ?
Na2 H2SA 2.11(5) . ?
Na2 H3SA 2.28(10) . ?
O1S H1SA 0.928(7) . ?
O1S H1SB 0.9282 . ?
O2S H2SA 0.956(10) . ?
O2S H2SB 0.953(10) . ?
O3S H3SA 0.944(10) . ?
O3S H3SB 0.9425 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 S1 C14 100.16(14) . . ?
O1 S2 O2 112.83(17) . . ?
O1 S2 O3 113.09(18) . . ?
O1 S2 C15 106.54(16) . . ?
O2 S2 O3 111.65(14) . . ?
O2 S2 C15 106.47(14) . . ?
O3 S2 C15 105.62(14) . . ?
C1 P1 C7 99.26(12) . . ?
C1 P1 C12 103.72(13) . . ?
C7 P1 C12 99.59(13) . . ?
C7 C00R H00R 119.7 . . ?
C7 C00R C11 120.7(3) . . ?
C11 C00R H00R 119.7 . . ?
C2 C1 P1 115.1(2) . . ?
C6 C1 P1 126.2(2) . . ?
C6 C1 C2 118.7(3) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 120.0 . . ?
C9 C3 C2 120.1(3) . . ?
C9 C3 H3 120.0 . . ?
C6 C5 H5 119.8 . . ?
C9 C5 H5 119.8 . . ?
C9 C5 C6 120.4(3) . . ?
C1 C6 C5 120.1(3) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C00R C7 P1 118.9(2) . . ?
C00R C7 C8 118.7(3) . . ?
C8 C7 P1 122.4(2) . . ?
C7 C8 H8 119.6 . . ?
C13 C8 C7 120.8(3) . . ?
C13 C8 H8 119.6 . . ?
C3 C9 C5 119.8(3) . . ?
C3 C9 H9 120.1 . . ?
C5 C9 H9 120.1 . . ?
C11 C10 H10 119.9 . . ?
C11 C10 C13 120.1(3) . . ?
C13 C10 H10 119.9 . . ?
C00R C11 H11 120.1 . . ?
C10 C11 C00R 119.7(3) . . ?
C10 C11 H11 120.1 . . ?
P1 C12 H12C 110.1 . . ?
P1 C12 H12D 110.1 . . ?
H12C C12 H12D 108.4 . . ?
C16 C12 P1 108.0(2) . . ?
C16 C12 H12C 110.1 . . ?
C16 C12 H12D 110.1 . . ?
C8 C13 C10 120.0(3) . . ?
C8 C13 H13 120.0 . . ?
C10 C13 H13 120.0 . . ?
S1 C14 H14C 109.0 . . ?
S1 C14 H14D 109.0 . . ?
H14C C14 H14D 107.8 . . ?
C15 C14 S1 113.0(2) . . ?
C15 C14 H14C 109.0 . . ?
C15 C14 H14D 109.0 . . ?
S2 C15 H15C 109.1 . . ?
S2 C15 H15D 109.1 . . ?
C14 C15 S2 112.4(2) . . ?
C14 C15 H15C 109.1 . . ?
C14 C15 H15D 109.1 . . ?
H15C C15 H15D 107.9 . . ?
S1 C16 H16A 109.7 . . ?
S1 C16 H16B 109.7 . . ?
C12 C16 S1 110.0(2) . . ?
C12 C16 H16A 109.7 . . ?
C12 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
C13A S1A C14A 99.44(15) . . ?
O1A S2A C15A 103.63(16) . . ?
O2A S2A O1A 111.4(3) . . ?
O2A S2A C15A 107.2(3) . . ?
O3A S2A O1A 110.2(2) . . ?
O3A S2A O2A 115.8(3) . . ?
O3A S2A C15A 107.71(16) . . ?
O1B S2A C15A 117.6(6) . . ?
O1B S2A O3B 104.5(11) . . ?
O1B S2A O2B 120.6(17) . . ?
O3B S2A C15A 97.8(6) . . ?
O2B S2A C15A 108.4(18) . . ?
O2B S2A O3B 104.4(14) . . ?
C1A P1A C7A 100.49(13) . . ?
C1A P1A C12A 101.72(13) . . ?
C7A P1A C12A 100.51(13) . . ?
C2A C1A P1A 124.5(2) . . ?
C2A C1A C6A 118.7(3) . . ?
C6A C1A P1A 116.7(2) . . ?
C1A C2A H2A 119.8 . . ?
C3A C2A C1A 120.4(3) . . ?
C3A C2A H2A 119.8 . . ?
C2A C3A H3A 119.8 . . ?
C4A C3A C2A 120.4(3) . . ?
C4A C3A H3A 119.8 . . ?
C7A C4 H4 119.6 . . ?
C7A C4 C11A 120.9(3) . . ?
C11A C4 H4 119.6 . . ?
C3A C4A H4A 120.2 . . ?
C3A C4A C5A 119.6(3) . . ?
C5A C4A H4A 120.2 . . ?
C4A C5A H5A 120.0 . . ?
C6A C5A C4A 120.0(3) . . ?
C6A C5A H5A 120.0 . . ?
C1A C6A H6A 119.6 . . ?
C5A C6A C1A 120.9(3) . . ?
C5A C6A H6A 119.6 . . ?
C4 C7A P1A 123.2(2) . . ?
C4 C7A C8A 118.8(3) . . ?
C8A C7A P1A 117.9(2) . . ?
C7A C8A H8A 119.7 . . ?
C9A C8A C7A 120.7(3) . . ?
C9A C8A H8A 119.7 . . ?
C8A C9A H9A 120.0 . . ?
C10A C9A C8A 120.0(3) . . ?
C10A C9A H9A 120.0 . . ?
C9A C10A H10A 119.9 . . ?
C9A C10A C11A 120.3(3) . . ?
C11A C10A H10A 119.9 . . ?
C4 C11A H11A 120.3 . . ?
C10A C11A C4 119.4(3) . . ?
C10A C11A H11A 120.3 . . ?
P1A C12A H12A 109.8 . . ?
P1A C12A H12B 109.8 . . ?
H12A C12A H12B 108.3 . . ?
C13A C12A P1A 109.3(2) . . ?
C13A C12A H12A 109.8 . . ?
C13A C12A H12B 109.8 . . ?
S1A C13A H13A 109.7 . . ?
S1A C13A H13B 109.7 . . ?
C12A C13A S1A 109.9(2) . . ?
C12A C13A H13A 109.7 . . ?
C12A C13A H13B 109.7 . . ?
H13A C13A H13B 108.2 . . ?
S1A C14A H14A 109.0 . . ?
S1A C14A H14B 109.0 . . ?
H14A C14A H14B 107.8 . . ?
C15A C14A S1A 113.0(2) . . ?
C15A C14A H14A 109.0 . . ?
C15A C14A H14B 109.0 . . ?
S2A C15A H15A 109.2 . . ?
S2A C15A H15B 109.2 . . ?
C14A C15A S2A 112.0(2) . . ?
C14A C15A H15A 109.2 . . ?
C14A C15A H15B 109.2 . . ?
H15A C15A H15B 107.9 . . ?
H2SA Na2 H3SA 100(3) . . ?
H1SA O1S H1SB 145.0 . . ?
H2SA O2S H2SB 131(2) . . ?
H3SA O3S H3SB 97.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1SA O1A 0.928(7) 1.91(3) 2.704(4) 142(4) 3_666

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C14 C15 S2 177.41(15) . . . . ?
P1 C1 C2 C3 179.6(2) . . . . ?
P1 C1 C6 C5 179.9(2) . . . . ?
P1 C7 C8 C13 179.0(2) . . . . ?
P1 C12 C16 S1 -172.90(14) . . . . ?
O1 S2 C15 C14 69.9(3) . . . . ?
O2 S2 C15 C14 -50.7(2) . . . . ?
O3 S2 C15 C14 -169.5(2) . . . . ?
C00R C7 C8 C13 -1.4(4) . . . . ?
C1 P1 C7 C00R 143.1(2) . . . . ?
C1 P1 C7 C8 -37.4(3) . . . . ?
C1 P1 C12 C16 174.05(19) . . . . ?
C1 C2 C3 C9 0.2(4) . . . . ?
C2 C1 C6 C5 -0.1(4) . . . . ?
C2 C3 C9 C5 0.4(4) . . . . ?
C6 C1 C2 C3 -0.4(4) . . . . ?
C6 C5 C9 C3 -0.9(4) . . . . ?
C7 P1 C1 C2 -74.8(2) . . . . ?
C7 P1 C1 C6 105.2(2) . . . . ?
C7 P1 C12 C16 72.0(2) . . . . ?
C7 C00R C11 C10 0.6(5) . . . . ?
C7 C8 C13 C10 1.1(5) . . . . ?
C9 C5 C6 C1 0.7(4) . . . . ?
C11 C00R C7 P1 -179.8(2) . . . . ?
C11 C00R C7 C8 0.6(4) . . . . ?
C11 C10 C13 C8 0.1(5) . . . . ?
C12 P1 C1 C2 -177.1(2) . . . . ?
C12 P1 C1 C6 2.8(3) . . . . ?
C12 P1 C7 C00R -111.2(2) . . . . ?
C12 P1 C7 C8 68.4(3) . . . . ?
C13 C10 C11 C00R -0.9(5) . . . . ?
C14 S1 C16 C12 174.8(2) . . . . ?
C16 S1 C14 C15 71.9(2) . . . . ?
S1A C14A C15A S2A 175.85(16) . . . . ?
P1A C1A C2A C3A -174.6(2) . . . . ?
P1A C1A C6A C5A 176.0(2) . . . . ?
P1A C7A C8A C9A -179.4(3) . . . . ?
P1A C12A C13A S1A 176.49(15) . . . . ?
O1A S2A C15A C14A -73.2(3) . . . . ?
O2A S2A C15A C14A 168.9(3) . . . . ?
O3A S2A C15A C14A 43.6(3) . . . . ?
C1A P1A C7A C4 34.8(3) . . . . ?
C1A P1A C7A C8A -145.3(2) . . . . ?
C1A P1A C12A C13A -171.5(2) . . . . ?
C1A C2A C3A C4A -1.1(4) . . . . ?
C2A C1A C6A C5A -0.2(4) . . . . ?
C2A C3A C4A C5A -0.1(4) . . . . ?
C3A C4A C5A C6A 1.1(4) . . . . ?
C4 C7A C8A C9A 0.5(5) . . . . ?
C4A C5A C6A C1A -1.0(4) . . . . ?
C6A C1A C2A C3A 1.2(4) . . . . ?
C7A P1A C1A C2A -114.0(2) . . . . ?
C7A P1A C1A C6A 70.0(2) . . . . ?
C7A P1A C12A C13A -68.4(2) . . . . ?
C7A C4 C11A C10A -0.8(5) . . . . ?
C7A C8A C9A C10A -0.9(5) . . . . ?
C8A C9A C10A C11A 0.4(5) . . . . ?
C9A C10A C11A C4 0.4(5) . . . . ?
C11A C4 C7A P1A -179.8(2) . . . . ?
C11A C4 C7A C8A 0.3(4) . . . . ?
C12A P1A C1A C2A -10.8(3) . . . . ?
C12A P1A C1A C6A 173.2(2) . . . . ?
C12A P1A C7A C4 -69.4(3) . . . . ?
C12A P1A C7A C8A 110.5(2) . . . . ?
C13A S1A C14A C15A -70.9(3) . . . . ?
C14A S1A C13A C12A -173.2(2) . . . . ?
O1B S2A C15A C14A -30.7(9) . . . . ?
O3B S2A C15A C14A 80.1(10) . . . . ?
O2B S2A C15A C14A -171.8(12) . . . . ?

_smtbx_masks_special_details     
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 340.4 Ang³ [8.5%]
Total electron count / cell = 78.5
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.358 -0.593 0.615 85.1 19.7 ?
2 0.358 -0.810 0.115 85.1 19.7 ?
3 0.642 -0.461 0.385 85.1 19.5 ?
4 0.642 -0.982 0.885 85.1 19.5 ?

_olex2_date_sample_data_collection 2015-10-12
_olex2_date_sample_submission    2015-10-09
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx0580
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cx0040a
_database_code_depnum_ccdc_archive 'CCDC 1469901'
_audit_update_record             
;
2016-03-21 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_audit_creation_date             2014-09-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C44 H46 N4 O3 P S), C H2 Cl2, 2(H2 O)'
_chemical_formula_sum            'C89 H98 Cl2 N8 O8 P2 S2'
_chemical_formula_weight         1604.71
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   48.8875(19)
_cell_length_b                   6.1721(2)
_cell_length_c                   13.7803(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.831(3)
_cell_angle_gamma                90
_cell_volume                     4037.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.073
_cell_measurement_theta_min      3.303
_shelx_estimated_absorpt_T_max   0.977
_shelx_estimated_absorpt_T_min   0.803
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0655 before and 0.0436 after correction.
The Ratio of minimum to maximum transmission is 0.8440.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15230
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.137
_diffrn_reflns_theta_min         3.303
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   microsource
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.883
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                6308
_reflns_number_total             6673
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 
;
 Flack x determined using 2613 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.019(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         6673
_refine_ls_number_restraints     251
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0488
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0754P)²+7.7088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1311
_refine_special_details          
'Rigid bond restraints were imposed on the displacement parameters as well as restraints on similar amplitudes separated by less than 1.7 Ang. on the disordered phenyl rings.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 C2, C3, C4, C5, C6, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C9, C10, C11, C12, C8A, C9A, C10A, C11A, C12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C2A \\sim C3A \\sim C4A \\sim C5A
\\sim C6A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C8A \\sim C9A \\sim C10A \\sim
C11A \\sim C12A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Sof(C2A)=Sof(H2AA)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4AA)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4A)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(H6)=FVAR(1)
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=
 Sof(C12A)=Sof(H12A)=1-FVAR(2)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=
 Sof(H12)=FVAR(2)
 Fixed Sof: H1SA(0.5) H1SB(0.5)
5.a Free rotating group:
 O1S(H1SC,H1SD)
5.b Ternary CH refined with riding coordinates:
 N4(H4), C25(H25), C36(H36), C38(H38), C42(H42)
5.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,
 H40B), C41(H41A,H41B), C43(H43A,H43B), C1S(H1SA,H1SB)
5.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C3(H3), C4(H4A), C5(H5), C6(H6), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C16(H16), C17(H17), C19(H19), C20(H20), C27(H27),
  C28(H28), C30(H30), C31(H31), C33(H33), C2A(H2AA), C3A(H3A), C4A(H4AA),
 C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A)
5.e Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.56946(2) 0.3372(2) 0.03066(9) 0.0291(3) Uani 1 1 d . . . . .
P1 P 0.56525(3) -0.1216(3) 0.27792(10) 0.0356(4) Uani 1 1 d . . . . .
O1 O 0.69953(6) 0.8248(5) 0.1158(2) 0.0145(6) Uani 1 1 d . . . . .
O2 O 0.76273(6) 0.8012(5) 0.2530(2) 0.0156(6) Uani 1 1 d . . . . .
O3 O 0.84836(7) 0.9193(5) 0.5264(2) 0.0215(7) Uani 1 1 d . . . . .
N1 N 0.69513(7) 0.2841(5) 0.1236(2) 0.0120(7) Uani 1 1 d . . . . .
H1 H 0.7018 0.1542 0.1163 0.014 Uiso 1 1 calc R . . . .
N2 N 0.75973(7) 0.2734(5) 0.2555(2) 0.0112(7) Uani 1 1 d . . . . .
H2 H 0.7541 0.1379 0.2472 0.013 Uiso 1 1 calc R . . . .
N4 N 0.80452(8) 0.2204(6) 0.1632(2) 0.0130(7) Uani 1 1 d . . . . .
H4 H 0.7849 0.1755 0.1290 0.016 Uiso 1 1 calc R . . . .
N28 N 0.79416(8) 0.1996(6) 0.6299(3) 0.0187(8) Uani 1 1 d . . . . .
C1 C 0.56897(11) -0.0224(9) 0.4060(4) 0.0305(12) Uani 1 1 d . . . . .
C2 C 0.5910(2) 0.1053(15) 0.4506(6) 0.040(2) Uani 0.739(11) 1 d . U . A 1
H2A H 0.6043 0.1468 0.4135 0.047 Uiso 0.739(11) 1 calc R . . A 1
C3 C 0.5950(2) 0.1769(17) 0.5477(6) 0.046(2) Uani 0.739(11) 1 d . U . A 1
H3 H 0.6103 0.2705 0.5756 0.055 Uiso 0.739(11) 1 calc R . . A 1
C4 C 0.5769(4) 0.113(4) 0.6034(19) 0.043(3) Uani 0.739(11) 1 d . U . A 1
H4A H 0.5792 0.1691 0.6691 0.052 Uiso 0.739(11) 1 calc R . . A 1
C5 C 0.5553(2) -0.0310(19) 0.5669(7) 0.045(2) Uani 0.739(11) 1 d . U . A 1
H5 H 0.5431 -0.0779 0.6071 0.054 Uiso 0.739(11) 1 calc R . . A 1
C6 C 0.5519(2) -0.1058(18) 0.4682(6) 0.043(2) Uani 0.739(11) 1 d . U . A 1
H6 H 0.5380 -0.2128 0.4426 0.051 Uiso 0.739(11) 1 calc R . . A 1
C7 C 0.52716(12) -0.1300(10) 0.2317(4) 0.0359(13) Uani 1 1 d . . . . .
C8 C 0.5105(9) 0.072(6) 0.252(3) 0.037(5) Uani 0.416(18) 1 d . U . B 1
H8 H 0.5202 0.1857 0.2928 0.044 Uiso 0.416(18) 1 calc R . . B 1
C9 C 0.4816(5) 0.091(4) 0.2107(17) 0.040(4) Uani 0.416(18) 1 d . U . B 1
H9 H 0.4718 0.2202 0.2191 0.048 Uiso 0.416(18) 1 calc R . . B 1
C10 C 0.4678(5) -0.078(4) 0.1588(17) 0.047(4) Uani 0.416(18) 1 d . U . B 1
H10 H 0.4482 -0.0622 0.1300 0.056 Uiso 0.416(18) 1 calc R . . B 1
C11 C 0.4795(5) -0.260(4) 0.1458(18) 0.045(4) Uani 0.416(18) 1 d . U . B 1
H11 H 0.4685 -0.3766 0.1117 0.054 Uiso 0.416(18) 1 calc R . . B 1
C12 C 0.5092(5) -0.284(4) 0.1835(18) 0.046(4) Uani 0.416(18) 1 d . U . B 1
H12 H 0.5172 -0.4208 0.1739 0.056 Uiso 0.416(18) 1 calc R . . B 1
C13 C 0.57263(11) 0.1282(10) 0.2138(4) 0.0316(12) Uani 1 1 d . . . . .
H13A H 0.5634 0.2535 0.2376 0.038 Uiso 1 1 calc R . . . .
H13B H 0.5932 0.1553 0.2301 0.038 Uiso 1 1 calc R . . . .
C14 C 0.56163(10) 0.1043(10) 0.1003(4) 0.0286(12) Uani 1 1 d . . . . .
H14A H 0.5410 0.0827 0.0847 0.034 Uiso 1 1 calc R . . . .
H14B H 0.5701 -0.0266 0.0780 0.034 Uiso 1 1 calc R . . . .
C15 C 0.60675(9) 0.3250(8) 0.0568(3) 0.0193(9) Uani 1 1 d . . . . .
C16 C 0.62039(9) 0.1424(7) 0.0333(3) 0.0168(9) Uani 1 1 d . . . . .
H16 H 0.6096 0.0224 0.0024 0.020 Uiso 1 1 calc R . . . .
C17 C 0.64955(9) 0.1318(7) 0.0541(3) 0.0135(8) Uani 1 1 d . . . . .
H17 H 0.6585 0.0045 0.0382 0.016 Uiso 1 1 calc R . . . .
C18 C 0.66581(9) 0.3081(7) 0.0983(3) 0.0112(8) Uani 1 1 d . . . . .
C19 C 0.65217(9) 0.4935(7) 0.1207(3) 0.0159(9) Uani 1 1 d . . . . .
H19 H 0.6629 0.6152 0.1499 0.019 Uiso 1 1 calc R . . . .
C20 C 0.62303(9) 0.5013(8) 0.1005(3) 0.0188(9) Uani 1 1 d . . . . .
H20 H 0.6140 0.6281 0.1166 0.023 Uiso 1 1 calc R . . . .
C21 C 0.71417(9) 0.4414(6) 0.1581(3) 0.0103(8) Uani 1 1 d . . . . .
C22 C 0.71521(9) 0.6780(7) 0.1539(3) 0.0106(8) Uani 1 1 d . . . . .
C23 C 0.74472(9) 0.6683(7) 0.2165(3) 0.0118(8) Uani 1 1 d . . . . .
C24 C 0.74233(9) 0.4301(6) 0.2153(3) 0.0107(8) Uani 1 1 d . . . . .
C25 C 0.78848(8) 0.3212(7) 0.3141(3) 0.0105(8) Uani 1 1 d . . . . .
H25 H 0.7925 0.4776 0.3045 0.013 Uiso 1 1 calc R . . . .
C26 C 0.79079(8) 0.2833(6) 0.4253(3) 0.0110(8) Uani 1 1 d . . . . .
C27 C 0.77825(9) 0.1062(7) 0.4562(3) 0.0145(9) Uani 1 1 d . . . . .
H27 H 0.7681 0.0065 0.4084 0.017 Uiso 1 1 calc R . . . .
C28 C 0.78035(9) 0.0718(7) 0.5583(3) 0.0172(9) Uani 1 1 d . . . . .
H28 H 0.7712 -0.0517 0.5770 0.021 Uiso 1 1 calc R . . . .
C29 C 0.80705(9) 0.3775(7) 0.6013(3) 0.0148(9) Uani 1 1 d . . . . .
C30 C 0.82287(10) 0.5113(7) 0.6765(3) 0.0176(9) Uani 1 1 d . . . . .
H30 H 0.8238 0.4768 0.7445 0.021 Uiso 1 1 calc R . . . .
C31 C 0.83691(10) 0.6900(7) 0.6551(3) 0.0175(9) Uani 1 1 d . . . . .
H31 H 0.8478 0.7764 0.7074 0.021 Uiso 1 1 calc R . . . .
C32 C 0.83512(9) 0.7442(7) 0.5546(3) 0.0146(9) Uani 1 1 d . . . . .
C33 C 0.81985(9) 0.6186(7) 0.4793(3) 0.0138(8) Uani 1 1 d . . . . .
H33 H 0.8188 0.6591 0.4119 0.017 Uiso 1 1 calc R . . . .
C34 C 0.80558(9) 0.4296(7) 0.4986(3) 0.0128(8) Uani 1 1 d . . . . .
C35 C 0.86462(10) 1.0561(8) 0.6014(3) 0.0218(10) Uani 1 1 d . . . . .
H35A H 0.8725 1.1753 0.5697 0.033 Uiso 1 1 calc GR . . . .
H35B H 0.8800 0.9723 0.6435 0.033 Uiso 1 1 calc GR . . . .
H35C H 0.8526 1.1151 0.6426 0.033 Uiso 1 1 calc GR . . . .
C36 C 0.80955(9) 0.1849(7) 0.2729(3) 0.0115(8) Uani 1 1 d . . . . .
H36 H 0.8055 0.0289 0.2835 0.014 Uiso 1 1 calc R . . . .
C37 C 0.84097(9) 0.2261(7) 0.3242(3) 0.0132(9) Uani 1 1 d . . . . .
H37A H 0.8425 0.3209 0.3831 0.016 Uiso 1 1 calc R . . . .
H37B H 0.8505 0.0871 0.3470 0.016 Uiso 1 1 calc R . . . .
C38 C 0.85510(9) 0.3346(7) 0.2490(3) 0.0146(8) Uani 1 1 d . . . . .
H38 H 0.8747 0.3806 0.2827 0.018 Uiso 1 1 calc R . . . .
C39 C 0.83755(9) 0.5305(7) 0.2051(3) 0.0179(9) Uani 1 1 d . . . . .
H39A H 0.8475 0.6152 0.1631 0.022 Uiso 1 1 calc R . . . .
H39B H 0.8345 0.6254 0.2595 0.022 Uiso 1 1 calc R . . . .
C40 C 0.80906(10) 0.4501(7) 0.1415(3) 0.0172(9) Uani 1 1 d . . . . .
H40A H 0.7937 0.5392 0.1560 0.021 Uiso 1 1 calc R . . . .
H40B H 0.8087 0.4667 0.0698 0.021 Uiso 1 1 calc R . . . .
C41 C 0.82528(9) 0.0887(7) 0.1266(3) 0.0148(9) Uani 1 1 d . . . . .
H41A H 0.8199 0.0847 0.0526 0.018 Uiso 1 1 calc R . . . .
H41B H 0.8250 -0.0617 0.1512 0.018 Uiso 1 1 calc R . . . .
C42 C 0.85566(9) 0.1816(7) 0.1618(3) 0.0150(9) Uani 1 1 d . . . . .
H42 H 0.8593 0.2723 0.1061 0.018 Uiso 1 1 calc R . . . .
C43 C 0.87825(9) 0.0080(7) 0.1840(3) 0.0182(9) Uani 1 1 d . . . . .
H43A H 0.8742 -0.1012 0.1299 0.022 Uiso 1 1 calc R . . . .
H43B H 0.8775 -0.0659 0.2471 0.022 Uiso 1 1 calc R . . . .
C44 C 0.90775(11) 0.0962(9) 0.1934(5) 0.0357(13) Uani 1 1 d . . . . .
H44A H 0.9084 0.1777 0.1329 0.054 Uiso 1 1 calc GR . . . .
H44B H 0.9212 -0.0243 0.2018 0.054 Uiso 1 1 calc GR . . . .
H44C H 0.9128 0.1922 0.2516 0.054 Uiso 1 1 calc GR . . . .
C2A C 0.5760(6) 0.201(5) 0.4356(17) 0.039(4) Uani 0.261(11) 1 d . U . A 2
H2AA H 0.5790 0.3076 0.3893 0.047 Uiso 0.261(11) 1 calc R . . A 2
C3A C 0.5781(6) 0.251(5) 0.5388(17) 0.041(4) Uani 0.261(11) 1 d . U . A 2
H3A H 0.5832 0.3932 0.5632 0.049 Uiso 0.261(11) 1 calc R . . A 2
C4A C 0.5726(14) 0.090(13) 0.604(6) 0.043(4) Uani 0.261(11) 1 d . U . A 2
H4AA H 0.5743 0.1154 0.6734 0.052 Uiso 0.261(11) 1 calc R . . A 2
C5A C 0.5650(7) -0.097(6) 0.562(2) 0.048(4) Uani 0.261(11) 1 d . U . A 2
H5A H 0.5586 -0.2034 0.6013 0.058 Uiso 0.261(11) 1 calc R . . A 2
C6A C 0.5654(8) -0.157(6) 0.463(2) 0.054(5) Uani 0.261(11) 1 d . U . A 2
H6A H 0.5627 -0.3043 0.4423 0.065 Uiso 0.261(11) 1 calc R . . A 2
C8A C 0.5095(6) 0.016(4) 0.242(2) 0.035(4) Uani 0.584(18) 1 d . U . B 2
H8A H 0.5162 0.1405 0.2804 0.042 Uiso 0.584(18) 1 calc R . . B 2
C9A C 0.4805(4) -0.003(3) 0.1971(12) 0.040(3) Uani 0.584(18) 1 d . U . B 2
H9A H 0.4677 0.1045 0.2083 0.048 Uiso 0.584(18) 1 calc R . . B 2
C10A C 0.4712(3) -0.177(3) 0.1377(12) 0.042(3) Uani 0.584(18) 1 d . U . B 2
H10A H 0.4518 -0.1897 0.1050 0.050 Uiso 0.584(18) 1 calc R . . B 2
C11A C 0.4905(3) -0.338(3) 0.1251(9) 0.046(3) Uani 0.584(18) 1 d . U . B 2
H11A H 0.4839 -0.4616 0.0857 0.055 Uiso 0.584(18) 1 calc R . . B 2
C12A C 0.5192(3) -0.318(3) 0.1694(11) 0.037(3) Uani 0.584(18) 1 d . U . B 2
H12A H 0.5326 -0.4221 0.1593 0.044 Uiso 0.584(18) 1 calc R . . B 2
Cl1S Cl 0.48930(5) 0.4910(5) 0.39154(16) 0.0873(7) Uani 1 1 d . . . . .
C1S C 0.5000 0.335(3) 0.5000 0.106(5) Uani 1 2 d S T P . .
H1SA H 0.4842 0.2400 0.5068 0.127 Uiso 0.5 1 calc R . . . .
H1SB H 0.5158 0.2401 0.4932 0.127 Uiso 0.5 1 calc R . . . .
O1S O 0.75154(7) 0.1197(6) 0.0317(2) 0.0258(8) Uani 1 1 d . . . . .
H1SC H 0.7397 0.0773 0.0656 0.039 Uiso 1 1 d G . . . .
H1SD H 0.7463 0.2442 0.0043 0.039 Uiso 1 1 d G . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C14 1.819(6) . ?
S1 C15 1.773(4) . ?
P1 C1 1.836(5) . ?
P1 C7 1.819(6) . ?
P1 C13 1.854(6) . ?
O1 C22 1.222(5) . ?
O2 C23 1.220(5) . ?
O3 C32 1.363(5) . ?
O3 C35 1.421(5) . ?
N1 H1 0.8800 . ?
N1 C18 1.400(5) . ?
N1 C21 1.350(5) . ?
N2 H2 0.8800 . ?
N2 C24 1.319(5) . ?
N2 C25 1.474(5) . ?
N4 H4 1.0000 . ?
N4 C36 1.489(5) . ?
N4 C40 1.477(6) . ?
N4 C41 1.480(5) . ?
N28 C28 1.317(6) . ?
N28 C29 1.370(6) . ?
C1 C2 1.359(10) . ?
C1 C6 1.429(10) . ?
C1 C2A 1.46(3) . ?
C1 C6A 1.19(3) . ?
C2 H2A 0.9500 . ?
C2 C3 1.378(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.36(2) . ?
C4 H4A 0.9500 . ?
C4 C5 1.38(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.409(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.55(4) . ?
C7 C12 1.35(3) . ?
C7 C8A 1.28(3) . ?
C7 C12A 1.441(17) . ?
C8 H8 0.9500 . ?
C8 C9 1.40(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.35(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.29(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.43(3) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.535(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.387(7) . ?
C15 C20 1.397(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.387(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.399(6) . ?
C18 C19 1.395(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.386(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.463(6) . ?
C21 C24 1.415(6) . ?
C22 C23 1.495(6) . ?
C23 C24 1.475(6) . ?
C25 H25 1.0000 . ?
C25 C26 1.527(5) . ?
C25 C36 1.540(6) . ?
C26 C27 1.370(6) . ?
C26 C34 1.418(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.402(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.404(6) . ?
C29 C34 1.437(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.368(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.407(6) . ?
C32 C33 1.366(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.417(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36 1.0000 . ?
C36 C37 1.551(6) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.530(6) . ?
C38 H38 1.0000 . ?
C38 C39 1.522(6) . ?
C38 C42 1.533(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.540(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.557(6) . ?
C42 H42 1.0000 . ?
C42 C43 1.516(6) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.518(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C2A H2AA 0.9500 . ?
C2A C3A 1.44(3) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.41(7) . ?
C4A H4AA 0.9500 . ?
C4A C5A 1.31(8) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.42(4) . ?
C6A H6A 0.9500 . ?
C8A H8A 0.9500 . ?
C8A C9A 1.41(3) . ?
C9A H9A 0.9500 . ?
C9A C10A 1.36(2) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.41(2) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.394(17) . ?
C12A H12A 0.9500 . ?
Cl1S C1S 1.751(11) . ?
C1S Cl1S 1.751(11) 2_656 ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
O1S H1SC 0.8672 . ?
O1S H1SD 0.8677 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 S1 C14 101.2(2) . . ?
C1 P1 C13 101.2(2) . . ?
C7 P1 C1 101.8(2) . . ?
C7 P1 C13 99.0(2) . . ?
C32 O3 C35 119.0(3) . . ?
C18 N1 H1 116.9 . . ?
C21 N1 H1 116.9 . . ?
C21 N1 C18 126.2(3) . . ?
C24 N2 H2 119.4 . . ?
C24 N2 C25 121.2(3) . . ?
C25 N2 H2 119.4 . . ?
C36 N4 H4 110.2 . . ?
C40 N4 H4 110.2 . . ?
C40 N4 C36 110.5(3) . . ?
C40 N4 C41 108.0(3) . . ?
C41 N4 H4 110.2 . . ?
C41 N4 C36 107.8(3) . . ?
C28 N28 C29 116.9(4) . . ?
C2 C1 P1 120.9(5) . . ?
C2 C1 C6 117.0(6) . . ?
C6 C1 P1 121.2(5) . . ?
C2A C1 P1 123.2(9) . . ?
C6A C1 P1 113.9(17) . . ?
C6A C1 C2A 122.9(19) . . ?
C1 C2 H2A 118.8 . . ?
C1 C2 C3 122.4(8) . . ?
C3 C2 H2A 118.8 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.8(12) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4A 119.2 . . ?
C3 C4 C5 122(2) . . ?
C5 C4 H4A 119.2 . . ?
C4 C5 H5 121.1 . . ?
C4 C5 C6 117.7(13) . . ?
C6 C5 H5 121.1 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.7(8) . . ?
C5 C6 H6 119.7 . . ?
C8 C7 P1 116.8(14) . . ?
C12 C7 P1 132.8(12) . . ?
C12 C7 C8 110.4(18) . . ?
C8A C7 P1 127.2(11) . . ?
C8A C7 C12A 122.6(12) . . ?
C12A C7 P1 109.9(7) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 C7 121(2) . . ?
C9 C8 H8 119.4 . . ?
C8 C9 H9 120.7 . . ?
C10 C9 C8 119(2) . . ?
C10 C9 H9 120.7 . . ?
C9 C10 H10 117.8 . . ?
C11 C10 C9 124(2) . . ?
C11 C10 H10 117.8 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119(2) . . ?
C12 C11 H11 120.5 . . ?
C7 C12 C11 126(2) . . ?
C7 C12 H12 117.0 . . ?
C11 C12 H12 117.0 . . ?
P1 C13 H13A 109.6 . . ?
P1 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 P1 110.2(4) . . ?
C14 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
S1 C14 H14A 108.9 . . ?
S1 C14 H14B 108.9 . . ?
C13 C14 S1 113.3(4) . . ?
C13 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 S1 121.0(4) . . ?
C16 C15 C20 118.5(4) . . ?
C20 C15 S1 120.5(3) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 C15 121.2(4) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.2(4) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 N1 117.9(4) . . ?
C19 C18 N1 123.1(4) . . ?
C19 C18 C17 118.9(4) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.5(4) . . ?
C20 C19 H19 119.8 . . ?
C15 C20 H20 119.6 . . ?
C19 C20 C15 120.8(4) . . ?
C19 C20 H20 119.6 . . ?
N1 C21 C22 137.0(4) . . ?
N1 C21 C24 131.1(4) . . ?
C24 C21 C22 91.9(3) . . ?
O1 C22 C21 137.2(4) . . ?
O1 C22 C23 134.3(4) . . ?
C21 C22 C23 88.6(3) . . ?
O2 C23 C22 135.4(4) . . ?
O2 C23 C24 136.2(4) . . ?
C24 C23 C22 88.3(3) . . ?
N2 C24 C21 135.6(4) . . ?
N2 C24 C23 133.2(4) . . ?
C21 C24 C23 91.2(3) . . ?
N2 C25 H25 108.1 . . ?
N2 C25 C26 110.6(3) . . ?
N2 C25 C36 108.9(3) . . ?
C26 C25 H25 108.1 . . ?
C26 C25 C36 113.0(3) . . ?
C36 C25 H25 108.1 . . ?
C27 C26 C25 120.2(4) . . ?
C27 C26 C34 118.4(4) . . ?
C34 C26 C25 121.3(4) . . ?
C26 C27 H27 119.9 . . ?
C26 C27 C28 120.2(4) . . ?
C28 C27 H27 119.9 . . ?
N28 C28 C27 124.3(4) . . ?
N28 C28 H28 117.9 . . ?
C27 C28 H28 117.9 . . ?
N28 C29 C30 118.0(4) . . ?
N28 C29 C34 123.0(4) . . ?
C30 C29 C34 119.0(4) . . ?
C29 C30 H30 119.0 . . ?
C31 C30 C29 122.0(4) . . ?
C31 C30 H30 119.0 . . ?
C30 C31 H31 120.4 . . ?
C30 C31 C32 119.2(4) . . ?
C32 C31 H31 120.4 . . ?
O3 C32 C31 123.2(4) . . ?
O3 C32 C33 116.4(4) . . ?
C33 C32 C31 120.5(4) . . ?
C32 C33 H33 119.0 . . ?
C32 C33 C34 121.9(4) . . ?
C34 C33 H33 119.0 . . ?
C26 C34 C29 117.1(4) . . ?
C33 C34 C26 125.5(4) . . ?
C33 C34 C29 117.3(4) . . ?
O3 C35 H35A 109.5 . . ?
O3 C35 H35B 109.5 . . ?
O3 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N4 C36 C25 109.3(3) . . ?
N4 C36 H36 107.4 . . ?
N4 C36 C37 110.1(3) . . ?
C25 C36 H36 107.4 . . ?
C25 C36 C37 114.8(3) . . ?
C37 C36 H36 107.4 . . ?
C36 C37 H37A 109.9 . . ?
C36 C37 H37B 109.9 . . ?
H37A C37 H37B 108.3 . . ?
C38 C37 C36 108.8(3) . . ?
C38 C37 H37A 109.9 . . ?
C38 C37 H37B 109.9 . . ?
C37 C38 H38 110.2 . . ?
C37 C38 C42 110.8(4) . . ?
C39 C38 C37 108.3(3) . . ?
C39 C38 H38 110.2 . . ?
C39 C38 C42 107.0(3) . . ?
C42 C38 H38 110.2 . . ?
C38 C39 H39A 110.0 . . ?
C38 C39 H39B 110.0 . . ?
C38 C39 C40 108.5(4) . . ?
H39A C39 H39B 108.4 . . ?
C40 C39 H39A 110.0 . . ?
C40 C39 H39B 110.0 . . ?
N4 C40 C39 110.7(4) . . ?
N4 C40 H40A 109.5 . . ?
N4 C40 H40B 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?
N4 C41 H41A 109.2 . . ?
N4 C41 H41B 109.2 . . ?
N4 C41 C42 111.8(3) . . ?
H41A C41 H41B 107.9 . . ?
C42 C41 H41A 109.2 . . ?
C42 C41 H41B 109.2 . . ?
C38 C42 C41 106.1(3) . . ?
C38 C42 H42 107.2 . . ?
C41 C42 H42 107.2 . . ?
C43 C42 C38 115.2(4) . . ?
C43 C42 C41 113.4(4) . . ?
C43 C42 H42 107.2 . . ?
C42 C43 H43A 108.9 . . ?
C42 C43 H43B 108.9 . . ?
C42 C43 C44 113.3(4) . . ?
H43A C43 H43B 107.7 . . ?
C44 C43 H43A 108.9 . . ?
C44 C43 H43B 108.9 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 C2A H2AA 122.0 . . ?
C3A C2A C1 116(2) . . ?
C3A C2A H2AA 122.0 . . ?
C2A C3A H3A 119.9 . . ?
C4A C3A C2A 120(4) . . ?
C4A C3A H3A 119.9 . . ?
C3A C4A H4AA 122.7 . . ?
C5A C4A C3A 115(6) . . ?
C5A C4A H4AA 122.7 . . ?
C4A C5A H5A 116.9 . . ?
C4A C5A C6A 126(4) . . ?
C6A C5A H5A 116.9 . . ?
C1 C6A C5A 119(3) . . ?
C1 C6A H6A 120.3 . . ?
C5A C6A H6A 120.3 . . ?
C7 C8A H8A 118.9 . . ?
C7 C8A C9A 122.2(16) . . ?
C9A C8A H8A 118.9 . . ?
C8A C9A H9A 120.5 . . ?
C10A C9A C8A 119.0(15) . . ?
C10A C9A H9A 120.5 . . ?
C9A C10A H10A 120.3 . . ?
C9A C10A C11A 119.3(13) . . ?
C11A C10A H10A 120.3 . . ?
C10A C11A H11A 119.3 . . ?
C12A C11A C10A 121.3(12) . . ?
C12A C11A H11A 119.3 . . ?
C7 C12A H12A 122.3 . . ?
C11A C12A C7 115.5(12) . . ?
C11A C12A H12A 122.3 . . ?
Cl1S C1S Cl1S 113.1(11) 2_656 . ?
Cl1S C1S H1SA 109.0 2_656 . ?
Cl1S C1S H1SA 109.0 . . ?
Cl1S C1S H1SB 109.0 2_656 . ?
Cl1S C1S H1SB 109.0 . . ?
H1SA C1S H1SB 107.8 . . ?
H1SC O1S H1SD 109.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C15 C16 C17 -179.7(3) . . . . ?
S1 C15 C20 C19 -179.6(3) . . . . ?
P1 C1 C2 C3 -177.9(8) . . . . ?
P1 C1 C6 C5 178.9(7) . . . . ?
P1 C1 C2A C3A -180.0(17) . . . . ?
P1 C1 C6A C5A -174(2) . . . . ?
P1 C7 C8 C9 173(2) . . . . ?
P1 C7 C12 C11 -175.6(15) . . . . ?
P1 C7 C8A C9A 175.9(13) . . . . ?
P1 C7 C12A C11A -176.9(9) . . . . ?
P1 C13 C14 S1 -177.2(3) . . . . ?
O1 C22 C23 O2 2.6(8) . . . . ?
O1 C22 C23 C24 -177.9(5) . . . . ?
O2 C23 C24 N2 0.1(8) . . . . ?
O2 C23 C24 C21 178.2(5) . . . . ?
O3 C32 C33 C34 178.7(4) . . . . ?
N1 C18 C19 C20 -175.1(4) . . . . ?
N1 C21 C22 O1 -2.1(9) . . . . ?
N1 C21 C22 C23 178.8(5) . . . . ?
N1 C21 C24 N2 -0.8(8) . . . . ?
N1 C21 C24 C23 -178.8(4) . . . . ?
N2 C25 C26 C27 41.6(5) . . . . ?
N2 C25 C26 C34 -137.8(4) . . . . ?
N2 C25 C36 N4 52.9(4) . . . . ?
N2 C25 C36 C37 177.2(3) . . . . ?
N4 C36 C37 C38 11.6(5) . . . . ?
N4 C41 C42 C38 17.5(4) . . . . ?
N4 C41 C42 C43 144.9(3) . . . . ?
N28 C29 C30 C31 178.7(4) . . . . ?
N28 C29 C34 C26 -2.3(6) . . . . ?
N28 C29 C34 C33 179.9(4) . . . . ?
C1 P1 C7 C8 47(2) . . . . ?
C1 P1 C7 C12 -130.9(15) . . . . ?
C1 P1 C7 C8A 45(2) . . . . ?
C1 P1 C7 C12A -141.7(7) . . . . ?
C1 P1 C13 C14 -161.9(3) . . . . ?
C1 C2 C3 C4 2(2) . . . . ?
C1 C2A C3A C4A -2(5) . . . . ?
C2 C1 C6 C5 9.5(14) . . . . ?
C2 C1 C2A C3A -81(3) . . . . ?
C2 C1 C6A C5A 47(3) . . . . ?
C2 C3 C4 C5 3(3) . . . . ?
C3 C4 C5 C6 -2(3) . . . . ?
C4 C5 C6 C1 -4.5(19) . . . . ?
C6 C1 C2 C3 -8.5(14) . . . . ?
C6 C1 C2A C3A 31(3) . . . . ?
C6 C1 C6A C5A -63(4) . . . . ?
C7 P1 C1 C2 -147.2(6) . . . . ?
C7 P1 C1 C6 43.9(7) . . . . ?
C7 P1 C1 C2A -101.7(14) . . . . ?
C7 P1 C1 C6A 79(2) . . . . ?
C7 P1 C13 C14 -57.8(4) . . . . ?
C7 C8 C9 C10 5(4) . . . . ?
C7 C8A C9A C10A -3(3) . . . . ?
C8 C7 C12 C11 6(3) . . . . ?
C8 C7 C8A C9A 168(20) . . . . ?
C8 C7 C12A C11A -7(3) . . . . ?
C8 C9 C10 C11 1(3) . . . . ?
C9 C10 C11 C12 -4(3) . . . . ?
C10 C11 C12 C7 -1(3) . . . . ?
C12 C7 C8 C9 -8(4) . . . . ?
C12 C7 C8A C9A -7(3) . . . . ?
C12 C7 C12A C11A 22(3) . . . . ?
C13 P1 C1 C2 -45.4(7) . . . . ?
C13 P1 C1 C6 145.7(7) . . . . ?
C13 P1 C1 C2A 0.1(15) . . . . ?
C13 P1 C1 C6A -179(2) . . . . ?
C13 P1 C7 C8 -57(2) . . . . ?
C13 P1 C7 C12 125.6(15) . . . . ?
C13 P1 C7 C8A -58(2) . . . . ?
C13 P1 C7 C12A 114.8(7) . . . . ?
C14 S1 C15 C16 58.0(4) . . . . ?
C14 S1 C15 C20 -122.9(4) . . . . ?
C15 S1 C14 C13 65.6(4) . . . . ?
C15 C16 C17 C18 -0.9(6) . . . . ?
C16 C15 C20 C19 -0.5(6) . . . . ?
C16 C17 C18 N1 176.0(3) . . . . ?
C16 C17 C18 C19 -0.2(6) . . . . ?
C17 C18 C19 C20 0.8(6) . . . . ?
C18 N1 C21 C22 -23.7(7) . . . . ?
C18 N1 C21 C24 156.5(4) . . . . ?
C18 C19 C20 C15 -0.5(6) . . . . ?
C20 C15 C16 C17 1.2(6) . . . . ?
C21 N1 C18 C17 173.5(4) . . . . ?
C21 N1 C18 C19 -10.5(6) . . . . ?
C21 C22 C23 O2 -178.2(5) . . . . ?
C21 C22 C23 C24 1.3(3) . . . . ?
C22 C21 C24 N2 179.3(4) . . . . ?
C22 C21 C24 C23 1.4(3) . . . . ?
C22 C23 C24 N2 -179.4(4) . . . . ?
C22 C23 C24 C21 -1.3(3) . . . . ?
C24 N2 C25 C26 107.2(4) . . . . ?
C24 N2 C25 C36 -128.1(4) . . . . ?
C24 C21 C22 O1 177.8(5) . . . . ?
C24 C21 C22 C23 -1.3(3) . . . . ?
C25 N2 C24 C21 -178.8(4) . . . . ?
C25 N2 C24 C23 -1.6(6) . . . . ?
C25 C26 C27 C28 -179.9(4) . . . . ?
C25 C26 C34 C29 -178.7(4) . . . . ?
C25 C26 C34 C33 -1.1(6) . . . . ?
C25 C36 C37 C38 -112.2(4) . . . . ?
C26 C25 C36 N4 176.2(3) . . . . ?
C26 C25 C36 C37 -59.6(4) . . . . ?
C26 C27 C28 N28 -0.7(7) . . . . ?
C27 C26 C34 C29 1.8(6) . . . . ?
C27 C26 C34 C33 179.4(4) . . . . ?
C28 N28 C29 C30 -177.5(4) . . . . ?
C28 N28 C29 C34 1.2(6) . . . . ?
C29 N28 C28 C27 0.4(6) . . . . ?
C29 C30 C31 C32 1.2(7) . . . . ?
C30 C29 C34 C26 176.4(4) . . . . ?
C30 C29 C34 C33 -1.4(6) . . . . ?
C30 C31 C32 O3 179.9(4) . . . . ?
C30 C31 C32 C33 -0.9(7) . . . . ?
C31 C32 C33 C34 -0.6(7) . . . . ?
C32 C33 C34 C26 -175.8(4) . . . . ?
C32 C33 C34 C29 1.8(6) . . . . ?
C34 C26 C27 C28 -0.5(6) . . . . ?
C34 C29 C30 C31 0.0(7) . . . . ?
C35 O3 C32 C31 -0.6(6) . . . . ?
C35 O3 C32 C33 -179.9(4) . . . . ?
C36 N4 C40 C39 50.1(4) . . . . ?
C36 N4 C41 C42 -70.8(4) . . . . ?
C36 C25 C26 C27 -80.7(5) . . . . ?
C36 C25 C26 C34 99.9(4) . . . . ?
C36 C37 C38 C39 51.9(4) . . . . ?
C36 C37 C38 C42 -65.2(4) . . . . ?
C37 C38 C39 C40 -67.2(4) . . . . ?
C37 C38 C42 C41 48.1(4) . . . . ?
C37 C38 C42 C43 -78.2(5) . . . . ?
C38 C39 C40 N4 14.8(4) . . . . ?
C38 C42 C43 C44 -71.6(5) . . . . ?
C39 C38 C42 C41 -69.8(4) . . . . ?
C39 C38 C42 C43 163.9(3) . . . . ?
C40 N4 C36 C25 61.6(4) . . . . ?
C40 N4 C36 C37 -65.4(4) . . . . ?
C40 N4 C41 C42 48.6(4) . . . . ?
C41 N4 C36 C25 179.5(3) . . . . ?
C41 N4 C36 C37 52.5(4) . . . . ?
C41 N4 C40 C39 -67.6(4) . . . . ?
C41 C42 C43 C44 165.8(4) . . . . ?
C42 C38 C39 C40 52.3(4) . . . . ?
C2A C1 C2 C3 76.4(18) . . . . ?
C2A C1 C6 C5 -30.9(16) . . . . ?
C2A C1 C6A C5A 7(4) . . . . ?
C2A C3A C4A C5A -2(8) . . . . ?
C3A C4A C5A C6A 9(9) . . . . ?
C4A C5A C6A C1 -11(7) . . . . ?
C6A C1 C2 C3 -42(2) . . . . ?
C6A C1 C6 C5 93(3) . . . . ?
C6A C1 C2A C3A -1(4) . . . . ?
C8A C7 C8 C9 -13(15) . . . . ?
C8A C7 C12 C11 7(3) . . . . ?
C8A C7 C12A C11A -4(2) . . . . ?
C8A C9A C10A C11A 2(2) . . . . ?
C9A C10A C11A C12A -2(2) . . . . ?
C10A C11A C12A C7 2.8(18) . . . . ?
C12A C7 C8 C9 4(5) . . . . ?
C12A C7 C12 C11 -151(5) . . . . ?
C12A C7 C8A C9A 4(3) . . . . ?

_olex2_submission_original_sample_id cx0040a
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Vapour deposition'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cx0591
_database_code_depnum_ccdc_archive 'CCDC 1469902'
_audit_update_record             
;
2016-03-21 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_audit_creation_date             2016-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H37 O3 P2 Pt S3, B F4'
_chemical_formula_sum            'C36 H37 B F4 O3 P2 Pt S3'
_chemical_formula_weight         957.67
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   18.1695(7)
_cell_length_b                   9.2664(4)
_cell_length_c                   22.3000(9)
_cell_angle_alpha                90
_cell_angle_beta                 101.881(3)
_cell_angle_gamma                90
_cell_volume                     3674.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7028
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.061
_cell_measurement_theta_min      2.865
_shelx_estimated_absorpt_T_max   0.942
_shelx_estimated_absorpt_T_min   0.520
_exptl_absorpt_coefficient_mu    10.046
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1027 before and 0.0687 after correction.
The Ratio of minimum to maximum transmission is 0.7666.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1896
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.006
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24761
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.439
_diffrn_reflns_theta_min         3.515
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   microsource
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4708
_reflns_number_total             6406
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     653
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0445
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0472P)²+1.8643P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1116
_refine_special_details          
'Distance restraints were imposed on the disordered rings. The enhanced rigid-bond restraint (SHELX keyword RIGU) was applied globally. (Acta Cryst. A68 (2012) 448-451).'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P1-C15A \\sim P1-C15
 with sigma of 0.01
 C15A-C16A \\sim C15A-C20A \\sim C16-C15 \\sim C20-C15 \\sim C19-C20 \\sim
C20A-C19A \\sim C18-C19 ~
 C18A-C19A \\sim C17A-C18A \\sim C18-C17 \\sim C17A-C16A \\sim C17-C16
 with sigma of 0.01
 C26-C21 \\sim C26A-C21A \\sim C25A-C26A \\sim C26-C25 \\sim C24-C25 \\sim
C25A-C24A \\sim C24-C23 ~
 C24A-C23A \\sim C22-C23 \\sim C23A-C22A \\sim C21A-C22A \\sim C22-C21
 with sigma of 0.01
 P2-C21 \\sim P2-C21A
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(C15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(2)
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C16A(H16A), C17(H17), C17A(H17A), C18(H18),
 C18A(H18A), C19(H19), C19A(H19A), C20(H20), C20A(H20A), C22(H22), C22A(H22A),
 C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A), C26(H26),
 C26A(H26A), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.42302(2) 0.69809(4) 0.75146(2) 0.03543(12) Uani 1 1 d . U . . .
S1 S 0.39388(9) 0.7665(2) 0.84702(7) 0.0387(4) Uani 1 1 d . U . . .
S2 S 0.29875(9) 0.6175(2) 0.71977(8) 0.0436(5) Uani 1 1 d . U . . .
S3 S 0.11841(11) 0.6742(2) 0.74969(8) 0.0451(5) Uani 1 1 d . U . . .
P1 P 0.54131(10) 0.7696(2) 0.79450(9) 0.0396(5) Uani 1 1 d D U . . .
P2 P 0.43637(11) 0.6457(2) 0.65478(8) 0.0406(5) Uani 1 1 d D U . . .
O2 O 0.0402(3) 0.7168(8) 0.7357(3) 0.0709(18) Uani 1 1 d . U . . .
O1 O 0.1285(3) 0.5223(6) 0.7397(2) 0.0438(12) Uani 1 1 d . U . . .
O3 O 0.1592(4) 0.7232(6) 0.8090(3) 0.0696(18) Uani 1 1 d . U . . .
C1 C 0.3847(4) 0.6100(9) 0.8912(3) 0.0435(16) Uani 1 1 d . U . . .
C2 C 0.4453(5) 0.5197(9) 0.9155(3) 0.0504(19) Uani 1 1 d . U . . .
H2 H 0.4945 0.5438 0.9105 0.060 Uiso 1 1 calc R . . . .
C3 C 0.4338(5) 0.3958(10) 0.9466(3) 0.056(2) Uani 1 1 d . U . . .
H3 H 0.4750 0.3345 0.9629 0.068 Uiso 1 1 calc R . . . .
C4 C 0.3620(6) 0.3610(11) 0.9541(4) 0.066(2) Uani 1 1 d . U . . .
H4 H 0.3539 0.2759 0.9757 0.079 Uiso 1 1 calc R . . . .
C5 C 0.3024(6) 0.4502(10) 0.9302(4) 0.064(2) Uani 1 1 d . U . . .
H5 H 0.2532 0.4264 0.9356 0.077 Uiso 1 1 calc R . . . .
C6 C 0.3136(5) 0.5758(10) 0.8981(4) 0.0529(19) Uani 1 1 d . U . . .
H6 H 0.2723 0.6364 0.8813 0.063 Uiso 1 1 calc R . . . .
C7 C 0.4786(4) 0.8532(9) 0.8911(3) 0.0483(19) Uani 1 1 d . U . . .
H7A H 0.4639 0.9338 0.9154 0.058 Uiso 1 1 calc R . . . .
H7B H 0.5074 0.7825 0.9200 0.058 Uiso 1 1 calc R . . . .
C8 C 0.5274(4) 0.9099(9) 0.8492(3) 0.0449(17) Uani 1 1 d . U . . .
H8A H 0.5767 0.9402 0.8738 0.054 Uiso 1 1 calc R . . . .
H8B H 0.5032 0.9952 0.8266 0.054 Uiso 1 1 calc R . . . .
C9 C 0.5945(4) 0.6239(9) 0.8383(3) 0.0449(17) Uani 1 1 d . U . . .
C10 C 0.6567(4) 0.6610(10) 0.8849(3) 0.052(2) Uani 1 1 d . U . . .
H10 H 0.6726 0.7584 0.8917 0.063 Uiso 1 1 calc R . . . .
C11 C 0.6932(5) 0.5508(11) 0.9199(4) 0.061(2) Uani 1 1 d . U . . .
H11 H 0.7345 0.5732 0.9521 0.073 Uiso 1 1 calc R . . . .
C12 C 0.6721(5) 0.4098(12) 0.9099(4) 0.066(2) Uani 1 1 d . U . . .
H12 H 0.6989 0.3363 0.9350 0.080 Uiso 1 1 calc R . . . .
C13 C 0.6120(5) 0.3738(11) 0.8635(4) 0.065(2) Uani 1 1 d . U . . .
H13 H 0.5977 0.2757 0.8562 0.078 Uiso 1 1 calc R . . . .
C14 C 0.5724(4) 0.4830(9) 0.8275(4) 0.053(2) Uani 1 1 d . U . . .
H14 H 0.5306 0.4600 0.7957 0.064 Uiso 1 1 calc R . . . .
C15 C 0.6133(8) 0.8367(16) 0.7572(9) 0.049(4) Uani 0.514(11) 1 d D U P A 1
C15A C 0.5939(8) 0.8618(18) 0.7447(8) 0.042(4) Uani 0.486(11) 1 d D U P A 2
C16 C 0.6132(8) 0.9857(16) 0.7510(9) 0.066(5) Uani 0.514(11) 1 d D U P A 1
H16 H 0.5753 1.0453 0.7617 0.079 Uiso 0.514(11) 1 calc R . P A 1
C16A C 0.5657(9) 0.9789(17) 0.7073(7) 0.052(4) Uani 0.486(11) 1 d D U P A 2
H16A H 0.5178 1.0144 0.7113 0.063 Uiso 0.486(11) 1 calc R . P A 2
C17 C 0.6731(8) 1.041(2) 0.7280(10) 0.089(6) Uani 0.514(11) 1 d D U P A 1
H17 H 0.6788 1.1426 0.7256 0.107 Uiso 0.514(11) 1 calc R . P A 1
C17A C 0.5995(8) 1.049(2) 0.6649(7) 0.062(5) Uani 0.486(11) 1 d D U P A 2
H17A H 0.5754 1.1250 0.6394 0.075 Uiso 0.486(11) 1 calc R . P A 2
C18 C 0.7247(10) 0.9511(17) 0.7084(10) 0.080(6) Uani 0.514(11) 1 d D U P A 1
H18 H 0.7633 0.9916 0.6908 0.095 Uiso 0.514(11) 1 calc R . P A 1
C18A C 0.6713(8) 1.001(2) 0.6624(9) 0.073(6) Uani 0.486(11) 1 d D U P A 2
H18A H 0.6985 1.0470 0.6357 0.088 Uiso 0.486(11) 1 calc R . P A 2
C19 C 0.7200(9) 0.8020(18) 0.7146(9) 0.072(5) Uani 0.514(11) 1 d D U P A 1
H19 H 0.7557 0.7417 0.7011 0.087 Uiso 0.514(11) 1 calc R . P A 1
C19A C 0.7041(10) 0.886(2) 0.6984(8) 0.061(5) Uani 0.486(11) 1 d D U P A 2
H19A H 0.7534 0.8556 0.6965 0.073 Uiso 0.486(11) 1 calc R . P A 2
C20 C 0.6637(9) 0.740(2) 0.7401(9) 0.053(4) Uani 0.514(11) 1 d D U P A 1
H20 H 0.6601 0.6390 0.7455 0.063 Uiso 0.514(11) 1 calc R . P A 1
C20A C 0.6647(8) 0.815(2) 0.7374(9) 0.056(5) Uani 0.486(11) 1 d D U P A 2
H20A H 0.6868 0.7331 0.7595 0.068 Uiso 0.486(11) 1 calc R . P A 2
C21 C 0.5156(8) 0.5519(18) 0.6355(10) 0.046(5) Uani 0.523(18) 1 d D U P B 2
C21A C 0.5280(8) 0.5769(19) 0.6485(10) 0.042(5) Uani 0.477(18) 1 d D U P B 1
C22 C 0.5666(17) 0.621(3) 0.607(2) 0.055(8) Uani 0.523(18) 1 d D U P B 2
H22 H 0.5594 0.7191 0.5947 0.066 Uiso 0.523(18) 1 calc R . P B 2
C22A C 0.574(2) 0.650(3) 0.616(2) 0.051(6) Uani 0.477(18) 1 d D U P B 1
H22A H 0.5566 0.7417 0.6000 0.061 Uiso 0.477(18) 1 calc R . P B 1
C23 C 0.6285(12) 0.545(2) 0.5982(12) 0.060(6) Uani 0.523(18) 1 d D U P B 2
H23 H 0.6665 0.5896 0.5811 0.072 Uiso 0.523(18) 1 calc R . P B 2
C23A C 0.6413(13) 0.601(2) 0.6040(13) 0.063(6) Uani 0.477(18) 1 d D U P B 1
H23A H 0.6665 0.6558 0.5782 0.075 Uiso 0.477(18) 1 calc R . P B 1
C24 C 0.6337(10) 0.4008(19) 0.6143(8) 0.062(5) Uani 0.523(18) 1 d D U P B 2
H24 H 0.6755 0.3467 0.6072 0.074 Uiso 0.523(18) 1 calc R . P B 2
C24A C 0.6719(11) 0.474(2) 0.6298(8) 0.058(5) Uani 0.477(18) 1 d D U P B 1
H24A H 0.7181 0.4379 0.6224 0.069 Uiso 0.477(18) 1 calc R . P B 1
C25 C 0.5807(9) 0.3320(19) 0.6405(8) 0.064(5) Uani 0.523(18) 1 d D U P B 2
H25 H 0.5859 0.2322 0.6502 0.077 Uiso 0.523(18) 1 calc R . P B 2
C25A C 0.6321(9) 0.402(2) 0.6670(8) 0.060(5) Uani 0.477(18) 1 d D U P B 1
H25A H 0.6530 0.3182 0.6885 0.072 Uiso 0.477(18) 1 calc R . P B 1
C26 C 0.5203(10) 0.4086(18) 0.6526(7) 0.054(4) Uani 0.523(18) 1 d D U P B 2
H26 H 0.4839 0.3648 0.6717 0.065 Uiso 0.523(18) 1 calc R . P B 2
C26A C 0.5620(10) 0.4503(19) 0.6730(9) 0.053(4) Uani 0.477(18) 1 d D U P B 1
H26A H 0.5349 0.3917 0.6959 0.063 Uiso 0.477(18) 1 calc R . P B 1
C27 C 0.4170(4) 0.7969(9) 0.6028(3) 0.0381(15) Uani 1 1 d . U . . .
C28 C 0.4093(6) 0.9329(9) 0.6224(4) 0.068(3) Uani 1 1 d . U . . .
H28 H 0.4121 0.9492 0.6649 0.082 Uiso 1 1 calc R . . . .
C29 C 0.3973(7) 1.0500(10) 0.5826(4) 0.082(3) Uani 1 1 d . U . . .
H29 H 0.3926 1.1448 0.5976 0.099 Uiso 1 1 calc R . . . .
C30 C 0.3923(5) 1.0259(11) 0.5204(4) 0.059(2) Uani 1 1 d . U . . .
H30 H 0.3846 1.1045 0.4925 0.071 Uiso 1 1 calc R . . . .
C31 C 0.3984(5) 0.8933(12) 0.5002(4) 0.065(2) Uani 1 1 d . U . . .
H31 H 0.3944 0.8775 0.4576 0.078 Uiso 1 1 calc R . . . .
C32 C 0.4107(5) 0.7751(10) 0.5406(4) 0.059(2) Uani 1 1 d . U . . .
H32 H 0.4146 0.6805 0.5251 0.071 Uiso 1 1 calc R . . . .
C33 C 0.3619(5) 0.5154(10) 0.6263(4) 0.061(2) Uani 1 1 d . U . . .
H33A H 0.3576 0.5009 0.5817 0.073 Uiso 1 1 calc R . . . .
H33B H 0.3743 0.4214 0.6470 0.073 Uiso 1 1 calc R . . . .
C34 C 0.2882(5) 0.5707(11) 0.6386(4) 0.065(2) Uani 1 1 d . U . . .
H34A H 0.2490 0.4957 0.6276 0.078 Uiso 1 1 calc R . . . .
H34B H 0.2722 0.6570 0.6131 0.078 Uiso 1 1 calc R . . . .
C35 C 0.2454(4) 0.7837(9) 0.7151(4) 0.052(2) Uani 1 1 d . U . . .
H35A H 0.2566 0.8311 0.7557 0.062 Uiso 1 1 calc R . . . .
H35B H 0.2628 0.8489 0.6857 0.062 Uiso 1 1 calc R . . . .
C36 C 0.1606(4) 0.7653(9) 0.6954(4) 0.051(2) Uani 1 1 d . U . . .
H36A H 0.1496 0.7110 0.6564 0.061 Uiso 1 1 calc R . . . .
H36B H 0.1373 0.8619 0.6876 0.061 Uiso 1 1 calc R . . . .
F1 F 0.2434(3) 0.6062(5) 0.4951(2) 0.0603(12) Uani 1 1 d . U . . .
F2 F 0.2458(3) 0.3671(6) 0.5137(2) 0.0852(19) Uani 1 1 d . U . . .
F3 F 0.1831(3) 0.4499(6) 0.4238(2) 0.0765(17) Uani 1 1 d . U . . .
F4 F 0.1380(4) 0.4972(8) 0.5083(4) 0.115(2) Uani 1 1 d . U . . .
B1 B 0.2018(6) 0.4788(12) 0.4857(5) 0.060(2) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 S1 2.3849(17) . ?
Pt1 S2 2.3449(16) . ?
Pt1 P1 2.2651(17) . ?
Pt1 P2 2.2711(19) . ?
S1 C1 1.780(8) . ?
S1 C7 1.832(7) . ?
S2 C34 1.831(8) . ?
S2 C35 1.811(9) . ?
S3 O2 1.445(6) . ?
S3 O1 1.443(5) . ?
S3 O3 1.450(6) . ?
S3 C36 1.774(8) . ?
P1 C8 1.835(8) . ?
P1 C9 1.823(8) . ?
P1 C15 1.799(11) . ?
P1 C15A 1.820(11) . ?
P2 C21 1.807(11) . ?
P2 C21A 1.815(11) . ?
P2 C27 1.806(8) . ?
P2 C33 1.827(8) . ?
C1 C2 1.401(11) . ?
C1 C6 1.369(11) . ?
C2 H2 0.9500 . ?
C2 C3 1.381(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(13) . ?
C5 H5 0.9500 . ?
C5 C6 1.403(13) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.510(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.410(10) . ?
C9 C14 1.373(12) . ?
C10 H10 0.9500 . ?
C10 C11 1.370(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.367(14) . ?
C12 H12 0.9500 . ?
C12 C13 1.383(12) . ?
C13 H13 0.9500 . ?
C13 C14 1.396(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(9) . ?
C15 C20 1.389(9) . ?
C15A C16A 1.401(9) . ?
C15A C20A 1.398(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.392(9) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.393(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(9) . ?
C17A H17A 0.9500 . ?
C17A C18A 1.391(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(9) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.390(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.392(9) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.396(9) . ?
C20 H20 0.9500 . ?
C20A H20A 0.9500 . ?
C21 C22 1.381(8) . ?
C21 C26 1.380(8) . ?
C21A C22A 1.383(8) . ?
C21A C26A 1.385(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.381(8) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.385(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.378(8) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.379(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.380(8) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.379(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.379(8) . ?
C25A H25A 0.9500 . ?
C25A C26A 1.382(8) . ?
C26 H26 0.9500 . ?
C26A H26A 0.9500 . ?
C27 C28 1.351(12) . ?
C27 C32 1.384(10) . ?
C28 H28 0.9500 . ?
C28 C29 1.391(12) . ?
C29 H29 0.9500 . ?
C29 C30 1.388(12) . ?
C30 H30 0.9500 . ?
C30 C31 1.321(13) . ?
C31 H31 0.9500 . ?
C31 C32 1.406(13) . ?
C32 H32 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.511(13) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.522(10) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
F1 B1 1.394(12) . ?
F2 B1 1.378(12) . ?
F3 B1 1.379(11) . ?
F4 B1 1.365(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Pt1 S1 88.68(6) . . ?
P1 Pt1 S1 84.80(7) . . ?
P1 Pt1 S2 172.62(7) . . ?
P1 Pt1 P2 100.80(7) . . ?
P2 Pt1 S1 172.65(6) . . ?
P2 Pt1 S2 86.00(7) . . ?
C1 S1 Pt1 110.0(3) . . ?
C1 S1 C7 103.0(3) . . ?
C7 S1 Pt1 106.3(3) . . ?
C34 S2 Pt1 105.7(3) . . ?
C35 S2 Pt1 102.5(2) . . ?
C35 S2 C34 101.4(4) . . ?
O2 S3 O3 114.0(4) . . ?
O2 S3 C36 105.4(4) . . ?
O1 S3 O2 112.6(4) . . ?
O1 S3 O3 112.9(3) . . ?
O1 S3 C36 105.8(4) . . ?
O3 S3 C36 105.2(4) . . ?
C8 P1 Pt1 103.9(2) . . ?
C9 P1 Pt1 111.2(3) . . ?
C9 P1 C8 107.4(4) . . ?
C15 P1 Pt1 128.4(7) . . ?
C15 P1 C8 106.0(6) . . ?
C15 P1 C9 98.6(6) . . ?
C15A P1 Pt1 116.8(6) . . ?
C15A P1 C8 103.6(7) . . ?
C15A P1 C9 112.8(5) . . ?
C21 P2 Pt1 125.1(7) . . ?
C21 P2 C33 99.7(7) . . ?
C21A P2 Pt1 115.3(7) . . ?
C21A P2 C33 111.5(8) . . ?
C27 P2 Pt1 113.5(2) . . ?
C27 P2 C21 106.3(6) . . ?
C27 P2 C21A 106.5(6) . . ?
C27 P2 C33 104.9(4) . . ?
C33 P2 Pt1 104.8(3) . . ?
C2 C1 S1 123.0(6) . . ?
C6 C1 S1 116.7(6) . . ?
C6 C1 C2 120.2(8) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 C1 120.2(8) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.9(9) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.8(9) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.6(9) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 119.3(9) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
S1 C7 H7A 109.5 . . ?
S1 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 S1 110.8(5) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
P1 C8 H8A 109.6 . . ?
P1 C8 H8B 109.6 . . ?
C7 C8 P1 110.1(5) . . ?
C7 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 P1 118.0(7) . . ?
C14 C9 P1 120.4(5) . . ?
C14 C9 C10 121.5(8) . . ?
C9 C10 H10 121.4 . . ?
C11 C10 C9 117.3(8) . . ?
C11 C10 H10 121.4 . . ?
C10 C11 H11 118.9 . . ?
C12 C11 C10 122.2(8) . . ?
C12 C11 H11 118.9 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.3(9) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.3(9) . . ?
C14 C13 H13 120.3 . . ?
C9 C14 C13 119.4(7) . . ?
C9 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 P1 113.8(10) . . ?
C16 C15 C20 127.0(13) . . ?
C20 C15 P1 119.2(10) . . ?
C16A C15A P1 123.6(10) . . ?
C20A C15A P1 122.6(11) . . ?
C20A C15A C16A 113.7(13) . . ?
C15 C16 H16 122.7 . . ?
C15 C16 C17 114.6(15) . . ?
C17 C16 H16 122.7 . . ?
C15A C16A H16A 116.2 . . ?
C17A C16A C15A 127.5(14) . . ?
C17A C16A H16A 116.2 . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.6(18) . . ?
C18 C17 H17 119.2 . . ?
C16A C17A H17A 122.5 . . ?
C18A C17A C16A 115.1(16) . . ?
C18A C17A H17A 122.5 . . ?
C17 C18 H18 119.8 . . ?
C17 C18 C19 120.3(18) . . ?
C19 C18 H18 119.8 . . ?
C17A C18A H18A 119.4 . . ?
C19A C18A C17A 121.2(17) . . ?
C19A C18A H18A 119.4 . . ?
C18 C19 H19 119.6 . . ?
C18 C19 C20 120.8(17) . . ?
C20 C19 H19 119.6 . . ?
C18A C19A H19A 119.8 . . ?
C18A C19A C20A 120.4(18) . . ?
C20A C19A H19A 119.8 . . ?
C15 C20 C19 115.4(15) . . ?
C15 C20 H20 122.3 . . ?
C19 C20 H20 122.3 . . ?
C15A C20A H20A 119.0 . . ?
C19A C20A C15A 121.9(16) . . ?
C19A C20A H20A 119.0 . . ?
C22 C21 P2 121.8(12) . . ?
C26 C21 P2 113.9(10) . . ?
C26 C21 C22 124.3(14) . . ?
C22A C21A P2 121.8(14) . . ?
C22A C21A C26A 110.7(16) . . ?
C26A C21A P2 127.5(12) . . ?
C21 C22 H22 120.9 . . ?
C21 C22 C23 118.1(19) . . ?
C23 C22 H22 120.9 . . ?
C21A C22A H22A 116.8 . . ?
C21A C22A C23A 126(2) . . ?
C23A C22A H22A 116.8 . . ?
C22 C23 H23 120.9 . . ?
C24 C23 C22 118(2) . . ?
C24 C23 H23 120.9 . . ?
C22A C23A H23A 120.2 . . ?
C24A C23A C22A 120(3) . . ?
C24A C23A H23A 120.2 . . ?
C23 C24 H24 118.6 . . ?
C23 C24 C25 122.7(17) . . ?
C25 C24 H24 118.6 . . ?
C23A C24A H24A 121.6 . . ?
C23A C24A C25A 116.7(19) . . ?
C25A C24A H24A 121.6 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.9(16) . . ?
C26 C25 H25 120.1 . . ?
C24A C25A H25A 119.7 . . ?
C24A C25A C26A 120.5(17) . . ?
C26A C25A H25A 119.7 . . ?
C21 C26 H26 121.7 . . ?
C25 C26 C21 116.6(14) . . ?
C25 C26 H26 121.7 . . ?
C21A C26A H26A 117.2 . . ?
C25A C26A C21A 125.6(15) . . ?
C25A C26A H26A 117.2 . . ?
C28 C27 P2 122.4(6) . . ?
C28 C27 C32 117.9(8) . . ?
C32 C27 P2 119.7(7) . . ?
C27 C28 H28 118.8 . . ?
C27 C28 C29 122.3(8) . . ?
C29 C28 H28 118.8 . . ?
C28 C29 H29 120.6 . . ?
C30 C29 C28 118.8(9) . . ?
C30 C29 H29 120.6 . . ?
C29 C30 H30 120.1 . . ?
C31 C30 C29 119.8(9) . . ?
C31 C30 H30 120.1 . . ?
C30 C31 H31 119.3 . . ?
C30 C31 C32 121.3(8) . . ?
C32 C31 H31 119.3 . . ?
C27 C32 C31 119.9(8) . . ?
C27 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
P2 C33 H33A 109.8 . . ?
P2 C33 H33B 109.8 . . ?
H33A C33 H33B 108.2 . . ?
C34 C33 P2 109.5(6) . . ?
C34 C33 H33A 109.8 . . ?
C34 C33 H33B 109.8 . . ?
S2 C34 H34A 109.6 . . ?
S2 C34 H34B 109.6 . . ?
C33 C34 S2 110.1(5) . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.2 . . ?
S2 C35 H35A 108.6 . . ?
S2 C35 H35B 108.6 . . ?
H35A C35 H35B 107.5 . . ?
C36 C35 S2 114.8(6) . . ?
C36 C35 H35A 108.6 . . ?
C36 C35 H35B 108.6 . . ?
S3 C36 H36A 108.7 . . ?
S3 C36 H36B 108.7 . . ?
C35 C36 S3 114.3(5) . . ?
C35 C36 H36A 108.7 . . ?
C35 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
F2 B1 F1 108.7(7) . . ?
F3 B1 F1 109.2(9) . . ?
F3 B1 F2 107.9(9) . . ?
F4 B1 F1 108.3(9) . . ?
F4 B1 F2 112.6(10) . . ?
F4 B1 F3 110.0(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pt1 S1 C1 C2 67.6(6) . . . . ?
Pt1 S1 C1 C6 -109.0(6) . . . . ?
Pt1 S1 C7 C8 22.8(6) . . . . ?
Pt1 S2 C34 C33 32.2(7) . . . . ?
Pt1 S2 C35 C36 -179.7(5) . . . . ?
Pt1 P1 C8 C7 53.0(5) . . . . ?
Pt1 P1 C9 C10 -157.4(6) . . . . ?
Pt1 P1 C9 C14 20.3(8) . . . . ?
Pt1 P1 C15 C16 91.4(16) . . . . ?
Pt1 P1 C15 C20 -91.3(16) . . . . ?
Pt1 P1 C15A C16A 50.4(19) . . . . ?
Pt1 P1 C15A C20A -125.2(17) . . . . ?
Pt1 P2 C21 C22 -110(3) . . . . ?
Pt1 P2 C21 C26 68.4(17) . . . . ?
Pt1 P2 C21A C22A -118(3) . . . . ?
Pt1 P2 C21A C26A 63(2) . . . . ?
Pt1 P2 C27 C28 11.5(8) . . . . ?
Pt1 P2 C27 C32 -169.3(6) . . . . ?
Pt1 P2 C33 C34 48.7(7) . . . . ?
S1 C1 C2 C3 -176.6(6) . . . . ?
S1 C1 C6 C5 177.3(6) . . . . ?
S1 C7 C8 P1 -49.2(6) . . . . ?
S2 C35 C36 S3 67.6(8) . . . . ?
P1 C9 C10 C11 176.1(7) . . . . ?
P1 C9 C14 C13 -177.1(7) . . . . ?
P1 C15 C16 C17 173.7(15) . . . . ?
P1 C15 C20 C19 -176.6(16) . . . . ?
P1 C15A C16A C17A -175.2(16) . . . . ?
P1 C15A C20A C19A 179.2(17) . . . . ?
P2 C21 C22 C23 175(3) . . . . ?
P2 C21 C26 C25 -178.4(14) . . . . ?
P2 C21A C22A C23A -174(3) . . . . ?
P2 C21A C26A C25A 179.9(17) . . . . ?
P2 C27 C28 C29 177.4(8) . . . . ?
P2 C27 C32 C31 -177.6(7) . . . . ?
P2 C33 C34 S2 -53.0(8) . . . . ?
O2 S3 C36 C35 157.8(7) . . . . ?
O1 S3 C36 C35 -82.7(7) . . . . ?
O3 S3 C36 C35 37.0(8) . . . . ?
C1 S1 C7 C8 138.4(6) . . . . ?
C1 C2 C3 C4 -0.3(12) . . . . ?
C2 C1 C6 C5 0.6(11) . . . . ?
C2 C3 C4 C5 0.2(12) . . . . ?
C3 C4 C5 C6 0.3(13) . . . . ?
C4 C5 C6 C1 -0.7(12) . . . . ?
C6 C1 C2 C3 -0.1(11) . . . . ?
C7 S1 C1 C2 -45.3(7) . . . . ?
C7 S1 C1 C6 138.1(6) . . . . ?
C8 P1 C9 C10 -44.3(8) . . . . ?
C8 P1 C9 C14 133.3(7) . . . . ?
C8 P1 C15 C16 -31.7(16) . . . . ?
C8 P1 C15 C20 145.6(15) . . . . ?
C8 P1 C15A C16A -63.1(18) . . . . ?
C8 P1 C15A C20A 121.3(18) . . . . ?
C9 P1 C8 C7 -65.0(6) . . . . ?
C9 P1 C15 C16 -142.7(14) . . . . ?
C9 P1 C15 C20 34.7(17) . . . . ?
C9 P1 C15A C16A -178.9(15) . . . . ?
C9 P1 C15A C20A 6(2) . . . . ?
C9 C10 C11 C12 1.4(14) . . . . ?
C10 C9 C14 C13 0.5(14) . . . . ?
C10 C11 C12 C13 -0.3(15) . . . . ?
C11 C12 C13 C14 -0.9(15) . . . . ?
C12 C13 C14 C9 0.7(14) . . . . ?
C14 C9 C10 C11 -1.5(13) . . . . ?
C15 P1 C8 C7 -169.6(7) . . . . ?
C15 P1 C9 C10 65.5(9) . . . . ?
C15 P1 C9 C14 -116.9(9) . . . . ?
C15 P1 C15A C16A -164(6) . . . . ?
C15 P1 C15A C20A 20(3) . . . . ?
C15 C16 C17 C18 5(3) . . . . ?
C15A P1 C8 C7 175.4(7) . . . . ?
C15A P1 C9 C10 69.2(10) . . . . ?
C15A P1 C9 C14 -113.2(10) . . . . ?
C15A P1 C15 C16 51(4) . . . . ?
C15A P1 C15 C20 -132(5) . . . . ?
C15A C16A C17A C18A -4(3) . . . . ?
C16 C15 C20 C19 0(3) . . . . ?
C16 C17 C18 C19 -4(3) . . . . ?
C16A C15A C20A C19A 3(3) . . . . ?
C16A C17A C18A C19A 3(3) . . . . ?
C17 C18 C19 C20 0(3) . . . . ?
C17A C18A C19A C20A 1(3) . . . . ?
C18 C19 C20 C15 1(3) . . . . ?
C18A C19A C20A C15A -4(3) . . . . ?
C20 C15 C16 C17 -3(3) . . . . ?
C20A C15A C16A C17A 1(3) . . . . ?
C21 P2 C21A C22A 100(6) . . . . ?
C21 P2 C21A C26A -79(5) . . . . ?
C21 P2 C27 C28 -129.6(10) . . . . ?
C21 P2 C27 C32 49.5(10) . . . . ?
C21 P2 C33 C34 179.0(9) . . . . ?
C21 C22 C23 C24 4(5) . . . . ?
C21A P2 C21 C22 -68(5) . . . . ?
C21A P2 C21 C26 111(5) . . . . ?
C21A P2 C27 C28 -116.3(11) . . . . ?
C21A P2 C27 C32 62.8(10) . . . . ?
C21A P2 C33 C34 174.0(9) . . . . ?
C21A C22A C23A C24A -5(6) . . . . ?
C22 C21 C26 C25 0(4) . . . . ?
C22 C23 C24 C25 -2(4) . . . . ?
C22A C21A C26A C25A 1(4) . . . . ?
C22A C23A C24A C25A 0(4) . . . . ?
C23 C24 C25 C26 -1(3) . . . . ?
C23A C24A C25A C26A 5(3) . . . . ?
C24 C25 C26 C21 2(3) . . . . ?
C24A C25A C26A C21A -6(3) . . . . ?
C26 C21 C22 C23 -3(6) . . . . ?
C26A C21A C22A C23A 5(6) . . . . ?
C27 P2 C21 C22 25(3) . . . . ?
C27 P2 C21 C26 -156.3(14) . . . . ?
C27 P2 C21A C22A 9(3) . . . . ?
C27 P2 C21A C26A -170.3(19) . . . . ?
C27 P2 C33 C34 -71.1(7) . . . . ?
C27 C28 C29 C30 0.7(17) . . . . ?
C28 C27 C32 C31 1.6(13) . . . . ?
C28 C29 C30 C31 0.5(16) . . . . ?
C29 C30 C31 C32 -0.7(15) . . . . ?
C30 C31 C32 C27 -0.4(14) . . . . ?
C32 C27 C28 C29 -1.7(15) . . . . ?
C33 P2 C21 C22 134(3) . . . . ?
C33 P2 C21 C26 -47.5(16) . . . . ?
C33 P2 C21A C22A 123(3) . . . . ?
C33 P2 C21A C26A -56(2) . . . . ?
C33 P2 C27 C28 125.3(8) . . . . ?
C33 P2 C27 C32 -55.5(7) . . . . ?
C34 S2 C35 C36 71.1(7) . . . . ?
C35 S2 C34 C33 138.9(7) . . . . ?

_olex2_date_sample_data_collection 2015-10-20
_olex2_date_sample_submission    2015-10-20
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx0591
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cx0613
_database_code_depnum_ccdc_archive 'CCDC 1469903'
_audit_update_record             
;
2016-03-21 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_audit_creation_date             2016-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        'pyridinium BArF'
_chemical_formula_moiety         'C32 H12 B F24, 2(C2.5 H3 N0.5)'
_chemical_formula_sum            'C37 H18 B F24 N'
_chemical_formula_weight         943.33
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.3832(6)
_cell_length_b                   12.7027(6)
_cell_length_c                   13.6428(6)
_cell_angle_alpha                79.884(3)
_cell_angle_beta                 76.218(3)
_cell_angle_gamma                63.750(3)
_cell_volume                     1863.20(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8509
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.560
_cell_measurement_theta_min      3.082
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.965
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0640 before and 0.0372 after correction.
The Ratio of minimum to maximum transmission is 0.9342.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.017
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27044
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         1.793
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   microsource
_diffrn_special_details          ?
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6936
_reflns_number_total             9629
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         9629
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0636
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0860P)²+1.9010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1830
_refine_special_details          
'Distance restraintes were imposed on the disordered flourine atoms. The enhanced rigid-bond restraint (SHELX keyword RIGU) was applied on the disordered flourine atoms. (Acta Cryst. A68 (2012) 448-451). The disordered pyridinium was constrained to certain positions.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Shared sites
{C38, N1}
{C35, N2}
{C33, N3}
3. Restrained distances
 C34-H34
 0.95 with sigma of 0.02
 F14A-F13A \\sim F14-F13
 with sigma of 0.01
 F15-C23 \\sim F14A-C23 \\sim F14-C23 \\sim F13A-C23 \\sim F13-C23 \\sim
F15A-C23
 with sigma of 0.01
4. Rigid bond restraints
 F13, F13A, F14, F14A, F15, F15A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
F13 \\sim F13A \\sim F14 \\sim F14A \\sim F15 \\sim F15A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.001
Uanis(C38) = Uanis(N1)
Uanis(C35) = Uanis(N2)
Uanis(C33) = Uanis(N3)
6. Others
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Fixed Sof: N1(0.5) H1(0.5) H36(0.5) H36A(0.5) H37(0.5) H37A(0.5) C38(0.5)
 H38(0.5) N2(0.25) H2A(0.25) N3(0.25) H3(0.25) C33(0.75) H33(0.75) C35(0.75)
 H35(0.75)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C10(H10), C12(H12), C14(H14), C17(H17), C19(H19),
 C21(H21), C26(H26), C28(H28), C30(H30), N1(H1), C36(H36), C36(H36A), C37(H37),
 C37(H37A), C38(H38), N2(H2A), N3(H3), C33(H33), C35(H35)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.44071(18) 0.65140(19) 0.05844(17) 0.0578(6) Uani 1 1 d . . . . .
F2 F 0.6024(2) 0.6136(2) -0.04892(15) 0.0676(7) Uani 1 1 d . . . . .
F3 F 0.5279(2) 0.76720(15) 0.03192(19) 0.0631(6) Uani 1 1 d . . . . .
F4 F 0.86278(19) 0.67532(17) 0.21311(18) 0.0562(5) Uani 1 1 d . . . . .
F5 F 0.74597(19) 0.6734(2) 0.35404(19) 0.0698(7) Uani 1 1 d . . . . .
F6 F 0.91582(17) 0.52416(15) 0.31548(17) 0.0499(5) Uani 1 1 d . . . . .
F7 F 0.5036(2) 0.3402(3) 0.61976(19) 0.0902(10) Uani 1 1 d . . . . .
F8 F 0.6421(3) 0.3962(3) 0.6079(2) 0.1005(12) Uani 1 1 d . . . . .
F9 F 0.6372(2) 0.2505(2) 0.70981(15) 0.0714(7) Uani 1 1 d . . . . .
F10 F 0.95116(18) -0.12262(17) 0.58376(15) 0.0517(5) Uani 1 1 d . . . . .
F11 F 0.9993(2) -0.14529(17) 0.42787(16) 0.0654(6) Uani 1 1 d . . . . .
F12 F 0.8356(2) -0.1564(2) 0.5136(3) 0.0999(12) Uani 1 1 d . . . . .
F13 F 0.2466(3) 0.4768(3) 0.2590(3) 0.0426(7) Uani 0.600(7) 1 d D U P A 1
F13A F 0.2556(5) 0.4848(4) 0.2927(5) 0.0419(7) Uani 0.400(7) 1 d D U P A 2
F14 F 0.2547(4) 0.3880(4) 0.4083(3) 0.0422(7) Uani 0.600(7) 1 d D U P A 1
F14A F 0.2386(5) 0.3562(5) 0.4123(4) 0.0415(7) Uani 0.400(7) 1 d D U P A 2
F15 F 0.1824(3) 0.3393(3) 0.3044(4) 0.0386(6) Uani 0.600(7) 1 d D U P A 1
F15A F 0.1853(4) 0.3662(5) 0.2696(5) 0.0402(6) Uani 0.400(7) 1 d D U P A 2
F16 F 0.48680(15) -0.06752(13) 0.25325(12) 0.0332(4) Uani 1 1 d . . . . .
F17 F 0.66547(13) -0.09508(12) 0.16742(13) 0.0330(4) Uani 1 1 d . . . . .
F18 F 0.50782(14) -0.00791(13) 0.09620(12) 0.0318(3) Uani 1 1 d . . . . .
F19 F 0.83425(15) 0.15961(15) -0.14852(12) 0.0355(4) Uani 1 1 d . . . . .
F20 F 1.02128(15) 0.13194(16) -0.20171(12) 0.0400(4) Uani 1 1 d . . . . .
F21 F 0.88316(17) 0.30460(13) -0.16985(12) 0.0388(4) Uani 1 1 d . . . . .
F22 F 1.28335(12) -0.01332(13) 0.05207(12) 0.0314(3) Uani 1 1 d . . . . .
F23 F 1.24132(14) 0.16350(14) 0.07744(14) 0.0369(4) Uani 1 1 d . . . . .
F24 F 1.21221(14) 0.04363(17) 0.20246(12) 0.0417(4) Uani 1 1 d . . . . .
C1 C 0.70753(19) 0.39401(18) 0.21858(17) 0.0183(4) Uani 1 1 d . . . . .
C2 C 0.6361(2) 0.46801(19) 0.14784(17) 0.0194(4) Uani 1 1 d . . . . .
H2 H 0.5946 0.4388 0.1172 0.023 Uiso 1 1 calc R . . . .
C3 C 0.6236(2) 0.58336(19) 0.12061(18) 0.0213(4) Uani 1 1 d . . . . .
C4 C 0.6834(2) 0.62914(19) 0.16325(19) 0.0236(5) Uani 1 1 d . . . . .
H4 H 0.6756 0.7075 0.1447 0.028 Uiso 1 1 calc R . . . .
C5 C 0.7546(2) 0.5573(2) 0.23349(19) 0.0226(5) Uani 1 1 d . . . . .
C6 C 0.7665(2) 0.44266(19) 0.26127(18) 0.0204(4) Uani 1 1 d . . . . .
H6 H 0.8155 0.3960 0.3102 0.025 Uiso 1 1 calc R . . . .
C7 C 0.5490(2) 0.6553(2) 0.0418(2) 0.0281(5) Uani 1 1 d . . . . .
C8 C 0.8192(2) 0.6059(2) 0.2815(2) 0.0315(6) Uani 1 1 d . . . . .
C9 C 0.7581(2) 0.19956(19) 0.35329(17) 0.0189(4) Uani 1 1 d . . . . .
C10 C 0.6929(2) 0.2687(2) 0.43556(18) 0.0232(5) Uani 1 1 d . . . . .
H10 H 0.6445 0.3504 0.4227 0.028 Uiso 1 1 calc R . . . .
C11 C 0.6970(2) 0.2213(2) 0.53546(19) 0.0281(5) Uani 1 1 d . . . . .
C12 C 0.7661(2) 0.1031(2) 0.55834(19) 0.0299(5) Uani 1 1 d . . . . .
H12 H 0.7689 0.0711 0.6266 0.036 Uiso 1 1 calc R . . . .
C13 C 0.8314(2) 0.0326(2) 0.47817(19) 0.0265(5) Uani 1 1 d . . . . .
C14 C 0.8279(2) 0.0797(2) 0.37848(18) 0.0212(4) Uani 1 1 d . . . . .
H14 H 0.8743 0.0292 0.3255 0.025 Uiso 1 1 calc R . . . .
C15 C 0.6223(3) 0.3018(3) 0.6191(2) 0.0395(7) Uani 1 1 d . . . . .
C16 C 0.9027(3) -0.0973(3) 0.5014(2) 0.0351(6) Uani 1 1 d . . . . .
C17 C 0.4962(2) 0.31048(19) 0.26686(17) 0.0189(4) Uani 1 1 d . . . . .
H17 H 0.4823 0.3833 0.2883 0.023 Uiso 1 1 calc R . . . .
C18 C 0.3966(2) 0.2846(2) 0.27261(17) 0.0209(4) Uani 1 1 d . . . . .
C19 C 0.4125(2) 0.1785(2) 0.24451(18) 0.0211(4) Uani 1 1 d . . . . .
H19 H 0.3445 0.1606 0.2494 0.025 Uiso 1 1 calc R . . . .
C20 C 0.5310(2) 0.09887(19) 0.20889(17) 0.0191(4) Uani 1 1 d . . . . .
C21 C 0.63047(19) 0.12530(18) 0.20043(17) 0.0177(4) Uani 1 1 d . . . . .
H21 H 0.7100 0.0699 0.1738 0.021 Uiso 1 1 calc R . . . .
C22 C 0.61687(19) 0.23185(18) 0.23015(16) 0.0169(4) Uani 1 1 d . . . . .
C23 C 0.2699(2) 0.3728(2) 0.31106(18) 0.0262(5) Uani 1 1 d D . . . .
C24 C 0.5476(2) -0.0169(2) 0.18065(18) 0.0221(5) Uani 1 1 d . . . . .
C25 C 0.85399(19) 0.19413(17) 0.14993(17) 0.0168(4) Uani 1 1 d . . . . .
C26 C 0.84011(19) 0.20148(18) 0.04926(17) 0.0181(4) Uani 1 1 d . . . . .
H26 H 0.7602 0.2289 0.0349 0.022 Uiso 1 1 calc R . . . .
C27 C 0.9402(2) 0.16974(18) -0.03013(17) 0.0186(4) Uani 1 1 d . . . . .
C28 C 1.0586(2) 0.12700(19) -0.01195(17) 0.0200(4) Uani 1 1 d . . . . .
H28 H 1.1269 0.1049 -0.0659 0.024 Uiso 1 1 calc R . . . .
C29 C 1.07466(19) 0.11727(19) 0.08719(18) 0.0198(4) Uani 1 1 d . . . . .
C30 C 0.97468(19) 0.15111(18) 0.16626(17) 0.0181(4) Uani 1 1 d . . . . .
H30 H 0.9884 0.1450 0.2331 0.022 Uiso 1 1 calc R . . . .
C31 C 0.9195(2) 0.1907(2) -0.13712(18) 0.0219(4) Uani 1 1 d . . . . .
C32 C 1.2023(2) 0.0766(2) 0.10531(19) 0.0246(5) Uani 1 1 d . . . . .
B1 B 0.7349(2) 0.2540(2) 0.23821(19) 0.0167(4) Uani 1 1 d . . . . .
N1 N 0.9532(2) 0.4184(2) 0.0338(2) 0.0363(6) Uani 0.5 1 d . . P B 2
H1 H 0.9228 0.3658 0.0555 0.044 Uiso 0.5 1 calc R . P B 2
C36 C 0.9661(3) 0.5756(3) -0.0834(2) 0.0402(7) Uani 1 1 d . . . . .
H36 H 0.9426 0.6281 -0.1411 0.048 Uiso 0.5 1 calc R . P C 1
H36A H 0.9426 0.6281 -0.1411 0.048 Uiso 0.5 1 calc R . P D 2
C37 C 0.9194(3) 0.4939(3) -0.0496(2) 0.0400(7) Uani 1 1 d . . . . .
H37 H 0.8635 0.4893 -0.0839 0.048 Uiso 0.5 1 calc R . P B 1
H37A H 0.8635 0.4893 -0.0839 0.048 Uiso 0.5 1 calc R . P B 2
C38 C 0.9532(2) 0.4184(2) 0.0338(2) 0.0363(6) Uani 0.5 1 d . . P B 1
H38 H 0.9204 0.3617 0.0573 0.044 Uiso 0.5 1 calc R . P B 1
N2 N 0.5589(2) 0.0680(2) 0.44883(19) 0.0300(5) Uani 0.25 1 d . . P E 4
H2A H 0.5971 0.1115 0.4159 0.036 Uiso 0.25 1 calc R . P E 4
N3 N 0.5468(3) -0.1164(3) 0.4822(2) 0.0386(6) Uani 0.25 1 d . . P E 6
H3 H 0.5769 -0.1911 0.4709 0.046 Uiso 0.25 1 calc R . P E 6
C33 C 0.5468(3) -0.1164(3) 0.4822(2) 0.0386(6) Uani 0.75 1 d . . P E .
H33 H 0.5793 -0.1971 0.4700 0.046 Uiso 0.75 1 calc R . P F 5
C34 C 0.6049(3) -0.0480(3) 0.4314(2) 0.0357(6) Uani 1 1 d D . . . .
H34 H 0.679(2) -0.075(3) 0.384(2) 0.061(11) Uiso 1 1 d D . . . .
C35 C 0.5589(2) 0.0680(2) 0.44883(19) 0.0300(5) Uani 0.75 1 d . . P E .
H35 H 0.6002 0.1149 0.4133 0.036 Uiso 0.75 1 calc R . P G 7


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C7 1.328(3) . ?
F2 C7 1.334(3) . ?
F3 C7 1.315(3) . ?
F4 C8 1.354(3) . ?
F5 C8 1.311(3) . ?
F6 C8 1.312(3) . ?
F7 C15 1.326(4) . ?
F8 C15 1.303(4) . ?
F9 C15 1.307(4) . ?
F10 C16 1.322(3) . ?
F11 C16 1.345(4) . ?
F12 C16 1.313(3) . ?
F13 C23 1.328(4) . ?
F13A C23 1.339(5) . ?
F14 C23 1.331(4) . ?
F14A C23 1.348(5) . ?
F15 C23 1.353(4) . ?
F15A C23 1.342(5) . ?
F16 C24 1.346(3) . ?
F17 C24 1.343(3) . ?
F18 C24 1.326(3) . ?
F19 C31 1.328(3) . ?
F20 C31 1.339(3) . ?
F21 C31 1.337(3) . ?
F22 C32 1.330(3) . ?
F23 C32 1.354(3) . ?
F24 C32 1.336(3) . ?
C1 C2 1.396(3) . ?
C1 C6 1.408(3) . ?
C1 B1 1.641(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.395(3) . ?
C3 C4 1.389(3) . ?
C3 C7 1.492(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(4) . ?
C5 C6 1.390(3) . ?
C5 C8 1.509(3) . ?
C6 H6 0.9500 . ?
C9 C10 1.403(3) . ?
C9 C14 1.406(3) . ?
C9 B1 1.638(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.393(4) . ?
C11 C12 1.382(4) . ?
C11 C15 1.508(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.391(4) . ?
C13 C14 1.389(3) . ?
C13 C16 1.505(4) . ?
C14 H14 0.9500 . ?
C17 H17 0.9500 . ?
C17 C18 1.393(3) . ?
C17 C22 1.407(3) . ?
C18 C19 1.383(3) . ?
C18 C23 1.501(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.390(3) . ?
C20 C21 1.389(3) . ?
C20 C24 1.498(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.408(3) . ?
C22 B1 1.637(3) . ?
C25 C26 1.406(3) . ?
C25 C30 1.406(3) . ?
C25 B1 1.639(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.394(3) . ?
C27 C28 1.388(3) . ?
C27 C31 1.500(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.390(3) . ?
C29 C30 1.392(3) . ?
C29 C32 1.499(3) . ?
C30 H30 0.9500 . ?
N1 H1 0.8800 . ?
N1 C36 1.368(4) 2_765 ?
N1 C37 1.370(4) . ?
C36 N1 1.368(4) 2_765 ?
C36 H36 0.9500 . ?
C36 H36A 0.9500 . ?
C36 C37 1.363(5) . ?
C36 C38 1.368(4) 2_765 ?
C37 H37 0.9500 . ?
C37 H37A 0.9500 . ?
N2 H2A 0.8800 . ?
N2 C33 1.372(4) 2_656 ?
N2 C34 1.366(4) . ?
N3 H3 0.8800 . ?
N3 C34 1.362(5) . ?
N3 C35 1.372(4) 2_656 ?
C34 H34 0.944(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 116.1(2) . . ?
C2 C1 B1 121.06(19) . . ?
C6 C1 B1 122.4(2) . . ?
C1 C2 H2 118.9 . . ?
C3 C2 C1 122.2(2) . . ?
C3 C2 H2 118.9 . . ?
C2 C3 C7 118.9(2) . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 C7 120.5(2) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 C3 118.1(2) . . ?
C5 C4 H4 121.0 . . ?
C4 C5 C6 121.4(2) . . ?
C4 C5 C8 118.9(2) . . ?
C6 C5 C8 119.7(2) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 C1 121.6(2) . . ?
C5 C6 H6 119.2 . . ?
F1 C7 F2 103.7(2) . . ?
F1 C7 C3 112.8(2) . . ?
F2 C7 C3 111.3(2) . . ?
F3 C7 F1 106.7(2) . . ?
F3 C7 F2 107.3(2) . . ?
F3 C7 C3 114.2(2) . . ?
F4 C8 C5 110.9(2) . . ?
F5 C8 F4 105.2(2) . . ?
F5 C8 F6 109.6(3) . . ?
F5 C8 C5 112.6(2) . . ?
F6 C8 F4 104.6(2) . . ?
F6 C8 C5 113.3(2) . . ?
C10 C9 C14 115.6(2) . . ?
C10 C9 B1 120.4(2) . . ?
C14 C9 B1 123.39(19) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 C9 122.1(2) . . ?
C11 C10 H10 119.0 . . ?
C10 C11 C15 118.4(3) . . ?
C12 C11 C10 121.3(2) . . ?
C12 C11 C15 120.3(3) . . ?
C11 C12 H12 121.1 . . ?
C11 C12 C13 117.8(2) . . ?
C13 C12 H12 121.1 . . ?
C12 C13 C16 118.6(2) . . ?
C14 C13 C12 121.1(2) . . ?
C14 C13 C16 120.3(2) . . ?
C9 C14 H14 118.9 . . ?
C13 C14 C9 122.2(2) . . ?
C13 C14 H14 118.9 . . ?
F7 C15 C11 110.5(2) . . ?
F8 C15 F7 105.5(3) . . ?
F8 C15 F9 109.0(3) . . ?
F8 C15 C11 112.7(2) . . ?
F9 C15 F7 104.8(3) . . ?
F9 C15 C11 113.7(3) . . ?
F10 C16 F11 104.1(2) . . ?
F10 C16 C13 113.4(2) . . ?
F11 C16 C13 112.3(2) . . ?
F12 C16 F10 107.0(2) . . ?
F12 C16 F11 107.0(3) . . ?
F12 C16 C13 112.4(2) . . ?
C18 C17 H17 119.1 . . ?
C18 C17 C22 121.9(2) . . ?
C22 C17 H17 119.1 . . ?
C17 C18 C23 119.4(2) . . ?
C19 C18 C17 121.2(2) . . ?
C19 C18 C23 119.4(2) . . ?
C18 C19 H19 121.0 . . ?
C18 C19 C20 118.0(2) . . ?
C20 C19 H19 121.0 . . ?
C19 C20 C24 117.66(19) . . ?
C21 C20 C19 121.2(2) . . ?
C21 C20 C24 121.17(19) . . ?
C20 C21 H21 119.1 . . ?
C20 C21 C22 121.9(2) . . ?
C22 C21 H21 119.1 . . ?
C17 C22 C21 115.84(19) . . ?
C17 C22 B1 121.66(18) . . ?
C21 C22 B1 121.83(18) . . ?
F13 C23 F14 107.9(3) . . ?
F13 C23 F15 107.6(3) . . ?
F13 C23 C18 110.9(2) . . ?
F13A C23 F14A 105.6(3) . . ?
F13A C23 F15A 106.1(4) . . ?
F13A C23 C18 114.0(3) . . ?
F14 C23 F15 106.0(3) . . ?
F14 C23 C18 111.7(2) . . ?
F14A C23 C18 111.4(3) . . ?
F15 C23 C18 112.4(2) . . ?
F15A C23 F14A 107.3(4) . . ?
F15A C23 C18 112.0(3) . . ?
F16 C24 C20 111.69(19) . . ?
F17 C24 F16 106.02(19) . . ?
F17 C24 C20 112.28(18) . . ?
F18 C24 F16 106.26(18) . . ?
F18 C24 F17 106.86(19) . . ?
F18 C24 C20 113.24(19) . . ?
C26 C25 B1 120.77(19) . . ?
C30 C25 C26 116.22(19) . . ?
C30 C25 B1 122.19(19) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 C25 121.9(2) . . ?
C27 C26 H26 119.0 . . ?
C26 C27 C31 119.7(2) . . ?
C28 C27 C26 120.7(2) . . ?
C28 C27 C31 119.4(2) . . ?
C27 C28 H28 120.8 . . ?
C27 C28 C29 118.3(2) . . ?
C29 C28 H28 120.8 . . ?
C28 C29 C30 121.0(2) . . ?
C28 C29 C32 117.9(2) . . ?
C30 C29 C32 121.0(2) . . ?
C25 C30 H30 119.1 . . ?
C29 C30 C25 121.8(2) . . ?
C29 C30 H30 119.1 . . ?
F19 C31 F20 106.81(18) . . ?
F19 C31 F21 106.5(2) . . ?
F19 C31 C27 113.19(19) . . ?
F20 C31 C27 112.33(19) . . ?
F21 C31 F20 106.3(2) . . ?
F21 C31 C27 111.26(18) . . ?
F22 C32 F23 105.90(19) . . ?
F22 C32 F24 107.25(19) . . ?
F22 C32 C29 112.8(2) . . ?
F23 C32 C29 111.01(19) . . ?
F24 C32 F23 106.4(2) . . ?
F24 C32 C29 113.07(19) . . ?
C9 B1 C1 112.76(17) . . ?
C9 B1 C25 113.83(18) . . ?
C22 B1 C1 111.88(17) . . ?
C22 B1 C9 103.03(16) . . ?
C22 B1 C25 112.96(17) . . ?
C25 B1 C1 102.74(16) . . ?
C36 N1 H1 119.9 2_765 . ?
C36 N1 C37 120.2(3) 2_765 . ?
C37 N1 H1 119.9 . . ?
N1 C36 H36A 120.1 2_765 . ?
C37 C36 N1 119.7(3) . 2_765 ?
C37 C36 H36 120.1 . . ?
C37 C36 H36A 120.1 . . ?
C37 C36 C38 119.7(3) . 2_765 ?
C38 C36 H36 120.1 2_765 . ?
N1 C37 H37A 120.0 . . ?
C36 C37 N1 120.1(3) . . ?
C36 C37 H37 120.0 . . ?
C36 C37 H37A 120.0 . . ?
C33 N2 H2A 120.1 2_656 . ?
C34 N2 H2A 120.1 . . ?
C34 N2 C33 119.9(3) . 2_656 ?
C34 N3 H3 120.3 . . ?
C34 N3 C35 119.5(3) . 2_656 ?
C35 N3 H3 120.3 2_656 . ?
N2 C34 H34 115(2) . . ?
N3 C34 H34 124(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.4(3) . . . . ?
C1 C2 C3 C7 177.9(2) . . . . ?
C2 C1 C6 C5 -0.6(3) . . . . ?
C2 C1 B1 C9 -151.82(19) . . . . ?
C2 C1 B1 C22 -36.2(3) . . . . ?
C2 C1 B1 C25 85.2(2) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
C2 C3 C7 F1 48.5(3) . . . . ?
C2 C3 C7 F2 -67.6(3) . . . . ?
C2 C3 C7 F3 170.6(2) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C3 C4 C5 C8 -179.3(2) . . . . ?
C4 C3 C7 F1 -133.9(2) . . . . ?
C4 C3 C7 F2 109.9(3) . . . . ?
C4 C3 C7 F3 -11.9(3) . . . . ?
C4 C5 C6 C1 0.6(3) . . . . ?
C4 C5 C8 F4 -38.7(3) . . . . ?
C4 C5 C8 F5 78.9(3) . . . . ?
C4 C5 C8 F6 -156.0(2) . . . . ?
C6 C1 C2 C3 0.1(3) . . . . ?
C6 C1 B1 C9 36.6(3) . . . . ?
C6 C1 B1 C22 152.2(2) . . . . ?
C6 C1 B1 C25 -86.3(2) . . . . ?
C6 C5 C8 F4 142.0(2) . . . . ?
C6 C5 C8 F5 -100.4(3) . . . . ?
C6 C5 C8 F6 24.7(4) . . . . ?
C7 C3 C4 C5 -177.9(2) . . . . ?
C8 C5 C6 C1 179.8(2) . . . . ?
C9 C10 C11 C12 0.1(4) . . . . ?
C9 C10 C11 C15 -179.0(2) . . . . ?
C10 C9 C14 C13 0.5(3) . . . . ?
C10 C9 B1 C1 35.6(3) . . . . ?
C10 C9 B1 C22 -85.2(2) . . . . ?
C10 C9 B1 C25 152.14(19) . . . . ?
C10 C11 C12 C13 -0.2(4) . . . . ?
C10 C11 C15 F7 65.9(3) . . . . ?
C10 C11 C15 F8 -51.9(4) . . . . ?
C10 C11 C15 F9 -176.6(2) . . . . ?
C11 C12 C13 C14 0.4(4) . . . . ?
C11 C12 C13 C16 -177.3(2) . . . . ?
C12 C11 C15 F7 -113.3(3) . . . . ?
C12 C11 C15 F8 129.0(3) . . . . ?
C12 C11 C15 F9 4.3(4) . . . . ?
C12 C13 C14 C9 -0.6(4) . . . . ?
C12 C13 C16 F10 -35.0(3) . . . . ?
C12 C13 C16 F11 -152.7(2) . . . . ?
C12 C13 C16 F12 86.6(3) . . . . ?
C14 C9 C10 C11 -0.3(3) . . . . ?
C14 C9 B1 C1 -154.0(2) . . . . ?
C14 C9 B1 C22 85.2(2) . . . . ?
C14 C9 B1 C25 -37.5(3) . . . . ?
C14 C13 C16 F10 147.3(2) . . . . ?
C14 C13 C16 F11 29.6(3) . . . . ?
C14 C13 C16 F12 -91.1(3) . . . . ?
C15 C11 C12 C13 178.9(2) . . . . ?
C16 C13 C14 C9 177.0(2) . . . . ?
C17 C18 C19 C20 -0.9(3) . . . . ?
C17 C18 C23 F13 54.4(4) . . . . ?
C17 C18 C23 F13A 29.6(5) . . . . ?
C17 C18 C23 F14 -66.0(4) . . . . ?
C17 C18 C23 F14A -89.8(4) . . . . ?
C17 C18 C23 F15 174.9(3) . . . . ?
C17 C18 C23 F15A 150.0(4) . . . . ?
C17 C22 B1 C1 -37.8(3) . . . . ?
C17 C22 B1 C9 83.6(2) . . . . ?
C17 C22 B1 C25 -153.2(2) . . . . ?
C18 C17 C22 C21 -0.5(3) . . . . ?
C18 C17 C22 B1 -171.3(2) . . . . ?
C18 C19 C20 C21 -0.8(3) . . . . ?
C18 C19 C20 C24 178.8(2) . . . . ?
C19 C18 C23 F13 -126.3(3) . . . . ?
C19 C18 C23 F13A -151.1(4) . . . . ?
C19 C18 C23 F14 113.3(3) . . . . ?
C19 C18 C23 F14A 89.5(4) . . . . ?
C19 C18 C23 F15 -5.7(4) . . . . ?
C19 C18 C23 F15A -30.6(5) . . . . ?
C19 C20 C21 C22 1.9(3) . . . . ?
C19 C20 C24 F16 -48.3(3) . . . . ?
C19 C20 C24 F17 -167.2(2) . . . . ?
C19 C20 C24 F18 71.7(3) . . . . ?
C20 C21 C22 C17 -1.2(3) . . . . ?
C20 C21 C22 B1 169.6(2) . . . . ?
C21 C20 C24 F16 131.3(2) . . . . ?
C21 C20 C24 F17 12.3(3) . . . . ?
C21 C20 C24 F18 -108.8(2) . . . . ?
C21 C22 B1 C1 151.9(2) . . . . ?
C21 C22 B1 C9 -86.7(2) . . . . ?
C21 C22 B1 C25 36.5(3) . . . . ?
C22 C17 C18 C19 1.6(3) . . . . ?
C22 C17 C18 C23 -179.1(2) . . . . ?
C23 C18 C19 C20 179.8(2) . . . . ?
C24 C20 C21 C22 -177.6(2) . . . . ?
C25 C26 C27 C28 1.4(3) . . . . ?
C25 C26 C27 C31 -173.87(19) . . . . ?
C26 C25 C30 C29 -0.3(3) . . . . ?
C26 C25 B1 C1 -78.3(2) . . . . ?
C26 C25 B1 C9 159.45(18) . . . . ?
C26 C25 B1 C22 42.4(3) . . . . ?
C26 C27 C28 C29 -0.4(3) . . . . ?
C26 C27 C31 F19 -44.3(3) . . . . ?
C26 C27 C31 F20 -165.41(19) . . . . ?
C26 C27 C31 F21 75.5(3) . . . . ?
C27 C28 C29 C30 -0.9(3) . . . . ?
C27 C28 C29 C32 -177.09(19) . . . . ?
C28 C27 C31 F19 140.4(2) . . . . ?
C28 C27 C31 F20 19.3(3) . . . . ?
C28 C27 C31 F21 -99.8(2) . . . . ?
C28 C29 C30 C25 1.3(3) . . . . ?
C28 C29 C32 F22 -43.2(3) . . . . ?
C28 C29 C32 F23 75.4(3) . . . . ?
C28 C29 C32 F24 -165.1(2) . . . . ?
C30 C25 C26 C27 -1.0(3) . . . . ?
C30 C25 B1 C1 90.9(2) . . . . ?
C30 C25 B1 C9 -31.4(3) . . . . ?
C30 C25 B1 C22 -148.44(19) . . . . ?
C30 C29 C32 F22 140.6(2) . . . . ?
C30 C29 C32 F23 -100.7(2) . . . . ?
C30 C29 C32 F24 18.7(3) . . . . ?
C31 C27 C28 C29 174.89(19) . . . . ?
C32 C29 C30 C25 177.3(2) . . . . ?
B1 C1 C2 C3 -172.0(2) . . . . ?
B1 C1 C6 C5 171.4(2) . . . . ?
B1 C9 C10 C11 170.8(2) . . . . ?
B1 C9 C14 C13 -170.3(2) . . . . ?
B1 C25 C26 C27 168.76(18) . . . . ?
B1 C25 C30 C29 -169.90(19) . . . . ?
N1 C36 C37 N1 0.1(4) 2_765 . . . ?
C36 N1 C37 C36 -0.1(4) 2_765 . . . ?
C38 C36 C37 N1 0.1(4) 2_765 . . . ?
C33 N2 C34 N3 -0.2(5) 2_656 . . . ?
C35 N3 C34 N2 0.2(5) 2_656 . . . ?

_olex2_date_sample_data_collection 2015-11-11
_olex2_date_sample_submission    2015-11-11
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx0613
_olex2_submission_special_instructions 'No special instructions were received'
