# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1865716'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;

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

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

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

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

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

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   12.7979(6)
_cell_length_b                   13.2777(6)
_cell_length_c                   16.1350(9)
_cell_angle_alpha                84.604(2)
_cell_angle_beta                 77.121(2)
_cell_angle_gamma                70.633(2)
_cell_volume                     2520.9(2)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

_chemical_formula_sum            'C52 H51 F6 N3 O6 P2 Pd1 S2'
_chemical_formula_moiety         'C50 H51 N3 P2 Pd, 2(C F3 O3 S)'
_chemical_compound_source        ?
_chemical_formula_weight         1160.46


_cell_measurement_reflns_used    9892
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25
_cell_measurement_temperature    100

_exptl_crystal_description       planar
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.180

_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1188
_exptl_absorpt_coefficient_mu    0.590

# Sheldrick geometric approximatio 0.92 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.95
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            72138
_reflns_number_total             9939
_diffrn_reflns_av_R_equivalents  0.069
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9939 
# Theoretical number of reflections is about 19974 


_diffrn_reflns_theta_min         1.295
_diffrn_reflns_theta_max         26.071
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        25.550
_diffrn_measured_fraction_theta_full 0.996


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

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

_refine_diff_density_min         -0.52
_refine_diff_density_max         0.74


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         7672
_refine_ls_number_restraints     0
_refine_ls_number_parameters     649
_oxford_refine_ls_R_factor_ref   0.0385
_refine_ls_wR_factor_ref         0.0403
_refine_ls_goodness_of_fit_ref   1.1235
_refine_ls_shift/su_max          0.0009283
_refine_ls_shift/su_mean         0.0000262


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9910
_refine_ls_R_factor_all          0.0570
_refine_ls_wR_factor_all         0.0576

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8162
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_gt          0.0418

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


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.242 0.129 0.991E-01 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.1866(3) 1.1007(3) 0.1499(2) 0.0568 0.7500 Uani . . . . . .
F2 F 0.09331(18) 1.19785(18) 0.05717(17) 0.0444 1.0000 Uani . . . . . .
F3 F 0.26187(19) 1.09153(18) 0.01698(17) 0.0487 1.0000 Uani . . . . . .
F4 F 0.8740(2) 1.0681(2) 0.38524(18) 0.0584 1.0000 Uani . . . . . .
F5 F 0.9027(2) 1.0851(2) 0.2492(2) 0.0667 1.0000 Uani . . . . . .
F6 F 0.9287(2) 0.92968(19) 0.30699(17) 0.0498 1.0000 Uani . . . . . .
O1 O 0.1741(3) 1.3218(3) 0.1634(2) 0.0395 0.7500 Uani . . . . . .
O2 O 0.2478(3) 1.3247(3) 0.0130(2) 0.0407 0.7500 Uani . . . . . .
O3 O 0.3630(3) 1.2084(3) 0.1038(2) 0.0379 0.7500 Uani . . . . . .
O4 O 0.6574(3) 1.1541(2) 0.3231(3) 0.0598 1.0000 Uani . . . . . .
O5 O 0.7221(2) 0.9928(2) 0.24142(17) 0.0408 1.0000 Uani . . . . . .
O6 O 0.6901(3) 0.9815(2) 0.39475(18) 0.0483 1.0000 Uani . . . . . .
P1 P 0.38195(7) 0.75093(6) 0.16356(5) 0.0201 1.0000 Uani . . . . . .
P2 P 0.76200(7) 0.65488(6) 0.38643(5) 0.0212 1.0000 Uani . . . . . .
N1 N 0.4775(2) 0.9864(2) 0.24185(18) 0.0238 1.0000 Uani . . . . . .
N2 N 0.4365(2) 0.9319(2) 0.37138(18) 0.0240 1.0000 Uani . . . . . .
N3 N 0.7375(2) 0.5320(2) 0.17875(16) 0.0200 1.0000 Uani . . . . . .
C1 C 0.4902(3) 0.8990(2) 0.2923(2) 0.0206 1.0000 Uani . . . . . .
C2 C 0.4132(3) 1.0759(3) 0.2897(3) 0.0324 1.0000 Uani . . . . . .
C3 C 0.3877(3) 1.0421(3) 0.3702(3) 0.0310 1.0000 Uani . . . . . .
C4 C 0.4335(3) 0.8551(3) 0.4417(2) 0.0277 1.0000 Uani . . . . . .
C5 C 0.5530(3) 0.7929(3) 0.4542(2) 0.0311 1.0000 Uani . . . . . .
C6 C 0.6412(3) 0.7603(3) 0.3703(2) 0.0232 1.0000 Uani . . . . . .
C7 C 0.5278(3) 0.9778(3) 0.1516(2) 0.0258 1.0000 Uani . . . . . .
C8 C 0.4837(3) 0.9060(3) 0.1095(2) 0.0249 1.0000 Uani . . . . . .
C9 C 0.5061(3) 0.7893(2) 0.14623(19) 0.0187 1.0000 Uani . . . . . .
C10 C 0.4150(3) 0.6072(3) 0.1673(2) 0.0241 1.0000 Uani . . . . . .
C11 C 0.3935(3) 0.5577(3) 0.1031(2) 0.0280 1.0000 Uani . . . . . .
C12 C 0.4124(3) 0.4485(3) 0.1080(2) 0.0327 1.0000 Uani . . . . . .
C13 C 0.4526(3) 0.3877(3) 0.1752(2) 0.0321 1.0000 Uani . . . . . .
C14 C 0.4758(3) 0.4359(3) 0.2384(2) 0.0327 1.0000 Uani . . . . . .
C15 C 0.4571(3) 0.5452(3) 0.2344(2) 0.0277 1.0000 Uani . . . . . .
C16 C 0.3030(3) 0.8031(3) 0.0797(2) 0.0236 1.0000 Uani . . . . . .
C17 C 0.3624(3) 0.8047(3) -0.0043(2) 0.0261 1.0000 Uani . . . . . .
C18 C 0.3040(3) 0.8453(3) -0.0691(2) 0.0294 1.0000 Uani . . . . . .
C19 C 0.1867(3) 0.8844(3) -0.0504(2) 0.0315 1.0000 Uani . . . . . .
C20 C 0.1278(3) 0.8830(3) 0.0319(2) 0.0320 1.0000 Uani . . . . . .
C21 C 0.1853(3) 0.8424(3) 0.0977(2) 0.0274 1.0000 Uani . . . . . .
C22 C 0.2815(3) 0.7986(3) 0.2613(2) 0.0263 1.0000 Uani . . . . . .
C23 C 0.2309(3) 0.7311(3) 0.3139(2) 0.0346 1.0000 Uani . . . . . .
C24 C 0.1515(3) 0.7698(4) 0.3870(3) 0.0456 1.0000 Uani . . . . . .
C25 C 0.1246(3) 0.8740(4) 0.4079(3) 0.0468 1.0000 Uani . . . . . .
C26 C 0.1714(3) 0.9417(4) 0.3563(3) 0.0442 1.0000 Uani . . . . . .
C27 C 0.2496(3) 0.9046(3) 0.2816(3) 0.0370 1.0000 Uani . . . . . .
C28 C 0.8059(3) 0.6734(3) 0.4819(2) 0.0266 1.0000 Uani . . . . . .
C29 C 0.8691(3) 0.7418(3) 0.4781(2) 0.0297 1.0000 Uani . . . . . .
C30 C 0.8945(3) 0.7651(3) 0.5522(2) 0.0330 1.0000 Uani . . . . . .
C31 C 0.8560(3) 0.7220(3) 0.6294(2) 0.0383 1.0000 Uani . . . . . .
C32 C 0.7920(3) 0.6564(3) 0.6338(2) 0.0399 1.0000 Uani . . . . . .
C33 C 0.7676(3) 0.6306(3) 0.5600(2) 0.0352 1.0000 Uani . . . . . .
C34 C 0.8783(3) 0.6519(3) 0.2989(2) 0.0246 1.0000 Uani . . . . . .
C35 C 0.8649(3) 0.7240(3) 0.2316(2) 0.0360 1.0000 Uani . . . . . .
C36 C 0.9569(4) 0.7180(4) 0.1642(3) 0.0467 1.0000 Uani . . . . . .
C37 C 1.0589(3) 0.6429(3) 0.1644(2) 0.0394 1.0000 Uani . . . . . .
C38 C 1.0743(4) 0.5729(3) 0.2313(3) 0.0495 1.0000 Uani . . . . . .
C39 C 0.9856(3) 0.5777(3) 0.2992(3) 0.0447 1.0000 Uani . . . . . .
C40 C 0.7352(3) 0.5283(3) 0.4021(2) 0.0277 1.0000 Uani . . . . . .
C41 C 0.6264(3) 0.5262(3) 0.4055(2) 0.0321 1.0000 Uani . . . . . .
C42 C 0.6052(4) 0.4297(3) 0.4171(2) 0.0379 1.0000 Uani . . . . . .
C43 C 0.6905(4) 0.3364(3) 0.4221(2) 0.0419 1.0000 Uani . . . . . .
C44 C 0.7993(4) 0.3375(3) 0.4191(3) 0.0466 1.0000 Uani . . . . . .
C45 C 0.8216(4) 0.4336(3) 0.4103(3) 0.0393 1.0000 Uani . . . . . .
C46 C 0.6803(3) 0.6095(2) 0.2115(2) 0.0203 1.0000 Uani . . . . . .
C47 C 0.8101(3) 0.4365(2) 0.1306(2) 0.0242 1.0000 Uani . . . . . .
C48 C 0.7460(3) 0.4235(3) 0.0656(2) 0.0372 1.0000 Uani . . . . . .
C49 C 0.8301(4) 0.3415(3) 0.1918(3) 0.0426 1.0000 Uani . . . . . .
C50 C 0.9182(3) 0.4584(3) 0.0871(3) 0.0376 1.0000 Uani . . . . . .
C51 C 0.1951(4) 1.1600(4) 0.0783(3) 0.0328 0.7500 Uani . . . . . .
C52 C 0.8621(3) 1.0306(3) 0.3146(3) 0.0383 1.0000 Uani . . . . . .
Pd1 Pd 0.579880(19) 0.753106(18) 0.256776(15) 0.0152 1.0000 Uani . . . . . .
S1 S 0.25219(7) 1.26592(7) 0.09105(6) 0.0205 0.7500 Uani . . . . . .
S2 S 0.71544(8) 1.04177(7) 0.31862(6) 0.0344 1.0000 Uani . . . . . .
F11 F 0.2233(3) 1.2367(3) -0.0483(2) 0.0544 0.2500 Uani . . . . . .
C53 C 0.2056(4) 1.1868(4) 0.0255(3) 0.0261 0.2500 Uani . . . . . .
O31 O 0.2348(3) 1.1735(3) 0.1785(2) 0.0622 0.2500 Uani . . . . . .
O11 O 0.1885(3) 1.3516(3) 0.1111(2) 0.0611 0.2500 Uani . . . . . .
O21 O 0.3740(3) 1.2178(3) 0.0699(2) 0.0371 0.2500 Uani . . . . . .
S11 S 0.24851(7) 1.24122(7) 0.10917(6) 0.0251 0.2500 Uani . . . . . .
H21 H 0.3920 1.1463 0.2686 0.0394 1.0000 Uiso R . . . . .
H31 H 0.3451 1.0827 0.4182 0.0384 1.0000 Uiso R . . . . .
H42 H 0.3894 0.8934 0.4939 0.0343 1.0000 Uiso R . . . . .
H41 H 0.3971 0.8063 0.4281 0.0337 1.0000 Uiso R . . . . .
H52 H 0.5773 0.8368 0.4852 0.0401 1.0000 Uiso R . . . . .
H51 H 0.5497 0.7290 0.4884 0.0398 1.0000 Uiso R . . . . .
H61 H 0.6719 0.8207 0.3571 0.0281 1.0000 Uiso R . . . . .
H72 H 0.5085 1.0486 0.1254 0.0322 1.0000 Uiso R . . . . .
H71 H 0.6105 0.9470 0.1445 0.0320 1.0000 Uiso R . . . . .
H81 H 0.5192 0.9032 0.0495 0.0307 1.0000 Uiso R . . . . .
H82 H 0.4025 0.9404 0.1153 0.0304 1.0000 Uiso R . . . . .
H91 H 0.5614 0.7419 0.1013 0.0244 1.0000 Uiso R . . . . .
H111 H 0.3669 0.5985 0.0570 0.0353 1.0000 Uiso R . . . . .
H121 H 0.3974 0.4164 0.0649 0.0393 1.0000 Uiso R . . . . .
H131 H 0.4648 0.3134 0.1780 0.0393 1.0000 Uiso R . . . . .
H141 H 0.5040 0.3951 0.2835 0.0402 1.0000 Uiso R . . . . .
H151 H 0.4712 0.5778 0.2775 0.0326 1.0000 Uiso R . . . . .
H171 H 0.4415 0.7784 -0.0161 0.0305 1.0000 Uiso R . . . . .
H181 H 0.3444 0.8454 -0.1254 0.0369 1.0000 Uiso R . . . . .
H191 H 0.1475 0.9116 -0.0940 0.0388 1.0000 Uiso R . . . . .
H201 H 0.0494 0.9091 0.0439 0.0391 1.0000 Uiso R . . . . .
H211 H 0.1445 0.8421 0.1534 0.0341 1.0000 Uiso R . . . . .
H231 H 0.2517 0.6578 0.2995 0.0433 1.0000 Uiso R . . . . .
H241 H 0.1155 0.7239 0.4231 0.0556 1.0000 Uiso R . . . . .
H251 H 0.0729 0.8994 0.4584 0.0562 1.0000 Uiso R . . . . .
H261 H 0.1503 1.0133 0.3702 0.0542 1.0000 Uiso R . . . . .
H271 H 0.2789 0.9519 0.2446 0.0459 1.0000 Uiso R . . . . .
H291 H 0.8951 0.7730 0.4253 0.0362 1.0000 Uiso R . . . . .
H301 H 0.9379 0.8107 0.5494 0.0418 1.0000 Uiso R . . . . .
H311 H 0.8734 0.7376 0.6790 0.0460 1.0000 Uiso R . . . . .
H321 H 0.7647 0.6289 0.6861 0.0484 1.0000 Uiso R . . . . .
H331 H 0.7252 0.5838 0.5618 0.0433 1.0000 Uiso R . . . . .
H351 H 0.7946 0.7765 0.2316 0.0445 1.0000 Uiso R . . . . .
H361 H 0.9488 0.7663 0.1184 0.0573 1.0000 Uiso R . . . . .
H371 H 1.1199 0.6382 0.1176 0.0484 1.0000 Uiso R . . . . .
H381 H 1.1456 0.5211 0.2309 0.0602 1.0000 Uiso R . . . . .
H391 H 0.9966 0.5311 0.3462 0.0543 1.0000 Uiso R . . . . .
H411 H 0.5666 0.5902 0.4002 0.0394 1.0000 Uiso R . . . . .
H421 H 0.5301 0.4295 0.4216 0.0483 1.0000 Uiso R . . . . .
H431 H 0.6754 0.2709 0.4275 0.0506 1.0000 Uiso R . . . . .
H441 H 0.8583 0.2731 0.4232 0.0572 1.0000 Uiso R . . . . .
H451 H 0.8954 0.4345 0.4109 0.0474 1.0000 Uiso R . . . . .
H482 H 0.7911 0.3599 0.0344 0.0578 1.0000 Uiso R . . . . .
H481 H 0.7357 0.4847 0.0263 0.0577 1.0000 Uiso R . . . . .
H483 H 0.6744 0.4168 0.0946 0.0579 1.0000 Uiso R . . . . .
H492 H 0.8744 0.2781 0.1591 0.0648 1.0000 Uiso R . . . . .
H491 H 0.8729 0.3534 0.2306 0.0647 1.0000 Uiso R . . . . .
H493 H 0.7582 0.3358 0.2217 0.0649 1.0000 Uiso R . . . . .
H502 H 0.9652 0.3977 0.0527 0.0590 1.0000 Uiso R . . . . .
H501 H 0.9545 0.4683 0.1307 0.0590 1.0000 Uiso R . . . . .
H503 H 0.8993 0.5211 0.0519 0.0590 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
F1 . C51 . 1.339(6) yes
F2 . C51 . 1.341(5) yes
F2 . C53 . 1.377(5) yes
F3 . C51 . 1.346(5) yes
F3 . C53 . 1.234(5) yes
F4 . C52 . 1.344(5) yes
F5 . C52 . 1.329(5) yes
F6 . C52 . 1.328(5) yes
O1 . S1 . 1.437(3) yes
O2 . S1 . 1.420(3) yes
O3 . S1 . 1.421(3) yes
O4 . S2 . 1.430(3) yes
O5 . S2 . 1.432(3) yes
O6 . S2 . 1.437(3) yes
P1 . C9 . 1.782(3) yes
P1 . C10 . 1.810(3) yes
P1 . C16 . 1.817(3) yes
P1 . C22 . 1.812(3) yes
P2 . C6 . 1.758(3) yes
P2 . C28 . 1.815(3) yes
P2 . C34 . 1.802(3) yes
P2 . C40 . 1.808(3) yes
N1 . C1 . 1.338(4) yes
N1 . C2 . 1.389(4) yes
N1 . C7 . 1.454(4) yes
N2 . C1 . 1.343(4) yes
N2 . C3 . 1.387(4) yes
N2 . C4 . 1.456(4) yes
N3 . C46 . 1.141(4) yes
N3 . C47 . 1.469(4) yes
C1 . Pd1 . 1.960(3) yes
C2 . C3 . 1.339(6) yes
C2 . H21 . 0.936 no
C3 . H31 . 0.940 no
C4 . C5 . 1.527(5) yes
C4 . H42 . 0.981 no
C4 . H41 . 0.979 no
C5 . C6 . 1.549(5) yes
C5 . H52 . 0.964 no
C5 . H51 . 0.975 no
C6 . Pd1 . 2.169(3) yes
C6 . H61 . 0.992 no
C7 . C8 . 1.530(4) yes
C7 . H72 . 0.971 no
C7 . H71 . 0.984 no
C8 . C9 . 1.563(4) yes
C8 . H81 . 0.971 no
C8 . H82 . 0.973 no
C9 . Pd1 . 2.143(3) yes
C9 . H91 . 0.992 no
C10 . C11 . 1.400(5) yes
C10 . C15 . 1.391(5) yes
C11 . C12 . 1.385(5) yes
C11 . H111 . 0.937 no
C12 . C13 . 1.380(5) yes
C12 . H121 . 0.934 no
C13 . C14 . 1.386(5) yes
C13 . H131 . 0.944 no
C14 . C15 . 1.388(5) yes
C14 . H141 . 0.931 no
C15 . H151 . 0.932 no
C16 . C17 . 1.401(5) yes
C16 . C21 . 1.391(5) yes
C17 . C18 . 1.386(5) yes
C17 . H171 . 0.936 no
C18 . C19 . 1.387(5) yes
C18 . H181 . 0.940 no
C19 . C20 . 1.376(5) yes
C19 . H191 . 0.931 no
C20 . C21 . 1.391(5) yes
C20 . H201 . 0.927 no
C21 . H211 . 0.934 no
C22 . C23 . 1.394(5) yes
C22 . C27 . 1.378(5) yes
C23 . C24 . 1.385(5) yes
C23 . H231 . 0.957 no
C24 . C25 . 1.366(7) yes
C24 . H241 . 0.961 no
C25 . C26 . 1.362(6) yes
C25 . H251 . 0.938 no
C26 . C27 . 1.394(5) yes
C26 . H261 . 0.932 no
C27 . H271 . 0.936 no
C28 . C29 . 1.392(5) yes
C28 . C33 . 1.388(5) yes
C29 . C30 . 1.393(5) yes
C29 . H291 . 0.953 no
C30 . C31 . 1.379(6) yes
C30 . H301 . 0.941 no
C31 . C32 . 1.368(6) yes
C31 . H311 . 0.935 no
C32 . C33 . 1.395(5) yes
C32 . H321 . 0.929 no
C33 . H331 . 0.947 no
C34 . C35 . 1.379(5) yes
C34 . C39 . 1.400(5) yes
C35 . C36 . 1.398(6) yes
C35 . H351 . 0.938 no
C36 . C37 . 1.356(6) yes
C36 . H361 . 0.933 no
C37 . C38 . 1.361(6) yes
C37 . H371 . 0.948 no
C38 . C39 . 1.379(6) yes
C38 . H381 . 0.942 no
C39 . H391 . 0.939 no
C40 . C41 . 1.392(5) yes
C40 . C45 . 1.390(5) yes
C41 . C42 . 1.382(5) yes
C41 . H411 . 0.948 no
C42 . C43 . 1.364(6) yes
C42 . H421 . 0.948 no
C43 . C44 . 1.387(6) yes
C43 . H431 . 0.944 no
C44 . C45 . 1.385(5) yes
C44 . H441 . 0.942 no
C45 . H451 . 0.951 no
C46 . Pd1 . 2.010(3) yes
C47 . C48 . 1.522(5) yes
C47 . C49 . 1.515(5) yes
C47 . C50 . 1.512(5) yes
C48 . H482 . 0.963 no
C48 . H481 . 0.973 no
C48 . H483 . 0.960 no
C49 . H492 . 0.970 no
C49 . H491 . 0.974 no
C49 . H493 . 0.964 no
C50 . H502 . 0.966 no
C50 . H501 . 0.965 no
C50 . H503 . 0.956 no
C51 . S1 . 1.832(5) yes
C52 . S2 . 1.820(4) yes
F11 . C53 . 1.320(6) yes
C53 . S11 . 1.849(5) yes
O31 . S11 . 1.385(4) yes
O11 . S11 . 1.411(4) yes
O21 . S11 . 1.527(4) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C9 . P1 . C10 . 111.88(15) yes
C9 . P1 . C16 . 111.39(14) yes
C10 . P1 . C16 . 107.50(15) yes
C9 . P1 . C22 . 114.66(15) yes
C10 . P1 . C22 . 105.95(16) yes
C16 . P1 . C22 . 104.93(15) yes
C6 . P2 . C28 . 111.24(15) yes
C6 . P2 . C34 . 109.60(16) yes
C28 . P2 . C34 . 106.68(16) yes
C6 . P2 . C40 . 111.74(16) yes
C28 . P2 . C40 . 105.59(16) yes
C34 . P2 . C40 . 111.83(15) yes
C1 . N1 . C2 . 109.4(3) yes
C1 . N1 . C7 . 120.6(3) yes
C2 . N1 . C7 . 130.0(3) yes
C1 . N2 . C3 . 109.4(3) yes
C1 . N2 . C4 . 120.6(3) yes
C3 . N2 . C4 . 130.0(3) yes
C46 . N3 . C47 . 175.8(3) yes
N2 . C1 . N1 . 107.0(3) yes
N2 . C1 . Pd1 . 127.4(2) yes
N1 . C1 . Pd1 . 125.5(2) yes
N1 . C2 . C3 . 107.2(3) yes
N1 . C2 . H21 . 125.5 no
C3 . C2 . H21 . 127.3 no
N2 . C3 . C2 . 107.0(3) yes
N2 . C3 . H31 . 124.5 no
C2 . C3 . H31 . 128.5 no
N2 . C4 . C5 . 110.6(3) yes
N2 . C4 . H42 . 109.0 no
C5 . C4 . H42 . 109.3 no
N2 . C4 . H41 . 107.6 no
C5 . C4 . H41 . 110.1 no
H42 . C4 . H41 . 110.2 no
C4 . C5 . C6 . 114.2(3) yes
C4 . C5 . H52 . 108.3 no
C6 . C5 . H52 . 108.2 no
C4 . C5 . H51 . 107.9 no
C6 . C5 . H51 . 109.3 no
H52 . C5 . H51 . 108.9 no
C5 . C6 . P2 . 112.0(2) yes
C5 . C6 . Pd1 . 118.0(2) yes
P2 . C6 . Pd1 . 116.11(16) yes
C5 . C6 . H61 . 103.7 no
P2 . C6 . H61 . 101.4 no
Pd1 . C6 . H61 . 102.7 no
N1 . C7 . C8 . 110.4(3) yes
N1 . C7 . H72 . 108.8 no
C8 . C7 . H72 . 109.6 no
N1 . C7 . H71 . 109.0 no
C8 . C7 . H71 . 109.3 no
H72 . C7 . H71 . 109.7 no
C7 . C8 . C9 . 115.8(3) yes
C7 . C8 . H81 . 107.3 no
C9 . C8 . H81 . 108.7 no
C7 . C8 . H82 . 107.1 no
C9 . C8 . H82 . 108.8 no
H81 . C8 . H82 . 109.0 no
C8 . C9 . P1 . 111.2(2) yes
C8 . C9 . Pd1 . 116.5(2) yes
P1 . C9 . Pd1 . 110.44(14) yes
C8 . C9 . H91 . 106.6 no
P1 . C9 . H91 . 105.6 no
Pd1 . C9 . H91 . 105.7 no
P1 . C10 . C11 . 119.2(3) yes
P1 . C10 . C15 . 121.6(3) yes
C11 . C10 . C15 . 119.1(3) yes
C10 . C11 . C12 . 119.7(3) yes
C10 . C11 . H111 . 119.8 no
C12 . C11 . H111 . 120.5 no
C11 . C12 . C13 . 120.9(3) yes
C11 . C12 . H121 . 118.9 no
C13 . C12 . H121 . 120.1 no
C12 . C13 . C14 . 119.7(3) yes
C12 . C13 . H131 . 120.1 no
C14 . C13 . H131 . 120.2 no
C13 . C14 . C15 . 120.0(3) yes
C13 . C14 . H141 . 120.1 no
C15 . C14 . H141 . 119.9 no
C10 . C15 . C14 . 120.5(3) yes
C10 . C15 . H151 . 119.5 no
C14 . C15 . H151 . 119.9 no
P1 . C16 . C17 . 118.9(2) yes
P1 . C16 . C21 . 121.3(3) yes
C17 . C16 . C21 . 119.8(3) yes
C16 . C17 . C18 . 120.0(3) yes
C16 . C17 . H171 . 119.6 no
C18 . C17 . H171 . 120.4 no
C17 . C18 . C19 . 119.7(3) yes
C17 . C18 . H181 . 119.5 no
C19 . C18 . H181 . 120.8 no
C18 . C19 . C20 . 120.7(3) yes
C18 . C19 . H191 . 119.7 no
C20 . C19 . H191 . 119.6 no
C19 . C20 . C21 . 120.2(3) yes
C19 . C20 . H201 . 120.1 no
C21 . C20 . H201 . 119.7 no
C16 . C21 . C20 . 119.7(3) yes
C16 . C21 . H211 . 120.7 no
C20 . C21 . H211 . 119.6 no
P1 . C22 . C23 . 120.9(3) yes
P1 . C22 . C27 . 119.7(3) yes
C23 . C22 . C27 . 119.3(3) yes
C22 . C23 . C24 . 120.1(4) yes
C22 . C23 . H231 . 119.6 no
C24 . C23 . H231 . 120.3 no
C23 . C24 . C25 . 119.7(4) yes
C23 . C24 . H241 . 120.5 no
C25 . C24 . H241 . 119.8 no
C24 . C25 . C26 . 121.0(4) yes
C24 . C25 . H251 . 119.6 no
C26 . C25 . H251 . 119.4 no
C25 . C26 . C27 . 120.0(4) yes
C25 . C26 . H261 . 120.2 no
C27 . C26 . H261 . 119.8 no
C26 . C27 . C22 . 119.8(4) yes
C26 . C27 . H271 . 120.1 no
C22 . C27 . H271 . 120.1 no
P2 . C28 . C29 . 118.9(3) yes
P2 . C28 . C33 . 121.5(3) yes
C29 . C28 . C33 . 119.2(3) yes
C28 . C29 . C30 . 119.8(3) yes
C28 . C29 . H291 . 120.7 no
C30 . C29 . H291 . 119.5 no
C29 . C30 . C31 . 120.4(4) yes
C29 . C30 . H301 . 119.7 no
C31 . C30 . H301 . 119.9 no
C30 . C31 . C32 . 120.1(3) yes
C30 . C31 . H311 . 120.2 no
C32 . C31 . H311 . 119.7 no
C31 . C32 . C33 . 120.2(4) yes
C31 . C32 . H321 . 119.9 no
C33 . C32 . H321 . 119.8 no
C32 . C33 . C28 . 120.2(4) yes
C32 . C33 . H331 . 121.2 no
C28 . C33 . H331 . 118.6 no
P2 . C34 . C35 . 121.2(3) yes
P2 . C34 . C39 . 120.3(3) yes
C35 . C34 . C39 . 118.5(3) yes
C34 . C35 . C36 . 119.4(4) yes
C34 . C35 . H351 . 119.8 no
C36 . C35 . H351 . 120.8 no
C35 . C36 . C37 . 120.9(4) yes
C35 . C36 . H361 . 120.2 no
C37 . C36 . H361 . 118.9 no
C36 . C37 . C38 . 120.4(4) yes
C36 . C37 . H371 . 120.2 no
C38 . C37 . H371 . 119.4 no
C37 . C38 . C39 . 120.0(4) yes
C37 . C38 . H381 . 119.7 no
C39 . C38 . H381 . 120.4 no
C34 . C39 . C38 . 120.6(4) yes
C34 . C39 . H391 . 119.2 no
C38 . C39 . H391 . 120.2 no
P2 . C40 . C41 . 119.2(3) yes
P2 . C40 . C45 . 121.1(3) yes
C41 . C40 . C45 . 119.8(3) yes
C40 . C41 . C42 . 119.6(4) yes
C40 . C41 . H411 . 120.7 no
C42 . C41 . H411 . 119.7 no
C41 . C42 . C43 . 120.7(4) yes
C41 . C42 . H421 . 118.9 no
C43 . C42 . H421 . 120.4 no
C42 . C43 . C44 . 120.2(4) yes
C42 . C43 . H431 . 119.8 no
C44 . C43 . H431 . 120.0 no
C43 . C44 . C45 . 120.0(4) yes
C43 . C44 . H441 . 120.3 no
C45 . C44 . H441 . 119.7 no
C40 . C45 . C44 . 119.7(4) yes
C40 . C45 . H451 . 120.4 no
C44 . C45 . H451 . 119.9 no
N3 . C46 . Pd1 . 173.9(3) yes
N3 . C47 . C48 . 106.2(3) yes
N3 . C47 . C49 . 108.6(3) yes
C48 . C47 . C49 . 111.1(3) yes
N3 . C47 . C50 . 107.0(3) yes
C48 . C47 . C50 . 110.9(3) yes
C49 . C47 . C50 . 112.7(3) yes
C47 . C48 . H482 . 107.7 no
C47 . C48 . H481 . 109.5 no
H482 . C48 . H481 . 109.0 no
C47 . C48 . H483 . 109.3 no
H482 . C48 . H483 . 110.3 no
H481 . C48 . H483 . 111.0 no
C47 . C49 . H492 . 108.2 no
C47 . C49 . H491 . 107.4 no
H492 . C49 . H491 . 109.7 no
C47 . C49 . H493 . 109.0 no
H492 . C49 . H493 . 111.0 no
H491 . C49 . H493 . 111.5 no
C47 . C50 . H502 . 107.9 no
C47 . C50 . H501 . 107.8 no
H502 . C50 . H501 . 111.2 no
C47 . C50 . H503 . 108.5 no
H502 . C50 . H503 . 110.1 no
H501 . C50 . H503 . 111.2 no
F3 . C51 . F2 . 105.8(4) yes
F3 . C51 . F1 . 105.9(4) yes
F2 . C51 . F1 . 108.6(4) yes
F3 . C51 . S1 . 112.6(3) yes
F2 . C51 . S1 . 112.7(3) yes
F1 . C51 . S1 . 110.8(3) yes
F4 . C52 . F5 . 106.8(3) yes
F4 . C52 . F6 . 107.6(3) yes
F5 . C52 . F6 . 106.9(4) yes
F4 . C52 . S2 . 111.5(3) yes
F5 . C52 . S2 . 112.4(3) yes
F6 . C52 . S2 . 111.3(2) yes
C6 . Pd1 . C9 . 165.42(11) yes
C6 . Pd1 . C46 . 101.99(12) yes
C9 . Pd1 . C46 . 91.26(12) yes
C6 . Pd1 . C1 . 79.53(12) yes
C9 . Pd1 . C1 . 86.74(12) yes
C46 . Pd1 . C1 . 174.65(13) yes
C51 . S1 . O1 . 102.7(2) yes
C51 . S1 . O3 . 103.1(2) yes
O1 . S1 . O3 . 115.8(2) yes
C51 . S1 . O2 . 103.4(2) yes
O1 . S1 . O2 . 114.5(2) yes
O3 . S1 . O2 . 114.9(2) yes
C52 . S2 . O6 . 102.07(19) yes
C52 . S2 . O5 . 102.70(18) yes
O6 . S2 . O5 . 114.65(17) yes
C52 . S2 . O4 . 103.91(18) yes
O6 . S2 . O4 . 115.0(2) yes
O5 . S2 . O4 . 115.8(2) yes
F2 . C53 . F11 . 113.3(4) yes
F2 . C53 . F3 . 110.3(4) yes
F11 . C53 . F3 . 108.3(4) yes
F2 . C53 . S11 . 104.3(3) yes
F11 . C53 . S11 . 111.8(3) yes
F3 . C53 . S11 . 108.7(3) yes
C53 . S11 . O21 . 99.2(2) yes
C53 . S11 . O11 . 106.1(2) yes
O21 . S11 . O11 . 112.3(2) yes
C53 . S11 . O31 . 103.7(2) yes
O21 . S11 . O31 . 110.06(18) yes
O11 . S11 . O31 . 122.4(2) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C4 . H42 . O6 2_676 165 0.98 2.38 3.333(6) yes
C6 . H61 . O6 . 151 0.99 2.37 3.274(6) yes
C7 . H72 . O3 . 147 0.97 2.37 3.227(6) yes
C7 . H72 . O21 . 154 0.97 2.56 3.460(6) yes
C7 . H71 . O5 . 123 0.98 2.57 3.211(6) yes
C8 . H81 . O21 2_675 144 0.97 2.47 3.309(6) yes
C17 . H171 . O21 2_675 157 0.94 2.34 3.223(6) yes
C23 . H231 . C15 . 123 0.96 2.59 3.212(6) yes
C31 . H311 . O1 2_676 133 0.94 2.59 3.297(6) yes
C31 . H311 . O31 2_676 137 0.94 2.57 3.319(6) yes
C43 . H431 . O4 1_545 133 0.94 2.49 3.209(6) yes
C50 . H503 . O2 2_675 151 0.96 2.60 3.465(6) yes



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 -1 3 x .
3 -1 2 x .
-2 0 3 x .
-1 2 0 x .
# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
####################################################################### 
# 
# 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_yc170214_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 1865719'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;

_audit_creation_date             2018-12-17T22:51:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C52 H49 Cl2 F6 N3 O6 P2 Pd S2'
_chemical_formula_moiety         'C50 H49 Cl2 N3 P2 Pd, 2(C F3 O3 S)'
_chemical_formula_weight         1229.29

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.8085(10)
_cell_length_b                   13.8014(6)
_cell_length_c                   18.8584(14)
_cell_angle_alpha                90
_cell_angle_beta                 126.5450(10)
_cell_angle_gamma                90
_cell_volume                     5396.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_theta_min      2.55
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_F_000             2504

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.7051
_exptl_absorpt_correction_T_max  0.7475

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_number            15653
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.554
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_reflns_Friedel_coverage         0
_reflns_number_total             5491
_reflns_number_gt                5045
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²+13.5995P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5491
_refine_ls_number_parameters     336
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0786
_refine_ls_wR_factor_gt          0.0756
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.063

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.5 0.5500(2) 0.75 0.0168(5) Uani 1 2 d S T P . .
C2 C 0.50037(12) 0.39488(16) 0.71462(15) 0.0292(5) Uani 1 1 d . . . . .
H2 H 0.5005 0.3396 0.6846 0.035 Uiso 1 1 calc R U . . .
C4 C 0.50330(10) 0.52352(16) 0.62174(13) 0.0217(4) Uani 1 1 d . . . . .
H4A H 0.5038 0.5952 0.6206 0.026 Uiso 1 1 calc R U . . .
H4B H 0.4642 0.5009 0.5647 0.026 Uiso 1 1 calc R U . . .
C5 C 0.56328(10) 0.48432(17) 0.63314(13) 0.0240(4) Uani 1 1 d . . . . .
H5A H 0.5588 0.4936 0.5776 0.029 Uiso 1 1 calc R U . . .
H5B H 0.5673 0.414 0.6458 0.029 Uiso 1 1 calc R U . . .
C6 C 0.62431(10) 0.53656(16) 0.70898(13) 0.0218(4) Uani 1 1 d . . . . .
H6A H 0.619 0.5519 0.7556 0.026 Uiso 1 1 calc R U . . .
H6B H 0.6284 0.5987 0.6865 0.026 Uiso 1 1 calc R U . . .
C11 C 0.71790(10) 0.45573(15) 0.68196(13) 0.0218(4) Uani 1 1 d . . . . .
C12 C 0.77185(11) 0.40170(17) 0.70544(16) 0.0285(5) Uani 1 1 d . . . . .
H12 H 0.7982 0.3713 0.7616 0.034 Uiso 1 1 calc R U . . .
C13 C 0.78638(12) 0.39296(19) 0.64561(18) 0.0364(6) Uani 1 1 d . . . . .
H13 H 0.8231 0.3567 0.6611 0.044 Uiso 1 1 calc R U . . .
C14 C 0.74775(14) 0.4367(2) 0.56376(18) 0.0404(6) Uani 1 1 d . . . . .
H14 H 0.7576 0.4297 0.5229 0.049 Uiso 1 1 calc R U . . .
C15 C 0.69499(13) 0.4905(2) 0.54116(17) 0.0414(6) Uani 1 1 d . . . . .
H15 H 0.6686 0.5204 0.4848 0.05 Uiso 1 1 calc R U . . .
C16 C 0.68011(11) 0.50133(18) 0.60029(15) 0.0300(5) Uani 1 1 d . . . . .
H16 H 0.6443 0.5397 0.585 0.036 Uiso 1 1 calc R U . . .
C21 C 0.76168(10) 0.53101(16) 0.85553(13) 0.0226(4) Uani 1 1 d . . . . .
C22 C 0.81508(12) 0.47717(19) 0.92075(16) 0.0351(5) Uani 1 1 d . . . . .
H22 H 0.8168 0.4094 0.9136 0.042 Uiso 1 1 calc R U . . .
C23 C 0.86572(12) 0.5236(2) 0.99635(16) 0.0403(6) Uani 1 1 d . . . . .
H23 H 0.9024 0.4876 1.041 0.048 Uiso 1 1 calc R U . . .
C24 C 0.86280(11) 0.62213(19) 1.00656(15) 0.0320(5) Uani 1 1 d . . . . .
H24 H 0.8976 0.6536 1.0583 0.038 Uiso 1 1 calc R U . . .
C25 C 0.80973(11) 0.67518(17) 0.94219(15) 0.0297(5) Uani 1 1 d . . . . .
H25 H 0.808 0.7428 0.9501 0.036 Uiso 1 1 calc R U . . .
C26 C 0.75888(11) 0.63020(16) 0.86605(14) 0.0260(4) Uani 1 1 d . . . . .
H26 H 0.7225 0.6668 0.8215 0.031 Uiso 1 1 calc R U . . .
C31 C 0.68795(11) 0.35232(16) 0.79067(14) 0.0255(4) Uani 1 1 d . . . . .
C32 C 0.68411(14) 0.26728(19) 0.74926(19) 0.0396(6) Uani 1 1 d . . . . .
H32 H 0.6881 0.2685 0.7024 0.047 Uiso 1 1 calc R U . . .
C33 C 0.67437(17) 0.1800(2) 0.7763(3) 0.0563(8) Uani 1 1 d . . . . .
H33 H 0.6723 0.1213 0.7484 0.068 Uiso 1 1 calc R U . . .
C34 C 0.66772(15) 0.1785(2) 0.8436(2) 0.0535(8) Uani 1 1 d . . . . .
H34 H 0.6611 0.1186 0.8619 0.064 Uiso 1 1 calc R U . . .
C35 C 0.67048(18) 0.2623(3) 0.8840(2) 0.0577(9) Uani 1 1 d . . . . .
H35 H 0.6651 0.2609 0.9297 0.069 Uiso 1 1 calc R U . . .
C36 C 0.68109(16) 0.3498(2) 0.85829(19) 0.0483(7) Uani 1 1 d . . . . .
H36 H 0.6837 0.4081 0.887 0.058 Uiso 1 1 calc R U . . .
C42 C 0.46853(17) 0.8932(2) 0.7744(2) 0.0749(13) Uani 1 1 d . . . . .
H42 H 0.4456 0.8587 0.7912 0.09 Uiso 1 1 calc R U . . .
C43 C 0.4685(2) 0.9941(3) 0.7758(3) 0.127(3) Uani 1 1 d . . . . .
H43 H 0.4466 1.0278 0.7946 0.152 Uiso 1 1 calc R U . . .
C44 C 0.5 1.0437(5) 0.75 0.170(6) Uani 1 2 d S T P . .
H44 H 0.5 1.1125 0.75 0.204 Uiso 1 2 calc R U P . .
C100 C 0.4907(2) 0.8134(3) 0.9961(3) 0.0780(13) Uani 1 1 d . . . . .
F1 F 0.51014(18) 0.7726(2) 0.9515(3) 0.1360(14) Uani 1 1 d . . . . .
F2 F 0.4759(2) 0.90431(18) 0.9700(3) 0.1467(16) Uani 1 1 d . . . . .
F3 F 0.53831(15) 0.8104(3) 1.0803(3) 0.1645(18) Uani 1 1 d . . . . .
N1 N 0.50094(8) 0.49101(13) 0.69395(11) 0.0196(3) Uani 1 1 d . . . . .
N3 N 0.5 0.8440(2) 0.75 0.0450(9) Uani 1 2 d S T P . .
O1 O 0.37388(14) 0.7638(2) 0.88175(16) 0.0895(10) Uani 1 1 d . . . . .
O2 O 0.41010(14) 0.79608(18) 1.03052(19) 0.0716(7) Uani 1 1 d . . . . .
O3 O 0.44519(10) 0.65199(14) 0.99680(15) 0.0531(5) Uani 1 1 d . . . . .
P1 P 0.69793(3) 0.46906(4) 0.75777(3) 0.01925(12) Uani 1 1 d . . . . .
Pd1 Pd 0.5 0.69170(2) 0.75 0.01968(7) Uani 1 2 d S T P . .
S1 S 0.42173(3) 0.74936(4) 0.97346(4) 0.03352(14) Uani 1 1 d . . . . .
Cl1 Cl 0.38901(2) 0.68715(4) 0.65018(3) 0.02653(12) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.346(2) 2_656 ?
C1 N1 1.346(2) . ?
C1 Pd1 1.955(3) . ?
C2 C2 1.346(4) 2_656 ?
C2 N1 1.385(3) . ?
C2 H2 0.95 . ?
C4 N1 1.469(2) . ?
C4 C5 1.529(3) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C6 1.537(3) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 P1 1.801(2) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C11 C16 1.390(3) . ?
C11 C12 1.399(3) . ?
C11 P1 1.795(2) . ?
C12 C13 1.390(3) . ?
C12 H12 0.95 . ?
C13 C14 1.382(4) . ?
C13 H13 0.95 . ?
C14 C15 1.377(4) . ?
C14 H14 0.95 . ?
C15 C16 1.387(3) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C21 C26 1.391(3) . ?
C21 C22 1.395(3) . ?
C21 P1 1.796(2) . ?
C22 C23 1.390(3) . ?
C22 H22 0.95 . ?
C23 C24 1.381(4) . ?
C23 H23 0.95 . ?
C24 C25 1.380(3) . ?
C24 H24 0.95 . ?
C25 C26 1.388(3) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C31 C32 1.380(3) . ?
C31 C36 1.388(3) . ?
C31 P1 1.799(2) . ?
C32 C33 1.388(4) . ?
C32 H32 0.95 . ?
C33 C34 1.378(5) . ?
C33 H33 0.95 . ?
C34 C35 1.364(5) . ?
C34 H34 0.95 . ?
C35 C36 1.387(4) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C42 N3 1.333(4) . ?
C42 C43 1.392(5) . ?
C42 H42 0.95 . ?
C43 C44 1.356(8) . ?
C43 H43 0.95 . ?
C44 C43 1.356(8) 2_656 ?
C44 H44 0.95 . ?
C100 F3 1.308(6) . ?
C100 F2 1.318(5) . ?
C100 F1 1.334(5) . ?
C100 S1 1.797(4) . ?
N3 C42 1.333(4) 2_656 ?
N3 Pd1 2.102(3) . ?
O1 S1 1.419(2) . ?
O2 S1 1.431(2) . ?
O3 S1 1.4314(19) . ?
Pd1 Cl1 2.3088(5) 2_656 ?
Pd1 Cl1 2.3089(5) . ?

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
N1 C1 N1 105.5(2) 2_656 . ?
N1 C1 Pd1 127.25(12) 2_656 . ?
N1 C1 Pd1 127.25(12) . . ?
C2 C2 N1 106.73(11) 2_656 . ?
C2 C2 H2 126.6 2_656 . ?
N1 C2 H2 126.6 . . ?
N1 C4 C5 111.03(17) . . ?
N1 C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
N1 C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108 . . ?
C4 C5 C6 110.82(17) . . ?
C4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C5 C6 P1 114.68(15) . . ?
C5 C6 H6A 108.6 . . ?
P1 C6 H6A 108.6 . . ?
C5 C6 H6B 108.6 . . ?
P1 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
C16 C11 C12 120.12(19) . . ?
C16 C11 P1 119.44(16) . . ?
C12 C11 P1 120.42(17) . . ?
C13 C12 C11 119.2(2) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 120.3(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 120.4(2) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 119.7(2) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
C26 C21 C22 120.4(2) . . ?
C26 C21 P1 121.42(17) . . ?
C22 C21 P1 118.16(17) . . ?
C23 C22 C21 119.4(2) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C24 C23 C22 120.1(2) . . ?
C24 C23 H23 120 . . ?
C22 C23 H23 120 . . ?
C25 C24 C23 120.5(2) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.3(2) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 119.4(2) . . ?
C25 C26 H26 120.3 . . ?
C21 C26 H26 120.3 . . ?
C32 C31 C36 119.5(2) . . ?
C32 C31 P1 122.89(18) . . ?
C36 C31 P1 117.53(19) . . ?
C31 C32 C33 119.9(3) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 120.0(3) . . ?
C34 C33 H33 120 . . ?
C32 C33 H33 120 . . ?
C35 C34 C33 120.6(3) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 119.9(3) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 120.2(3) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
N3 C42 C43 121.6(5) . . ?
N3 C42 H42 119.2 . . ?
C43 C42 H42 119.2 . . ?
C44 C43 C42 119.4(6) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
C43 C44 C43 119.3(6) . 2_656 ?
C43 C44 H44 120.4 . . ?
C43 C44 H44 120.4 2_656 . ?
F3 C100 F2 109.6(4) . . ?
F3 C100 F1 108.6(4) . . ?
F2 C100 F1 107.5(4) . . ?
F3 C100 S1 110.7(3) . . ?
F2 C100 S1 110.7(3) . . ?
F1 C100 S1 109.5(3) . . ?
C1 N1 C2 110.52(17) . . ?
C1 N1 C4 124.97(18) . . ?
C2 N1 C4 124.51(17) . . ?
C42 N3 C42 118.7(5) 2_656 . ?
C42 N3 Pd1 120.6(2) 2_656 . ?
C42 N3 Pd1 120.6(2) . . ?
C11 P1 C21 110.15(10) . . ?
C11 P1 C31 110.54(10) . . ?
C21 P1 C31 107.70(10) . . ?
C11 P1 C6 111.23(10) . . ?
C21 P1 C6 108.74(10) . . ?
C31 P1 C6 108.38(10) . . ?
C1 Pd1 N3 180 . . ?
C1 Pd1 Cl1 88.445(14) . 2_656 ?
N3 Pd1 Cl1 91.555(14) . 2_656 ?
C1 Pd1 Cl1 88.444(14) . . ?
N3 Pd1 Cl1 91.556(14) . . ?
Cl1 Pd1 Cl1 176.89(3) 2_656 . ?
O1 S1 O2 115.66(18) . . ?
O1 S1 O3 114.12(15) . . ?
O2 S1 O3 115.56(14) . . ?
O1 S1 C100 103.9(2) . . ?
O2 S1 C100 102.81(18) . . ?
O3 S1 C100 102.20(18) . . ?


####################################################################### 
# 
# 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_yc171102_3_0m
_database_code_depnum_ccdc_archive 'CCDC 1865720'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;

_audit_creation_date             2018-06-20T15:07:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C54 H54.45 Cl F6 N4 O6 P2 Pd S2'
_chemical_formula_moiety         
'C48 H48.45 Cl N2 P2 Pd, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_weight         1237.82

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.9726(6)
_cell_length_b                   14.7721(7)
_cell_length_c                   16.7001(8)
_cell_angle_alpha                88.0820(10)
_cell_angle_beta                 73.5710(10)
_cell_angle_gamma                65.1440(10)
_cell_volume                     2771.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      2.85
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_F_000             1266.9
_exptl_crystal_density_method    'not measured'
_exptl_special_details           
;
 ?
;


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.6322
_exptl_absorpt_correction_T_max  0.7465

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_number            74501
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.846
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             11316
_reflns_number_gt                10685
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0434P)²+4.5916P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         11316
_refine_ls_number_parameters     712
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0914
_refine_ls_wR_factor_gt          0.089
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.03
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.815
_refine_diff_density_min         -0.59
_refine_diff_density_rms         0.077

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#


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 0 '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'
O O 0.0106 0.006 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.16790(17) 0.09830(16) 0.74346(12) 0.0144(4) Uani 1 1 d . . . . .
C2 C 0.23368(18) -0.06288(16) 0.69293(13) 0.0166(4) Uani 1 1 d . . . . .
H2 H 0.276 -0.1231 0.6564 0.02 Uiso 1 1 calc R U . . .
C3 C 0.15455(18) -0.04822(16) 0.76920(13) 0.0180(4) Uani 1 1 d . . . . .
H3 H 0.1301 -0.0963 0.7969 0.022 Uiso 1 1 calc R U . . .
C4 C 0.31494(17) 0.04476(16) 0.60100(12) 0.0145(4) Uani 1 1 d . . . . .
H4A H 0.3916 -0.0155 0.5814 0.017 Uiso 1 1 calc R U . . .
H4B H 0.332 0.1016 0.6124 0.017 Uiso 1 1 calc R U . . .
C5 C 0.25350(17) 0.06797(16) 0.53254(12) 0.0143(4) Uani 1 1 d . . . . .
H5A H 0.1851 0.1349 0.5469 0.017 Uiso 1 1 calc R U . . .
H5B H 0.2233 0.0176 0.5279 0.017 Uiso 1 1 calc R U . . .
C6 C 0.34280(17) 0.06597(15) 0.44871(12) 0.0129(4) Uani 1 1 d . . . . .
H6A H 0.407 -0.0029 0.4324 0.015 Uiso 1 1 calc R U . . .
H6B H 0.3794 0.1108 0.4559 0.015 Uiso 1 1 calc R U . . .
C7 C 0.02836(19) 0.09622(18) 0.88063(13) 0.0200(4) Uani 1 1 d . . . . .
H7A H 0.0364 0.1557 0.8981 0.024 Uiso 1 1 calc R U . . .
H7B H 0.0442 0.0479 0.9231 0.024 Uiso 1 1 calc R U . . .
C8 C -0.09723(18) 0.12759(16) 0.87709(13) 0.0187(4) Uani 1 1 d . . . . .
H8A H -0.102 0.0713 0.8503 0.022 Uiso 1 1 calc R U . . .
H8B H -0.1184 0.1847 0.8426 0.022 Uiso 1 1 calc R U . . .
C9 C -0.18630(18) 0.15856(16) 0.96657(13) 0.0185(4) Uani 1 1 d . . . . .
H9A H -0.1419 0.1535 1.0072 0.022 Uiso 1 1 calc R U . . .
H9B H -0.2221 0.1104 0.9795 0.022 Uiso 1 1 calc R U . . .
C11 C 0.17847(18) 0.04506(16) 0.36985(12) 0.0145(4) Uani 1 1 d . . . . .
C12 C 0.2302(2) -0.05786(17) 0.34670(15) 0.0233(5) Uani 1 1 d . . . . .
H12 H 0.3143 -0.0948 0.3298 0.028 Uiso 1 1 calc R U . . .
C13 C 0.1578(2) -0.10566(19) 0.34852(17) 0.0291(5) Uani 1 1 d . . . . .
H13 H 0.1923 -0.1755 0.3317 0.035 Uiso 1 1 calc R U . . .
C14 C 0.0352(2) -0.05197(19) 0.37481(15) 0.0255(5) Uani 1 1 d . . . . .
H14 H -0.0139 -0.0848 0.3749 0.031 Uiso 1 1 calc R U . . .
C15 C -0.0158(2) 0.04899(19) 0.40094(15) 0.0239(5) Uani 1 1 d . . . . .
H15 H -0.1 0.0847 0.4209 0.029 Uiso 1 1 calc R U . . .
C16 C 0.05505(19) 0.09880(17) 0.39831(13) 0.0186(4) Uani 1 1 d . . . . .
H16 H 0.0199 0.1685 0.4157 0.022 Uiso 1 1 calc R U . . .
C21 C 0.19363(18) 0.23870(15) 0.37537(13) 0.0151(4) Uani 1 1 d . . . . .
C22 C 0.19354(19) 0.29961(17) 0.43727(14) 0.0205(4) Uani 1 1 d . . . . .
H22 H 0.2301 0.2708 0.4795 0.025 Uiso 1 1 calc R U . . .
C23 C 0.1391(2) 0.40340(18) 0.43638(17) 0.0286(5) Uani 1 1 d . . . . .
H23 H 0.1385 0.4458 0.4782 0.034 Uiso 1 1 calc R U . . .
C24 C 0.0859(2) 0.44493(18) 0.37480(17) 0.0309(6) Uani 1 1 d . . . . .
H24 H 0.0493 0.5157 0.3743 0.037 Uiso 1 1 calc R U . . .
C25 C 0.0858(2) 0.38389(19) 0.31392(16) 0.0296(5) Uani 1 1 d . . . . .
H25 H 0.0487 0.413 0.272 0.035 Uiso 1 1 calc R U . . .
C26 C 0.1392(2) 0.28058(17) 0.31347(14) 0.0221(4) Uani 1 1 d . . . . .
H26 H 0.1389 0.2388 0.2716 0.027 Uiso 1 1 calc R U . . .
C31 C 0.38741(17) 0.06777(15) 0.26682(12) 0.0133(4) Uani 1 1 d . . . . .
C32 C 0.49626(18) 0.06974(16) 0.25990(13) 0.0164(4) Uani 1 1 d . . . . .
H32 H 0.5117 0.0872 0.3081 0.02 Uiso 1 1 calc R U . . .
C33 C 0.58174(19) 0.04615(17) 0.18226(14) 0.0200(4) Uani 1 1 d . . . . .
H33 H 0.6563 0.0466 0.1775 0.024 Uiso 1 1 calc R U . . .
C34 C 0.5589(2) 0.02203(19) 0.11180(14) 0.0249(5) Uani 1 1 d . . . . .
H34 H 0.6179 0.0054 0.0588 0.03 Uiso 1 1 calc R U . . .
C35 C 0.4497(2) 0.0222(2) 0.11862(14) 0.0300(5) Uani 1 1 d . . . . .
H35 H 0.4338 0.0067 0.0699 0.036 Uiso 1 1 calc R U . . .
C36 C 0.3634(2) 0.04486(19) 0.19582(14) 0.0225(5) Uani 1 1 d . . . . .
H36 H 0.2888 0.0447 0.2002 0.027 Uiso 1 1 calc R U . . .
C41 C -0.37747(19) 0.29861(17) 0.90245(14) 0.0201(4) Uani 1 1 d . . . . .
C42 C -0.4203(2) 0.3901(2) 0.86915(18) 0.0314(5) Uani 1 1 d . . . . .
H42 H -0.4066 0.444 0.8857 0.038 Uiso 1 1 calc R U . . .
C43 C -0.4828(3) 0.4021(2) 0.8117(2) 0.0413(7) Uani 1 1 d . . . . .
H43 H -0.5116 0.4643 0.7885 0.05 Uiso 1 1 calc R U . . .
C44 C -0.5034(2) 0.3238(2) 0.78811(18) 0.0394(7) Uani 1 1 d . . . . .
H44 H -0.546 0.3323 0.7484 0.047 Uiso 1 1 calc R U . . .
C45 C -0.4626(2) 0.2336(2) 0.82188(17) 0.0341(6) Uani 1 1 d . . . . .
H45 H -0.4783 0.1805 0.8062 0.041 Uiso 1 1 calc R U . . .
C46 C -0.3985(2) 0.22001(19) 0.87881(16) 0.0263(5) Uani 1 1 d . . . . .
H46 H -0.3692 0.1575 0.9014 0.032 Uiso 1 1 calc R U . . .
C51 C -0.40880(19) 0.29948(16) 1.08260(14) 0.0191(4) Uani 1 1 d . . . . .
C52 C -0.5303(2) 0.33718(18) 1.09110(16) 0.0266(5) Uani 1 1 d . . . . .
H52 H -0.558 0.3542 1.0433 0.032 Uiso 1 1 calc R U . . .
C53 C -0.6102(2) 0.3495(2) 1.16988(18) 0.0355(6) Uani 1 1 d . . . . .
H53 H -0.6928 0.3744 1.1759 0.043 Uiso 1 1 calc R U . . .
C54 C -0.5704(2) 0.32593(19) 1.23966(17) 0.0341(6) Uani 1 1 d . . . . .
H54 H -0.6258 0.335 1.2934 0.041 Uiso 1 1 calc R U . . .
C55 C -0.4503(2) 0.28909(19) 1.23165(16) 0.0307(5) Uani 1 1 d . . . . .
H55 H -0.4235 0.2734 1.2799 0.037 Uiso 1 1 calc R U . . .
C56 C -0.3690(2) 0.27510(17) 1.15306(15) 0.0242(5) Uani 1 1 d . . . . .
H56 H -0.2865 0.2489 1.1474 0.029 Uiso 1 1 calc R U . . .
C61 C -0.2436(2) 0.37344(17) 0.97480(15) 0.0221(4) Uani 1 1 d . . . . .
C62 C -0.2558(3) 0.4250(2) 1.04745(18) 0.0341(6) Uani 1 1 d . . . . .
H62 H -0.3002 0.4158 1.1004 0.041 Uiso 1 1 calc R U . . .
C63 C -0.2026(3) 0.4901(2) 1.0422(2) 0.0467(8) Uani 1 1 d . . . . .
H63 H -0.2102 0.5253 1.0918 0.056 Uiso 1 1 calc R U . . .
C64 C -0.1387(3) 0.5038(2) 0.9655(2) 0.0459(8) Uani 1 1 d . . . . .
H64 H -0.1025 0.5484 0.9623 0.055 Uiso 1 1 calc R U . . .
C65 C -0.1270(3) 0.4531(2) 0.8930(2) 0.0401(7) Uani 1 1 d . . . . .
H65 H -0.0833 0.4635 0.8402 0.048 Uiso 1 1 calc R U . . .
C66 C -0.1786(2) 0.3874(2) 0.89674(17) 0.0307(5) Uani 1 1 d . . . . .
H66 H -0.1701 0.3521 0.847 0.037 Uiso 1 1 calc R U . . .
C67 C 0.2864(2) 0.2206(2) 0.79358(17) 0.0281(5) Uani 1 1 d D . . . .
C68A C 0.2067(3) 0.3231(2) 0.8086(2) 0.0285(9) Uani 0.889(10) 1 d D . P . .
C68B C 0.2642(18) 0.3086(16) 0.7497(14) 0.021(7) Uani 0.111(10) 1 d . . P . .
C69 C 0.1770(3) 0.3779(2) 0.7444(2) 0.0367(6) Uani 1 1 d D . . . .
C81 C 0.1772(3) 0.7044(2) 0.6734(2) 0.0451(7) Uani 1 1 d . . . . .
H81A H 0.1147 0.7588 0.7152 0.068 Uiso 1 1 calc R U . . .
H81B H 0.1412 0.6812 0.6393 0.068 Uiso 1 1 calc R U . . .
H81C H 0.2321 0.7289 0.6372 0.068 Uiso 1 1 calc R U . . .
C82 C 0.2412(3) 0.6230(2) 0.71524(18) 0.0363(6) Uani 1 1 d . . . . .
C91 C 0.2837(3) 0.5920(4) 0.3717(3) 0.0718(12) Uani 1 1 d . . . . .
H91A H 0.2494 0.597 0.3255 0.108 Uiso 1 1 calc R U . . .
H91B H 0.3388 0.5222 0.3724 0.108 Uiso 1 1 calc R U . . .
H91C H 0.3266 0.6342 0.3638 0.108 Uiso 1 1 calc R U . . .
C92 C 0.1912(3) 0.6248(2) 0.4489(2) 0.0451(7) Uani 1 1 d . . . . .
C101 C 0.5418(3) 0.63713(19) 0.47841(16) 0.0310(5) Uani 1 1 d . . . . .
C111 C 0.8956(2) 0.7511(2) 0.92373(16) 0.0297(5) Uani 1 1 d . . . . .
N1 N 0.24100(15) 0.02736(13) 0.67842(10) 0.0134(3) Uani 1 1 d . . . . .
N2 N 0.11577(15) 0.05028(14) 0.79941(11) 0.0156(3) Uani 1 1 d . . . . .
N3 N 0.2912(3) 0.5592(2) 0.7491(2) 0.0624(9) Uani 1 1 d . . . . .
N4 N 0.1164(3) 0.6493(3) 0.5103(2) 0.0592(8) Uani 1 1 d . . . . .
O4 O 0.35157(17) 0.80155(16) 0.50931(13) 0.0408(5) Uani 1 1 d . . . . .
O5 O 0.5312(2) 0.80045(17) 0.41411(15) 0.0585(7) Uani 1 1 d . . . . .
O6 O 0.50938(17) 0.79305(15) 0.56296(14) 0.0402(5) Uani 1 1 d . . . . .
O11 O 0.8162(2) 0.93975(16) 0.95877(15) 0.0519(6) Uani 1 1 d . . . . .
O12 O 0.91476(16) 0.87249(14) 0.81291(11) 0.0300(4) Uani 1 1 d . . . . .
O13 O 1.02947(17) 0.84173(16) 0.91069(11) 0.0345(4) Uani 1 1 d . . . . .
F1 F 0.97944(18) 0.67235(12) 0.87050(12) 0.0469(4) Uani 1 1 d . . . . .
F2 F 0.79181(17) 0.75979(15) 0.91869(14) 0.0525(5) Uani 1 1 d . . . . .
F3 F 0.9018(2) 0.72828(15) 1.00036(11) 0.0513(5) Uani 1 1 d . . . . .
F4 F 0.5216(2) 0.60391(14) 0.41461(12) 0.0551(5) Uani 1 1 d . . . . .
F5 F 0.4970(2) 0.60173(14) 0.54692(12) 0.0596(6) Uani 1 1 d . . . . .
F6 F 0.65901(17) 0.59856(14) 0.46332(13) 0.0557(5) Uani 1 1 d . . . . .
P1 P 0.27396(4) 0.10495(4) 0.36619(3) 0.01104(10) Uani 1 1 d . . . . .
P2 P -0.30399(5) 0.28318(4) 0.98119(3) 0.01588(11) Uani 1 1 d . . . . .
S1 S 0.91562(5) 0.86474(4) 0.89865(3) 0.02141(12) Uani 1 1 d . . . . .
S2 S 0.47623(5) 0.77316(4) 0.49210(4) 0.02598(13) Uani 1 1 d . . . . .
Cl1 Cl -0.01254(4) 0.29315(4) 0.68252(3) 0.01806(11) Uani 1 1 d . . . . .
Pd1 Pd 0.14538(2) 0.24204(2) 0.74625(2) 0.01667(6) Uani 1 1 d . . . . .
H67A H 0.294(3) 0.187(2) 0.8426(12) 0.05 Uiso 0.889(10) 1 d D U P . .
H67B H 0.352(2) 0.193(3) 0.7446(13) 0.05 Uiso 0.889(10) 1 d D U P . .
H68 H 0.155(3) 0.351(3) 0.8635(9) 0.05 Uiso 0.889(10) 1 d D U P . .
H69A H 0.115(2) 0.4440(11) 0.753(2) 0.05 Uiso 0.889(10) 1 d D U P . .
H69B H 0.233(2) 0.357(3) 0.6901(10) 0.05 Uiso 0.889(10) 1 d D U P . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N2 1.355(3) . ?
C1 N1 1.355(3) . ?
C1 Pd1 2.018(2) . ?
C2 C3 1.347(3) . ?
C2 N1 1.384(3) . ?
C2 H2 0.95 . ?
C3 N2 1.384(3) . ?
C3 H3 0.95 . ?
C4 N1 1.463(2) . ?
C4 C5 1.523(3) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C6 1.536(3) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 P1 1.7998(19) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C7 N2 1.460(3) . ?
C7 C8 1.513(3) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 C9 1.550(3) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 P2 1.799(2) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C11 C16 1.395(3) . ?
C11 C12 1.395(3) . ?
C11 P1 1.788(2) . ?
C12 C13 1.387(3) . ?
C12 H12 0.95 . ?
C13 C14 1.385(4) . ?
C13 H13 0.95 . ?
C14 C15 1.379(4) . ?
C14 H14 0.95 . ?
C15 C16 1.390(3) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C21 C22 1.392(3) . ?
C21 C26 1.397(3) . ?
C21 P1 1.792(2) . ?
C22 C23 1.394(3) . ?
C22 H22 0.95 . ?
C23 C24 1.383(4) . ?
C23 H23 0.95 . ?
C24 C25 1.382(4) . ?
C24 H24 0.95 . ?
C25 C26 1.385(3) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C31 C36 1.394(3) . ?
C31 C32 1.397(3) . ?
C31 P1 1.795(2) . ?
C32 C33 1.387(3) . ?
C32 H32 0.95 . ?
C33 C34 1.383(3) . ?
C33 H33 0.95 . ?
C34 C35 1.388(3) . ?
C34 H34 0.95 . ?
C35 C36 1.387(3) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C41 C46 1.392(3) . ?
C41 C42 1.393(3) . ?
C41 P2 1.788(2) . ?
C42 C43 1.385(4) . ?
C42 H42 0.95 . ?
C43 C44 1.385(5) . ?
C43 H43 0.95 . ?
C44 C45 1.379(4) . ?
C44 H44 0.95 . ?
C45 C46 1.389(3) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C51 C56 1.392(3) . ?
C51 C52 1.399(3) . ?
C51 P2 1.796(2) . ?
C52 C53 1.387(4) . ?
C52 H52 0.95 . ?
C53 C54 1.381(4) . ?
C53 H53 0.95 . ?
C54 C55 1.384(4) . ?
C54 H54 0.95 . ?
C55 C56 1.389(3) . ?
C55 H55 0.95 . ?
C56 H56 0.95 . ?
C61 C62 1.389(4) . ?
C61 C66 1.399(3) . ?
C61 P2 1.796(2) . ?
C62 C63 1.388(4) . ?
C62 H62 0.95 . ?
C63 C64 1.376(5) . ?
C63 H63 0.95 . ?
C64 C65 1.383(5) . ?
C64 H64 0.95 . ?
C65 C66 1.383(4) . ?
C65 H65 0.95 . ?
C66 H66 0.95 . ?
C67 C68A 1.411(4) . ?
C67 C68B 1.43(2) . ?
C67 Pd1 2.094(2) . ?
C67 H67A 0.9500(10) . ?
C67 H67B 0.9500(10) . ?
C68A C68B 1.02(2) . ?
C68A C69 1.365(4) . ?
C68A Pd1 2.123(3) . ?
C68A H68 0.9500(10) . ?
C68B C69 1.19(2) . ?
C68B Pd1 2.163(19) . ?
C68B H69B 1.27(4) . ?
C69 Pd1 2.209(3) . ?
C69 H69A 0.9500(10) . ?
C69 H69B 0.9501(11) . ?
C81 C82 1.434(4) . ?
C81 H81A 0.98 . ?
C81 H81B 0.98 . ?
C81 H81C 0.98 . ?
C82 N3 1.134(4) . ?
C91 C92 1.420(5) . ?
C91 H91A 0.98 . ?
C91 H91B 0.98 . ?
C91 H91C 0.98 . ?
C92 N4 1.136(4) . ?
C101 F4 1.321(3) . ?
C101 F5 1.327(3) . ?
C101 F6 1.329(3) . ?
C101 S2 1.816(3) . ?
C111 F2 1.324(3) . ?
C111 F3 1.328(3) . ?
C111 F1 1.336(3) . ?
C111 S1 1.822(3) . ?
O4 S2 1.431(2) . ?
O5 S2 1.431(2) . ?
O6 S2 1.445(2) . ?
O11 S1 1.428(2) . ?
O12 S1 1.4354(18) . ?
O13 S1 1.4417(19) . ?
Cl1 Pd1 2.4039(5) . ?

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
N2 C1 N1 104.08(18) . . ?
N2 C1 Pd1 131.24(15) . . ?
N1 C1 Pd1 124.64(14) . . ?
C3 C2 N1 106.33(19) . . ?
C3 C2 H2 126.8 . . ?
N1 C2 H2 126.8 . . ?
C2 C3 N2 106.79(18) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
N1 C4 C5 111.33(16) . . ?
N1 C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
N1 C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108 . . ?
C4 C5 C6 109.22(16) . . ?
C4 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C4 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
C5 C6 P1 112.22(13) . . ?
C5 C6 H6A 109.2 . . ?
P1 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
P1 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C8 111.50(17) . . ?
N2 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N2 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108 . . ?
C7 C8 C9 110.48(17) . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C8 C9 P2 114.46(15) . . ?
C8 C9 H9A 108.6 . . ?
P2 C9 H9A 108.6 . . ?
C8 C9 H9B 108.6 . . ?
P2 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C16 C11 C12 120.50(19) . . ?
C16 C11 P1 121.03(16) . . ?
C12 C11 P1 118.43(16) . . ?
C13 C12 C11 119.4(2) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C14 C13 C12 120.2(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 120.3(2) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 120.4(2) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 119.1(2) . . ?
C15 C16 H16 120.4 . . ?
C11 C16 H16 120.4 . . ?
C22 C21 C26 120.7(2) . . ?
C22 C21 P1 121.68(16) . . ?
C26 C21 P1 117.37(16) . . ?
C21 C22 C23 119.1(2) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 120.3(2) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 120.6(2) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 119.1(2) . . ?
C25 C26 H26 120.4 . . ?
C21 C26 H26 120.4 . . ?
C36 C31 C32 120.27(19) . . ?
C36 C31 P1 119.99(16) . . ?
C32 C31 P1 119.54(15) . . ?
C33 C32 C31 119.65(19) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.3(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 119.9(2) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C36 C35 C34 120.7(2) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C31 119.2(2) . . ?
C35 C36 H36 120.4 . . ?
C31 C36 H36 120.4 . . ?
C46 C41 C42 120.2(2) . . ?
C46 C41 P2 119.09(18) . . ?
C42 C41 P2 120.58(19) . . ?
C43 C42 C41 119.6(3) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 120.1(3) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C45 C44 C43 120.3(3) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 120.2(3) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C45 C46 C41 119.5(2) . . ?
C45 C46 H46 120.2 . . ?
C41 C46 H46 120.2 . . ?
C56 C51 C52 119.9(2) . . ?
C56 C51 P2 119.90(17) . . ?
C52 C51 P2 120.19(18) . . ?
C53 C52 C51 119.5(2) . . ?
C53 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C54 C53 C52 120.4(2) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C53 C54 C55 120.4(2) . . ?
C53 C54 H54 119.8 . . ?
C55 C54 H54 119.8 . . ?
C54 C55 C56 120.0(3) . . ?
C54 C55 H55 120 . . ?
C56 C55 H55 120 . . ?
C55 C56 C51 119.9(2) . . ?
C55 C56 H56 120.1 . . ?
C51 C56 H56 120.1 . . ?
C62 C61 C66 120.2(2) . . ?
C62 C61 P2 120.08(19) . . ?
C66 C61 P2 119.59(19) . . ?
C63 C62 C61 119.6(3) . . ?
C63 C62 H62 120.2 . . ?
C61 C62 H62 120.2 . . ?
C64 C63 C62 120.1(3) . . ?
C64 C63 H63 119.9 . . ?
C62 C63 H63 119.9 . . ?
C63 C64 C65 120.5(3) . . ?
C63 C64 H64 119.8 . . ?
C65 C64 H64 119.8 . . ?
C64 C65 C66 120.4(3) . . ?
C64 C65 H65 119.8 . . ?
C66 C65 H65 119.8 . . ?
C65 C66 C61 119.2(3) . . ?
C65 C66 H66 120.4 . . ?
C61 C66 H66 120.4 . . ?
C68A C67 C68B 41.9(9) . . ?
C68A C67 Pd1 71.53(15) . . ?
C68B C67 Pd1 72.9(7) . . ?
C68A C67 H67A 115(2) . . ?
C68B C67 H67A 152(2) . . ?
Pd1 C67 H67A 121(2) . . ?
C68A C67 H67B 123(2) . . ?
C68B C67 H67B 82(3) . . ?
Pd1 C67 H67B 101(2) . . ?
H67A C67 H67B 116(3) . . ?
C68B C68A C69 57.6(12) . . ?
C68B C68A C67 70.2(12) . . ?
C69 C68A C67 121.2(3) . . ?
C68B C68A Pd1 78.5(10) . . ?
C69 C68A Pd1 75.09(17) . . ?
C67 C68A Pd1 69.38(14) . . ?
C68B C68A H68 166(3) . . ?
C69 C68A H68 116(2) . . ?
C67 C68A H68 120(2) . . ?
Pd1 C68A H68 113(2) . . ?
C68A C68B C69 76.1(14) . . ?
C68A C68B C67 67.9(13) . . ?
C69 C68B C67 134.4(18) . . ?
C68A C68B Pd1 74.1(11) . . ?
C69 C68B Pd1 76.4(9) . . ?
C67 C68B Pd1 67.8(8) . . ?
C68A C68B H69B 121(2) . . ?
C69 C68B H69B 45.4(11) . . ?
C67 C68B H69B 150(2) . . ?
Pd1 C68B H69B 87(2) . . ?
C68B C69 C68A 46.3(11) . . ?
C68B C69 Pd1 72.1(9) . . ?
C68A C69 Pd1 68.23(16) . . ?
C68B C69 H69A 160(3) . . ?
C68A C69 H69A 123(2) . . ?
Pd1 C69 H69A 123(2) . . ?
C68B C69 H69B 72(3) . . ?
C68A C69 H69B 118(2) . . ?
Pd1 C69 H69B 93(3) . . ?
H69A C69 H69B 116(3) . . ?
C82 C81 H81A 109.5 . . ?
C82 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C82 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
N3 C82 C81 179.3(4) . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
N4 C92 C91 178.3(4) . . ?
F4 C101 F5 108.0(2) . . ?
F4 C101 F6 107.1(2) . . ?
F5 C101 F6 108.3(2) . . ?
F4 C101 S2 111.75(19) . . ?
F5 C101 S2 110.38(18) . . ?
F6 C101 S2 111.14(19) . . ?
F2 C111 F3 108.1(2) . . ?
F2 C111 F1 106.8(2) . . ?
F3 C111 F1 107.0(2) . . ?
F2 C111 S1 111.60(19) . . ?
F3 C111 S1 111.81(18) . . ?
F1 C111 S1 111.32(17) . . ?
C1 N1 C2 111.53(17) . . ?
C1 N1 C4 124.37(17) . . ?
C2 N1 C4 124.06(17) . . ?
C1 N2 C3 111.27(17) . . ?
C1 N2 C7 124.78(18) . . ?
C3 N2 C7 123.94(18) . . ?
C11 P1 C21 111.25(10) . . ?
C11 P1 C31 109.01(9) . . ?
C21 P1 C31 107.55(9) . . ?
C11 P1 C6 109.12(9) . . ?
C21 P1 C6 110.74(10) . . ?
C31 P1 C6 109.11(9) . . ?
C41 P2 C61 109.73(11) . . ?
C41 P2 C51 109.12(10) . . ?
C61 P2 C51 110.26(11) . . ?
C41 P2 C9 109.87(10) . . ?
C61 P2 C9 109.67(11) . . ?
C51 P2 C9 108.17(10) . . ?
O11 S1 O12 115.84(14) . . ?
O11 S1 O13 114.84(14) . . ?
O12 S1 O13 114.32(11) . . ?
O11 S1 C111 102.95(12) . . ?
O12 S1 C111 103.44(11) . . ?
O13 S1 C111 102.98(12) . . ?
O5 S2 O4 115.05(16) . . ?
O5 S2 O6 114.92(16) . . ?
O4 S2 O6 114.05(12) . . ?
O5 S2 C101 104.23(13) . . ?
O4 S2 C101 103.73(13) . . ?
O6 S2 C101 102.74(12) . . ?
C1 Pd1 C67 97.00(9) . . ?
C1 Pd1 C68A 133.03(10) . . ?
C67 Pd1 C68A 39.08(11) . . ?
C1 Pd1 C68B 132.0(6) . . ?
C67 Pd1 C68B 39.3(6) . . ?
C68A Pd1 C68B 27.4(6) . . ?
C1 Pd1 C69 163.26(10) . . ?
C67 Pd1 C69 68.33(11) . . ?
C68A Pd1 C69 36.69(11) . . ?
C68B Pd1 C69 31.5(6) . . ?
C1 Pd1 Cl1 92.57(6) . . ?
C67 Pd1 Cl1 169.64(7) . . ?
C68A Pd1 Cl1 132.87(8) . . ?
C68B Pd1 Cl1 130.3(6) . . ?
C69 Pd1 Cl1 101.62(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
N1 C2 C3 N2 -0.1(2) . . . . ?
N1 C4 C5 C6 -169.44(16) . . . . ?
C4 C5 C6 P1 -174.17(14) . . . . ?
N2 C7 C8 C9 170.01(18) . . . . ?
C7 C8 C9 P2 123.66(18) . . . . ?
C16 C11 C12 C13 3.0(3) . . . . ?
P1 C11 C12 C13 -179.55(19) . . . . ?
C11 C12 C13 C14 -1.4(4) . . . . ?
C12 C13 C14 C15 -1.3(4) . . . . ?
C13 C14 C15 C16 2.3(4) . . . . ?
C14 C15 C16 C11 -0.8(3) . . . . ?
C12 C11 C16 C15 -1.9(3) . . . . ?
P1 C11 C16 C15 -179.33(16) . . . . ?
C26 C21 C22 C23 -0.5(3) . . . . ?
P1 C21 C22 C23 173.85(17) . . . . ?
C21 C22 C23 C24 0.1(3) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C23 C24 C25 C26 -0.3(4) . . . . ?
C24 C25 C26 C21 -0.1(4) . . . . ?
C22 C21 C26 C25 0.5(3) . . . . ?
P1 C21 C26 C25 -174.06(18) . . . . ?
C36 C31 C32 C33 -1.7(3) . . . . ?
P1 C31 C32 C33 -176.61(16) . . . . ?
C31 C32 C33 C34 0.8(3) . . . . ?
C32 C33 C34 C35 0.5(4) . . . . ?
C33 C34 C35 C36 -1.0(4) . . . . ?
C34 C35 C36 C31 0.2(4) . . . . ?
C32 C31 C36 C35 1.2(3) . . . . ?
P1 C31 C36 C35 176.1(2) . . . . ?
C46 C41 C42 C43 -0.7(4) . . . . ?
P2 C41 C42 C43 -176.3(2) . . . . ?
C41 C42 C43 C44 0.5(4) . . . . ?
C42 C43 C44 C45 0.4(4) . . . . ?
C43 C44 C45 C46 -1.1(4) . . . . ?
C44 C45 C46 C41 1.0(4) . . . . ?
C42 C41 C46 C45 -0.1(4) . . . . ?
P2 C41 C46 C45 175.67(19) . . . . ?
C56 C51 C52 C53 -0.2(4) . . . . ?
P2 C51 C52 C53 -179.9(2) . . . . ?
C51 C52 C53 C54 0.7(4) . . . . ?
C52 C53 C54 C55 -0.4(4) . . . . ?
C53 C54 C55 C56 -0.4(4) . . . . ?
C54 C55 C56 C51 0.9(4) . . . . ?
C52 C51 C56 C55 -0.5(3) . . . . ?
P2 C51 C56 C55 179.07(18) . . . . ?
C66 C61 C62 C63 -0.3(4) . . . . ?
P2 C61 C62 C63 176.1(2) . . . . ?
C61 C62 C63 C64 0.3(5) . . . . ?
C62 C63 C64 C65 0.0(5) . . . . ?
C63 C64 C65 C66 -0.5(5) . . . . ?
C64 C65 C66 C61 0.5(4) . . . . ?
C62 C61 C66 C65 -0.1(4) . . . . ?
P2 C61 C66 C65 -176.5(2) . . . . ?
Pd1 C67 C68A C68B -84.7(11) . . . . ?
C68B C67 C68A C69 28.0(11) . . . . ?
Pd1 C67 C68A C69 -56.7(2) . . . . ?
C68B C67 C68A Pd1 84.7(11) . . . . ?
C67 C68A C68B C69 151.6(10) . . . . ?
Pd1 C68A C68B C69 79.5(7) . . . . ?
C69 C68A C68B C67 -151.6(10) . . . . ?
Pd1 C68A C68B C67 -72.0(4) . . . . ?
C69 C68A C68B Pd1 -79.5(7) . . . . ?
C67 C68A C68B Pd1 72.0(4) . . . . ?
Pd1 C67 C68B C68A 81.2(8) . . . . ?
C68A C67 C68B C69 -40.3(17) . . . . ?
Pd1 C67 C68B C69 40.8(19) . . . . ?
C68A C67 C68B Pd1 -81.2(8) . . . . ?
C67 C68B C69 C68A 38.2(16) . . . . ?
Pd1 C68B C69 C68A 76.7(9) . . . . ?
C68A C68B C69 Pd1 -76.7(9) . . . . ?
C67 C68B C69 Pd1 -38.5(17) . . . . ?
C67 C68A C69 C68B -31.6(12) . . . . ?
Pd1 C68A C69 C68B -85.6(12) . . . . ?
C68B C68A C69 Pd1 85.6(12) . . . . ?
C67 C68A C69 Pd1 54.1(2) . . . . ?
N2 C1 N1 C2 0.7(2) . . . . ?
Pd1 C1 N1 C2 -177.18(14) . . . . ?
N2 C1 N1 C4 178.41(17) . . . . ?
Pd1 C1 N1 C4 0.5(3) . . . . ?
C3 C2 N1 C1 -0.4(2) . . . . ?
C3 C2 N1 C4 -178.07(18) . . . . ?
C5 C4 N1 C1 -95.7(2) . . . . ?
C5 C4 N1 C2 81.7(2) . . . . ?
N1 C1 N2 C3 -0.8(2) . . . . ?
Pd1 C1 N2 C3 176.90(15) . . . . ?
N1 C1 N2 C7 -179.82(17) . . . . ?
Pd1 C1 N2 C7 -2.1(3) . . . . ?
C2 C3 N2 C1 0.6(2) . . . . ?
C2 C3 N2 C7 179.63(18) . . . . ?
C8 C7 N2 C1 98.8(2) . . . . ?
C8 C7 N2 C3 -80.1(2) . . . . ?
C16 C11 P1 C21 -15.3(2) . . . . ?
C12 C11 P1 C21 167.18(17) . . . . ?
C16 C11 P1 C31 -133.78(17) . . . . ?
C12 C11 P1 C31 48.74(19) . . . . ?
C16 C11 P1 C6 107.14(18) . . . . ?
C12 C11 P1 C6 -70.34(19) . . . . ?
C22 C21 P1 C11 124.44(18) . . . . ?
C26 C21 P1 C11 -61.02(19) . . . . ?
C22 C21 P1 C31 -116.24(18) . . . . ?
C26 C21 P1 C31 58.30(18) . . . . ?
C22 C21 P1 C6 2.9(2) . . . . ?
C26 C21 P1 C6 177.44(16) . . . . ?
C36 C31 P1 C11 30.6(2) . . . . ?
C32 C31 P1 C11 -154.47(16) . . . . ?
C36 C31 P1 C21 -90.11(19) . . . . ?
C32 C31 P1 C21 84.80(18) . . . . ?
C36 C31 P1 C6 149.71(18) . . . . ?
C32 C31 P1 C6 -35.38(19) . . . . ?
C5 C6 P1 C11 -44.99(17) . . . . ?
C5 C6 P1 C21 77.79(16) . . . . ?
C5 C6 P1 C31 -164.01(14) . . . . ?
C46 C41 P2 C61 160.52(18) . . . . ?
C42 C41 P2 C61 -23.7(2) . . . . ?
C46 C41 P2 C51 -78.6(2) . . . . ?
C42 C41 P2 C51 97.2(2) . . . . ?
C46 C41 P2 C9 39.9(2) . . . . ?
C42 C41 P2 C9 -144.40(19) . . . . ?
C62 C61 P2 C41 136.4(2) . . . . ?
C66 C61 P2 C41 -47.2(2) . . . . ?
C62 C61 P2 C51 16.2(2) . . . . ?
C66 C61 P2 C51 -167.41(19) . . . . ?
C62 C61 P2 C9 -102.8(2) . . . . ?
C66 C61 P2 C9 73.6(2) . . . . ?
C56 C51 P2 C41 169.52(18) . . . . ?
C52 C51 P2 C41 -10.9(2) . . . . ?
C56 C51 P2 C61 -69.9(2) . . . . ?
C52 C51 P2 C61 109.73(19) . . . . ?
C56 C51 P2 C9 50.0(2) . . . . ?
C52 C51 P2 C9 -130.36(19) . . . . ?
C8 C9 P2 C41 53.07(19) . . . . ?
C8 C9 P2 C61 -67.62(18) . . . . ?
C8 C9 P2 C51 172.10(16) . . . . ?
F2 C111 S1 O11 58.2(2) . . . . ?
F3 C111 S1 O11 -63.0(2) . . . . ?
F1 C111 S1 O11 177.4(2) . . . . ?
F2 C111 S1 O12 -62.8(2) . . . . ?
F3 C111 S1 O12 175.97(19) . . . . ?
F1 C111 S1 O12 56.4(2) . . . . ?
F2 C111 S1 O13 177.91(19) . . . . ?
F3 C111 S1 O13 56.7(2) . . . . ?
F1 C111 S1 O13 -62.9(2) . . . . ?
F4 C101 S2 O5 -59.2(2) . . . . ?
F5 C101 S2 O5 -179.4(2) . . . . ?
F6 C101 S2 O5 60.4(2) . . . . ?
F4 C101 S2 O4 61.6(2) . . . . ?
F5 C101 S2 O4 -58.6(2) . . . . ?
F6 C101 S2 O4 -178.82(19) . . . . ?
F4 C101 S2 O6 -179.4(2) . . . . ?
F5 C101 S2 O6 60.4(2) . . . . ?
F6 C101 S2 O6 -59.8(2) . . . . ?


####################################################################### 
# 
# 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_platon_sq
_database_code_depnum_ccdc_archive 'CCDC 1865721'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;

_audit_creation_date             2018-09-03T15:15:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C48 H45 F9 N2 O9 P2 S3'
_chemical_formula_moiety         'C45 H45 N2 P2, 3(C F3 O3 S)'

_chemical_formula_weight         1122.98

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.000(7)
_cell_length_b                   13.831(10)
_cell_length_c                   21.778(14)
_cell_angle_alpha                85.044(17)
_cell_angle_beta                 79.313(18)
_cell_angle_gamma                89.59(2)
_cell_volume                     2949(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      1.80
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             1156
_exptl_crystal_density_method    'not measured'
_exptl_special_details           
;
 ?
;


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.5561
_exptl_absorpt_correction_T_max  0.7462


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_number            168988
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.072
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             12060
_reflns_number_gt                11273
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0239P)²+9.6744P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         12060
_refine_ls_number_parameters     731
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1438
_refine_ls_wR_factor_gt          0.1416
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.57
_refine_diff_density_rms         0.08

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C72A C 0.6686(9) 0.5666(8) 0.3792(4) 0.0319(19) Uani 0.755(8) 1 d . . P A 1
F7A F 0.7066(4) 0.5076(3) 0.3328(2) 0.0502(11) Uani 0.755(8) 1 d . . P A 1
F8A F 0.5914(4) 0.5148(3) 0.42681(18) 0.0496(12) Uani 0.755(8) 1 d . . P A 1
F9A F 0.7809(3) 0.5944(3) 0.39683(16) 0.0448(12) Uani 0.755(8) 1 d . . P A 1
O7A O 0.6778(10) 0.7145(7) 0.2983(4) 0.0238(15) Uani 0.755(8) 1 d . . P A 1
O8A O 0.4620(12) 0.6259(8) 0.3324(6) 0.055(3) Uani 0.755(8) 1 d . . P A 1
O9A O 0.5458(5) 0.7262(4) 0.4041(2) 0.0442(12) Uani 0.755(8) 1 d . . P A 1
S3A S 0.5762(4) 0.6733(2) 0.35003(15) 0.0226(5) Uani 0.755(8) 1 d . . P A 1
F8B F 0.7399(13) 0.6677(14) 0.4222(6) 0.076(6) Uani 0.245(8) 1 d . . P A 2
F9B F 0.5524(14) 0.5873(16) 0.4528(7) 0.086(7) Uani 0.245(8) 1 d . . P A 2
F7B F 0.704(2) 0.540(2) 0.3754(17) 0.085(10) Uani 0.245(8) 1 d . . P A 2
C72B C 0.643(2) 0.619(2) 0.4049(13) 0.061(7) Uani 0.245(8) 1 d . . P A 2
O7B O 0.659(4) 0.719(3) 0.3023(19) 0.063(13) Uani 0.245(8) 1 d . U P A 2
O8B O 0.463(3) 0.6276(13) 0.3317(10) 0.013(5) Uani 0.245(8) 1 d . U P A 2
O9B O 0.5089(14) 0.7704(14) 0.3844(8) 0.049(4) Uani 0.245(8) 1 d . . P A 2
S3B S 0.5617(17) 0.6815(13) 0.3500(8) 0.077(5) Uani 0.245(8) 1 d . . P A 2
C1 C 0.4078(3) 0.4934(2) 0.20956(14) 0.0172(6) Uani 1 1 d . . . . .
H1 H 0.391 0.5059 0.2525 0.021 Uiso 1 1 calc R U . . .
C2 C 0.4009(3) 0.4280(2) 0.12170(15) 0.0218(6) Uani 1 1 d . . . . .
H2 H 0.3779 0.3861 0.0928 0.026 Uiso 1 1 calc R U . . .
C3 C 0.4897(3) 0.5032(2) 0.10836(14) 0.0192(6) Uani 1 1 d . . . . .
H3 H 0.5403 0.5248 0.0682 0.023 Uiso 1 1 calc R U . . .
C4 C 0.2415(3) 0.3561(2) 0.21792(16) 0.0236(7) Uani 1 1 d . . . . .
H4A H 0.1785 0.3445 0.1892 0.028 Uiso 1 1 calc R U . . .
H4B H 0.1891 0.3867 0.2542 0.028 Uiso 1 1 calc R U . . .
C5 C 0.2959(3) 0.2589(2) 0.24104(15) 0.0195(6) Uani 1 1 d . . . . .
H5A H 0.3512 0.2679 0.2734 0.023 Uiso 1 1 calc R U . . .
H5B H 0.3532 0.2286 0.2059 0.023 Uiso 1 1 calc R U . . .
C6 C 0.1703(3) 0.1949(2) 0.26879(15) 0.0207(6) Uani 1 1 d . . . . .
H6A H 0.1187 0.1866 0.2349 0.025 Uiso 1 1 calc R U . . .
H6B H 0.1112 0.2305 0.3008 0.025 Uiso 1 1 calc R U . . .
C7 C 0.5677(3) 0.6321(2) 0.17028(14) 0.0167(6) Uani 1 1 d . . . . .
H7A H 0.5488 0.6467 0.2147 0.02 Uiso 1 1 calc R U . . .
H7B H 0.5343 0.687 0.1452 0.02 Uiso 1 1 calc R U . . .
C8 C 0.7214(3) 0.62283(19) 0.14867(13) 0.0142(5) Uani 1 1 d . . . . .
H8A H 0.7425 0.6056 0.1048 0.017 Uiso 1 1 calc R U . . .
H8B H 0.7583 0.572 0.1756 0.017 Uiso 1 1 calc R U . . .
C9 C 0.7833(3) 0.72239(19) 0.15411(13) 0.0133(5) Uani 1 1 d . . . . .
H9A H 0.7531 0.7393 0.1978 0.016 Uiso 1 1 calc R U . . .
H9B H 0.7436 0.7708 0.1266 0.016 Uiso 1 1 calc R U . . .
C11 C 0.2613(3) 0.0863(2) 0.37614(15) 0.0244(7) Uani 1 1 d . . . . .
C12 C 0.3957(4) 0.1090(3) 0.37543(17) 0.0331(8) Uani 1 1 d . . . . .
H12 H 0.4584 0.1158 0.3368 0.04 Uiso 1 1 calc R U . . .
C13 C 0.4399(4) 0.1219(3) 0.4313(2) 0.0437(10) Uani 1 1 d . . . . .
H13 H 0.533 0.136 0.4307 0.052 Uiso 1 1 calc R U . . .
C14 C 0.3499(5) 0.1142(4) 0.4865(2) 0.0566(13) Uani 1 1 d . . . . .
H14 H 0.3799 0.1234 0.5245 0.068 Uiso 1 1 calc R U . . .
C15 C 0.2145(6) 0.0929(6) 0.4874(2) 0.078(2) Uani 1 1 d . . . . .
H15 H 0.1518 0.0881 0.5261 0.094 Uiso 1 1 calc R U . . .
C16 C 0.1698(5) 0.0786(4) 0.43240(19) 0.0540(13) Uani 1 1 d . . . . .
H16 H 0.0769 0.0635 0.4333 0.065 Uiso 1 1 calc R U . . .
C21 C 0.3213(3) 0.0136(2) 0.25082(14) 0.0171(6) Uani 1 1 d . . . . .
C22 C 0.4133(3) -0.0526(2) 0.27205(15) 0.0224(6) Uani 1 1 d . . . . .
H22 H 0.4142 -0.0645 0.3156 0.027 Uiso 1 1 calc R U . . .
C23 C 0.5033(3) -0.1004(2) 0.22829(16) 0.0274(7) Uani 1 1 d . . . . .
H23 H 0.5654 -0.1458 0.2421 0.033 Uiso 1 1 calc R U . . .
C24 C 0.5030(3) -0.0823(2) 0.16471(16) 0.0277(7) Uani 1 1 d . . . . .
H24 H 0.5665 -0.1141 0.1352 0.033 Uiso 1 1 calc R U . . .
C25 C 0.4108(4) -0.0183(2) 0.14405(15) 0.0260(7) Uani 1 1 d . . . . .
H25 H 0.409 -0.0076 0.1005 0.031 Uiso 1 1 calc R U . . .
C26 C 0.3207(3) 0.0306(2) 0.18702(14) 0.0206(6) Uani 1 1 d . . . . .
H26 H 0.2585 0.0756 0.1728 0.025 Uiso 1 1 calc R U . . .
C31 C 0.0413(3) 0.0122(2) 0.32059(14) 0.0192(6) Uani 1 1 d . . . . .
C32 C 0.0401(4) -0.0886(2) 0.32551(18) 0.0307(8) Uani 1 1 d . . . . .
H32 H 0.1236 -0.1227 0.3209 0.037 Uiso 1 1 calc R U . . .
C33 C -0.0821(4) -0.1398(3) 0.33706(18) 0.0359(8) Uani 1 1 d . . . . .
H33 H -0.0818 -0.2087 0.3402 0.043 Uiso 1 1 calc R U . . .
C34 C -0.2030(4) -0.0914(3) 0.34391(16) 0.0309(8) Uani 1 1 d . . . . .
H34 H -0.2867 -0.1265 0.3523 0.037 Uiso 1 1 calc R U . . .
C35 C -0.2025(4) 0.0082(3) 0.3385(2) 0.0400(9) Uani 1 1 d . . . . .
H35 H -0.2866 0.0417 0.3431 0.048 Uiso 1 1 calc R U . . .
C36 C -0.0815(4) 0.0610(3) 0.32659(19) 0.0342(8) Uani 1 1 d . . . . .
H36 H -0.0827 0.13 0.3226 0.041 Uiso 1 1 calc R U . . .
C41 C 0.9970(3) 0.8651(2) 0.12028(13) 0.0150(5) Uani 1 1 d . . . . .
C42 C 1.0899(3) 0.9046(2) 0.06887(14) 0.0182(6) Uani 1 1 d . . . . .
H42 H 1.1388 0.8636 0.0399 0.022 Uiso 1 1 calc R U . . .
C43 C 1.1109(3) 1.0049(2) 0.06013(16) 0.0234(7) Uani 1 1 d . . . . .
H43 H 1.1747 1.0324 0.0253 0.028 Uiso 1 1 calc R U . . .
C44 C 1.0385(3) 1.0644(2) 0.10230(16) 0.0233(7) Uani 1 1 d . . . . .
H44 H 1.0526 1.1327 0.096 0.028 Uiso 1 1 calc R U . . .
C45 C 0.9460(3) 1.0253(2) 0.15337(16) 0.0253(7) Uani 1 1 d . . . . .
H45 H 0.8964 1.0666 0.1819 0.03 Uiso 1 1 calc R U . . .
C46 C 0.9256(3) 0.9259(2) 0.16302(15) 0.0204(6) Uani 1 1 d . . . . .
H46 H 0.8631 0.8989 0.1986 0.025 Uiso 1 1 calc R U . . .
C51 C 1.0437(3) 0.6934(2) 0.19983(13) 0.0141(5) Uani 1 1 d . . . . .
C52 C 0.9877(3) 0.6146(2) 0.24054(15) 0.0227(6) Uani 1 1 d . . . . .
H52 H 0.9071 0.5839 0.2344 0.027 Uiso 1 1 calc R U . . .
C53 C 1.0502(3) 0.5813(3) 0.29000(16) 0.0276(7) Uani 1 1 d . . . . .
H53 H 1.0126 0.5274 0.3176 0.033 Uiso 1 1 calc R U . . .
C54 C 1.1673(3) 0.6263(2) 0.29943(15) 0.0236(7) Uani 1 1 d . . . . .
H54 H 1.2086 0.6041 0.3339 0.028 Uiso 1 1 calc R U . . .
C55 C 1.2238(3) 0.7035(2) 0.25855(16) 0.0225(6) Uani 1 1 d . . . . .
H55 H 1.3049 0.7333 0.2648 0.027 Uiso 1 1 calc R U . . .
C56 C 1.1633(3) 0.7379(2) 0.20840(15) 0.0202(6) Uani 1 1 d . . . . .
H56 H 1.2026 0.7909 0.1804 0.024 Uiso 1 1 calc R U . . .
C61 C 1.0344(3) 0.67529(19) 0.06708(13) 0.0135(5) Uani 1 1 d . . . . .
C62 C 0.9927(3) 0.7051(2) 0.01063(14) 0.0184(6) Uani 1 1 d . . . . .
H62 H 0.9292 0.7563 0.009 0.022 Uiso 1 1 calc R U . . .
C63 C 1.0440(3) 0.6600(2) -0.04282(15) 0.0211(6) Uani 1 1 d . . . . .
H63 H 1.0169 0.6806 -0.0814 0.025 Uiso 1 1 calc R U . . .
C64 C 1.1352(3) 0.5845(2) -0.04006(15) 0.0224(6) Uani 1 1 d . . . . .
H64 H 1.1708 0.5539 -0.077 0.027 Uiso 1 1 calc R U . . .
C65 C 1.1751(3) 0.5530(2) 0.01610(16) 0.0237(7) Uani 1 1 d . . . . .
H65 H 1.2362 0.5004 0.0177 0.028 Uiso 1 1 calc R U . . .
C66 C 1.1254(3) 0.5990(2) 0.06974(14) 0.0184(6) Uani 1 1 d . . . . .
H66 H 1.1532 0.5785 0.1082 0.022 Uiso 1 1 calc R U . . .
N1 N 0.3500(2) 0.42352(17) 0.18507(12) 0.0175(5) Uani 1 1 d . . . . .
N2 N 0.4932(2) 0.54298(17) 0.16381(11) 0.0153(5) Uani 1 1 d . . . . .
P1 P 0.20090(7) 0.07631(5) 0.30425(4) 0.01645(16) Uani 1 1 d . . . . .
P2 P 0.96610(7) 0.73645(5) 0.13509(3) 0.01145(14) Uani 1 1 d . . . . .
C70 C 0.6890(4) 0.2915(4) 0.2360(2) 0.0452(10) Uani 1 1 d . . . . .
F1 F 0.6076(3) 0.3517(3) 0.26981(16) 0.0820(11) Uani 1 1 d . . . . .
F2 F 0.6625(3) 0.2029(3) 0.26416(19) 0.0880(12) Uani 1 1 d . . . . .
F3 F 0.6511(3) 0.2954(2) 0.18085(14) 0.0638(8) Uani 1 1 d . . . . .
S1 S 0.86760(8) 0.32507(6) 0.22857(4) 0.02201(17) Uani 1 1 d . . . . .
O1 O 0.8894(3) 0.3223(2) 0.29190(12) 0.0406(7) Uani 1 1 d . . . . .
O2 O 0.9350(2) 0.24978(16) 0.19299(11) 0.0262(5) Uani 1 1 d . . . . .
O3 O 0.8768(3) 0.41951(17) 0.19503(13) 0.0385(6) Uani 1 1 d . . . . .
C71 C 0.4481(3) 0.7959(2) 0.99924(16) 0.0252(7) Uani 1 1 d . . . . .
F4 F 0.3856(2) 0.74977(19) 0.96144(11) 0.0438(6) Uani 1 1 d . . . . .
F5 F 0.4290(2) 0.89085(15) 0.98881(11) 0.0381(5) Uani 1 1 d . . . . .
F6 F 0.3862(2) 0.76951(16) 1.05848(10) 0.0361(5) Uani 1 1 d . . . . .
S2 S 0.62938(7) 0.76669(5) 0.98813(3) 0.01451(14) Uani 1 1 d . . . . .
O4 O 0.6280(2) 0.66372(16) 1.00661(10) 0.0231(5) Uani 1 1 d . . . . .
O5 O 0.6789(2) 0.82616(16) 1.03052(10) 0.0218(5) Uani 1 1 d . . . . .
O6 O 0.6790(2) 0.79193(15) 0.92241(10) 0.0205(4) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C72A F9A 1.322(10) . ?
C72A F8A 1.331(10) . ?
C72A F7A 1.351(11) . ?
C72A S3A 1.863(11) . ?
O7A S3A 1.449(9) . ?
O8A S3A 1.449(12) . ?
O9A S3A 1.423(5) . ?
F8B C72B 1.31(3) . ?
F9B C72B 1.30(2) . ?
F7B C72B 1.39(4) . ?
C72B S3B 1.74(3) . ?
O7B S3B 1.35(4) . ?
O8B S3B 1.38(3) . ?
O9B S3B 1.54(2) . ?
C1 N1 1.328(4) . ?
C1 N2 1.329(4) . ?
C1 H1 0.95 . ?
C2 C3 1.350(4) . ?
C2 N1 1.376(4) . ?
C2 H2 0.95 . ?
C3 N2 1.375(4) . ?
C3 H3 0.95 . ?
C4 N1 1.473(4) . ?
C4 C5 1.527(4) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C6 1.538(4) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 P1 1.801(3) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C7 N2 1.475(4) . ?
C7 C8 1.530(4) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 C9 1.536(4) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 P2 1.806(3) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C11 C12 1.380(5) . ?
C11 C16 1.383(5) . ?
C11 P1 1.795(3) . ?
C12 C13 1.394(5) . ?
C12 H12 0.95 . ?
C13 C14 1.359(6) . ?
C13 H13 0.95 . ?
C14 C15 1.383(7) . ?
C14 H14 0.95 . ?
C15 C16 1.384(6) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C21 C26 1.390(4) . ?
C21 C22 1.403(4) . ?
C21 P1 1.788(3) . ?
C22 C23 1.392(5) . ?
C22 H22 0.95 . ?
C23 C24 1.386(5) . ?
C23 H23 0.95 . ?
C24 C25 1.382(5) . ?
C24 H24 0.95 . ?
C25 C26 1.390(5) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C31 C36 1.387(5) . ?
C31 C32 1.388(5) . ?
C31 P1 1.793(3) . ?
C32 C33 1.388(5) . ?
C32 H32 0.95 . ?
C33 C34 1.368(5) . ?
C33 H33 0.95 . ?
C34 C35 1.373(6) . ?
C34 H34 0.95 . ?
C35 C36 1.389(5) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C41 C42 1.389(4) . ?
C41 C46 1.402(4) . ?
C41 P2 1.799(3) . ?
C42 C43 1.397(4) . ?
C42 H42 0.95 . ?
C43 C44 1.386(5) . ?
C43 H43 0.95 . ?
C44 C45 1.381(5) . ?
C44 H44 0.95 . ?
C45 C46 1.383(4) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C51 C52 1.394(4) . ?
C51 C56 1.399(4) . ?
C51 P2 1.789(3) . ?
C52 C53 1.387(4) . ?
C52 H52 0.95 . ?
C53 C54 1.386(5) . ?
C53 H53 0.95 . ?
C54 C55 1.381(5) . ?
C54 H54 0.95 . ?
C55 C56 1.392(4) . ?
C55 H55 0.95 . ?
C56 H56 0.95 . ?
C61 C66 1.392(4) . ?
C61 C62 1.399(4) . ?
C61 P2 1.791(3) . ?
C62 C63 1.381(4) . ?
C62 H62 0.95 . ?
C63 C64 1.387(4) . ?
C63 H63 0.95 . ?
C64 C65 1.390(5) . ?
C64 H64 0.95 . ?
C65 C66 1.387(4) . ?
C65 H65 0.95 . ?
C66 H66 0.95 . ?
C70 F3 1.322(5) . ?
C70 F2 1.327(5) . ?
C70 F1 1.331(5) . ?
C70 S1 1.823(4) . ?
S1 O1 1.433(3) . ?
S1 O3 1.435(3) . ?
S1 O2 1.441(2) . ?
C71 F4 1.327(4) . ?
C71 F5 1.332(4) . ?
C71 F6 1.344(4) . ?
C71 S2 1.831(3) . ?
S2 O6 1.438(2) . ?
S2 O5 1.442(2) . ?
S2 O4 1.446(2) . ?

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
F9A C72A F8A 109.3(6) . . ?
F9A C72A F7A 107.1(7) . . ?
F8A C72A F7A 107.7(8) . . ?
F9A C72A S3A 110.8(7) . . ?
F8A C72A S3A 111.8(6) . . ?
F7A C72A S3A 110.0(5) . . ?
O9A S3A O8A 116.1(6) . . ?
O9A S3A O7A 117.2(4) . . ?
O8A S3A O7A 115.4(6) . . ?
O9A S3A C72A 102.0(4) . . ?
O8A S3A C72A 100.9(6) . . ?
O7A S3A C72A 101.1(5) . . ?
F9B C72B F8B 111(2) . . ?
F9B C72B F7B 109(3) . . ?
F8B C72B F7B 107(2) . . ?
F9B C72B S3B 108.6(16) . . ?
F8B C72B S3B 114.9(19) . . ?
F7B C72B S3B 105(2) . . ?
O7B S3B O8B 114(2) . . ?
O7B S3B O9B 104(2) . . ?
O8B S3B O9B 114.9(15) . . ?
O7B S3B C72B 108(2) . . ?
O8B S3B C72B 113.7(17) . . ?
O9B S3B C72B 101.4(17) . . ?
N1 C1 N2 108.5(3) . . ?
N1 C1 H1 125.8 . . ?
N2 C1 H1 125.8 . . ?
C3 C2 N1 106.9(3) . . ?
C3 C2 H2 126.5 . . ?
N1 C2 H2 126.5 . . ?
C2 C3 N2 107.2(3) . . ?
C2 C3 H3 126.4 . . ?
N2 C3 H3 126.4 . . ?
N1 C4 C5 113.0(2) . . ?
N1 C4 H4A 109 . . ?
C5 C4 H4A 109 . . ?
N1 C4 H4B 109 . . ?
C5 C4 H4B 109 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 106.2(2) . . ?
C4 C5 H5A 110.5 . . ?
C6 C5 H5A 110.5 . . ?
C4 C5 H5B 110.5 . . ?
C6 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
C5 C6 P1 117.0(2) . . ?
C5 C6 H6A 108 . . ?
P1 C6 H6A 108 . . ?
C5 C6 H6B 108 . . ?
P1 C6 H6B 108 . . ?
H6A C6 H6B 107.3 . . ?
N2 C7 C8 112.4(2) . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 C9 106.2(2) . . ?
C7 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
C7 C8 H8B 110.5 . . ?
C9 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
C8 C9 P2 118.25(19) . . ?
C8 C9 H9A 107.7 . . ?
P2 C9 H9A 107.7 . . ?
C8 C9 H9B 107.7 . . ?
P2 C9 H9B 107.7 . . ?
H9A C9 H9B 107.1 . . ?
C12 C11 C16 119.6(3) . . ?
C12 C11 P1 120.7(3) . . ?
C16 C11 P1 119.5(3) . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120 . . ?
C12 C13 H13 120 . . ?
C13 C14 C15 120.0(4) . . ?
C13 C14 H14 120 . . ?
C15 C14 H14 120 . . ?
C14 C15 C16 120.5(4) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C11 C16 C15 119.6(4) . . ?
C11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C26 C21 C22 120.2(3) . . ?
C26 C21 P1 118.3(2) . . ?
C22 C21 P1 121.5(2) . . ?
C23 C22 C21 118.9(3) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C24 C23 C22 120.6(3) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C25 C24 C23 120.3(3) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 119.9(3) . . ?
C24 C25 H25 120 . . ?
C26 C25 H25 120 . . ?
C25 C26 C21 120.0(3) . . ?
C25 C26 H26 120 . . ?
C21 C26 H26 120 . . ?
C36 C31 C32 119.0(3) . . ?
C36 C31 P1 121.5(3) . . ?
C32 C31 P1 119.5(2) . . ?
C31 C32 C33 120.6(3) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C34 C33 C32 120.2(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 119.5(3) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C34 C35 C36 121.3(4) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C31 C36 C35 119.4(3) . . ?
C31 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
C42 C41 C46 120.0(3) . . ?
C42 C41 P2 122.0(2) . . ?
C46 C41 P2 118.0(2) . . ?
C41 C42 C43 119.5(3) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 H42 120.2 . . ?
C44 C43 C42 120.0(3) . . ?
C44 C43 H43 120 . . ?
C42 C43 H43 120 . . ?
C45 C44 C43 120.5(3) . . ?
C45 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C44 C45 C46 120.1(3) . . ?
C44 C45 H45 120 . . ?
C46 C45 H45 120 . . ?
C45 C46 C41 119.9(3) . . ?
C45 C46 H46 120 . . ?
C41 C46 H46 120 . . ?
C52 C51 C56 120.2(3) . . ?
C52 C51 P2 120.4(2) . . ?
C56 C51 P2 119.4(2) . . ?
C53 C52 C51 119.7(3) . . ?
C53 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C54 C53 C52 120.4(3) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C55 C54 C53 119.9(3) . . ?
C55 C54 H54 120.1 . . ?
C53 C54 H54 120.1 . . ?
C54 C55 C56 120.8(3) . . ?
C54 C55 H55 119.6 . . ?
C56 C55 H55 119.6 . . ?
C55 C56 C51 119.1(3) . . ?
C55 C56 H56 120.5 . . ?
C51 C56 H56 120.5 . . ?
C66 C61 C62 120.2(3) . . ?
C66 C61 P2 121.6(2) . . ?
C62 C61 P2 118.3(2) . . ?
C63 C62 C61 119.8(3) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C62 C63 C64 119.9(3) . . ?
C62 C63 H63 120.1 . . ?
C64 C63 H63 120.1 . . ?
C63 C64 C65 120.7(3) . . ?
C63 C64 H64 119.6 . . ?
C65 C64 H64 119.6 . . ?
C66 C65 C64 119.6(3) . . ?
C66 C65 H65 120.2 . . ?
C64 C65 H65 120.2 . . ?
C65 C66 C61 119.8(3) . . ?
C65 C66 H66 120.1 . . ?
C61 C66 H66 120.1 . . ?
C1 N1 C2 108.8(2) . . ?
C1 N1 C4 126.8(3) . . ?
C2 N1 C4 124.3(3) . . ?
C1 N2 C3 108.6(2) . . ?
C1 N2 C7 125.5(3) . . ?
C3 N2 C7 125.5(2) . . ?
C21 P1 C31 109.65(15) . . ?
C21 P1 C11 110.59(15) . . ?
C31 P1 C11 109.48(15) . . ?
C21 P1 C6 109.80(15) . . ?
C31 P1 C6 106.93(15) . . ?
C11 P1 C6 110.31(16) . . ?
C51 P2 C61 110.52(14) . . ?
C51 P2 C41 108.08(13) . . ?
C61 P2 C41 110.70(14) . . ?
C51 P2 C9 111.35(13) . . ?
C61 P2 C9 110.60(13) . . ?
C41 P2 C9 105.46(13) . . ?
F3 C70 F2 108.4(4) . . ?
F3 C70 F1 106.1(4) . . ?
F2 C70 F1 106.8(4) . . ?
F3 C70 S1 111.8(3) . . ?
F2 C70 S1 112.0(3) . . ?
F1 C70 S1 111.6(3) . . ?
O1 S1 O3 115.43(17) . . ?
O1 S1 O2 114.76(15) . . ?
O3 S1 O2 114.35(16) . . ?
O1 S1 C70 104.50(19) . . ?
O3 S1 C70 103.58(19) . . ?
O2 S1 C70 101.91(19) . . ?
F4 C71 F5 108.6(3) . . ?
F4 C71 F6 107.6(3) . . ?
F5 C71 F6 107.1(3) . . ?
F4 C71 S2 111.4(2) . . ?
F5 C71 S2 111.4(2) . . ?
F6 C71 S2 110.6(2) . . ?
O6 S2 O5 115.85(14) . . ?
O6 S2 O4 114.32(13) . . ?
O5 S2 O4 114.43(14) . . ?
O6 S2 C71 104.22(14) . . ?
O5 S2 C71 102.90(15) . . ?
O4 S2 C71 102.79(15) . . ?

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
F9A C72A S3A O9A -61.4(6) . . . . ?
F8A C72A S3A O9A 60.7(7) . . . . ?
F7A C72A S3A O9A -179.7(6) . . . . ?
F9A C72A S3A O8A 178.6(7) . . . . ?
F8A C72A S3A O8A -59.2(8) . . . . ?
F7A C72A S3A O8A 60.4(8) . . . . ?
F9A C72A S3A O7A 59.8(7) . . . . ?
F8A C72A S3A O7A -178.0(6) . . . . ?
F7A C72A S3A O7A -58.4(7) . . . . ?
F9B C72B S3B O7B 176(3) . . . . ?
F8B C72B S3B O7B 51(3) . . . . ?
F7B C72B S3B O7B -67(3) . . . . ?
F9B C72B S3B O8B -56(3) . . . . ?
F8B C72B S3B O8B 179(2) . . . . ?
F7B C72B S3B O8B 61(2) . . . . ?
F9B C72B S3B O9B 68(3) . . . . ?
F8B C72B S3B O9B -58(2) . . . . ?
F7B C72B S3B O9B -175.3(19) . . . . ?
N1 C2 C3 N2 0.7(3) . . . . ?
N1 C4 C5 C6 -175.3(3) . . . . ?
C4 C5 C6 P1 -176.7(2) . . . . ?
N2 C7 C8 C9 176.4(2) . . . . ?
C7 C8 C9 P2 177.58(19) . . . . ?
C16 C11 C12 C13 1.4(6) . . . . ?
P1 C11 C12 C13 176.4(3) . . . . ?
C11 C12 C13 C14 -1.4(7) . . . . ?
C12 C13 C14 C15 0.4(8) . . . . ?
C13 C14 C15 C16 0.5(10) . . . . ?
C12 C11 C16 C15 -0.5(8) . . . . ?
P1 C11 C16 C15 -175.6(5) . . . . ?
C14 C15 C16 C11 -0.4(10) . . . . ?
C26 C21 C22 C23 0.1(5) . . . . ?
P1 C21 C22 C23 179.0(2) . . . . ?
C21 C22 C23 C24 0.6(5) . . . . ?
C22 C23 C24 C25 -1.7(5) . . . . ?
C23 C24 C25 C26 2.0(5) . . . . ?
C24 C25 C26 C21 -1.3(5) . . . . ?
C22 C21 C26 C25 0.3(5) . . . . ?
P1 C21 C26 C25 -178.7(2) . . . . ?
C36 C31 C32 C33 -0.8(5) . . . . ?
P1 C31 C32 C33 -178.9(3) . . . . ?
C31 C32 C33 C34 -0.2(6) . . . . ?
C32 C33 C34 C35 0.8(6) . . . . ?
C33 C34 C35 C36 -0.3(6) . . . . ?
C32 C31 C36 C35 1.2(6) . . . . ?
P1 C31 C36 C35 179.3(3) . . . . ?
C34 C35 C36 C31 -0.7(6) . . . . ?
C46 C41 C42 C43 -0.2(4) . . . . ?
P2 C41 C42 C43 -179.3(2) . . . . ?
C41 C42 C43 C44 -0.5(4) . . . . ?
C42 C43 C44 C45 0.4(5) . . . . ?
C43 C44 C45 C46 0.4(5) . . . . ?
C44 C45 C46 C41 -1.1(5) . . . . ?
C42 C41 C46 C45 1.1(4) . . . . ?
P2 C41 C46 C45 -179.9(2) . . . . ?
C56 C51 C52 C53 0.7(5) . . . . ?
P2 C51 C52 C53 179.1(3) . . . . ?
C51 C52 C53 C54 0.5(5) . . . . ?
C52 C53 C54 C55 -1.4(5) . . . . ?
C53 C54 C55 C56 1.1(5) . . . . ?
C54 C55 C56 C51 0.1(5) . . . . ?
C52 C51 C56 C55 -1.0(4) . . . . ?
P2 C51 C56 C55 -179.4(2) . . . . ?
C66 C61 C62 C63 -1.3(4) . . . . ?
P2 C61 C62 C63 179.6(2) . . . . ?
C61 C62 C63 C64 0.9(5) . . . . ?
C62 C63 C64 C65 0.4(5) . . . . ?
C63 C64 C65 C66 -1.3(5) . . . . ?
C64 C65 C66 C61 0.9(5) . . . . ?
C62 C61 C66 C65 0.4(4) . . . . ?
P2 C61 C66 C65 179.5(2) . . . . ?
N2 C1 N1 C2 0.5(3) . . . . ?
N2 C1 N1 C4 -175.1(3) . . . . ?
C3 C2 N1 C1 -0.8(3) . . . . ?
C3 C2 N1 C4 175.0(3) . . . . ?
C5 C4 N1 C1 -96.0(4) . . . . ?
C5 C4 N1 C2 89.0(4) . . . . ?
N1 C1 N2 C3 -0.1(3) . . . . ?
N1 C1 N2 C7 173.8(2) . . . . ?
C2 C3 N2 C1 -0.4(3) . . . . ?
C2 C3 N2 C7 -174.3(3) . . . . ?
C8 C7 N2 C1 124.9(3) . . . . ?
C8 C7 N2 C3 -62.2(4) . . . . ?
C26 C21 P1 C31 83.7(3) . . . . ?
C22 C21 P1 C31 -95.2(3) . . . . ?
C26 C21 P1 C11 -155.5(2) . . . . ?
C22 C21 P1 C11 25.6(3) . . . . ?
C26 C21 P1 C6 -33.5(3) . . . . ?
C22 C21 P1 C6 147.5(3) . . . . ?
C36 C31 P1 C21 -141.1(3) . . . . ?
C32 C31 P1 C21 36.9(3) . . . . ?
C36 C31 P1 C11 97.4(3) . . . . ?
C32 C31 P1 C11 -84.6(3) . . . . ?
C36 C31 P1 C6 -22.1(3) . . . . ?
C32 C31 P1 C6 155.9(3) . . . . ?
C12 C11 P1 C21 41.9(3) . . . . ?
C16 C11 P1 C21 -143.1(4) . . . . ?
C12 C11 P1 C31 162.8(3) . . . . ?
C16 C11 P1 C31 -22.2(4) . . . . ?
C12 C11 P1 C6 -79.8(3) . . . . ?
C16 C11 P1 C6 95.2(4) . . . . ?
C5 C6 P1 C21 -52.0(3) . . . . ?
C5 C6 P1 C31 -170.9(2) . . . . ?
C5 C6 P1 C11 70.2(3) . . . . ?
C52 C51 P2 C61 -89.8(3) . . . . ?
C56 C51 P2 C61 88.6(3) . . . . ?
C52 C51 P2 C41 148.9(2) . . . . ?
C56 C51 P2 C41 -32.6(3) . . . . ?
C52 C51 P2 C9 33.6(3) . . . . ?
C56 C51 P2 C9 -148.0(2) . . . . ?
C66 C61 P2 C51 5.6(3) . . . . ?
C62 C61 P2 C51 -175.2(2) . . . . ?
C66 C61 P2 C41 125.3(2) . . . . ?
C62 C61 P2 C41 -55.5(3) . . . . ?
C66 C61 P2 C9 -118.2(2) . . . . ?
C62 C61 P2 C9 61.0(3) . . . . ?
C42 C41 P2 C51 106.5(3) . . . . ?
C46 C41 P2 C51 -72.6(3) . . . . ?
C42 C41 P2 C61 -14.7(3) . . . . ?
C46 C41 P2 C61 166.3(2) . . . . ?
C42 C41 P2 C9 -134.3(2) . . . . ?
C46 C41 P2 C9 46.6(3) . . . . ?
C8 C9 P2 C51 -82.3(2) . . . . ?
C8 C9 P2 C61 41.0(3) . . . . ?
C8 C9 P2 C41 160.7(2) . . . . ?
F3 C70 S1 O1 176.9(3) . . . . ?
F2 C70 S1 O1 -61.3(4) . . . . ?
F1 C70 S1 O1 58.3(4) . . . . ?
F3 C70 S1 O3 55.7(4) . . . . ?
F2 C70 S1 O3 177.4(3) . . . . ?
F1 C70 S1 O3 -62.9(4) . . . . ?
F3 C70 S1 O2 -63.3(4) . . . . ?
F2 C70 S1 O2 58.5(4) . . . . ?
F1 C70 S1 O2 178.1(3) . . . . ?
F4 C71 S2 O6 56.2(3) . . . . ?
F5 C71 S2 O6 -65.2(3) . . . . ?
F6 C71 S2 O6 175.8(2) . . . . ?
F4 C71 S2 O5 177.5(2) . . . . ?
F5 C71 S2 O5 56.1(3) . . . . ?
F6 C71 S2 O5 -62.9(3) . . . . ?
F4 C71 S2 O4 -63.3(3) . . . . ?
F5 C71 S2 O4 175.3(2) . . . . ?
F6 C71 S2 O4 56.3(3) . . . . ?




# END of CIF
####################################################################### 
# 
# 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_I_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1865717'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;

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

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

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

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

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

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   13.6658(9)
_cell_length_b                   17.1283(10)
_cell_length_c                   21.6507(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.366(2)
_cell_angle_gamma                90
_cell_volume                     5066.4(5)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

_chemical_formula_sum            'C52 H52.2 F6 N3 O6.60 P2 Pd1 S2'
_chemical_formula_moiety         'C50 H51 N3 P2 Pd, 2(C F3 O3 S), 0.6(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         1171.27


_cell_measurement_reflns_used    7112
_cell_measurement_theta_min      3
_cell_measurement_theta_max      21
_cell_measurement_temperature    100

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.010
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_max          0.180

_exptl_crystal_density_diffrn    1.54
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2395.200
_exptl_absorpt_coefficient_mu    0.589

# Sheldrick geometric approximatio 0.99 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_T_max  0.99
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            103825
_reflns_number_total             9276
_diffrn_reflns_av_R_equivalents  0.170
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9276 
# Theoretical number of reflections is about 18651 


_diffrn_reflns_theta_min         1.516
_diffrn_reflns_theta_max         25.396
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        25.396
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              26


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

_refine_diff_density_min         -1.73
_refine_diff_density_max         1.94


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>2.2\s(I)
_refine_ls_number_reflns         5636
_refine_ls_number_restraints     61
_refine_ls_number_parameters     556
_oxford_refine_ls_R_factor_ref   0.0808
_refine_ls_wR_factor_ref         0.0857
_refine_ls_goodness_of_fit_ref   1.1047
_refine_ls_shift/su_max          0.0010463
_refine_ls_shift/su_mean         0.0000247


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9252
_refine_ls_R_factor_all          0.1383
_refine_ls_wR_factor_all         0.1306

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5841
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_gt          0.0871

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


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.839 0.704 0.507 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pd1 Pd 0.45344(4) 0.57440(3) 0.24161(3) 0.0242 1.0000 Uani . . . . . .
P1 P 0.45137(15) 0.46765(12) 0.35987(9) 0.0260 1.0000 Uani . . . . . .
P2 P 0.48576(15) 0.70553(12) 0.14003(9) 0.0271 1.0000 Uani . . . . . .
C1 C 0.3107(5) 0.5790(5) 0.2404(3) 0.0256 1.0000 Uani . . . . . .
C2 C 0.1530(7) 0.5428(6) 0.2258(4) 0.0422 1.0000 Uani . . . . . .
C3 C 0.1544(7) 0.6165(7) 0.2473(4) 0.0447 1.0000 Uani . . . . . .
C4 C 0.2915(8) 0.7117(5) 0.2778(4) 0.0448 1.0000 Uani . . . . . .
C5 C 0.3583(8) 0.7452(5) 0.2287(4) 0.0437 1.0000 Uani . . . . . .
C6 C 0.4514(6) 0.6971(5) 0.2181(4) 0.0331 1.0000 Uani . . . . . .
C7 C 0.2881(6) 0.4451(5) 0.2039(4) 0.0361 1.0000 Uani . . . . . .
C8 C 0.3471(6) 0.4101(5) 0.2570(3) 0.0293 1.0000 Uani . . . . . .
C9 C 0.4392(6) 0.4587(4) 0.2775(3) 0.0253 1.0000 Uani . . . . . .
C10 C 0.5778(6) 0.4877(6) 0.3807(4) 0.0386 1.0000 Uani . . . . . .
C11 C 0.6372(6) 0.4277(8) 0.4046(4) 0.0510 1.0000 Uani . . . . . .
C12 C 0.7332(8) 0.4359(9) 0.4170(6) 0.0667 1.0000 Uani . . . . . .
C13 C 0.7767(9) 0.5037(9) 0.4065(6) 0.0719 1.0000 Uani . . . . . .
C14 C 0.7239(10) 0.5683(8) 0.3840(5) 0.0714 1.0000 Uani . . . . . .
C15 C 0.6199(8) 0.5592(7) 0.3692(4) 0.0538 1.0000 Uani . . . . . .
C16 C 0.4213(6) 0.3773(5) 0.3979(4) 0.0384 1.0000 Uani . . . . . .
C17 C 0.4425(7) 0.3066(5) 0.3687(5) 0.0439 1.0000 Uani . . . . . .
C18 C 0.4241(8) 0.2372(6) 0.4018(7) 0.0650 1.0000 Uani . . . . . .
C19 C 0.3910(9) 0.2402(8) 0.4613(6) 0.0663 1.0000 Uani . . . . . .
C20 C 0.3699(9) 0.3085(8) 0.4885(5) 0.0639 1.0000 Uani . . . . . .
C21 C 0.3836(7) 0.3783(6) 0.4577(4) 0.0439 1.0000 Uani . . . . . .
C22 C 0.3728(6) 0.5417(5) 0.3930(3) 0.0298 1.0000 Uani . . . . . .
C23 C 0.4106(8) 0.6022(6) 0.4292(4) 0.0453 1.0000 Uani . . . . . .
C24 C 0.3509(9) 0.6585(6) 0.4505(5) 0.0509 1.0000 Uani . . . . . .
C25 C 0.2515(9) 0.6563(6) 0.4383(4) 0.0483 1.0000 Uani . . . . . .
C26 C 0.2129(7) 0.5985(5) 0.4029(4) 0.0377 1.0000 Uani . . . . . .
C27 C 0.2731(7) 0.5393(5) 0.3803(4) 0.0368 1.0000 Uani . . . . . .
C34 C 0.4608(6) 0.8004(5) 0.1074(4) 0.0376 1.0000 Uani . . . . . .
C40 C 0.6146(5) 0.6949(4) 0.1275(4) 0.0240 1.0000 Uani . . . . . .
C41 C 0.6840(7) 0.7162(5) 0.1733(4) 0.0370 1.0000 Uani . . . . . .
C42 C 0.7828(7) 0.7202(5) 0.1576(5) 0.0440 1.0000 Uani . . . . . .
C43 C 0.8098(7) 0.7042(5) 0.0987(5) 0.0445 1.0000 Uani . . . . . .
C44 C 0.7432(7) 0.6845(5) 0.0537(5) 0.0434 1.0000 Uani . . . . . .
C45 C 0.6455(6) 0.6803(5) 0.0679(4) 0.0328 1.0000 Uani . . . . . .
C46 C 0.5967(7) 0.5523(4) 0.2308(4) 0.0310 1.0000 Uani . . . . . .
C47 C 0.7629(7) 0.4829(6) 0.2082(4) 0.0404 1.0000 Uani . . . . . .
C48 C 0.7583(8) 0.4059(5) 0.2432(5) 0.0470 1.0000 Uani . . . . . .
C49 C 0.8494(7) 0.5324(6) 0.2321(6) 0.0541 1.0000 Uani . . . . . .
C50 C 0.7620(8) 0.4733(9) 0.1387(5) 0.0694 1.0000 Uani . . . . . .
C51 C 0.4977(9) 0.3039(6) 0.1262(5) 0.0524 1.0000 Uani . . . . . .
N1 N 0.2500(5) 0.5209(4) 0.2218(3) 0.0318 1.0000 Uani . . . . . .
N2 N 0.2506(5) 0.6381(4) 0.2561(3) 0.0355 1.0000 Uani . . . . . .
N3 N 0.6705(6) 0.5259(4) 0.2221(3) 0.0349 1.0000 Uani . . . . . .
F1 F 0.5200(5) 0.3759(3) 0.1504(3) 0.0554 1.0000 Uani . . . . . .
F2 F 0.3998(5) 0.2991(4) 0.1255(3) 0.0752 1.0000 Uani . . . . . .
F3 F 0.5230(8) 0.3096(5) 0.0661(3) 0.1084 1.0000 Uani . . . . . .
O1 O 0.5220(6) 0.2391(4) 0.2279(3) 0.0559 1.0000 Uani . . . . . .
O2 O 0.6594(5) 0.2447(5) 0.1585(5) 0.0845 1.0000 Uani . . . . . .
O3 O 0.5247(5) 0.1583(4) 0.1354(3) 0.0522 1.0000 Uani . . . . . .
O9 O 0.6389(7) 0.7353(6) 0.3237(5) 0.0419 0.6000 Uani . . . . . .
S1 S 0.55809(16) 0.22734(14) 0.16645(11) 0.0412 1.0000 Uani . . . . . .
C330 C 0.3232(3) 0.6392(3) 0.0822(2) 0.0422 0.5000 Uani . . . . . .
C33 C 0.3314(3) 0.6536(3) 0.0642(2) 0.0422 0.5000 Uani . . . . . .
C320 C 0.2690(3) 0.5756(3) 0.0575(2) 0.0644 0.5000 Uani . . . . . .
C32 C 0.2823(3) 0.5950(3) 0.0301(2) 0.0644 0.5000 Uani . . . . . .
C31 C 0.3177(3) 0.5203(3) 0.0287(2) 0.0739 0.5000 Uani . . . . . .
C310 C 0.3161(3) 0.5079(3) 0.0390(2) 0.0739 0.5000 Uani . . . . . .
C30 C 0.4075(3) 0.5039(3) 0.0524(2) 0.0461 0.5000 Uani . . . . . .
C300 C 0.4171(3) 0.4999(3) 0.0543(2) 0.0461 0.5000 Uani . . . . . .
C29 C 0.4589(3) 0.5598(3) 0.0836(2) 0.0337 0.5000 Uani . . . . . .
C290 C 0.4690(3) 0.5595(3) 0.0840(2) 0.0337 0.5000 Uani . . . . . .
C28 C 0.4207(3) 0.6354(3) 0.0935(2) 0.0479 1.0000 Uani . . . . . .
C350 C 0.4241(4) 0.8042(3) 0.0452(2) 0.0540 0.5000 Uani . . . . . .
C35 C 0.4440(4) 0.8171(3) 0.0456(2) 0.0540 0.5000 Uani . . . . . .
C360 C 0.4104(4) 0.8763(3) 0.0215(2) 0.0541 0.5000 Uani . . . . . .
C36 C 0.4453(4) 0.8916(3) 0.0214(2) 0.0541 0.5000 Uani . . . . . .
C370 C 0.4309(4) 0.9434(3) 0.0556(2) 0.0566 0.5000 Uani . . . . . .
C37 C 0.4496(4) 0.9538(3) 0.0605(2) 0.0566 0.5000 Uani . . . . . .
C380 C 0.4633(4) 0.9388(3) 0.1176(2) 0.0463 0.5000 Uani . . . . . .
C38 C 0.4691(4) 0.9406(3) 0.1233(2) 0.0463 0.5000 Uani . . . . . .
C39 C 0.4787(4) 0.8680(3) 0.1489(2) 0.0449 0.5000 Uani . . . . . .
C390 C 0.4784(4) 0.8664(3) 0.1432(2) 0.0449 0.5000 Uani . . . . . .
S2 S 0.4470(3) 0.8632(3) 0.38678(19) 0.0630 0.6000 Uani D . . . . .
S3 S 0.5049(6) 0.8342(4) 0.3698(3) 0.0913 0.4000 Uani D . . . . .
O4 O 0.5226(6) 0.8124(5) 0.4113(4) 0.0986 0.6000 Uani D . . . . .
O5 O 0.3443(6) 0.8422(5) 0.3939(3) 0.0702 0.6000 Uani D . . . . .
O6 O 0.4741(5) 0.8889(4) 0.3229(3) 0.0962 1.0000 Uani D . . . . .
O7 O 0.4483(12) 0.7646(6) 0.3798(5) 0.1242 0.4000 Uani D . . . . .
O8 O 0.6112(9) 0.8221(9) 0.3660(5) 0.1248 0.4000 Uani D . . . . .
C52 C 0.4648(4) 0.9440(4) 0.4409(3) 0.0731 0.6000 Uani D . . . . .
C53 C 0.4791(6) 0.8947(6) 0.4371(3) 0.0632 0.4000 Uani D . . . . .
F4 F 0.4400(7) 0.9217(6) 0.4977(3) 0.0909 0.6000 Uani D . . . . .
F5 F 0.4088(8) 1.0042(5) 0.4246(4) 0.1007 0.6000 Uani D . . . . .
F6 F 0.5586(6) 0.9650(6) 0.4432(4) 0.1008 0.6000 Uani D . . . . .
F7 F 0.4191(8) 0.9527(7) 0.4207(5) 0.0742 0.4000 Uani D . . . . .
F8 F 0.4356(11) 0.8528(8) 0.4802(5) 0.1399 0.4000 Uani D . . . . .
F9 F 0.5618(7) 0.9262(7) 0.4596(5) 0.0632 0.4000 Uani D . . . . .
H21 H 0.0979 0.5128 0.2160 0.0500 1.0000 Uiso . . . . . .
H31 H 0.0984 0.6488 0.2547 0.0540 1.0000 Uiso . . . . . .
H41 H 0.2378 0.7484 0.2866 0.0540 1.0000 Uiso . . . . . .
H42 H 0.3287 0.7033 0.3164 0.0540 1.0000 Uiso . . . . . .
H51 H 0.3769 0.7983 0.2399 0.0520 1.0000 Uiso . . . . . .
H52 H 0.3212 0.7467 0.1893 0.0520 1.0000 Uiso . . . . . .
H61 H 0.5028 0.7235 0.2432 0.0421 1.0000 Uiso . . . . . .
H71 H 0.3297 0.4499 0.1682 0.0419 1.0000 Uiso . . . . . .
H72 H 0.2340 0.4100 0.1929 0.0420 1.0000 Uiso . . . . . .
H81 H 0.3038 0.4050 0.2919 0.0380 1.0000 Uiso . . . . . .
H82 H 0.3681 0.3579 0.2445 0.0381 1.0000 Uiso . . . . . .
H91 H 0.4970 0.4285 0.2640 0.0311 1.0000 Uiso . . . . . .
H111 H 0.6071 0.3782 0.4113 0.0651 1.0000 Uiso . . . . . .
H121 H 0.7730 0.3913 0.4320 0.0911 1.0000 Uiso . . . . . .
H131 H 0.8422 0.5113 0.4141 0.0871 1.0000 Uiso . . . . . .
H141 H 0.7564 0.6177 0.3803 0.0920 1.0000 Uiso . . . . . .
H151 H 0.5795 0.6026 0.3529 0.0779 1.0000 Uiso . . . . . .
H171 H 0.4649 0.3044 0.3276 0.0440 1.0000 Uiso . . . . . .
H181 H 0.4367 0.1891 0.3828 0.0760 1.0000 Uiso . . . . . .
H191 H 0.3826 0.1938 0.4836 0.0770 1.0000 Uiso . . . . . .
H201 H 0.3481 0.3077 0.5285 0.0781 1.0000 Uiso . . . . . .
H211 H 0.3668 0.4265 0.4771 0.0561 1.0000 Uiso . . . . . .
H231 H 0.4806 0.6038 0.4384 0.0570 1.0000 Uiso . . . . . .
H241 H 0.3790 0.7001 0.4747 0.0631 1.0000 Uiso . . . . . .
H251 H 0.2116 0.6949 0.4544 0.0600 1.0000 Uiso . . . . . .
H261 H 0.1445 0.5967 0.3936 0.0461 1.0000 Uiso . . . . . .
H271 H 0.2467 0.4967 0.3568 0.0440 1.0000 Uiso . . . . . .
H411 H 0.6633 0.7278 0.2136 0.0460 1.0000 Uiso . . . . . .
H421 H 0.8290 0.7350 0.1885 0.0570 1.0000 Uiso . . . . . .
H431 H 0.8784 0.7049 0.0904 0.0541 1.0000 Uiso . . . . . .
H441 H 0.7629 0.6740 0.0124 0.0551 1.0000 Uiso . . . . . .
H451 H 0.5971 0.6683 0.0374 0.0401 1.0000 Uiso . . . . . .
H481 H 0.7049 0.3741 0.2261 0.0751 1.0000 Uiso . . . . . .
H482 H 0.7461 0.4145 0.2866 0.0750 1.0000 Uiso . . . . . .
H483 H 0.8184 0.3775 0.2399 0.0751 1.0000 Uiso . . . . . .
H491 H 0.8544 0.5788 0.2081 0.0830 1.0000 Uiso . . . . . .
H492 H 0.8390 0.5466 0.2751 0.0830 1.0000 Uiso . . . . . .
H493 H 0.9082 0.5026 0.2301 0.0830 1.0000 Uiso . . . . . .
H501 H 0.7570 0.5231 0.1174 0.0990 1.0000 Uiso . . . . . .
H502 H 0.8221 0.4483 0.1253 0.0990 1.0000 Uiso . . . . . .
H503 H 0.7078 0.4409 0.1248 0.0990 1.0000 Uiso . . . . . .
H3501 H 0.4098 0.7588 0.0218 0.0640 0.5000 Uiso . . . . . .
H3601 H 0.3858 0.8815 -0.0196 0.0642 0.5000 Uiso . . . . . .
H351 H 0.4308 0.7751 0.0183 0.0640 0.5000 Uiso . . . . . .
H361 H 0.4428 0.8995 -0.0219 0.0642 0.5000 Uiso . . . . . .
H3701 H 0.4225 0.9932 0.0369 0.0671 0.5000 Uiso . . . . . .
H371 H 0.4392 1.0055 0.0455 0.0671 0.5000 Uiso . . . . . .
H381 H 0.4759 0.9848 0.1499 0.0548 0.5000 Uiso . . . . . .
H3801 H 0.4743 0.9849 0.1414 0.0548 0.5000 Uiso . . . . . .
H3901 H 0.5005 0.8618 0.1851 0.0531 0.5000 Uiso . . . . . .
H391 H 0.4958 0.8615 0.1915 0.0531 0.5000 Uiso . . . . . .
H331 H 0.3047 0.7048 0.0667 0.0518 0.5000 Uiso . . . . . .
H321 H 0.2242 0.6078 0.0070 0.0784 0.5000 Uiso . . . . . .
H3201 H 0.2001 0.5795 0.0530 0.0784 0.5000 Uiso . . . . . .
H311 H 0.2792 0.4801 0.0103 0.0898 0.5000 Uiso . . . . . .
H3101 H 0.2822 0.4686 0.0162 0.0898 0.5000 Uiso . . . . . .
H3001 H 0.4503 0.4533 0.0434 0.0565 0.5000 Uiso . . . . . .
H301 H 0.4352 0.4536 0.0468 0.0565 0.5000 Uiso . . . . . .
H2901 H 0.5351 0.5517 0.0973 0.0415 0.5000 Uiso . . . . . .
H291 H 0.5231 0.5481 0.0987 0.0415 0.5000 Uiso . . . . . .
H3301 H 0.2902 0.6866 0.0906 0.0518 0.5000 Uiso . . . . . .

_refine_ls_extinction_method     None

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . C1 . 1.951(7) yes
Pd1 . C6 . 2.162(9) yes
Pd1 . C9 . 2.138(7) yes
Pd1 . C46 . 2.013(9) yes
P1 . C9 . 1.794(8) yes
P1 . C10 . 1.808(8) yes
P1 . C16 . 1.805(8) yes
P1 . C22 . 1.820(9) yes
P2 . C6 . 1.770(8) yes
P2 . C34 . 1.801(9) yes
P2 . C40 . 1.798(7) yes
P2 . C28 . 1.790(5) yes
C1 . N1 . 1.351(11) yes
C1 . N2 . 1.352(10) yes
C2 . C3 . 1.346(15) yes
C2 . N1 . 1.382(11) yes
C2 . H21 . 0.932 no
C3 . N2 . 1.375(12) yes
C3 . H31 . 0.960 no
C4 . C5 . 1.531(13) yes
C4 . N2 . 1.453(13) yes
C4 . H41 . 0.987 no
C4 . H42 . 0.979 no
C5 . C6 . 1.538(12) yes
C5 . H51 . 0.973 no
C5 . H52 . 0.981 no
C6 . H61 . 0.989 no
C7 . C8 . 1.512(12) yes
C7 . N1 . 1.455(12) yes
C7 . H71 . 0.975 no
C7 . H72 . 0.977 no
C8 . C9 . 1.565(11) yes
C8 . H81 . 0.975 no
C8 . H82 . 0.979 no
C9 . H91 . 0.994 no
C10 . C11 . 1.400(14) yes
C10 . C15 . 1.379(14) yes
C11 . C12 . 1.340(14) yes
C11 . H111 . 0.956 no
C12 . C13 . 1.327(19) yes
C12 . H121 . 0.988 no
C13 . C14 . 1.40(2) yes
C13 . H131 . 0.916 no
C14 . C15 . 1.458(16) yes
C14 . H141 . 0.961 no
C15 . H151 . 0.985 no
C16 . C17 . 1.400(14) yes
C16 . C21 . 1.405(14) yes
C17 . C18 . 1.413(14) yes
C17 . H171 . 0.949 no
C18 . C19 . 1.376(19) yes
C18 . H181 . 0.938 no
C19 . C20 . 1.344(19) yes
C19 . H191 . 0.939 no
C20 . C21 . 1.385(14) yes
C20 . H201 . 0.923 no
C21 . H211 . 0.955 no
C22 . C23 . 1.391(12) yes
C22 . C27 . 1.384(13) yes
C23 . C24 . 1.350(15) yes
C23 . H231 . 0.973 no
C24 . C25 . 1.379(16) yes
C24 . H241 . 0.959 no
C25 . C26 . 1.351(14) yes
C25 . H251 . 0.930 no
C26 . C27 . 1.402(13) yes
C26 . H261 . 0.951 no
C27 . H271 . 0.956 no
C34 . C350 . 1.428(10) yes
C34 . C35 . 1.382(10) yes
C34 . C39 . 1.482(11) yes
C34 . C390 . 1.389(11) yes
C40 . C41 . 1.404(12) yes
C40 . C45 . 1.390(11) yes
C41 . C42 . 1.402(13) yes
C41 . H411 . 0.944 no
C42 . C43 . 1.364(14) yes
C42 . H421 . 0.944 no
C43 . C44 . 1.360(14) yes
C43 . H431 . 0.958 no
C44 . C45 . 1.379(13) yes
C44 . H441 . 0.957 no
C45 . H451 . 0.945 no
C46 . N3 . 1.126(10) yes
C47 . C48 . 1.524(13) yes
C47 . C49 . 1.535(15) yes
C47 . C50 . 1.513(15) yes
C47 . N3 . 1.499(11) yes
C48 . H481 . 0.977 no
C48 . H482 . 0.969 no
C48 . H483 . 0.958 no
C49 . H491 . 0.952 no
C49 . H492 . 0.976 no
C49 . H493 . 0.954 no
C50 . H501 . 0.971 no
C50 . H502 . 0.976 no
C50 . H503 . 0.968 no
C51 . F1 . 1.372(12) yes
C51 . F2 . 1.340(13) yes
C51 . F3 . 1.359(12) yes
C51 . S1 . 1.767(11) yes
O1 . S1 . 1.444(7) yes
O2 . S1 . 1.430(8) yes
O3 . S1 . 1.429(7) yes
C330 . C320 . 1.41523(6) yes
C330 . C28 . 1.34990(9) yes
C330 . H3301 . 0.950 no
C33 . C32 . 1.40763(5) yes
C33 . C28 . 1.39694(7) yes
C33 . H331 . 0.952 no
C320 . C310 . 1.38976(6) yes
C320 . H3201 . 0.946 no
C32 . C31 . 1.36847(7) yes
C32 . H321 . 0.953 no
C31 . C30 . 1.34989(8) yes
C31 . C300 . 1.49628(8) yes
C31 . H311 . 0.948 no
C310 . C30 . 1.27809(8) yes
C310 . C300 . 1.41792(9) yes
C310 . H3101 . 0.950 no
C30 . C29 . 1.35863(5) yes
C30 . H301 . 0.949 no
C300 . C290 . 1.39225(5) yes
C300 . H3001 . 0.951 no
C29 . C28 . 1.41466(7) yes
C29 . H2901 . 1.085 no
C29 . H291 . 0.950 no
C290 . C28 . 1.47582(7) yes
C290 . H2901 . 0.951 no
C350 . C360 . 1.34746(7) yes
C350 . H3501 . 0.947 no
C35 . C36 . 1.38025(7) yes
C35 . H351 . 0.946 no
C360 . C370 . 1.39121(6) yes
C360 . H3601 . 0.948 no
C36 . C37 . 1.36177(6) yes
C36 . H361 . 0.946 no
C370 . C380 . 1.40465(8) yes
C370 . H3701 . 0.951 no
C37 . C38 . 1.39831(8) yes
C37 . H371 . 0.951 no
C380 . C390 . 1.37208(7) yes
C380 . H3801 . 0.954 no
C38 . C39 . 1.36645(7) yes
C38 . H381 . 0.954 no
C39 . H3901 . 0.840 no
C39 . H391 . 0.953 no
C390 . H3901 . 0.953 no
S2 . O4 . 1.443(8) yes
S2 . O5 . 1.461(7) yes
S2 . O6 . 1.507(6) yes
S2 . C52 . 1.826(7) yes
S3 . O6 . 1.438(7) yes
S3 . O7 . 1.441(9) yes
S3 . O8 . 1.472(9) yes
S3 . C53 . 1.828(8) yes
C52 . F4 . 1.340(6) yes
C52 . F5 . 1.326(6) yes
C52 . F6 . 1.330(6) yes
C53 . F7 . 1.331(7) yes
C53 . F8 . 1.329(7) yes
C53 . F9 . 1.334(7) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 . Pd1 . C6 . 87.2(3) yes
C1 . Pd1 . C9 . 86.7(3) yes
C6 . Pd1 . C9 . 170.1(3) yes
C1 . Pd1 . C46 . 168.7(3) yes
C6 . Pd1 . C46 . 99.3(3) yes
C9 . Pd1 . C46 . 88.0(3) yes
C9 . P1 . C10 . 109.3(4) yes
C9 . P1 . C16 . 111.4(4) yes
C10 . P1 . C16 . 106.0(4) yes
C9 . P1 . C22 . 114.2(3) yes
C10 . P1 . C22 . 109.8(4) yes
C16 . P1 . C22 . 105.9(4) yes
C6 . P2 . C34 . 113.4(4) yes
C6 . P2 . C40 . 114.8(4) yes
C34 . P2 . C40 . 102.0(4) yes
C6 . P2 . C28 . 110.0(3) yes
C34 . P2 . C28 . 107.3(3) yes
C40 . P2 . C28 . 108.8(3) yes
Pd1 . C1 . N1 . 125.5(6) yes
Pd1 . C1 . N2 . 129.8(7) yes
N1 . C1 . N2 . 104.7(6) yes
C3 . C2 . N1 . 105.8(9) yes
C3 . C2 . H21 . 126.9 no
N1 . C2 . H21 . 127.3 no
C2 . C3 . N2 . 107.7(8) yes
C2 . C3 . H31 . 126.4 no
N2 . C3 . H31 . 125.9 no
C5 . C4 . N2 . 109.3(7) yes
C5 . C4 . H41 . 110.7 no
N2 . C4 . H41 . 109.4 no
C5 . C4 . H42 . 110.0 no
N2 . C4 . H42 . 109.7 no
H41 . C4 . H42 . 107.7 no
C4 . C5 . C6 . 114.3(7) yes
C4 . C5 . H51 . 109.5 no
C6 . C5 . H51 . 109.0 no
C4 . C5 . H52 . 107.9 no
C6 . C5 . H52 . 107.3 no
H51 . C5 . H52 . 108.6 no
C5 . C6 . P2 . 109.7(6) yes
C5 . C6 . Pd1 . 119.5(6) yes
P2 . C6 . Pd1 . 107.6(4) yes
C5 . C6 . H61 . 104.6 no
P2 . C6 . H61 . 106.6 no
Pd1 . C6 . H61 . 108.1 no
C8 . C7 . N1 . 109.8(7) yes
C8 . C7 . H71 . 109.0 no
N1 . C7 . H71 . 110.8 no
C8 . C7 . H72 . 109.1 no
N1 . C7 . H72 . 109.9 no
H71 . C7 . H72 . 108.2 no
C7 . C8 . C9 . 114.6(6) yes
C7 . C8 . H81 . 107.6 no
C9 . C8 . H81 . 109.1 no
C7 . C8 . H82 . 107.9 no
C9 . C8 . H82 . 109.0 no
H81 . C8 . H82 . 108.6 no
C8 . C9 . P1 . 112.5(5) yes
C8 . C9 . Pd1 . 118.0(5) yes
P1 . C9 . Pd1 . 106.0(4) yes
C8 . C9 . H91 . 106.2 no
P1 . C9 . H91 . 106.3 no
Pd1 . C9 . H91 . 107.2 no
P1 . C10 . C11 . 119.7(7) yes
P1 . C10 . C15 . 121.6(8) yes
C11 . C10 . C15 . 118.6(9) yes
C10 . C11 . C12 . 123.6(11) yes
C10 . C11 . H111 . 117.3 no
C12 . C11 . H111 . 119.0 no
C11 . C12 . C13 . 119.9(13) yes
C11 . C12 . H121 . 120.9 no
C13 . C12 . H121 . 119.2 no
C12 . C13 . C14 . 121.4(11) yes
C12 . C13 . H131 . 122.3 no
C14 . C13 . H131 . 116.3 no
C13 . C14 . C15 . 119.0(11) yes
C13 . C14 . H141 . 119.3 no
C15 . C14 . H141 . 121.7 no
C14 . C15 . C10 . 117.6(11) yes
C14 . C15 . H151 . 122.3 no
C10 . C15 . H151 . 120.1 no
P1 . C16 . C17 . 118.9(7) yes
P1 . C16 . C21 . 120.2(7) yes
C17 . C16 . C21 . 120.7(8) yes
C16 . C17 . C18 . 117.3(10) yes
C16 . C17 . H171 . 122.2 no
C18 . C17 . H171 . 120.5 no
C17 . C18 . C19 . 120.6(11) yes
C17 . C18 . H181 . 118.7 no
C19 . C18 . H181 . 120.7 no
C18 . C19 . C20 . 121.4(10) yes
C18 . C19 . H191 . 119.9 no
C20 . C19 . H191 . 118.7 no
C19 . C20 . C21 . 120.5(11) yes
C19 . C20 . H201 . 118.4 no
C21 . C20 . H201 . 121.0 no
C16 . C21 . C20 . 119.3(10) yes
C16 . C21 . H211 . 120.8 no
C20 . C21 . H211 . 119.9 no
P1 . C22 . C23 . 121.8(7) yes
P1 . C22 . C27 . 119.2(6) yes
C23 . C22 . C27 . 119.0(8) yes
C22 . C23 . C24 . 120.4(9) yes
C22 . C23 . H231 . 119.0 no
C24 . C23 . H231 . 120.6 no
C23 . C24 . C25 . 121.0(9) yes
C23 . C24 . H241 . 118.7 no
C25 . C24 . H241 . 120.3 no
C24 . C25 . C26 . 119.9(9) yes
C24 . C25 . H251 . 119.5 no
C26 . C25 . H251 . 120.6 no
C25 . C26 . C27 . 120.2(9) yes
C25 . C26 . H261 . 120.8 no
C27 . C26 . H261 . 119.0 no
C26 . C27 . C22 . 119.5(8) yes
C26 . C27 . H271 . 121.4 no
C22 . C27 . H271 . 119.1 no
P2 . C34 . C350 . 118.1(6) yes
P2 . C34 . C35 . 126.3(6) yes
P2 . C34 . C39 . 116.1(5) yes
C350 . C34 . C39 . 125.7(7) yes
C35 . C34 . C39 . 116.5(7) yes
P2 . C34 . C390 . 119.1(6) yes
C350 . C34 . C390 . 122.8(7) yes
C35 . C34 . C390 . 113.2(7) yes
P2 . C40 . C41 . 120.9(6) yes
P2 . C40 . C45 . 118.6(6) yes
C41 . C40 . C45 . 119.3(7) yes
C40 . C41 . C42 . 118.6(8) yes
C40 . C41 . H411 . 119.7 no
C42 . C41 . H411 . 121.7 no
C41 . C42 . C43 . 120.1(8) yes
C41 . C42 . H421 . 118.3 no
C43 . C42 . H421 . 121.6 no
C42 . C43 . C44 . 121.8(9) yes
C42 . C43 . H431 . 117.5 no
C44 . C43 . H431 . 120.6 no
C43 . C44 . C45 . 119.3(9) yes
C43 . C44 . H441 . 121.2 no
C45 . C44 . H441 . 119.5 no
C40 . C45 . C44 . 120.9(8) yes
C40 . C45 . H451 . 117.7 no
C44 . C45 . H451 . 121.5 no
Pd1 . C46 . N3 . 166.7(7) yes
C48 . C47 . C49 . 110.6(8) yes
C48 . C47 . C50 . 113.7(9) yes
C49 . C47 . C50 . 112.5(9) yes
C48 . C47 . N3 . 106.3(7) yes
C49 . C47 . N3 . 107.8(8) yes
C50 . C47 . N3 . 105.5(8) yes
C47 . C48 . H481 . 109.4 no
C47 . C48 . H482 . 111.1 no
H481 . C48 . H482 . 108.0 no
C47 . C48 . H483 . 110.8 no
H481 . C48 . H483 . 108.9 no
H482 . C48 . H483 . 108.6 no
C47 . C49 . H491 . 110.1 no
C47 . C49 . H492 . 109.3 no
H491 . C49 . H492 . 109.0 no
C47 . C49 . H493 . 109.3 no
H491 . C49 . H493 . 110.6 no
H492 . C49 . H493 . 108.5 no
C47 . C50 . H501 . 112.0 no
C47 . C50 . H502 . 110.8 no
H501 . C50 . H502 . 107.1 no
C47 . C50 . H503 . 111.0 no
H501 . C50 . H503 . 108.3 no
H502 . C50 . H503 . 107.4 no
F1 . C51 . F2 . 105.8(8) yes
F1 . C51 . F3 . 104.0(9) yes
F2 . C51 . F3 . 105.6(9) yes
F1 . C51 . S1 . 112.4(7) yes
F2 . C51 . S1 . 114.5(8) yes
F3 . C51 . S1 . 113.6(7) yes
C7 . N1 . C2 . 127.5(8) yes
C7 . N1 . C1 . 121.1(6) yes
C2 . N1 . C1 . 111.4(7) yes
C4 . N2 . C3 . 129.5(8) yes
C4 . N2 . C1 . 120.0(7) yes
C3 . N2 . C1 . 110.4(8) yes
C47 . N3 . C46 . 173.6(8) yes
C51 . S1 . O1 . 100.6(4) yes
C51 . S1 . O2 . 103.2(6) yes
O1 . S1 . O2 . 115.8(6) yes
C51 . S1 . O3 . 104.0(5) yes
O1 . S1 . O3 . 115.9(4) yes
O2 . S1 . O3 . 114.5(5) yes
C320 . C330 . C28 . 122.550(4) yes
C320 . C330 . H3301 . 118.9 no
C28 . C330 . H3301 . 118.5 no
C32 . C33 . C28 . 118.659(4) yes
C32 . C33 . H331 . 120.6 no
C28 . C33 . H331 . 120.7 no
C330 . C320 . C310 . 120.550(4) yes
C330 . C320 . H3201 . 119.7 no
C310 . C320 . H3201 . 119.8 no
C33 . C32 . C31 . 120.991(4) yes
C33 . C32 . H321 . 119.4 no
C31 . C32 . H321 . 119.6 no
C32 . C31 . C30 . 120.303(3) yes
C32 . C31 . C300 . 121.845 yes
C32 . C31 . H311 . 119.7 no
C30 . C31 . H311 . 120.0 no
C300 . C31 . H311 . 118.4 no
C320 . C310 . C30 . 115.932(4) yes
C320 . C310 . C300 . 117.965(4) yes
C320 . C310 . H3101 . 121.2 no
C30 . C310 . H3101 . 122.9 no
C300 . C310 . H3101 . 120.9 no
C31 . C30 . C29 . 119.824 yes
C310 . C30 . C29 . 124.443 yes
C31 . C30 . H301 . 120.1 no
C310 . C30 . H301 . 114.2 no
C29 . C30 . H301 . 120.1 no
C31 . C300 . C290 . 116.665 yes
C310 . C300 . C290 . 121.292 yes
C31 . C300 . H3001 . 122.6 no
C310 . C300 . H3001 . 119.5 no
C290 . C300 . H3001 . 119.2 no
C30 . C29 . C28 . 122.203(4) yes
C30 . C29 . H2901 . 121.8 no
C28 . C29 . H2901 . 115.6 no
C30 . C29 . H291 . 119.0 no
C28 . C29 . H291 . 118.8 no
C300 . C290 . C28 . 119.068(4) yes
C300 . C290 . H2901 . 120.5 no
C28 . C290 . H2901 . 120.4 no
C290 . C28 . P2 . 116.87(16) yes
P2 . C28 . C29 . 121.26(16) yes
C290 . C28 . C33 . 121.468(3) yes
P2 . C28 . C33 . 121.53(16) yes
C29 . C28 . C33 . 117.192(3) yes
C290 . C28 . C330 . 117.351(4) yes
P2 . C28 . C330 . 123.04(16) yes
C29 . C28 . C330 . 112.477(4) yes
C34 . C350 . C360 . 116.4(4) yes
C34 . C350 . H3501 . 122.0 no
C360 . C350 . H3501 . 121.7 no
C34 . C35 . C36 . 123.8(4) yes
C34 . C35 . H351 . 118.2 no
C36 . C35 . H351 . 118.0 no
C350 . C360 . C370 . 122.014(3) yes
C350 . C360 . H3601 . 119.1 no
C370 . C360 . H3601 . 118.8 no
C35 . C36 . C37 . 119.222(3) yes
C35 . C36 . H361 . 120.6 no
C37 . C36 . H361 . 120.2 no
C360 . C370 . C380 . 121.052(4) yes
C360 . C370 . H3701 . 119.7 no
C380 . C370 . H3701 . 119.3 no
C36 . C37 . C38 . 118.858(5) yes
C36 . C37 . H371 . 120.8 no
C38 . C37 . H371 . 120.3 no
C370 . C380 . C390 . 118.542 yes
C370 . C380 . H3801 . 120.8 no
C390 . C380 . H3801 . 120.7 no
C37 . C38 . C39 . 123.733 yes
C37 . C38 . H381 . 118.2 no
C39 . C38 . H381 . 118.1 no
C34 . C39 . C38 . 117.0(4) yes
C34 . C39 . H3901 . 121.1 no
C38 . C39 . H3901 . 121.5 no
C34 . C39 . H391 . 121.8 no
C38 . C39 . H391 . 121.2 no
C34 . C390 . C380 . 119.2(4) yes
C34 . C390 . H3901 . 120.7 no
C380 . C390 . H3901 . 120.1 no
O4 . S2 . O5 . 119.65(9) yes
O4 . S2 . O6 . 108.91(9) yes
O5 . S2 . O6 . 115.27(9) yes
O4 . S2 . C52 . 97.90(9) yes
O5 . S2 . C52 . 103.47(9) yes
O6 . S2 . C52 . 109.64(9) yes
O6 . S3 . O7 . 119.71(9) yes
O6 . S3 . O8 . 108.93(9) yes
O7 . S3 . O8 . 115.25(9) yes
O6 . S3 . C53 . 97.78(9) yes
O7 . S3 . C53 . 103.56(9) yes
O8 . S3 . C53 . 109.58(9) yes
S2 . C52 . F4 . 109.87(9) yes
S2 . C52 . F5 . 110.57(9) yes
F4 . C52 . F5 . 107.95(9) yes
S2 . C52 . F6 . 110.02(9) yes
F4 . C52 . F6 . 107.87(9) yes
F5 . C52 . F6 . 110.48(9) yes
S3 . C53 . F7 . 109.91(9) yes
S3 . C53 . F8 . 110.59(9) yes
F7 . C53 . F8 . 107.95(9) yes
S3 . C53 . F9 . 109.97(9) yes
F7 . C53 . F9 . 107.83(9) yes
F8 . C53 . F9 . 110.53(9) yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C2 . H21 . O6 4_545 150 0.93 2.48 3.315(11) yes
C3 . H31 . O1 4_555 173 0.96 2.30 3.251(11) yes
C4 . H42 . O7 . 140 0.98 2.36 3.173(11) yes
C6 . H61 . O9 . 157 0.99 2.53 3.456(11) yes
C7 . H72 . O5 4_545 143 0.98 2.44 3.267(11) yes
C15 . H151 . O9 . 126 0.99 2.50 3.185(11) yes
C17 . H171 . O1 . 156 0.95 2.57 3.460(11) yes
C23 . H231 . C15 . 128 0.97 2.57 3.254(11) yes
C41 . H411 . O9 . 167 0.94 2.42 3.343(11) yes
C50 . H502 . O8 4_645 135 0.98 2.35 3.119(11) yes
C350 . H3501 . C33 . 122 0.95 2.30 2.908(11) yes
C330 . H331 . C350 . 125 1.20 2.41 3.254(11) yes



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-2 2 3 x .
# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
####################################################################### 
# 
# 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_220218
_database_code_depnum_ccdc_archive 'CCDC 1865718'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;

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

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

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

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

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

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   15.3294(6)
_cell_length_b                   15.1363(6)
_cell_length_c                   18.3583(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4259.7(3)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_space_group_name_Hall  '-P 2ac 2ab '

_audit_creation_method           CRYSTALS_ver_14.61_build_6236

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8


_chemical_formula_sum            'C24 H24 Br1 N2 P1'
_chemical_formula_moiety         'C24 H24 N2 P, Br '
_chemical_compound_source        ?
_chemical_formula_weight         451.35


_cell_measurement_reflns_used    9943
_cell_measurement_theta_min      3
_cell_measurement_theta_max      26
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.160

_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    2.017

# Sheldrick geometric approximatio 0.74 0.82 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.82
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            79348
_reflns_number_total             4053
_diffrn_reflns_av_R_equivalents  0.043
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4053 
# Theoretical number of reflections is about 8113 


_diffrn_reflns_theta_min         2.219
_diffrn_reflns_theta_max         25.716
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        25.716
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              0
_reflns_limit_h_max              18
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              22

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

_refine_diff_density_min         -0.38
_refine_diff_density_max         0.44


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         3399
_refine_ls_number_restraints     0
_refine_ls_number_parameters     253
_oxford_refine_ls_R_factor_ref   0.0239
_refine_ls_wR_factor_ref         0.0243
_refine_ls_goodness_of_fit_ref   1.0921
_refine_ls_shift/su_max          0.0027122
_refine_ls_shift/su_mean         0.0000730


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4042
_refine_ls_R_factor_all          0.0309
_refine_ls_wR_factor_all         0.0331

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3531
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_gt          0.0251

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


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.120 0.798E-01 0.381E-01 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.26279(11) 0.08749(11) 0.82388(9) 0.0216 1.0000 Uani . . . . . .
C2 C 0.13160(11) 0.04263(11) 0.79592(9) 0.0222 1.0000 Uani . . . . . .
C3 C 0.18042(12) -0.02607(11) 0.81919(9) 0.0220 1.0000 Uani . . . . . .
C4 C 0.15860(12) 0.20528(11) 0.77924(9) 0.0240 1.0000 Uani . . . . . .
C5 C 0.21325(11) 0.24455(11) 0.71880(10) 0.0213 1.0000 Uani . . . . . .
C6 C 0.17939(10) 0.33735(10) 0.70069(8) 0.0158 1.0000 Uani . . . . . .
C7 C 0.15430(10) 0.48167(10) 0.59821(9) 0.0159 1.0000 Uani . . . . . .
C8 C 0.12952(11) 0.53708(11) 0.65545(10) 0.0223 1.0000 Uani . . . . . .
C9 C 0.08117(12) 0.61227(12) 0.64105(11) 0.0280 1.0000 Uani . . . . . .
C10 C 0.05729(11) 0.63189(11) 0.57016(11) 0.0292 1.0000 Uani . . . . . .
C11 C 0.08186(12) 0.57748(12) 0.51331(11) 0.0278 1.0000 Uani . . . . . .
C12 C 0.13080(11) 0.50206(11) 0.52676(9) 0.0210 1.0000 Uani . . . . . .
C13 C 0.20818(11) 0.30664(10) 0.54616(8) 0.0166 1.0000 Uani . . . . . .
C14 C 0.12806(11) 0.26298(10) 0.54017(9) 0.0195 1.0000 Uani . . . . . .
C15 C 0.11820(12) 0.19672(11) 0.48899(9) 0.0223 1.0000 Uani . . . . . .
C16 C 0.18769(13) 0.17341(11) 0.44438(9) 0.0259 1.0000 Uani . . . . . .
C17 C 0.26565(13) 0.21817(13) 0.44941(10) 0.0302 1.0000 Uani . . . . . .
C18 C 0.27658(11) 0.28509(12) 0.50025(9) 0.0234 1.0000 Uani . . . . . .
C19 C 0.33189(10) 0.42060(10) 0.62466(9) 0.0170 1.0000 Uani . . . . . .
C20 C 0.35656(12) 0.50599(12) 0.60477(11) 0.0286 1.0000 Uani . . . . . .
C21 C 0.44321(12) 0.53180(13) 0.61271(12) 0.0324 1.0000 Uani . . . . . .
C22 C 0.50456(11) 0.47310(12) 0.63896(10) 0.0244 1.0000 Uani . . . . . .
C23 C 0.47970(11) 0.38988(12) 0.66006(9) 0.0230 1.0000 Uani . . . . . .
C24 C 0.39358(11) 0.36317(11) 0.65341(9) 0.0211 1.0000 Uani . . . . . .
Br1 Br -0.049516(10) 0.247011(11) 0.675727(9) 0.0227 1.0000 Uani . . . . . .
P1 P 0.22005(2) 0.38657(3) 0.61745(2) 0.0135 1.0000 Uani . . . . . .
N1 N 0.18471(9) 0.11552(9) 0.79875(7) 0.0175 1.0000 Uani . . . . . .
N2 N 0.26350(9) 0.00174(9) 0.83645(8) 0.0238 1.0000 Uani . . . . . .
H11 H 0.3096 0.1247 0.8307 0.0266 1.0000 Uiso R . . . . .
H21 H 0.0736 0.0425 0.7800 0.0277 1.0000 Uiso R . . . . .
H31 H 0.1620 -0.0851 0.8231 0.0258 1.0000 Uiso R . . . . .
H42 H 0.1620 0.2434 0.8211 0.0298 1.0000 Uiso R . . . . .
H41 H 0.0978 0.2031 0.7619 0.0304 1.0000 Uiso R . . . . .
H51 H 0.2734 0.2469 0.7340 0.0272 1.0000 Uiso R . . . . .
H52 H 0.2083 0.2065 0.6776 0.0258 1.0000 Uiso R . . . . .
H62 H 0.1937 0.3766 0.7418 0.0197 1.0000 Uiso R . . . . .
H61 H 0.1165 0.3346 0.6953 0.0197 1.0000 Uiso R . . . . .
H81 H 0.1461 0.5235 0.7022 0.0266 1.0000 Uiso R . . . . .
H91 H 0.0658 0.6481 0.6792 0.0340 1.0000 Uiso R . . . . .
H101 H 0.0234 0.6824 0.5610 0.0346 1.0000 Uiso R . . . . .
H111 H 0.0648 0.5911 0.4660 0.0337 1.0000 Uiso R . . . . .
H121 H 0.1477 0.4645 0.4886 0.0246 1.0000 Uiso R . . . . .
H141 H 0.0817 0.2775 0.5694 0.0234 1.0000 Uiso R . . . . .
H151 H 0.0638 0.1683 0.4848 0.0270 1.0000 Uiso R . . . . .
H161 H 0.1819 0.1278 0.4099 0.0315 1.0000 Uiso R . . . . .
H171 H 0.3114 0.2043 0.4191 0.0364 1.0000 Uiso R . . . . .
H181 H 0.3292 0.3161 0.5040 0.0275 1.0000 Uiso R . . . . .
H201 H 0.3149 0.5449 0.5867 0.0352 1.0000 Uiso R . . . . .
H211 H 0.4607 0.5899 0.6008 0.0397 1.0000 Uiso R . . . . .
H221 H 0.5622 0.4901 0.6434 0.0284 1.0000 Uiso R . . . . .
H231 H 0.5205 0.3509 0.6792 0.0273 1.0000 Uiso R . . . . .
H241 H 0.3773 0.3073 0.6684 0.0258 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . N1 . 1.351(2) yes
C1 . N2 . 1.318(2) yes
C1 . H11 . 0.920 no
C2 . C3 . 1.351(2) yes
C2 . N1 . 1.372(2) yes
C2 . H21 . 0.936 no
C3 . N2 . 1.378(2) yes
C3 . H31 . 0.939 no
C4 . C5 . 1.512(2) yes
C4 . N1 . 1.461(2) yes
C4 . H42 . 0.963 no
C4 . H41 . 0.986 no
C5 . C6 . 1.534(2) yes
C5 . H51 . 0.964 no
C5 . H52 . 0.954 no
C6 . P1 . 1.8107(15) yes
C6 . H62 . 0.985 no
C6 . H61 . 0.970 no
C7 . C8 . 1.397(2) yes
C7 . C12 . 1.395(2) yes
C7 . P1 . 1.7924(16) yes
C8 . C9 . 1.384(2) yes
C8 . H81 . 0.918 no
C9 . C10 . 1.384(3) yes
C9 . H91 . 0.916 no
C10 . C11 . 1.382(3) yes
C10 . H101 . 0.939 no
C11 . C12 . 1.388(2) yes
C11 . H111 . 0.931 no
C12 . H121 . 0.938 no
C13 . C14 . 1.399(2) yes
C13 . C18 . 1.384(2) yes
C13 . P1 . 1.7916(16) yes
C14 . C15 . 1.383(2) yes
C14 . H141 . 0.918 no
C15 . C16 . 1.389(3) yes
C15 . H151 . 0.941 no
C16 . C17 . 1.377(3) yes
C16 . H161 . 0.942 no
C17 . C18 . 1.388(3) yes
C17 . H171 . 0.920 no
C18 . H181 . 0.936 no
C19 . C20 . 1.395(2) yes
C19 . C24 . 1.389(2) yes
C19 . P1 . 1.7951(16) yes
C20 . C21 . 1.392(3) yes
C20 . H201 . 0.929 no
C21 . C22 . 1.381(3) yes
C21 . H211 . 0.944 no
C22 . C23 . 1.372(3) yes
C22 . H221 . 0.924 no
C23 . C24 . 1.386(2) yes
C23 . H231 . 0.929 no
C24 . H241 . 0.924 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . C1 . N2 . 112.09(15) yes
N1 . C1 . H11 . 123.0 no
N2 . C1 . H11 . 124.9 no
C3 . C2 . N1 . 106.15(15) yes
C3 . C2 . H21 . 128.6 no
N1 . C2 . H21 . 125.2 no
C2 . C3 . N2 . 110.46(15) yes
C2 . C3 . H31 . 126.1 no
N2 . C3 . H31 . 123.4 no
C5 . C4 . N1 . 113.18(14) yes
C5 . C4 . H42 . 108.7 no
N1 . C4 . H42 . 110.3 no
C5 . C4 . H41 . 107.5 no
N1 . C4 . H41 . 107.9 no
H42 . C4 . H41 . 109.2 no
C4 . C5 . C6 . 109.36(13) yes
C4 . C5 . H51 . 109.4 no
C6 . C5 . H51 . 110.7 no
C4 . C5 . H52 . 107.5 no
C6 . C5 . H52 . 110.8 no
H51 . C5 . H52 . 109.0 no
C5 . C6 . P1 . 116.31(11) yes
C5 . C6 . H62 . 108.2 no
P1 . C6 . H62 . 108.7 no
C5 . C6 . H61 . 108.6 no
P1 . C6 . H61 . 105.9 no
H62 . C6 . H61 . 108.9 no
C8 . C7 . C12 . 120.28(15) yes
C8 . C7 . P1 . 119.13(12) yes
C12 . C7 . P1 . 120.54(12) yes
C7 . C8 . C9 . 119.71(16) yes
C7 . C8 . H81 . 119.5 no
C9 . C8 . H81 . 120.7 no
C8 . C9 . C10 . 119.86(17) yes
C8 . C9 . H91 . 118.6 no
C10 . C9 . H91 . 121.5 no
C9 . C10 . C11 . 120.67(16) yes
C9 . C10 . H101 . 119.3 no
C11 . C10 . H101 . 120.1 no
C10 . C11 . C12 . 120.21(17) yes
C10 . C11 . H111 . 119.8 no
C12 . C11 . H111 . 120.0 no
C7 . C12 . C11 . 119.26(16) yes
C7 . C12 . H121 . 119.8 no
C11 . C12 . H121 . 121.0 no
C14 . C13 . C18 . 120.39(15) yes
C14 . C13 . P1 . 117.74(12) yes
C18 . C13 . P1 . 121.80(13) yes
C13 . C14 . C15 . 119.47(15) yes
C13 . C14 . H141 . 121.4 no
C15 . C14 . H141 . 119.1 no
C14 . C15 . C16 . 120.07(16) yes
C14 . C15 . H151 . 118.9 no
C16 . C15 . H151 . 121.0 no
C15 . C16 . C17 . 120.07(16) yes
C15 . C16 . H161 . 120.7 no
C17 . C16 . H161 . 119.2 no
C16 . C17 . C18 . 120.61(17) yes
C16 . C17 . H171 . 120.6 no
C18 . C17 . H171 . 118.8 no
C17 . C18 . C13 . 119.35(17) yes
C17 . C18 . H181 . 121.3 no
C13 . C18 . H181 . 119.4 no
C20 . C19 . C24 . 119.65(15) yes
C20 . C19 . P1 . 120.36(13) yes
C24 . C19 . P1 . 119.92(12) yes
C19 . C20 . C21 . 119.42(16) yes
C19 . C20 . H201 . 119.6 no
C21 . C20 . H201 . 121.0 no
C20 . C21 . C22 . 120.39(17) yes
C20 . C21 . H211 . 120.5 no
C22 . C21 . H211 . 119.1 no
C21 . C22 . C23 . 120.02(16) yes
C21 . C22 . H221 . 120.2 no
C23 . C22 . H221 . 119.7 no
C22 . C23 . C24 . 120.50(16) yes
C22 . C23 . H231 . 120.2 no
C24 . C23 . H231 . 119.3 no
C19 . C24 . C23 . 119.97(15) yes
C19 . C24 . H241 . 120.1 no
C23 . C24 . H241 . 119.9 no
C6 . P1 . C19 . 112.62(7) yes
C6 . P1 . C7 . 107.65(7) yes
C19 . P1 . C7 . 108.73(7) yes
C6 . P1 . C13 . 107.68(7) yes
C19 . P1 . C13 . 110.16(8) yes
C7 . P1 . C13 . 109.95(7) yes
C4 . N1 . C2 . 125.15(14) yes
C4 . N1 . C1 . 128.21(14) yes
C2 . N1 . C1 . 106.63(14) yes
C3 . N2 . C1 . 104.65(14) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C16 . H161 . N2 5_554 154 0.94 2.52 3.393(2) yes



# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
