# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_8.1
_database_code_depnum_ccdc_archive 'CCDC 1031965'
_audit_update_record             
;
2014-10-31 deposited with the CCDC.
2015-06-16 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          ?
#--------------------------------------------------------------- 
_cell_length_a                   12.8008(2)
_cell_length_b                   16.6628(3)
_cell_length_c                   17.8668(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.6830(17)
_cell_angle_gamma                90
_cell_volume                     3756.64(11)
_cell_measurement_reflns_used    31838
_cell_measurement_theta_min      2.8568
_cell_measurement_theta_max      28.9856


_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'
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'
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'
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'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

_chemical_formula_sum            'C86 H71 N13 O4 P4'
_chemical_formula_moiety         '2(C42 H34 N6 O2 P2), C2 H3 N'
_chemical_compound_source        ?
_chemical_formula_weight         1474.44


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.250
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_max          0.430
_exptl_absorpt_correction_T_min  0.95533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1540
_exptl_absorpt_coefficient_mu    0.163
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_detector_area_resol_mean 8.4205

_diffrn_measurement_device       Serial
_diffrn_radiation_wavelength     0.71073


#End reflection statistics
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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_orient_matrix_UB_11      -0.0124929000
_diffrn_orient_matrix_UB_12      0.0381873000
_diffrn_orient_matrix_UB_13      -0.0166372000
_diffrn_orient_matrix_UB_21      0.0259241000
_diffrn_orient_matrix_UB_22      -0.0105436000
_diffrn_orient_matrix_UB_23      -0.0307026000
_diffrn_orient_matrix_UB_31      -0.0483052000
_diffrn_orient_matrix_UB_32      -0.0155360000
_diffrn_orient_matrix_UB_33      -0.0200684000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    3.00  101.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4101   77.0000  120.0000 98

#__ type_ start__ end____ width___ exp.time_
  2 omega  -14.00  101.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4101   77.0000 -120.0000 115

#__ type_ start__ end____ width___ exp.time_
  3 omega  -19.00   85.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4101   77.0000   30.0000 104

#__ type_ start__ end____ width___ exp.time_
  4 omega  -57.00   69.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   77.0000  120.0000 126

#__ type_ start__ end____ width___ exp.time_
  5 omega  -61.00   50.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   77.0000    0.0000 111

#__ type_ start__ end____ width___ exp.time_
  6 omega  -61.00   50.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   77.0000 -120.0000 111

#__ type_ start__ end____ width___ exp.time_
  7 omega   34.00  118.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4101  179.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  8 omega  -59.00  -24.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   38.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
  9 omega  -59.00   67.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   38.0000 -150.0000 126

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            64742
_reflns_number_total             9225
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.0559
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9225 
# Theoretical number of reflections is about 20072 


_diffrn_reflns_theta_min         2.863
_diffrn_reflns_theta_max         29.050
_diffrn_measured_fraction_theta_max 0.918

_diffrn_reflns_theta_full        26.726
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -17
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              24



_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.67
_refine_diff_density_max         0.49

_refine_ls_number_reflns         9225
_refine_ls_number_restraints     2
_refine_ls_number_parameters     476
_refine_ls_wR_factor_ref         0.1425
_refine_ls_goodness_of_fit_ref   0.8507
_refine_ls_shift/su_max          0.0008743
_refine_ls_shift/su_mean         0.0000359

_refine_ls_R_factor_all          0.0534
_refine_ls_wR_factor_all         0.1425

_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7926
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_gt          0.1325


_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.10P)² + 3.94P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# Insert your own references if required - in alphabetical order 



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
P1 P 0.48697(3) 0.66183(2) 0.29645(2) 0.0206 1.0000 Uani . . . . . .
O2 O 0.59269(9) 0.69755(7) 0.29319(7) 0.0250 1.0000 Uani . . . . . .
C3 C 0.38623(12) 0.72613(9) 0.24610(9) 0.0208 1.0000 Uani . . . . . .
N4 N 0.27921(11) 0.71586(9) 0.24064(9) 0.0270 1.0000 Uani . . . . . .
N5 N 0.23094(11) 0.77880(9) 0.20772(9) 0.0280 1.0000 Uani . . . . . .
N6 N 0.30575(11) 0.83023(8) 0.19184(8) 0.0223 1.0000 Uani . . . . . .
C7 C 0.40390(12) 0.79973(9) 0.21469(8) 0.0192 1.0000 Uani . . . . . .
C8 C 0.50267(12) 0.83923(9) 0.20498(8) 0.0192 1.0000 Uani . . . . . .
N9 N 0.56466(11) 0.81154(8) 0.15590(8) 0.0219 1.0000 Uani . . . . . .
N10 N 0.65510(12) 0.85402(9) 0.16180(8) 0.0266 1.0000 Uani . . . . . .
N11 N 0.65213(12) 0.90950(9) 0.21336(8) 0.0263 1.0000 Uani . . . . . .
C12 C 0.55909(13) 0.90239(10) 0.24125(9) 0.0212 1.0000 Uani . . . . . .
P13 P 0.52744(3) 0.96110(3) 0.31884(2) 0.0218 1.0000 Uani . . . . . .
O14 O 0.41441(10) 0.95052(8) 0.32668(7) 0.0302 1.0000 Uani . . . . . .
C15 C 0.56194(13) 1.06335(10) 0.30239(9) 0.0229 1.0000 Uani . . . . . .
C16 C 0.66417(14) 1.08319(11) 0.29018(11) 0.0290 1.0000 Uani . . . . . .
C17 C 0.69025(15) 1.16238(11) 0.27897(11) 0.0319 1.0000 Uani . . . . . .
C18 C 0.61599(16) 1.22233(11) 0.28275(11) 0.0329 1.0000 Uani . . . . . .
C19 C 0.51527(15) 1.20355(11) 0.29571(11) 0.0324 1.0000 Uani . . . . . .
C20 C 0.48738(14) 1.12386(11) 0.30480(10) 0.0281 1.0000 Uani . . . . . .
H201 H 0.4174 1.1113 0.3144 0.0323 1.0000 Uiso R . . . . .
H191 H 0.4637 1.2450 0.2967 0.0367 1.0000 Uiso R . . . . .
H181 H 0.6334 1.2782 0.2778 0.0396 1.0000 Uiso R . . . . .
H171 H 0.7561 1.1742 0.2671 0.0380 1.0000 Uiso R . . . . .
H161 H 0.7176 1.0418 0.2865 0.0336 1.0000 Uiso R . . . . .
C21 C 0.62157(14) 0.92985(10) 0.40040(10) 0.0258 1.0000 Uani . . . . . .
C22 C 0.68918(16) 0.86460(12) 0.39983(11) 0.0343 1.0000 Uani . . . . . .
C23 C 0.7569(2) 0.84275(14) 0.46620(13) 0.0464 1.0000 Uani . . . . . .
C24 C 0.7550(2) 0.88420(16) 0.53289(13) 0.0499 1.0000 Uani . . . . . .
C25 C 0.6876(2) 0.94871(16) 0.53390(12) 0.0482 1.0000 Uani . . . . . .
C26 C 0.62222(17) 0.97217(13) 0.46778(11) 0.0378 1.0000 Uani . . . . . .
H261 H 0.5769 1.0161 0.4675 0.0441 1.0000 Uiso R . . . . .
H251 H 0.6836 0.9779 0.5786 0.0566 1.0000 Uiso R . . . . .
H241 H 0.7978 0.8685 0.5779 0.0576 1.0000 Uiso R . . . . .
H231 H 0.8017 0.7979 0.4663 0.0545 1.0000 Uiso R . . . . .
H221 H 0.6855 0.8343 0.3551 0.0410 1.0000 Uiso R . . . . .
C27 C 0.54863(15) 0.74049(10) 0.10632(10) 0.0289 1.0000 Uani . . . . . .
C28 C 0.57834(14) 0.75676(11) 0.02955(10) 0.0276 1.0000 Uani . . . . . .
C29 C 0.51093(16) 0.80245(12) -0.02281(11) 0.0337 1.0000 Uani . . . . . .
C30 C 0.5356(2) 0.81913(14) -0.09386(12) 0.0428 1.0000 Uani . . . . . .
C31 C 0.62912(19) 0.79018(16) -0.11207(12) 0.0480 1.0000 Uani . . . . . .
C32 C 0.69614(18) 0.74526(19) -0.06138(14) 0.0554 1.0000 Uani . . . . . .
C33 C 0.67146(17) 0.72824(17) 0.01041(12) 0.0456 1.0000 Uani . . . . . .
H331 H 0.7171 0.6971 0.0452 0.0542 1.0000 Uiso R . . . . .
H321 H 0.7582 0.7231 -0.0746 0.0642 1.0000 Uiso R . . . . .
H311 H 0.6483 0.8021 -0.1610 0.0570 1.0000 Uiso R . . . . .
H301 H 0.4856 0.8519 -0.1299 0.0504 1.0000 Uiso R . . . . .
H291 H 0.4424 0.8232 -0.0105 0.0403 1.0000 Uiso R . . . . .
H272 H 0.4730 0.7271 0.1003 0.0340 1.0000 Uiso R . . . . .
H271 H 0.5933 0.6961 0.1327 0.0338 1.0000 Uiso R . . . . .
C34 C 0.27404(14) 0.90953(10) 0.15986(10) 0.0270 1.0000 Uani . . . . . .
C35 C 0.28922(13) 0.92000(10) 0.07877(10) 0.0236 1.0000 Uani . . . . . .
C36 C 0.23681(14) 0.87090(11) 0.02183(10) 0.0301 1.0000 Uani . . . . . .
C37 C 0.24493(16) 0.88523(13) -0.05368(11) 0.0354 1.0000 Uani . . . . . .
C38 C 0.30455(17) 0.94897(13) -0.07223(11) 0.0385 1.0000 Uani . . . . . .
C39 C 0.35720(18) 0.99768(13) -0.01607(12) 0.0408 1.0000 Uani . . . . . .
C40 C 0.35025(16) 0.98313(12) 0.05934(11) 0.0343 1.0000 Uani . . . . . .
H401 H 0.3918 1.0163 0.0976 0.0410 1.0000 Uiso R . . . . .
H391 H 0.3994 1.0391 -0.0295 0.0486 1.0000 Uiso R . . . . .
H381 H 0.3095 0.9595 -0.1236 0.0442 1.0000 Uiso R . . . . .
H371 H 0.2109 0.8503 -0.0922 0.0425 1.0000 Uiso R . . . . .
H361 H 0.1959 0.8273 0.0340 0.0363 1.0000 Uiso R . . . . .
H342 H 0.3144 0.9480 0.1913 0.0322 1.0000 Uiso R . . . . .
H341 H 0.1992 0.9131 0.1644 0.0313 1.0000 Uiso R . . . . .
C41 C 0.47110(13) 0.56355(10) 0.25486(10) 0.0245 1.0000 Uani . . . . . .
C42 C 0.37382(14) 0.52982(11) 0.22335(10) 0.0295 1.0000 Uani . . . . . .
C43 C 0.37013(17) 0.45311(12) 0.19273(12) 0.0373 1.0000 Uani . . . . . .
C44 C 0.4629(2) 0.41023(12) 0.19339(14) 0.0455 1.0000 Uani . . . . . .
C45 C 0.55980(19) 0.44308(13) 0.22466(16) 0.0482 1.0000 Uani . . . . . .
C46 C 0.56405(16) 0.51966(11) 0.25567(13) 0.0362 1.0000 Uani . . . . . .
H461 H 0.6292 0.5428 0.2759 0.0416 1.0000 Uiso R . . . . .
H451 H 0.6207 0.4141 0.2269 0.0558 1.0000 Uiso R . . . . .
H441 H 0.4591 0.3599 0.1743 0.0528 1.0000 Uiso R . . . . .
H431 H 0.3069 0.4316 0.1698 0.0424 1.0000 Uiso R . . . . .
H421 H 0.3141 0.5591 0.2218 0.0326 1.0000 Uiso R . . . . .
C47 C 0.45861(13) 0.65532(10) 0.39161(9) 0.0243 1.0000 Uani . . . . . .
C48 C 0.42232(18) 0.58616(13) 0.42173(11) 0.0385 1.0000 Uani . . . . . .
C49 C 0.4065(2) 0.58483(15) 0.49710(12) 0.0472 1.0000 Uani . . . . . .
C50 C 0.42777(19) 0.65177(15) 0.54191(12) 0.0433 1.0000 Uani . . . . . .
C51 C 0.46499(19) 0.72107(14) 0.51278(12) 0.0426 1.0000 Uani . . . . . .
C52 C 0.47985(16) 0.72295(12) 0.43742(11) 0.0345 1.0000 Uani . . . . . .
H521 H 0.5056 0.7705 0.4190 0.0413 1.0000 Uiso R . . . . .
H511 H 0.4745 0.7678 0.5417 0.0528 1.0000 Uiso R . . . . .
H501 H 0.4167 0.6499 0.5931 0.0494 1.0000 Uiso R . . . . .
H491 H 0.3807 0.5379 0.5199 0.0555 1.0000 Uiso R . . . . .
H481 H 0.4107 0.5406 0.3911 0.0462 1.0000 Uiso R . . . . .
C53 C 0.5343(4) 0.5252(3) 0.0274(3) 0.1155(14) 1.0000 Uiso D . . . . .
N54 N 0.5923(6) 0.5556(5) 0.0724(5) 0.1155(14) 0.5000 Uiso D . . . . .
H531 H 0.5542 0.4930 0.0714 0.0600 0.5000 Uiso R . . . . .
H532 H 0.5958 0.5402 0.0076 0.0600 0.5000 Uiso R . . . . .
H533 H 0.4989 0.5720 0.0404 0.0600 0.5000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.16(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
P1 . O2 . 1.4885(12) yes
P1 . C3 . 1.7971(16) yes
P1 . C41 . 1.7957(18) yes
P1 . C47 . 1.8006(17) yes
C3 . N4 . 1.368(2) yes
C3 . C7 . 1.383(2) yes
N4 . N5 . 1.306(2) yes
N5 . N6 . 1.3503(19) yes
N6 . C7 . 1.353(2) yes
N6 . C34 . 1.469(2) yes
C7 . C8 . 1.461(2) yes
C8 . N9 . 1.359(2) yes
C8 . C12 . 1.375(2) yes
N9 . N10 . 1.3458(19) yes
N9 . C27 . 1.472(2) yes
N10 . N11 . 1.310(2) yes
N11 . C12 . 1.371(2) yes
C12 . P13 . 1.7977(16) yes
P13 . O14 . 1.4874(12) yes
P13 . C15 . 1.7965(17) yes
P13 . C21 . 1.8044(18) yes
C15 . C16 . 1.402(2) yes
C15 . C20 . 1.394(2) yes
C16 . C17 . 1.384(3) yes
C16 . H161 . 0.981 no
C17 . C18 . 1.388(3) yes
C17 . H171 . 0.924 no
C18 . C19 . 1.384(3) yes
C18 . H181 . 0.966 no
C19 . C20 . 1.392(3) yes
C19 . H191 . 0.958 no
C20 . H201 . 0.963 no
C21 . C22 . 1.391(3) yes
C21 . C26 . 1.394(2) yes
C22 . C23 . 1.394(3) yes
C22 . H221 . 0.940 no
C23 . C24 . 1.381(3) yes
C23 . H231 . 0.942 no
C24 . C25 . 1.381(3) yes
C24 . H241 . 0.930 no
C25 . C26 . 1.384(3) yes
C25 . H251 . 0.944 no
C26 . H261 . 0.934 no
C27 . C28 . 1.508(2) yes
C27 . H272 . 0.982 no
C27 . H271 . 1.003 no
C28 . C29 . 1.388(3) yes
C28 . C33 . 1.379(3) yes
C29 . C30 . 1.387(3) yes
C29 . H291 . 1.001 no
C30 . C31 . 1.379(3) yes
C30 . H301 . 0.992 no
C31 . C32 . 1.362(4) yes
C31 . H311 . 0.967 no
C32 . C33 . 1.401(3) yes
C32 . H321 . 0.942 no
C33 . H331 . 0.935 no
C34 . C35 . 1.504(2) yes
C34 . H342 . 0.946 no
C34 . H341 . 0.977 no
C35 . C36 . 1.387(2) yes
C35 . C40 . 1.389(2) yes
C36 . C37 . 1.391(3) yes
C36 . H361 . 0.942 no
C37 . C38 . 1.380(3) yes
C37 . H371 . 0.949 no
C38 . C39 . 1.376(3) yes
C38 . H381 . 0.947 no
C39 . C40 . 1.386(3) yes
C39 . H391 . 0.933 no
C40 . H401 . 0.966 no
C41 . C42 . 1.396(2) yes
C41 . C46 . 1.395(3) yes
C42 . C43 . 1.388(3) yes
C42 . H421 . 0.903 no
C43 . C44 . 1.384(3) yes
C43 . H431 . 0.917 no
C44 . C45 . 1.385(3) yes
C44 . H441 . 0.903 no
C45 . C46 . 1.389(3) yes
C45 . H451 . 0.911 no
C46 . H461 . 0.934 no
C47 . C48 . 1.385(2) yes
C47 . C52 . 1.392(3) yes
C48 . C49 . 1.395(3) yes
C48 . H481 . 0.933 no
C49 . C50 . 1.373(3) yes
C49 . H491 . 0.965 no
C50 . C51 . 1.384(3) yes
C50 . H501 . 0.950 no
C51 . C52 . 1.391(3) yes
C51 . H511 . 0.931 no
C52 . H521 . 0.939 no
C53 . C53 2_665 1.465(7) yes
C53 . N54 . 1.119(7) yes
C53 . H531 . 0.950 no
C53 . H532 . 0.950 no
C53 . H533 . 0.950 no
N54 . H531 . 1.149 no
N54 . H532 . 1.193 no
N54 . H533 . 1.264 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
O2 . P1 . C3 . 108.82(7) yes
O2 . P1 . C41 . 112.88(8) yes
C3 . P1 . C41 . 108.35(8) yes
O2 . P1 . C47 . 112.96(7) yes
C3 . P1 . C47 . 105.48(7) yes
C41 . P1 . C47 . 108.00(8) yes
P1 . C3 . N4 . 125.94(12) yes
P1 . C3 . C7 . 125.39(12) yes
N4 . C3 . C7 . 108.19(14) yes
C3 . N4 . N5 . 108.91(14) yes
N4 . N5 . N6 . 107.80(13) yes
N5 . N6 . C7 . 110.71(13) yes
N5 . N6 . C34 . 119.54(14) yes
C7 . N6 . C34 . 129.55(14) yes
C3 . C7 . N6 . 104.39(13) yes
C3 . C7 . C8 . 130.64(14) yes
N6 . C7 . C8 . 124.97(14) yes
C7 . C8 . N9 . 122.33(14) yes
C7 . C8 . C12 . 133.22(14) yes
N9 . C8 . C12 . 104.27(13) yes
C8 . N9 . N10 . 111.04(13) yes
C8 . N9 . C27 . 128.61(14) yes
N10 . N9 . C27 . 120.07(13) yes
N9 . N10 . N11 . 107.45(13) yes
N10 . N11 . C12 . 108.92(13) yes
C8 . C12 . N11 . 108.31(14) yes
C8 . C12 . P13 . 127.68(12) yes
N11 . C12 . P13 . 123.73(12) yes
C12 . P13 . O14 . 110.92(7) yes
C12 . P13 . C15 . 107.24(7) yes
O14 . P13 . C15 . 113.43(8) yes
C12 . P13 . C21 . 105.03(8) yes
O14 . P13 . C21 . 114.69(8) yes
C15 . P13 . C21 . 104.87(8) yes
P13 . C15 . C16 . 120.71(13) yes
P13 . C15 . C20 . 119.50(13) yes
C16 . C15 . C20 . 119.74(16) yes
C15 . C16 . C17 . 120.11(16) yes
C15 . C16 . H161 . 121.6 no
C17 . C16 . H161 . 118.2 no
C16 . C17 . C18 . 119.69(17) yes
C16 . C17 . H171 . 119.2 no
C18 . C17 . H171 . 121.1 no
C17 . C18 . C19 . 120.69(17) yes
C17 . C18 . H181 . 121.3 no
C19 . C18 . H181 . 118.0 no
C18 . C19 . C20 . 119.99(17) yes
C18 . C19 . H191 . 120.3 no
C20 . C19 . H191 . 119.7 no
C15 . C20 . C19 . 119.75(16) yes
C15 . C20 . H201 . 120.7 no
C19 . C20 . H201 . 119.5 no
P13 . C21 . C22 . 123.47(14) yes
P13 . C21 . C26 . 117.23(14) yes
C22 . C21 . C26 . 119.25(17) yes
C21 . C22 . C23 . 119.77(18) yes
C21 . C22 . H221 . 119.0 no
C23 . C22 . H221 . 121.1 no
C22 . C23 . C24 . 120.3(2) yes
C22 . C23 . H231 . 120.0 no
C24 . C23 . H231 . 119.6 no
C23 . C24 . C25 . 120.1(2) yes
C23 . C24 . H241 . 120.8 no
C25 . C24 . H241 . 119.0 no
C24 . C25 . C26 . 119.9(2) yes
C24 . C25 . H251 . 122.4 no
C26 . C25 . H251 . 117.8 no
C21 . C26 . C25 . 120.6(2) yes
C21 . C26 . H261 . 118.6 no
C25 . C26 . H261 . 120.8 no
N9 . C27 . C28 . 111.82(14) yes
N9 . C27 . H272 . 106.5 no
C28 . C27 . H272 . 109.6 no
N9 . C27 . H271 . 107.5 no
C28 . C27 . H271 . 110.4 no
H272 . C27 . H271 . 110.9 no
C27 . C28 . C29 . 119.22(16) yes
C27 . C28 . C33 . 121.62(18) yes
C29 . C28 . C33 . 119.16(18) yes
C28 . C29 . C30 . 121.01(19) yes
C28 . C29 . H291 . 120.6 no
C30 . C29 . H291 . 118.4 no
C29 . C30 . C31 . 119.1(2) yes
C29 . C30 . H301 . 118.9 no
C31 . C30 . H301 . 122.1 no
C30 . C31 . C32 . 120.7(2) yes
C30 . C31 . H311 . 120.2 no
C32 . C31 . H311 . 119.1 no
C31 . C32 . C33 . 120.4(2) yes
C31 . C32 . H321 . 120.8 no
C33 . C32 . H321 . 118.7 no
C32 . C33 . C28 . 119.7(2) yes
C32 . C33 . H331 . 120.6 no
C28 . C33 . H331 . 119.7 no
N6 . C34 . C35 . 114.02(14) yes
N6 . C34 . H342 . 106.9 no
C35 . C34 . H342 . 110.3 no
N6 . C34 . H341 . 103.5 no
C35 . C34 . H341 . 111.1 no
H342 . C34 . H341 . 110.8 no
C34 . C35 . C36 . 120.86(16) yes
C34 . C35 . C40 . 119.86(16) yes
C36 . C35 . C40 . 119.11(16) yes
C35 . C36 . C37 . 120.27(17) yes
C35 . C36 . H361 . 120.3 no
C37 . C36 . H361 . 119.4 no
C36 . C37 . C38 . 119.96(18) yes
C36 . C37 . H371 . 119.9 no
C38 . C37 . H371 . 120.1 no
C37 . C38 . C39 . 120.11(18) yes
C37 . C38 . H381 . 120.4 no
C39 . C38 . H381 . 119.5 no
C38 . C39 . C40 . 120.13(18) yes
C38 . C39 . H391 . 118.9 no
C40 . C39 . H391 . 120.9 no
C35 . C40 . C39 . 120.41(18) yes
C35 . C40 . H401 . 121.5 no
C39 . C40 . H401 . 118.1 no
P1 . C41 . C42 . 124.43(14) yes
P1 . C41 . C46 . 115.92(14) yes
C42 . C41 . C46 . 119.66(17) yes
C41 . C42 . C43 . 119.91(18) yes
C41 . C42 . H421 . 119.2 no
C43 . C42 . H421 . 120.9 no
C42 . C43 . C44 . 119.99(19) yes
C42 . C43 . H431 . 120.3 no
C44 . C43 . H431 . 119.6 no
C43 . C44 . C45 . 120.56(19) yes
C43 . C44 . H441 . 119.0 no
C45 . C44 . H441 . 120.4 no
C44 . C45 . C46 . 119.8(2) yes
C44 . C45 . H451 . 120.6 no
C46 . C45 . H451 . 119.6 no
C41 . C46 . C45 . 120.12(19) yes
C41 . C46 . H461 . 119.4 no
C45 . C46 . H461 . 120.4 no
P1 . C47 . C48 . 123.44(14) yes
P1 . C47 . C52 . 117.12(13) yes
C48 . C47 . C52 . 119.36(17) yes
C47 . C48 . C49 . 120.05(19) yes
C47 . C48 . H481 . 118.7 no
C49 . C48 . H481 . 121.3 no
C48 . C49 . C50 . 120.2(2) yes
C48 . C49 . H491 . 122.4 no
C50 . C49 . H491 . 117.4 no
C49 . C50 . C51 . 120.36(19) yes
C49 . C50 . H501 . 119.2 no
C51 . C50 . H501 . 120.5 no
C50 . C51 . C52 . 119.6(2) yes
C50 . C51 . H511 . 120.7 no
C52 . C51 . H511 . 119.4 no
C47 . C52 . C51 . 120.37(18) yes
C47 . C52 . H521 . 121.5 no
C51 . C52 . H521 . 118.1 no
C53 2_665 C53 . N54 . 171.9(9) yes
C53 2_665 C53 . H531 . 106.1 no
N54 . C53 . H531 . 66.9 no
C53 2_665 C53 . H532 . 110.0 no
N54 . C53 . H532 . 69.9 no
H531 . C53 . H532 . 109.5 no
C53 2_665 C53 . H533 . 112.2 no
N54 . C53 . H533 . 74.9 no
H531 . C53 . H533 . 109.5 no
H532 . C53 . H533 . 109.5 no
C53 . N54 . H531 . 49.5 no
C53 . N54 . H532 . 48.4 no
H531 . N54 . H532 . 82.9 no
C53 . N54 . H533 . 46.5 no
H531 . N54 . H533 . 79.8 no
H532 . N54 . H533 . 78.2 no
N54 . H531 . C53 . 63.6 no
N54 . H532 . C53 . 61.7 no
C53 . H533 . N54 . 58.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C19 . H191 . N5 4_555 146 0.96 2.54 3.383(3) yes
C17 . H171 . O2 4_655 167 0.92 2.40 3.306(3) yes
C25 . H251 . O14 2_676 154 0.94 2.56 3.438(3) yes
C27 . H271 . N54 . 121 1.00 2.58 3.208(3) yes
C37 . H371 . O2 3_464 161 0.95 2.46 3.375(3) yes
C34 . H342 . O14 . 136 0.95 2.54 3.283(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 08/12/11 at 15:26:31
#
#LIST     12                                                                    
BLOCK SCALE P(1,X'S, U'S) UNTIL C(20) 
CONT  C(21,X'S, U'S) UNTIL C(26) 
CONT  C(27,X'S, U'S) UNTIL C(33) 
CONT  C(34,X'S, U'S) UNTIL C(40) 
CONT  C(41,X'S, U'S) UNTIL C(46) 
CONT  C(47,X'S, U'S) UNTIL C(52) 
CONT  C(53,X'S) UNTIL N(54) 
EQUIV C(53,U[ISO]) N(54,U[ISO]) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 272,X'S) H   ( 271,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 342,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) H   ( 533,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 08/12/11 at 15:26:31
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
DIST  1.08 , .01 =      C(53) TO N(54) 
DIST  1.47 , .01 =      C(53) TO C(53,-1,1,1,1) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8.3
_database_code_depnum_ccdc_archive 'CCDC 1031966'
_audit_update_record             
;
2014-10-31 deposited with the CCDC.
2015-06-16 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          ?
#--------------------------------------------------------------- 
_cell_length_a                   23.4908(5)
_cell_length_b                   11.0856(2)
_cell_length_c                   25.9333(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.8818(18)
_cell_angle_gamma                90
_cell_volume                     6752.5(2)
_cell_measurement_reflns_used    10890
_cell_measurement_theta_min      1.5890
_cell_measurement_theta_max      28.8960


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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
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'

_cell_formula_units_Z            8

_chemical_formula_sum            'C36 H38 N6 O2 P2'
_chemical_formula_moiety         'C36 H38 N6 O2 P2'
_chemical_compound_source        ?
_chemical_formula_weight         648.66

_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_max          0.300
_exptl_absorpt_correction_T_min  0.87684
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2736
_exptl_absorpt_coefficient_mu    0.171
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 16.0143

_diffrn_measurement_device       Area
_diffrn_radiation_wavelength     0.71073

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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_orient_matrix_UB_11      0.0245429000
_diffrn_orient_matrix_UB_12      0.0199455000
_diffrn_orient_matrix_UB_13      -0.0131162000
_diffrn_orient_matrix_UB_21      -0.0033961000
_diffrn_orient_matrix_UB_22      0.0584174000
_diffrn_orient_matrix_UB_23      0.0106869000
_diffrn_orient_matrix_UB_31      0.0172527000
_diffrn_orient_matrix_UB_32      -0.0168612000
_diffrn_orient_matrix_UB_33      0.0214986000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -10.00   71.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   77.0000  150.0000 81

#__ type_ start__ end____ width___ exp.time_
  2 omega   -6.00   83.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   77.0000  -90.0000 89

#__ type_ start__ end____ width___ exp.time_
  3 omega  -11.00   83.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   77.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega   52.00   82.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   77.0000 -180.0000 30

#__ type_ start__ end____ width___ exp.time_
  5 omega  -14.00   47.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2704   77.0000 -150.0000 61

#__ type_ start__ end____ width___ exp.time_
  6 omega   25.00   46.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2704   77.0000  150.0000 21

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            27328
_reflns_number_total             8090
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.0566
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8090 
# Theoretical number of reflections is about 18451 


_diffrn_reflns_theta_min         1.571
_diffrn_reflns_theta_max         29.290
_diffrn_measured_fraction_theta_max 0.878

_diffrn_reflns_theta_full        25.190
_diffrn_measured_fraction_theta_full 0.966


_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -31
_reflns_limit_h_max              30
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              32


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

_refine_diff_density_min         -0.27
_refine_diff_density_max         0.40


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



_refine_ls_number_reflns         6655
_refine_ls_number_restraints     0
_refine_ls_number_parameters     415
_refine_ls_wR_factor_ref         0.0552
_refine_ls_goodness_of_fit_ref   1.0885
_refine_ls_shift/su_max          0.0020464
_refine_ls_shift/su_mean         0.0000649


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8090
_refine_ls_R_factor_all          0.0614
_refine_ls_wR_factor_all         0.0602

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6655
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_gt          0.0552

_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: 
 8.12 6.38 7.13 2.16 
;

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
P1 P 0.354043(15) 0.70245(3) 0.734348(13) 0.0185 1.0000 Uani . . . . . .
O2 O 0.29452(4) 0.67979(11) 0.71686(4) 0.0268 1.0000 Uani . . . . . .
C3 C 0.39849(6) 0.73353(13) 0.67985(5) 0.0195 1.0000 Uani . . . . . .
N4 N 0.44973(6) 0.78972(13) 0.68173(5) 0.0256 1.0000 Uani . . . . . .
N5 N 0.46999(6) 0.79628(13) 0.63483(5) 0.0286 1.0000 Uani . . . . . .
N6 N 0.43173(5) 0.74452(12) 0.60281(5) 0.0229 1.0000 Uani . . . . . .
C7 C 0.38655(6) 0.70342(12) 0.62913(5) 0.0180 1.0000 Uani . . . . . .
C8 C 0.33915(6) 0.63849(12) 0.60504(5) 0.0175 1.0000 Uani . . . . . .
N9 N 0.28631(5) 0.68542(11) 0.59806(5) 0.0192 1.0000 Uani . . . . . .
N10 N 0.25113(6) 0.60395(12) 0.57600(5) 0.0237 1.0000 Uani . . . . . .
N11 N 0.28049(5) 0.50539(12) 0.56821(5) 0.0232 1.0000 Uani . . . . . .
C12 C 0.33497(6) 0.52242(13) 0.58569(5) 0.0196 1.0000 Uani . . . . . .
P13 P 0.390842(16) 0.41241(3) 0.580182(14) 0.0198 1.0000 Uani . . . . . .
O14 O 0.44766(5) 0.46908(11) 0.58584(5) 0.0295 1.0000 Uani . . . . . .
C15 C 0.37890(7) 0.34434(14) 0.51789(6) 0.0234 1.0000 Uani . . . . . .
C16 C 0.33812(8) 0.25566(15) 0.50942(7) 0.0334 1.0000 Uani . . . . . .
C17 C 0.33021(10) 0.20649(18) 0.46052(8) 0.0459 1.0000 Uani . . . . . .
C18 C 0.36330(11) 0.2466(2) 0.42063(8) 0.0520 1.0000 Uani . . . . . .
C19 C 0.40342(10) 0.3348(3) 0.42830(8) 0.0526 1.0000 Uani . . . . . .
C20 C 0.41190(8) 0.38486(19) 0.47723(7) 0.0357 1.0000 Uani . . . . . .
H201 H 0.4396 0.4456 0.4833 0.0423 1.0000 Uiso . . . . . .
H191 H 0.4257 0.3617 0.4009 0.0629 1.0000 Uiso . . . . . .
H181 H 0.3581 0.2140 0.3878 0.0626 1.0000 Uiso . . . . . .
H171 H 0.3027 0.1464 0.4551 0.0555 1.0000 Uiso . . . . . .
H161 H 0.3156 0.2290 0.5373 0.0391 1.0000 Uiso . . . . . .
C21 C 0.37724(7) 0.29688(14) 0.62713(6) 0.0257 1.0000 Uani . . . . . .
C22 C 0.32411(8) 0.27545(16) 0.64790(7) 0.0347 1.0000 Uani . . . . . .
C23 C 0.31738(10) 0.18151(19) 0.68292(8) 0.0453 1.0000 Uani . . . . . .
C24 C 0.36272(12) 0.1088(2) 0.69592(9) 0.0529 1.0000 Uani . . . . . .
C25 C 0.41533(12) 0.1297(2) 0.67560(10) 0.0598 1.0000 Uani . . . . . .
C26 C 0.42312(9) 0.2244(2) 0.64144(8) 0.0439 1.0000 Uani . . . . . .
H261 H 0.4587 0.2403 0.6282 0.0534 1.0000 Uiso . . . . . .
H251 H 0.4463 0.0798 0.6848 0.0725 1.0000 Uiso . . . . . .
H241 H 0.3581 0.0447 0.7191 0.0627 1.0000 Uiso . . . . . .
H231 H 0.2816 0.1676 0.6978 0.0549 1.0000 Uiso . . . . . .
H221 H 0.2936 0.3240 0.6385 0.0422 1.0000 Uiso . . . . . .
C27 C 0.26621(7) 0.80615(14) 0.61201(6) 0.0247 1.0000 Uani . . . . . .
C28 C 0.24224(7) 0.87804(15) 0.56600(6) 0.0291 1.0000 Uani . . . . . .
C29 C 0.18233(8) 0.84026(18) 0.55143(8) 0.0401 1.0000 Uani . . . . . .
H291 H 0.1698 0.8838 0.5216 0.0588 1.0000 Uiso . . . . . .
H292 H 0.1581 0.8550 0.5800 0.0593 1.0000 Uiso . . . . . .
H293 H 0.1811 0.7559 0.5439 0.0593 1.0000 Uiso . . . . . .
C30 C 0.24410(10) 1.01139(18) 0.57921(10) 0.0492 1.0000 Uani . . . . . .
H303 H 0.2305 1.0582 0.5499 0.0735 1.0000 Uiso . . . . . .
H302 H 0.2824 1.0351 0.5873 0.0737 1.0000 Uiso . . . . . .
H301 H 0.2206 1.0272 0.6088 0.0727 1.0000 Uiso . . . . . .
H281 H 0.2670 0.8661 0.5365 0.0343 1.0000 Uiso . . . . . .
H271 H 0.2974 0.8481 0.6268 0.0294 1.0000 Uiso . . . . . .
H272 H 0.2384 0.7962 0.6371 0.0302 1.0000 Uiso . . . . . .
C31 C 0.44248(7) 0.73585(15) 0.54725(6) 0.0280 1.0000 Uani . . . . . .
C32 C 0.45513(8) 0.85635(18) 0.52207(7) 0.0353 1.0000 Uani . . . . . .
C33 C 0.46539(10) 0.8321(2) 0.46504(8) 0.0482 1.0000 Uani . . . . . .
H331 H 0.4730 0.9070 0.4468 0.0717 1.0000 Uiso . . . . . .
H332 H 0.4975 0.7742 0.4610 0.0719 1.0000 Uiso . . . . . .
H333 H 0.4309 0.7967 0.4507 0.0709 1.0000 Uiso . . . . . .
C34 C 0.40752(10) 0.9469(2) 0.52986(9) 0.0510 1.0000 Uani . . . . . .
H341 H 0.4167 1.0221 0.5137 0.0761 1.0000 Uiso . . . . . .
H342 H 0.4027 0.9619 0.5661 0.0751 1.0000 Uiso . . . . . .
H343 H 0.3725 0.9149 0.5162 0.0752 1.0000 Uiso . . . . . .
H321 H 0.4903 0.8885 0.5382 0.0421 1.0000 Uiso . . . . . .
H311 H 0.4728 0.6818 0.5420 0.0341 1.0000 Uiso . . . . . .
H312 H 0.4085 0.7022 0.5319 0.0350 1.0000 Uiso . . . . . .
C35 C 0.36020(6) 0.83273(13) 0.77560(5) 0.0196 1.0000 Uani . . . . . .
C36 C 0.41121(6) 0.87976(14) 0.79474(6) 0.0246 1.0000 Uani . . . . . .
C37 C 0.41065(8) 0.97988(16) 0.82679(7) 0.0319 1.0000 Uani . . . . . .
C38 C 0.35956(8) 1.03461(15) 0.83900(7) 0.0331 1.0000 Uani . . . . . .
C39 C 0.30894(8) 0.99086(16) 0.81907(7) 0.0317 1.0000 Uani . . . . . .
C40 C 0.30892(6) 0.88875(15) 0.78791(6) 0.0257 1.0000 Uani . . . . . .
H401 H 0.2752 0.8568 0.7739 0.0316 1.0000 Uiso . . . . . .
H391 H 0.2749 1.0298 0.8266 0.0382 1.0000 Uiso . . . . . .
H381 H 0.3594 1.1019 0.8614 0.0405 1.0000 Uiso . . . . . .
H371 H 0.4450 1.0097 0.8405 0.0380 1.0000 Uiso . . . . . .
H361 H 0.4468 0.8429 0.7862 0.0295 1.0000 Uiso . . . . . .
C41 C 0.38451(7) 0.57293(13) 0.76656(5) 0.0228 1.0000 Uani . . . . . .
C42 C 0.43774(9) 0.57188(17) 0.78945(9) 0.0447 1.0000 Uani . . . . . .
C43 C 0.45812(11) 0.4673(2) 0.81345(10) 0.0545 1.0000 Uani . . . . . .
C44 C 0.42559(11) 0.36548(19) 0.81294(9) 0.0521 1.0000 Uani . . . . . .
C45 C 0.37183(12) 0.36529(19) 0.79051(11) 0.0578 1.0000 Uani . . . . . .
C46 C 0.35125(9) 0.46901(18) 0.76741(9) 0.0461 1.0000 Uani . . . . . .
H461 H 0.3150 0.4697 0.7518 0.0545 1.0000 Uiso . . . . . .
H451 H 0.3496 0.2949 0.7908 0.0694 1.0000 Uiso . . . . . .
H441 H 0.4396 0.2952 0.8281 0.0629 1.0000 Uiso . . . . . .
H431 H 0.4938 0.4684 0.8294 0.0661 1.0000 Uiso . . . . . .
H421 H 0.4604 0.6416 0.7893 0.0542 1.0000 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
P1 . O2 . 1.4847(11) yes
P1 . C3 . 1.8033(15) yes
P1 . C35 . 1.8018(15) yes
P1 . C41 . 1.8038(15) yes
C3 . N4 . 1.3556(19) yes
C3 . C7 . 1.3816(19) yes
N4 . N5 . 1.3148(19) yes
N5 . N6 . 1.3428(18) yes
N6 . C7 . 1.3500(18) yes
N6 . C31 . 1.4698(19) yes
C7 . C8 . 1.4582(19) yes
C8 . N9 . 1.3555(18) yes
C8 . C12 . 1.3840(19) yes
N9 . N10 . 1.3457(17) yes
N9 . C27 . 1.4664(19) yes
N10 . N11 . 1.3094(19) yes
N11 . C12 . 1.3642(19) yes
C12 . P13 . 1.7990(15) yes
P13 . O14 . 1.4804(12) yes
P13 . C15 . 1.8010(15) yes
P13 . C21 . 1.7991(16) yes
C15 . C16 . 1.388(2) yes
C15 . C20 . 1.393(2) yes
C16 . C17 . 1.390(3) yes
C16 . H161 . 0.951 no
C17 . C18 . 1.377(4) yes
C17 . H171 . 0.938 no
C18 . C19 . 1.370(4) yes
C18 . H181 . 0.931 no
C19 . C20 . 1.396(3) yes
C19 . H191 . 0.937 no
C20 . H201 . 0.947 no
C21 . C22 . 1.387(2) yes
C21 . C26 . 1.390(2) yes
C22 . C23 . 1.392(3) yes
C22 . H221 . 0.925 no
C23 . C24 . 1.373(3) yes
C23 . H231 . 0.944 no
C24 . C25 . 1.370(4) yes
C24 . H241 . 0.940 no
C25 . C26 . 1.388(3) yes
C25 . H251 . 0.942 no
C26 . H261 . 0.926 no
C27 . C28 . 1.535(2) yes
C27 . H271 . 0.945 no
C27 . H272 . 0.935 no
C28 . C29 . 1.511(2) yes
C28 . C30 . 1.518(3) yes
C28 . H281 . 0.977 no
C29 . H291 . 0.954 no
C29 . H292 . 0.954 no
C29 . H293 . 0.956 no
C30 . H303 . 0.970 no
C30 . H302 . 0.957 no
C30 . H301 . 0.968 no
C31 . C32 . 1.518(2) yes
C31 . H311 . 0.942 no
C31 . H312 . 0.962 no
C32 . C33 . 1.526(3) yes
C32 . C34 . 1.519(3) yes
C32 . H321 . 0.986 no
C33 . H331 . 0.973 no
C33 . H332 . 0.996 no
C33 . H333 . 0.969 no
C34 . H341 . 0.959 no
C34 . H342 . 0.962 no
C34 . H343 . 0.959 no
C35 . C36 . 1.391(2) yes
C35 . C40 . 1.397(2) yes
C36 . C37 . 1.387(2) yes
C36 . H361 . 0.960 no
C37 . C38 . 1.386(3) yes
C37 . H371 . 0.937 no
C38 . C39 . 1.377(3) yes
C38 . H381 . 0.946 no
C39 . C40 . 1.391(2) yes
C39 . H391 . 0.932 no
C40 . H401 . 0.937 no
C41 . C42 . 1.376(2) yes
C41 . C46 . 1.392(2) yes
C42 . C43 . 1.397(3) yes
C42 . H421 . 0.939 no
C43 . C44 . 1.363(4) yes
C43 . H431 . 0.930 no
C44 . C45 . 1.382(4) yes
C44 . H441 . 0.930 no
C45 . C46 . 1.380(3) yes
C45 . H451 . 0.939 no
C46 . H461 . 0.938 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
O2 . P1 . C3 . 110.29(6) yes
O2 . P1 . C35 . 112.56(7) yes
C3 . P1 . C35 . 105.67(7) yes
O2 . P1 . C41 . 111.84(7) yes
C3 . P1 . C41 . 106.54(7) yes
C35 . P1 . C41 . 109.60(7) yes
P1 . C3 . N4 . 125.74(11) yes
P1 . C3 . C7 . 126.05(11) yes
N4 . C3 . C7 . 108.21(13) yes
C3 . N4 . N5 . 109.02(12) yes
N4 . N5 . N6 . 107.47(12) yes
N5 . N6 . C7 . 110.82(12) yes
N5 . N6 . C31 . 120.72(12) yes
C7 . N6 . C31 . 128.45(13) yes
C3 . C7 . N6 . 104.48(12) yes
C3 . C7 . C8 . 132.03(13) yes
N6 . C7 . C8 . 123.44(12) yes
C7 . C8 . N9 . 124.01(12) yes
C7 . C8 . C12 . 131.59(13) yes
N9 . C8 . C12 . 104.39(12) yes
C8 . N9 . N10 . 110.75(12) yes
C8 . N9 . C27 . 127.95(12) yes
N10 . N9 . C27 . 121.30(12) yes
N9 . N10 . N11 . 107.71(12) yes
N10 . N11 . C12 . 109.07(12) yes
C8 . C12 . N11 . 108.07(12) yes
C8 . C12 . P13 . 127.68(11) yes
N11 . C12 . P13 . 124.17(11) yes
C12 . P13 . O14 . 111.24(7) yes
C12 . P13 . C15 . 104.57(7) yes
O14 . P13 . C15 . 113.23(7) yes
C12 . P13 . C21 . 106.94(7) yes
O14 . P13 . C21 . 113.84(7) yes
C15 . P13 . C21 . 106.37(7) yes
P13 . C15 . C16 . 122.44(12) yes
P13 . C15 . C20 . 117.59(13) yes
C16 . C15 . C20 . 119.96(15) yes
C15 . C16 . C17 . 120.30(18) yes
C15 . C16 . H161 . 119.4 no
C17 . C16 . H161 . 120.3 no
C16 . C17 . C18 . 119.3(2) yes
C16 . C17 . H171 . 119.9 no
C18 . C17 . H171 . 120.8 no
C17 . C18 . C19 . 121.10(18) yes
C17 . C18 . H181 . 119.5 no
C19 . C18 . H181 . 119.4 no
C18 . C19 . C20 . 120.2(2) yes
C18 . C19 . H191 . 120.5 no
C20 . C19 . H191 . 119.2 no
C19 . C20 . C15 . 119.12(19) yes
C19 . C20 . H201 . 121.4 no
C15 . C20 . H201 . 119.5 no
P13 . C21 . C22 . 123.70(13) yes
P13 . C21 . C26 . 116.55(13) yes
C22 . C21 . C26 . 119.73(16) yes
C21 . C22 . C23 . 119.54(17) yes
C21 . C22 . H221 . 119.7 no
C23 . C22 . H221 . 120.7 no
C22 . C23 . C24 . 120.22(19) yes
C22 . C23 . H231 . 120.0 no
C24 . C23 . H231 . 119.7 no
C23 . C24 . C25 . 120.49(18) yes
C23 . C24 . H241 . 120.2 no
C25 . C24 . H241 . 119.3 no
C24 . C25 . C26 . 120.1(2) yes
C24 . C25 . H251 . 120.1 no
C26 . C25 . H251 . 119.8 no
C21 . C26 . C25 . 119.9(2) yes
C21 . C26 . H261 . 119.5 no
C25 . C26 . H261 . 120.6 no
N9 . C27 . C28 . 113.44(13) yes
N9 . C27 . H271 . 107.4 no
C28 . C27 . H271 . 109.5 no
N9 . C27 . H272 . 107.1 no
C28 . C27 . H272 . 110.5 no
H271 . C27 . H272 . 108.7 no
C27 . C28 . C29 . 112.31(14) yes
C27 . C28 . C30 . 108.74(15) yes
C29 . C28 . C30 . 110.48(15) yes
C27 . C28 . H281 . 108.9 no
C29 . C28 . H281 . 109.2 no
C30 . C28 . H281 . 107.1 no
C28 . C29 . H291 . 109.7 no
C28 . C29 . H292 . 108.8 no
H291 . C29 . H292 . 111.2 no
C28 . C29 . H293 . 110.4 no
H291 . C29 . H293 . 108.7 no
H292 . C29 . H293 . 108.0 no
C28 . C30 . H303 . 109.6 no
C28 . C30 . H302 . 109.9 no
H303 . C30 . H302 . 108.8 no
C28 . C30 . H301 . 109.9 no
H303 . C30 . H301 . 109.8 no
H302 . C30 . H301 . 108.8 no
N6 . C31 . C32 . 113.69(14) yes
N6 . C31 . H311 . 108.9 no
C32 . C31 . H311 . 110.1 no
N6 . C31 . H312 . 106.1 no
C32 . C31 . H312 . 109.3 no
H311 . C31 . H312 . 108.5 no
C31 . C32 . C33 . 107.26(16) yes
C31 . C32 . C34 . 112.01(15) yes
C33 . C32 . C34 . 111.90(18) yes
C31 . C32 . H321 . 107.7 no
C33 . C32 . H321 . 109.3 no
C34 . C32 . H321 . 108.6 no
C32 . C33 . H331 . 110.7 no
C32 . C33 . H332 . 110.2 no
H331 . C33 . H332 . 110.8 no
C32 . C33 . H333 . 107.5 no
H331 . C33 . H333 . 108.5 no
H332 . C33 . H333 . 109.2 no
C32 . C34 . H341 . 110.2 no
C32 . C34 . H342 . 110.0 no
H341 . C34 . H342 . 107.8 no
C32 . C34 . H343 . 109.6 no
H341 . C34 . H343 . 111.0 no
H342 . C34 . H343 . 108.2 no
P1 . C35 . C36 . 124.96(11) yes
P1 . C35 . C40 . 115.49(11) yes
C36 . C35 . C40 . 119.54(14) yes
C35 . C36 . C37 . 119.84(15) yes
C35 . C36 . H361 . 120.4 no
C37 . C36 . H361 . 119.7 no
C36 . C37 . C38 . 120.24(16) yes
C36 . C37 . H371 . 119.6 no
C38 . C37 . H371 . 120.2 no
C37 . C38 . C39 . 120.38(15) yes
C37 . C38 . H381 . 119.8 no
C39 . C38 . H381 . 119.8 no
C38 . C39 . C40 . 119.82(15) yes
C38 . C39 . H391 . 119.8 no
C40 . C39 . H391 . 120.4 no
C35 . C40 . C39 . 120.13(15) yes
C35 . C40 . H401 . 118.1 no
C39 . C40 . H401 . 121.7 no
P1 . C41 . C42 . 123.92(13) yes
P1 . C41 . C46 . 116.56(13) yes
C42 . C41 . C46 . 119.52(16) yes
C41 . C42 . C43 . 120.14(19) yes
C41 . C42 . H421 . 120.2 no
C43 . C42 . H421 . 119.6 no
C42 . C43 . C44 . 119.7(2) yes
C42 . C43 . H431 . 119.2 no
C44 . C43 . H431 . 121.1 no
C43 . C44 . C45 . 120.91(19) yes
C43 . C44 . H441 . 119.7 no
C45 . C44 . H441 . 119.4 no
C44 . C45 . C46 . 119.5(2) yes
C44 . C45 . H451 . 120.1 no
C46 . C45 . H451 . 120.3 no
C41 . C46 . C45 . 120.2(2) yes
C41 . C46 . H461 . 119.5 no
C45 . C46 . H461 . 120.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C29 . H293 . N10 . 125.12(11) 0.956 2.489 3.138(3) yes
C39 . H391 . O2 8_556 138.36(11) 0.932 2.576 3.330(3) yes
C43 . H431 . O14 6_656 147.86(18) 0.930 2.574 3.397(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 11/04/13 at 11:33:08
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 11/04/13 at 11:33:08
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_13.1
_database_code_depnum_ccdc_archive 'CCDC 1031967'
_audit_update_record             
;
2014-10-31 deposited with the CCDC.
2015-06-16 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          ?
#--------------------------------------------------------------- 
_cell_length_a                   20.0222(3)
_cell_length_b                   18.8861(4)
_cell_length_c                   22.6056(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.2374(16)
_cell_angle_gamma                90
_cell_volume                     8524.8(3)
_cell_measurement_reflns_used    8620
_cell_measurement_theta_min      2.0090
_cell_measurement_theta_max      26.2780


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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

_chemical_formula_sum            'C43 H35 Cl5 N6 P2 Pd'
_chemical_formula_moiety         'C42 H34 Cl2 N6 P2 Pd, C H Cl3'
_chemical_compound_source        ?
_chemical_formula_weight         981.36


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.250
_exptl_absorpt_correction_T_min  0.98999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3968
_exptl_absorpt_coefficient_mu    0.864
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 16.0143

_diffrn_measurement_device       Area
_diffrn_radiation_wavelength     0.71073


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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_orient_matrix_UB_11      0.0099175000
_diffrn_orient_matrix_UB_12      0.0183588000
_diffrn_orient_matrix_UB_13      0.0265859000
_diffrn_orient_matrix_UB_21      0.0164357000
_diffrn_orient_matrix_UB_22      0.0257492000
_diffrn_orient_matrix_UB_23      -0.0165561000
_diffrn_orient_matrix_UB_31      -0.0298946000
_diffrn_orient_matrix_UB_32      0.0202421000
_diffrn_orient_matrix_UB_33      -0.0030392000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   51.00   77.00   1.0000  420.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3939  179.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -48.00   84.00   1.0000  420.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3939    0.0000  -90.0000 132

#__ type_ start__ end____ width___ exp.time_
  3 omega  -20.00   35.00   1.0000  420.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3939  -38.0000 -150.0000 55

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            32286
_reflns_number_total             14409
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0527
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 14409 
# Theoretical number of reflections is about 35141


_diffrn_reflns_theta_min         1.484
_diffrn_reflns_theta_max         26.446
_diffrn_measured_fraction_theta_max 0.820

_diffrn_reflns_theta_full        25.123
_diffrn_measured_fraction_theta_full 0.852


_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -25
_reflns_limit_h_max              25
_reflns_limit_k_min              0
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              25


_atom_sites_solution_primary     other
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.63
_refine_diff_density_max         1.64


_refine_ls_number_reflns         10170
_refine_ls_number_restraints     0
_refine_ls_number_parameters     1027
_refine_ls_wR_factor_ref         0.0247
_refine_ls_goodness_of_fit_ref   1.1177
_refine_ls_shift/su_max          0.0013347
_refine_ls_shift/su_mean         0.0000401


_refine_ls_R_factor_all          0.0727
_refine_ls_wR_factor_all         0.0313

_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10170
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_gt          0.0247


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr
_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: 
 1.94 -8.31 -1.20 -2.49 -1.94 
;

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 0.264294(14) 0.633158(16) 0.505675(14) 0.0214 1.0000 Uani . . . . . .
Cl3 Cl 0.24132(6) 0.75384(6) 0.50307(6) 0.0413 1.0000 Uani . . . . . .
Cl7 Cl 0.36881(5) 0.65767(6) 0.47034(6) 0.0370 1.0000 Uani . . . . . .
P10 P 0.29919(5) 0.51900(5) 0.50505(5) 0.0197 1.0000 Uani . . . . . .
P15 P 0.16447(5) 0.61050(5) 0.54293(5) 0.0223 1.0000 Uani . . . . . .
C17 C 0.37969(18) 0.5076(2) 0.54701(19) 0.0230 1.0000 Uani . . . . . .
C18 C 0.3923(2) 0.5457(3) 0.5980(2) 0.0536 1.0000 Uani . . . . . .
C19 C 0.4516(3) 0.5352(4) 0.6328(3) 0.0669 1.0000 Uani . . . . . .
C20 C 0.4979(2) 0.4883(3) 0.6168(2) 0.0473 1.0000 Uani . . . . . .
C21 C 0.4855(2) 0.4503(3) 0.5662(3) 0.0539 1.0000 Uani . . . . . .
C22 C 0.4267(2) 0.4594(3) 0.5311(3) 0.0484 1.0000 Uani . . . . . .
Pd23 Pd 0.769913(14) 0.865812(17) 0.533604(15) 0.0262 1.0000 Uani . . . . . .
P24 P 0.66982(5) 0.89102(6) 0.56742(5) 0.0246 1.0000 Uani . . . . . .
Cl29 Cl 0.75477(6) 0.74510(6) 0.54739(7) 0.0553 1.0000 Uani . . . . . .
Cl32 Cl 0.86849(6) 0.84259(6) 0.48768(7) 0.0478 1.0000 Uani . . . . . .
N36 N 0.78576(18) 1.09295(18) 0.60655(15) 0.0299 1.0000 Uani . . . . . .
C37 C 0.6088(2) 0.8193(2) 0.56601(19) 0.0273 1.0000 Uani . . . . . .
C38 C 0.5907(2) 0.7847(2) 0.5126(2) 0.0393 1.0000 Uani . . . . . .
C39 C 0.5437(2) 0.7319(3) 0.5112(2) 0.0455 1.0000 Uani . . . . . .
C40 C 0.5148(2) 0.7112(3) 0.5614(3) 0.0472 1.0000 Uani . . . . . .
C41 C 0.5329(2) 0.7451(3) 0.6144(2) 0.0422 1.0000 Uani . . . . . .
C42 C 0.5793(2) 0.7994(2) 0.6170(2) 0.0330 1.0000 Uani . . . . . .
C43 C 0.62505(19) 0.9586(2) 0.52264(19) 0.0266 1.0000 Uani . . . . . .
N44 N 0.57432(18) 0.9427(2) 0.48210(18) 0.0378 1.0000 Uani . . . . . .
N45 N 0.55609(18) 1.0005(2) 0.45304(18) 0.0393 1.0000 Uani . . . . . .
N46 N 0.59516(17) 1.05394(19) 0.47448(16) 0.0305 1.0000 Uani . . . . . .
C47 C 0.63913(19) 1.0305(2) 0.51873(18) 0.0244 1.0000 Uani . . . . . .
C48 C 0.6903(2) 1.0692(2) 0.55350(17) 0.0225 1.0000 Uani . . . . . .
N49 N 0.68312(18) 1.12601(18) 0.58967(15) 0.0293 1.0000 Uani . . . . . .
N50 N 0.74144(19) 1.1396(2) 0.62138(16) 0.0361 1.0000 Uani . . . . . .
C52 C 0.75613(19) 1.0489(2) 0.56522(17) 0.0226 1.0000 Uani . . . . . .
C53 C 0.6261(2) 1.1745(3) 0.5956(2) 0.0409 1.0000 Uani . . . . . .
C54 C 0.5824(2) 1.1564(2) 0.6444(2) 0.0326 1.0000 Uani . . . . . .
C55 C 0.5999(2) 1.1780(2) 0.7019(2) 0.0353 1.0000 Uani . . . . . .
C56 C 0.5575(3) 1.1655(3) 0.7466(2) 0.0487 1.0000 Uani . . . . . .
C57 C 0.4979(3) 1.1310(3) 0.7339(3) 0.0550 1.0000 Uani . . . . . .
C58 C 0.4811(3) 1.1085(3) 0.6771(3) 0.0574 1.0000 Uani . . . . . .
C59 C 0.5229(3) 1.1214(3) 0.6324(3) 0.0507 1.0000 Uani . . . . . .
C60 C 0.5867(2) 1.1256(2) 0.44876(19) 0.0346 1.0000 Uani . . . . . .
C61 C 0.5962(2) 1.1292(2) 0.3834(2) 0.0335 1.0000 Uani . . . . . .
C62 C 0.6426(3) 1.1760(3) 0.3655(3) 0.0539 1.0000 Uani . . . . . .
C63 C 0.6499(3) 1.1854(4) 0.3058(3) 0.0761 1.0000 Uani . . . . . .
C64 C 0.6113(4) 1.1480(4) 0.2641(3) 0.0772 1.0000 Uani . . . . . .
C65 C 0.5636(4) 1.1019(3) 0.2815(3) 0.0777 1.0000 Uani . . . . . .
C66 C 0.5558(3) 1.0926(3) 0.3422(2) 0.0547 1.0000 Uani . . . . . .
C67 C 0.6754(2) 0.9225(2) 0.64319(19) 0.0313 1.0000 Uani . . . . . .
C68 C 0.6270(3) 0.9668(2) 0.6640(2) 0.0373 1.0000 Uani . . . . . .
C69 C 0.6279(3) 0.9813(3) 0.7239(2) 0.0531 1.0000 Uani . . . . . .
C70 C 0.6768(3) 0.9533(3) 0.7633(2) 0.0546 1.0000 Uani . . . . . .
C71 C 0.7261(3) 0.9110(3) 0.7425(2) 0.0499 1.0000 Uani . . . . . .
C72 C 0.7262(2) 0.8954(2) 0.6821(2) 0.0372 1.0000 Uani . . . . . .
Cl73 Cl 0.66473(12) 0.73904(9) 0.75407(7) 0.0921 1.0000 Uani . . . . . .
C74 C 0.6587(3) 0.7641(3) 0.8275(2) 0.0532 1.0000 Uani . . . . . .
Cl75 Cl 0.68138(9) 0.69241(11) 0.87320(8) 0.0797 1.0000 Uani . . . . . .
Cl76 Cl 0.57867(10) 0.79305(10) 0.84010(12) 0.1028 1.0000 Uani . . . . . .
Cl77 Cl 0.14770(8) 0.63470(9) 0.35916(7) 0.0673 1.0000 Uani . . . . . .
C78 C 0.1697(3) 0.7192(4) 0.3407(3) 0.0804 1.0000 Uani . . . . . .
Cl79 Cl 0.09922(14) 0.77349(12) 0.33032(16) 0.1564 1.0000 Uani . . . . . .
C82 C 0.11504(18) 0.5434(2) 0.50182(18) 0.0239 1.0000 Uani . . . . . .
N83 N 0.05939(17) 0.55706(19) 0.46545(17) 0.0310 1.0000 Uani . . . . . .
N84 N 0.04061(17) 0.4982(2) 0.43834(17) 0.0328 1.0000 Uani . . . . . .
N85 N 0.08331(15) 0.44640(18) 0.45689(15) 0.0259 1.0000 Uani . . . . . .
C86 C 0.13049(18) 0.4727(2) 0.49706(18) 0.0210 1.0000 Uani . . . . . .
C87 C 0.18391(19) 0.4334(2) 0.52950(17) 0.0202 1.0000 Uani . . . . . .
N88 N 0.17549(16) 0.37706(17) 0.56523(14) 0.0234 1.0000 Uani . . . . . .
N89 N 0.23411(17) 0.35953(19) 0.59467(16) 0.0311 1.0000 Uani . . . . . .
N90 N 0.27983(16) 0.40404(18) 0.57938(16) 0.0290 1.0000 Uani . . . . . .
C91 C 0.25088(18) 0.45068(19) 0.53909(17) 0.0205 1.0000 Uani . . . . . .
C92 C 0.1150(2) 0.3341(2) 0.57391(19) 0.0303 1.0000 Uani . . . . . .
C93 C 0.0998(2) 0.3282(2) 0.6378(2) 0.0337 1.0000 Uani . . . . . .
C94 C 0.0443(2) 0.3622(3) 0.6573(2) 0.0439 1.0000 Uani . . . . . .
C95 C 0.0293(3) 0.3570(4) 0.7157(2) 0.0605 1.0000 Uani . . . . . .
C96 C 0.0701(3) 0.3179(4) 0.7546(2) 0.0656 1.0000 Uani . . . . . .
C97 C 0.1247(3) 0.2841(4) 0.7369(3) 0.0689 1.0000 Uani . . . . . .
C98 C 0.1390(3) 0.2884(3) 0.6776(3) 0.0545 1.0000 Uani . . . . . .
C99 C 0.0782(2) 0.3763(2) 0.42844(19) 0.0292 1.0000 Uani . . . . . .
C100 C 0.0854(2) 0.3825(2) 0.3627(2) 0.0305 1.0000 Uani . . . . . .
C101 C 0.0308(2) 0.3814(3) 0.3222(2) 0.0425 1.0000 Uani . . . . . .
C102 C 0.0385(3) 0.3880(3) 0.2618(2) 0.0511 1.0000 Uani . . . . . .
C103 C 0.1002(3) 0.3968(4) 0.2421(2) 0.0671 1.0000 Uani . . . . . .
C104 C 0.1550(3) 0.3940(5) 0.2812(3) 0.0948 1.0000 Uani . . . . . .
C105 C 0.1480(3) 0.3876(4) 0.3415(3) 0.0736 1.0000 Uani . . . . . .
C106 C 0.17361(19) 0.5800(2) 0.61884(19) 0.0266 1.0000 Uani . . . . . .
C107 C 0.2244(2) 0.6107(2) 0.6565(2) 0.0357 1.0000 Uani . . . . . .
C108 C 0.2259(3) 0.5993(3) 0.7171(2) 0.0470 1.0000 Uani . . . . . .
C109 C 0.1780(3) 0.5577(3) 0.7403(2) 0.0477 1.0000 Uani . . . . . .
C110 C 0.1294(3) 0.5258(3) 0.7034(2) 0.0425 1.0000 Uani . . . . . .
C111 C 0.1267(2) 0.5365(2) 0.6434(2) 0.0325 1.0000 Uani . . . . . .
C112 C 0.10714(18) 0.6849(2) 0.5465(2) 0.0270 1.0000 Uani . . . . . .
C113 C 0.0756(2) 0.7137(2) 0.4953(2) 0.0367 1.0000 Uani . . . . . .
C114 C 0.0339(2) 0.7717(2) 0.4981(2) 0.0428 1.0000 Uani . . . . . .
C115 C 0.0239(2) 0.8014(3) 0.5522(3) 0.0466 1.0000 Uani . . . . . .
C116 C 0.0551(2) 0.7748(3) 0.6035(3) 0.0498 1.0000 Uani . . . . . .
C117 C 0.0971(2) 0.7163(2) 0.6005(2) 0.0362 1.0000 Uani . . . . . .
C118 C 0.3038(2) 0.5295(2) 0.3816(2) 0.0299 1.0000 Uani . . . . . .
C119 C 0.30696(19) 0.4842(2) 0.43031(19) 0.0249 1.0000 Uani . . . . . .
C120 C 0.3187(2) 0.4129(2) 0.42234(19) 0.0270 1.0000 Uani . . . . . .
C121 C 0.3290(2) 0.3869(2) 0.3662(2) 0.0377 1.0000 Uani . . . . . .
C122 C 0.3272(2) 0.4324(3) 0.3185(2) 0.0385 1.0000 Uani . . . . . .
C123 C 0.3131(2) 0.5030(3) 0.3259(2) 0.0387 1.0000 Uani . . . . . .
C124 C 0.79682(19) 1.0127(2) 0.45222(18) 0.0255 1.0000 Uani . . . . . .
C125 C 0.7807(2) 0.9668(3) 0.4056(2) 0.0405 1.0000 Uani . . . . . .
C126 C 0.7760(3) 0.9905(3) 0.3482(2) 0.0556 1.0000 Uani . . . . . .
C127 C 0.7871(3) 1.0601(3) 0.3358(2) 0.0545 1.0000 Uani . . . . . .
C128 C 0.8033(3) 1.1068(3) 0.3815(2) 0.0443 1.0000 Uani . . . . . .
C129 C 0.8071(2) 1.0842(2) 0.4391(2) 0.0348 1.0000 Uani . . . . . .
C130 C 0.9026(2) 0.9565(3) 0.6144(2) 0.0472 1.0000 Uani . . . . . .
C131 C 0.8853(2) 0.9923(2) 0.5632(2) 0.0285 1.0000 Uani . . . . . .
C132 C 0.9313(2) 1.0368(3) 0.5403(3) 0.0581 1.0000 Uani . . . . . .
C133 C 0.9946(3) 1.0433(3) 0.5692(3) 0.0705 1.0000 Uani . . . . . .
C134 C 1.0121(2) 1.0068(3) 0.6191(3) 0.0515 1.0000 Uani . . . . . .
C135 C 0.9665(3) 0.9644(3) 0.6423(2) 0.0605 1.0000 Uani . . . . . .
P1 P 0.80129(5) 0.98045(5) 0.52781(5) 0.0224 1.0000 Uani . . . . . .
Cl1 Cl 0.2185(3) 0.71475(18) 0.28176(18) 0.2882 1.0000 Uani . . . . . .
H181 H 0.3612 0.5785 0.6087 0.0649 1.0000 Uiso R . . . . .
H191 H 0.4596 0.5609 0.6672 0.0802 1.0000 Uiso R . . . . .
H201 H 0.5373 0.4816 0.6401 0.0569 1.0000 Uiso R . . . . .
H211 H 0.5179 0.4180 0.5547 0.0640 1.0000 Uiso R . . . . .
H221 H 0.4190 0.4331 0.4963 0.0579 1.0000 Uiso R . . . . .
H381 H 0.6113 0.7967 0.4782 0.0469 1.0000 Uiso R . . . . .
H391 H 0.5310 0.7097 0.4753 0.0542 1.0000 Uiso R . . . . .
H401 H 0.4832 0.6746 0.5600 0.0562 1.0000 Uiso R . . . . .
H411 H 0.5137 0.7311 0.6485 0.0498 1.0000 Uiso R . . . . .
H421 H 0.5907 0.8221 0.6525 0.0405 1.0000 Uiso R . . . . .
H531 H 0.6444 1.2220 0.6018 0.0492 1.0000 Uiso R . . . . .
H532 H 0.5979 1.1731 0.5593 0.0491 1.0000 Uiso R . . . . .
H551 H 0.6404 1.2007 0.7106 0.0416 1.0000 Uiso R . . . . .
H561 H 0.5693 1.1805 0.7851 0.0580 1.0000 Uiso R . . . . .
H571 H 0.4688 1.1234 0.7635 0.0650 1.0000 Uiso R . . . . .
H581 H 0.4409 1.0838 0.6686 0.0690 1.0000 Uiso R . . . . .
H591 H 0.5109 1.1072 0.5939 0.0611 1.0000 Uiso R . . . . .
H601 H 0.6192 1.1561 0.4692 0.0417 1.0000 Uiso R . . . . .
H602 H 0.5421 1.1416 0.4549 0.0424 1.0000 Uiso R . . . . .
H621 H 0.6694 1.2016 0.3936 0.0639 1.0000 Uiso R . . . . .
H631 H 0.6819 1.2174 0.2939 0.0909 1.0000 Uiso R . . . . .
H641 H 0.6170 1.1538 0.2241 0.0920 1.0000 Uiso R . . . . .
H651 H 0.5360 1.0773 0.2540 0.0929 1.0000 Uiso R . . . . .
H661 H 0.5227 1.0619 0.3544 0.0650 1.0000 Uiso R . . . . .
H681 H 0.5933 0.9858 0.6378 0.0451 1.0000 Uiso R . . . . .
H691 H 0.5952 1.0100 0.7381 0.0633 1.0000 Uiso R . . . . .
H701 H 0.6764 0.9624 0.8041 0.0660 1.0000 Uiso R . . . . .
H711 H 0.7601 0.8917 0.7685 0.0591 1.0000 Uiso R . . . . .
H721 H 0.7593 0.8663 0.6685 0.0440 1.0000 Uiso R . . . . .
H741 H 0.6902 0.8022 0.8371 0.0642 1.0000 Uiso R . . . . .
H781 H 0.1973 0.7383 0.3742 0.0959 1.0000 Uiso R . . . . .
H921 H 0.0775 0.3564 0.5517 0.0354 1.0000 Uiso R . . . . .
H922 H 0.1216 0.2873 0.5585 0.0360 1.0000 Uiso R . . . . .
H941 H 0.0173 0.3884 0.6305 0.0527 1.0000 Uiso R . . . . .
H951 H -0.0087 0.3795 0.7283 0.0723 1.0000 Uiso R . . . . .
H961 H 0.0598 0.3143 0.7941 0.0778 1.0000 Uiso R . . . . .
H971 H 0.1517 0.2579 0.7637 0.0820 1.0000 Uiso R . . . . .
H981 H 0.1748 0.2635 0.6644 0.0649 1.0000 Uiso R . . . . .
H991 H 0.1124 0.3461 0.4464 0.0346 1.0000 Uiso R . . . . .
H992 H 0.0353 0.3559 0.4346 0.0348 1.0000 Uiso R . . . . .
H1011 H -0.0122 0.3771 0.3354 0.0511 1.0000 Uiso R . . . . .
H1021 H 0.0003 0.3867 0.2347 0.0609 1.0000 Uiso R . . . . .
H1031 H 0.1044 0.4043 0.2019 0.0810 1.0000 Uiso R . . . . .
H1041 H 0.1981 0.3968 0.2670 0.1129 1.0000 Uiso R . . . . .
H1051 H 0.1858 0.3871 0.3688 0.0870 1.0000 Uiso R . . . . .
H1071 H 0.2567 0.6389 0.6409 0.0427 1.0000 Uiso R . . . . .
H1081 H 0.2596 0.6204 0.7415 0.0561 1.0000 Uiso R . . . . .
H1091 H 0.1779 0.5512 0.7813 0.0580 1.0000 Uiso R . . . . .
H1101 H 0.0984 0.4963 0.7195 0.0512 1.0000 Uiso R . . . . .
H1111 H 0.0937 0.5155 0.6185 0.0389 1.0000 Uiso R . . . . .
H1131 H 0.0830 0.6937 0.4585 0.0439 1.0000 Uiso R . . . . .
H1141 H 0.0128 0.7905 0.4637 0.0507 1.0000 Uiso R . . . . .
H1151 H -0.0043 0.8401 0.5543 0.0558 1.0000 Uiso R . . . . .
H1161 H 0.0486 0.7956 0.6399 0.0599 1.0000 Uiso R . . . . .
H1171 H 0.1192 0.6979 0.6349 0.0440 1.0000 Uiso R . . . . .
H1181 H 0.2966 0.5774 0.3862 0.0360 1.0000 Uiso R . . . . .
H1201 H 0.3187 0.3820 0.4552 0.0318 1.0000 Uiso R . . . . .
H1211 H 0.3368 0.3393 0.3612 0.0452 1.0000 Uiso R . . . . .
H1221 H 0.3349 0.4156 0.2810 0.0457 1.0000 Uiso R . . . . .
H1231 H 0.3100 0.5333 0.2935 0.0457 1.0000 Uiso R . . . . .
H1251 H 0.7730 0.9195 0.4143 0.0483 1.0000 Uiso R . . . . .
H1261 H 0.7652 0.9588 0.3172 0.0672 1.0000 Uiso R . . . . .
H1271 H 0.7829 1.0763 0.2972 0.0665 1.0000 Uiso R . . . . .
H1281 H 0.8117 1.1539 0.3728 0.0525 1.0000 Uiso R . . . . .
H1291 H 0.8158 1.1162 0.4702 0.0414 1.0000 Uiso R . . . . .
H1301 H 0.8717 0.9268 0.6304 0.0569 1.0000 Uiso R . . . . .
H1321 H 0.9198 1.0622 0.5058 0.0701 1.0000 Uiso R . . . . .
H1331 H 1.0260 1.0729 0.5530 0.0842 1.0000 Uiso R . . . . .
H1341 H 1.0549 1.0112 0.6381 0.0621 1.0000 Uiso R . . . . .
H1351 H 0.9779 0.9407 0.6773 0.0720 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.5393(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl3 . 2.3250(11) yes
Pd1 . Cl7 . 2.3407(11) yes
Pd1 . P10 . 2.2667(10) yes
Pd1 . P15 . 2.2663(10) yes
P10 . C17 . 1.822(4) yes
P10 . C91 . 1.817(4) yes
P10 . C119 . 1.830(4) yes
P15 . C82 . 1.820(4) yes
P15 . C106 . 1.807(4) yes
P15 . C112 . 1.821(4) yes
C17 . C18 . 1.367(6) yes
C17 . C22 . 1.377(6) yes
C18 . C19 . 1.389(7) yes
C18 . H181 . 0.922 no
C19 . C20 . 1.352(8) yes
C19 . H191 . 0.921 no
C20 . C21 . 1.357(8) yes
C20 . H201 . 0.924 no
C21 . C22 . 1.380(7) yes
C21 . H211 . 0.941 no
C22 . H221 . 0.934 no
Pd23 . P24 . 2.2480(11) yes
Pd23 . Cl29 . 2.3238(12) yes
Pd23 . Cl32 . 2.3386(12) yes
Pd23 . P1 . 2.2609(11) yes
P24 . C37 . 1.822(4) yes
P24 . C43 . 1.823(4) yes
P24 . C67 . 1.809(5) yes
N36 . N50 . 1.311(5) yes
N36 . C52 . 1.355(5) yes
C37 . C38 . 1.397(6) yes
C37 . C42 . 1.386(6) yes
C38 . C39 . 1.370(6) yes
C38 . H381 . 0.935 no
C39 . C40 . 1.368(7) yes
C39 . H391 . 0.932 no
C40 . C41 . 1.384(7) yes
C40 . H401 . 0.935 no
C41 . C42 . 1.381(6) yes
C41 . H411 . 0.926 no
C42 . H421 . 0.924 no
C43 . N44 . 1.351(5) yes
C43 . C47 . 1.390(6) yes
N44 . N45 . 1.311(5) yes
N45 . N46 . 1.345(5) yes
N46 . C47 . 1.357(5) yes
N46 . C60 . 1.477(5) yes
C47 . C48 . 1.444(5) yes
C48 . N49 . 1.363(5) yes
C48 . C52 . 1.379(5) yes
N49 . N50 . 1.349(5) yes
N49 . C53 . 1.478(5) yes
C52 . P1 . 1.821(4) yes
C53 . C54 . 1.496(6) yes
C53 . H531 . 0.976 no
C53 . H532 . 0.962 no
C54 . C55 . 1.382(6) yes
C54 . C59 . 1.372(7) yes
C55 . C56 . 1.386(6) yes
C55 . H551 . 0.926 no
C56 . C57 . 1.371(7) yes
C56 . H561 . 0.930 no
C57 . C58 . 1.372(8) yes
C57 . H571 . 0.930 no
C58 . C59 . 1.381(8) yes
C58 . H581 . 0.936 no
C59 . H591 . 0.926 no
C60 . C61 . 1.504(6) yes
C60 . H601 . 0.961 no
C60 . H602 . 0.962 no
C61 . C62 . 1.366(7) yes
C61 . C66 . 1.376(7) yes
C62 . C63 . 1.378(8) yes
C62 . H621 . 0.934 no
C63 . C64 . 1.371(10) yes
C63 . H631 . 0.936 no
C64 . C65 . 1.372(9) yes
C64 . H641 . 0.927 no
C65 . C66 . 1.402(8) yes
C65 . H651 . 0.925 no
C66 . H661 . 0.936 no
C67 . C68 . 1.387(6) yes
C67 . C72 . 1.392(6) yes
C68 . C69 . 1.379(7) yes
C68 . H681 . 0.936 no
C69 . C70 . 1.380(8) yes
C69 . H691 . 0.927 no
C70 . C71 . 1.378(8) yes
C70 . H701 . 0.938 no
C71 . C72 . 1.398(7) yes
C71 . H711 . 0.941 no
C72 . H721 . 0.930 no
Cl73 . C74 . 1.739(5) yes
C74 . Cl75 . 1.742(6) yes
C74 . Cl76 . 1.737(6) yes
C74 . H741 . 0.971 no
Cl77 . C78 . 1.715(7) yes
C78 . Cl79 . 1.745(8) yes
C78 . Cl1 . 1.712(6) yes
C78 . H781 . 0.974 no
C82 . N83 . 1.360(5) yes
C82 . C86 . 1.377(5) yes
N83 . N84 . 1.311(5) yes
N84 . N85 . 1.345(5) yes
N85 . C86 . 1.355(5) yes
N85 . C99 . 1.472(5) yes
C86 . C87 . 1.454(5) yes
C87 . N88 . 1.355(5) yes
C87 . C91 . 1.381(5) yes
N88 . N89 . 1.347(5) yes
N88 . C92 . 1.483(5) yes
N89 . N90 . 1.308(5) yes
N90 . C91 . 1.365(5) yes
C92 . C93 . 1.503(6) yes
C92 . H921 . 0.968 no
C92 . H922 . 0.961 no
C93 . C94 . 1.383(7) yes
C93 . C98 . 1.373(7) yes
C94 . C95 . 1.379(7) yes
C94 . H941 . 0.924 no
C95 . C96 . 1.371(9) yes
C95 . H951 . 0.934 no
C96 . C97 . 1.352(9) yes
C96 . H961 . 0.934 no
C97 . C98 . 1.395(8) yes
C97 . H971 . 0.924 no
C98 . H981 . 0.924 no
C99 . C100 . 1.509(6) yes
C99 . H991 . 0.958 no
C99 . H992 . 0.961 no
C100 . C101 . 1.373(6) yes
C100 . C105 . 1.376(7) yes
C101 . C102 . 1.392(7) yes
C101 . H1011 . 0.934 no
C102 . C103 . 1.353(7) yes
C102 . H1021 . 0.943 no
C103 . C104 . 1.358(8) yes
C103 . H1031 . 0.930 no
C104 . C105 . 1.386(8) yes
C104 . H1041 . 0.944 no
C105 . H1051 . 0.940 no
C106 . C107 . 1.402(6) yes
C106 . C111 . 1.394(6) yes
C107 . C108 . 1.385(7) yes
C107 . H1071 . 0.927 no
C108 . C109 . 1.374(7) yes
C108 . H1081 . 0.928 no
C109 . C110 . 1.372(7) yes
C109 . H1091 . 0.934 no
C110 . C111 . 1.369(6) yes
C110 . H1101 . 0.929 no
C111 . H1111 . 0.925 no
C112 . C113 . 1.388(6) yes
C112 . C117 . 1.384(6) yes
C113 . C114 . 1.383(6) yes
C113 . H1131 . 0.935 no
C114 . C115 . 1.374(7) yes
C114 . H1141 . 0.927 no
C115 . C116 . 1.371(8) yes
C115 . H1151 . 0.928 no
C116 . C117 . 1.395(6) yes
C116 . H1161 . 0.931 no
C117 . H1171 . 0.933 no
C118 . C119 . 1.392(6) yes
C118 . C123 . 1.379(6) yes
C118 . H1181 . 0.922 no
C119 . C120 . 1.381(6) yes
C120 . C121 . 1.390(6) yes
C120 . H1201 . 0.944 no
C121 . C122 . 1.376(7) yes
C121 . H1211 . 0.922 no
C122 . C123 . 1.377(7) yes
C122 . H1221 . 0.928 no
C123 . H1231 . 0.928 no
C124 . C125 . 1.383(6) yes
C124 . C129 . 1.403(6) yes
C124 . P1 . 1.810(4) yes
C125 . C126 . 1.370(7) yes
C125 . H1251 . 0.931 no
C126 . C127 . 1.366(8) yes
C126 . H1261 . 0.934 no
C127 . C128 . 1.379(7) yes
C127 . H1271 . 0.923 no
C128 . C129 . 1.367(6) yes
C128 . H1281 . 0.928 no
C129 . H1291 . 0.933 no
C130 . C131 . 1.364(6) yes
C130 . C135 . 1.392(6) yes
C130 . H1301 . 0.928 no
C131 . C132 . 1.377(6) yes
C131 . P1 . 1.822(4) yes
C132 . C133 . 1.387(7) yes
C132 . H1321 . 0.930 no
C133 . C134 . 1.346(8) yes
C133 . H1331 . 0.936 no
C134 . C135 . 1.350(8) yes
C134 . H1341 . 0.934 no
C135 . H1351 . 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
Cl3 . Pd1 . Cl7 . 88.72(4) yes
Cl3 . Pd1 . P10 . 173.08(4) yes
Cl7 . Pd1 . P10 . 84.39(4) yes
Cl3 . Pd1 . P15 . 90.93(4) yes
Cl7 . Pd1 . P15 . 178.11(4) yes
P10 . Pd1 . P15 . 95.93(4) yes
Pd1 . P10 . C17 . 111.76(13) yes
Pd1 . P10 . C91 . 119.92(12) yes
C17 . P10 . C91 . 100.00(17) yes
Pd1 . P10 . C119 . 113.24(13) yes
C17 . P10 . C119 . 107.80(19) yes
C91 . P10 . C119 . 102.72(18) yes
Pd1 . P15 . C82 . 113.76(14) yes
Pd1 . P15 . C106 . 112.52(13) yes
C82 . P15 . C106 . 106.02(19) yes
Pd1 . P15 . C112 . 116.54(13) yes
C82 . P15 . C112 . 103.86(18) yes
C106 . P15 . C112 . 102.96(19) yes
P10 . C17 . C18 . 118.5(3) yes
P10 . C17 . C22 . 122.6(3) yes
C18 . C17 . C22 . 118.8(4) yes
C17 . C18 . C19 . 119.9(5) yes
C17 . C18 . H181 . 119.2 no
C19 . C18 . H181 . 120.9 no
C18 . C19 . C20 . 121.1(5) yes
C18 . C19 . H191 . 119.5 no
C20 . C19 . H191 . 119.4 no
C19 . C20 . C21 . 119.0(5) yes
C19 . C20 . H201 . 120.6 no
C21 . C20 . H201 . 120.3 no
C20 . C21 . C22 . 120.9(5) yes
C20 . C21 . H211 . 119.2 no
C22 . C21 . H211 . 119.9 no
C21 . C22 . C17 . 120.2(5) yes
C21 . C22 . H221 . 120.0 no
C17 . C22 . H221 . 119.8 no
P24 . Pd23 . Cl29 . 91.93(4) yes
P24 . Pd23 . Cl32 . 173.48(5) yes
Cl29 . Pd23 . Cl32 . 89.90(5) yes
P24 . Pd23 . P1 . 94.33(4) yes
Cl29 . Pd23 . P1 . 170.68(5) yes
Cl32 . Pd23 . P1 . 84.64(4) yes
Pd23 . P24 . C37 . 116.74(14) yes
Pd23 . P24 . C43 . 111.94(13) yes
C37 . P24 . C43 . 102.08(18) yes
Pd23 . P24 . C67 . 113.44(15) yes
C37 . P24 . C67 . 104.8(2) yes
C43 . P24 . C67 . 106.8(2) yes
N50 . N36 . C52 . 108.6(3) yes
P24 . C37 . C38 . 119.6(3) yes
P24 . C37 . C42 . 120.9(3) yes
C38 . C37 . C42 . 119.5(4) yes
C37 . C38 . C39 . 119.6(5) yes
C37 . C38 . H381 . 120.2 no
C39 . C38 . H381 . 120.2 no
C38 . C39 . C40 . 121.4(5) yes
C38 . C39 . H391 . 119.4 no
C40 . C39 . H391 . 119.2 no
C39 . C40 . C41 . 119.1(5) yes
C39 . C40 . H401 . 120.7 no
C41 . C40 . H401 . 120.3 no
C40 . C41 . C42 . 120.8(5) yes
C40 . C41 . H411 . 119.3 no
C42 . C41 . H411 . 119.8 no
C37 . C42 . C41 . 119.6(5) yes
C37 . C42 . H421 . 120.2 no
C41 . C42 . H421 . 120.3 no
P24 . C43 . N44 . 122.4(3) yes
P24 . C43 . C47 . 128.7(3) yes
N44 . C43 . C47 . 108.6(4) yes
C43 . N44 . N45 . 108.8(4) yes
N44 . N45 . N46 . 108.1(3) yes
N45 . N46 . C47 . 110.4(3) yes
N45 . N46 . C60 . 119.9(3) yes
C47 . N46 . C60 . 129.6(4) yes
C43 . C47 . N46 . 104.0(4) yes
C43 . C47 . C48 . 126.8(4) yes
N46 . C47 . C48 . 129.2(4) yes
C47 . C48 . N49 . 128.5(4) yes
C47 . C48 . C52 . 126.4(4) yes
N49 . C48 . C52 . 104.2(3) yes
C48 . N49 . N50 . 110.0(3) yes
C48 . N49 . C53 . 131.2(4) yes
N50 . N49 . C53 . 118.6(4) yes
N49 . N50 . N36 . 108.2(3) yes
C48 . C52 . N36 . 108.9(3) yes
C48 . C52 . P1 . 127.5(3) yes
N36 . C52 . P1 . 123.3(3) yes
N49 . C53 . C54 . 115.1(4) yes
N49 . C53 . H531 . 107.3 no
C54 . C53 . H531 . 109.8 no
N49 . C53 . H532 . 108.3 no
C54 . C53 . H532 . 106.6 no
H531 . C53 . H532 . 109.8 no
C53 . C54 . C55 . 120.3(4) yes
C53 . C54 . C59 . 120.7(5) yes
C55 . C54 . C59 . 118.9(5) yes
C54 . C55 . C56 . 120.6(4) yes
C54 . C55 . H551 . 119.6 no
C56 . C55 . H551 . 119.8 no
C55 . C56 . C57 . 119.9(5) yes
C55 . C56 . H561 . 120.3 no
C57 . C56 . H561 . 119.8 no
C56 . C57 . C58 . 119.5(5) yes
C56 . C57 . H571 . 120.3 no
C58 . C57 . H571 . 120.1 no
C57 . C58 . C59 . 120.6(5) yes
C57 . C58 . H581 . 119.5 no
C59 . C58 . H581 . 119.9 no
C58 . C59 . C54 . 120.4(5) yes
C58 . C59 . H591 . 120.4 no
C54 . C59 . H591 . 119.2 no
N46 . C60 . C61 . 114.2(4) yes
N46 . C60 . H601 . 107.8 no
C61 . C60 . H601 . 108.3 no
N46 . C60 . H602 . 108.1 no
C61 . C60 . H602 . 108.2 no
H601 . C60 . H602 . 110.2 no
C60 . C61 . C62 . 117.3(5) yes
C60 . C61 . C66 . 122.2(4) yes
C62 . C61 . C66 . 120.2(5) yes
C61 . C62 . C63 . 119.8(6) yes
C61 . C62 . H621 . 120.1 no
C63 . C62 . H621 . 120.1 no
C62 . C63 . C64 . 120.8(6) yes
C62 . C63 . H631 . 119.3 no
C64 . C63 . H631 . 119.8 no
C63 . C64 . C65 . 119.9(6) yes
C63 . C64 . H641 . 120.5 no
C65 . C64 . H641 . 119.5 no
C64 . C65 . C66 . 119.4(6) yes
C64 . C65 . H651 . 121.3 no
C66 . C65 . H651 . 119.3 no
C65 . C66 . C61 . 119.8(6) yes
C65 . C66 . H661 . 119.9 no
C61 . C66 . H661 . 120.3 no
P24 . C67 . C68 . 121.6(3) yes
P24 . C67 . C72 . 117.9(4) yes
C68 . C67 . C72 . 120.2(4) yes
C67 . C68 . C69 . 119.6(5) yes
C67 . C68 . H681 . 120.3 no
C69 . C68 . H681 . 120.1 no
C68 . C69 . C70 . 121.0(5) yes
C68 . C69 . H691 . 119.9 no
C70 . C69 . H691 . 119.1 no
C69 . C70 . C71 . 119.5(5) yes
C69 . C70 . H701 . 120.4 no
C71 . C70 . H701 . 120.0 no
C70 . C71 . C72 . 120.6(5) yes
C70 . C71 . H711 . 121.0 no
C72 . C71 . H711 . 118.4 no
C71 . C72 . C67 . 119.0(5) yes
C71 . C72 . H721 . 120.0 no
C67 . C72 . H721 . 120.9 no
Cl73 . C74 . Cl75 . 108.7(3) yes
Cl73 . C74 . Cl76 . 111.8(3) yes
Cl75 . C74 . Cl76 . 110.5(3) yes
Cl73 . C74 . H741 . 109.0 no
Cl75 . C74 . H741 . 107.8 no
Cl76 . C74 . H741 . 108.8 no
Cl77 . C78 . Cl79 . 111.1(3) yes
Cl77 . C78 . Cl1 . 108.4(4) yes
Cl79 . C78 . Cl1 . 115.3(5) yes
Cl77 . C78 . H781 . 107.3 no
Cl79 . C78 . H781 . 107.0 no
Cl1 . C78 . H781 . 107.5 no
P15 . C82 . N83 . 124.5(3) yes
P15 . C82 . C86 . 126.8(3) yes
N83 . C82 . C86 . 108.4(4) yes
C82 . N83 . N84 . 108.4(3) yes
N83 . N84 . N85 . 108.5(3) yes
N84 . N85 . C86 . 109.8(3) yes
N84 . N85 . C99 . 119.7(3) yes
C86 . N85 . C99 . 130.1(3) yes
C82 . C86 . N85 . 105.0(3) yes
C82 . C86 . C87 . 128.0(4) yes
N85 . C86 . C87 . 127.0(3) yes
C86 . C87 . N88 . 125.6(3) yes
C86 . C87 . C91 . 128.9(3) yes
N88 . C87 . C91 . 104.7(3) yes
C87 . N88 . N89 . 110.2(3) yes
C87 . N88 . C92 . 130.4(3) yes
N89 . N88 . C92 . 119.3(3) yes
N88 . N89 . N90 . 108.2(3) yes
N89 . N90 . C91 . 108.7(3) yes
P10 . C91 . C87 . 129.9(3) yes
P10 . C91 . N90 . 121.8(3) yes
C87 . C91 . N90 . 108.2(3) yes
N88 . C92 . C93 . 113.1(3) yes
N88 . C92 . H921 . 107.6 no
C93 . C92 . H921 . 109.0 no
N88 . C92 . H922 . 108.6 no
C93 . C92 . H922 . 108.9 no
H921 . C92 . H922 . 109.6 no
C92 . C93 . C94 . 119.7(4) yes
C92 . C93 . C98 . 121.5(4) yes
C94 . C93 . C98 . 118.7(5) yes
C93 . C94 . C95 . 120.5(5) yes
C93 . C94 . H941 . 119.1 no
C95 . C94 . H941 . 120.4 no
C94 . C95 . C96 . 119.4(6) yes
C94 . C95 . H951 . 120.0 no
C96 . C95 . H951 . 120.6 no
C95 . C96 . C97 . 121.4(5) yes
C95 . C96 . H961 . 119.3 no
C97 . C96 . H961 . 119.3 no
C96 . C97 . C98 . 119.0(6) yes
C96 . C97 . H971 . 120.3 no
C98 . C97 . H971 . 120.7 no
C97 . C98 . C93 . 120.9(5) yes
C97 . C98 . H981 . 120.0 no
C93 . C98 . H981 . 119.1 no
N85 . C99 . C100 . 110.6(3) yes
N85 . C99 . H991 . 109.0 no
C100 . C99 . H991 . 110.3 no
N85 . C99 . H992 . 109.3 no
C100 . C99 . H992 . 109.0 no
H991 . C99 . H992 . 108.5 no
C99 . C100 . C101 . 121.7(4) yes
C99 . C100 . C105 . 120.2(4) yes
C101 . C100 . C105 . 118.1(5) yes
C100 . C101 . C102 . 120.8(4) yes
C100 . C101 . H1011 . 119.7 no
C102 . C101 . H1011 . 119.5 no
C101 . C102 . C103 . 120.2(5) yes
C101 . C102 . H1021 . 119.4 no
C103 . C102 . H1021 . 120.4 no
C102 . C103 . C104 . 119.6(5) yes
C102 . C103 . H1031 . 119.5 no
C104 . C103 . H1031 . 120.9 no
C103 . C104 . C105 . 120.5(6) yes
C103 . C104 . H1041 . 119.4 no
C105 . C104 . H1041 . 120.1 no
C104 . C105 . C100 . 120.6(5) yes
C104 . C105 . H1051 . 120.7 no
C100 . C105 . H1051 . 118.8 no
P15 . C106 . C107 . 117.5(3) yes
P15 . C106 . C111 . 122.8(3) yes
C107 . C106 . C111 . 118.8(4) yes
C106 . C107 . C108 . 119.8(4) yes
C106 . C107 . H1071 . 120.2 no
C108 . C107 . H1071 . 120.0 no
C107 . C108 . C109 . 120.2(5) yes
C107 . C108 . H1081 . 118.8 no
C109 . C108 . H1081 . 121.1 no
C108 . C109 . C110 . 120.1(5) yes
C108 . C109 . H1091 . 120.5 no
C110 . C109 . H1091 . 119.4 no
C109 . C110 . C111 . 120.8(5) yes
C109 . C110 . H1101 . 119.3 no
C111 . C110 . H1101 . 119.8 no
C106 . C111 . C110 . 120.2(4) yes
C106 . C111 . H1111 . 118.8 no
C110 . C111 . H1111 . 121.0 no
P15 . C112 . C113 . 120.9(3) yes
P15 . C112 . C117 . 120.1(3) yes
C113 . C112 . C117 . 118.8(4) yes
C112 . C113 . C114 . 120.7(5) yes
C112 . C113 . H1131 . 119.5 no
C114 . C113 . H1131 . 119.8 no
C113 . C114 . C115 . 119.5(5) yes
C113 . C114 . H1141 . 120.3 no
C115 . C114 . H1141 . 120.2 no
C114 . C115 . C116 . 121.1(5) yes
C114 . C115 . H1151 . 119.9 no
C116 . C115 . H1151 . 119.0 no
C115 . C116 . C117 . 119.2(5) yes
C115 . C116 . H1161 . 120.7 no
C117 . C116 . H1161 . 120.0 no
C116 . C117 . C112 . 120.6(5) yes
C116 . C117 . H1171 . 120.3 no
C112 . C117 . H1171 . 119.1 no
C119 . C118 . C123 . 119.9(4) yes
C119 . C118 . H1181 . 120.8 no
C123 . C118 . H1181 . 119.3 no
P10 . C119 . C118 . 120.5(3) yes
P10 . C119 . C120 . 119.8(3) yes
C118 . C119 . C120 . 119.6(4) yes
C119 . C120 . C121 . 120.1(4) yes
C119 . C120 . H1201 . 119.4 no
C121 . C120 . H1201 . 120.5 no
C120 . C121 . C122 . 119.8(4) yes
C120 . C121 . H1211 . 119.7 no
C122 . C121 . H1211 . 120.5 no
C121 . C122 . C123 . 120.2(4) yes
C121 . C122 . H1221 . 120.3 no
C123 . C122 . H1221 . 119.5 no
C118 . C123 . C122 . 120.3(4) yes
C118 . C123 . H1231 . 119.5 no
C122 . C123 . H1231 . 120.2 no
C125 . C124 . C129 . 118.1(4) yes
C125 . C124 . P1 . 120.1(3) yes
C129 . C124 . P1 . 121.7(3) yes
C124 . C125 . C126 . 120.9(5) yes
C124 . C125 . H1251 . 118.2 no
C126 . C125 . H1251 . 120.9 no
C125 . C126 . C127 . 120.5(5) yes
C125 . C126 . H1261 . 119.8 no
C127 . C126 . H1261 . 119.7 no
C126 . C127 . C128 . 119.7(5) yes
C126 . C127 . H1271 . 120.5 no
C128 . C127 . H1271 . 119.8 no
C127 . C128 . C129 . 120.4(5) yes
C127 . C128 . H1281 . 119.4 no
C129 . C128 . H1281 . 120.1 no
C124 . C129 . C128 . 120.3(4) yes
C124 . C129 . H1291 . 119.1 no
C128 . C129 . H1291 . 120.6 no
C131 . C130 . C135 . 119.9(5) yes
C131 . C130 . H1301 . 119.7 no
C135 . C130 . H1301 . 120.3 no
C130 . C131 . C132 . 119.1(4) yes
C130 . C131 . P1 . 118.7(3) yes
C132 . C131 . P1 . 122.1(4) yes
C131 . C132 . C133 . 119.4(5) yes
C131 . C132 . H1321 . 119.9 no
C133 . C132 . H1321 . 120.7 no
C132 . C133 . C134 . 121.4(5) yes
C132 . C133 . H1331 . 119.0 no
C134 . C133 . H1331 . 119.6 no
C133 . C134 . C135 . 119.3(5) yes
C133 . C134 . H1341 . 120.9 no
C135 . C134 . H1341 . 119.9 no
C130 . C135 . C134 . 120.8(5) yes
C130 . C135 . H1351 . 119.8 no
C134 . C135 . H1351 . 119.4 no
C131 . P1 . C52 . 100.53(18) yes
C131 . P1 . C124 . 110.66(19) yes
C52 . P1 . C124 . 102.03(19) yes
C131 . P1 . Pd23 . 110.11(14) yes
C52 . P1 . Pd23 . 120.20(13) yes
C124 . P1 . Pd23 . 112.45(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
C22 . H221 . C120 . 135.01(15) 0.934 2.545 3.273(7) yes
C59 . H591 . N44 2_676 150.21(16) 0.926 2.513 3.349(7) yes
C74 . H741 . N89 4_656 150.11(17) 0.971 2.345 3.223(7) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 21/01/13 at 14:15:13
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) H   ( 922,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) 
RIDE C   (  95,X'S) H   ( 951,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) 
RIDE C   (  97,X'S) H   ( 971,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) H   ( 992,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 121,X'S) H   (1211,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 21/01/13 at 14:15:13
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

_vrf_PLAT029_13.1                
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.852 Note  
RESPONSE: inherently weak scatterer
;
####################################################################### 
# 
# 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_13.11
_database_code_depnum_ccdc_archive 'CCDC 1031968'
_audit_update_record             
;
2014-10-31 deposited with the CCDC.
2015-06-16 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          ?
#--------------------------------------------------------------- 
_cell_length_a                   22.5985(2)
_cell_length_b                   10.81823(12)
_cell_length_c                   20.4451(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.0860(10)
_cell_angle_gamma                90
_cell_volume                     4998.32(9)
_cell_measurement_reflns_used    14336
_cell_measurement_theta_min      2.1590
_cell_measurement_theta_max      67.4550


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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd 0.1215 3.9337 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'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

_chemical_formula_sum            'C50 H46 Cl2 N10 P2 Pd'
_chemical_formula_moiety         'C42 H34 Cl2 N6 P2 Pd, 4(C2 H3 N)'
_chemical_compound_source        ?
_chemical_formula_weight         1026.21


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            'yellow transparent'
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.250
_exptl_absorpt_correction_T_min  0.18829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2104
_exptl_absorpt_coefficient_mu    4.937
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 16.0143

_diffrn_measurement_device       Area
_diffrn_radiation_wavelength     1.54180


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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_orient_matrix_UB_11      0.0604893000
_diffrn_orient_matrix_UB_12      0.0305777000
_diffrn_orient_matrix_UB_13      0.0308878000
_diffrn_orient_matrix_UB_21      0.0142212000
_diffrn_orient_matrix_UB_22      -0.1390091000
_diffrn_orient_matrix_UB_23      0.0045932000
_diffrn_orient_matrix_UB_31      0.0280727000
_diffrn_orient_matrix_UB_32      0.0044655000
_diffrn_orient_matrix_UB_33      -0.0685592000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -106.00  -40.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.6428 -179.0000 -150.0000 66

#__ type_ start__ end____ width___ exp.time_
  2 omega -102.00  -13.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.6428  -57.0000  120.0000 89

#__ type_ start__ end____ width___ exp.time_
  3 omega  -45.00    5.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.6428   57.0000   60.0000 50

#__ type_ start__ end____ width___ exp.time_
  4 omega  -45.00  -17.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -120.0000 28

#__ type_ start__ end____ width___ exp.time_
  5 omega -113.00  -87.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000 -140.0000   48.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega   39.00   91.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -25.0000  150.0000 52

#__ type_ start__ end____ width___ exp.time_
  7 omega  126.00  172.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   25.0000  150.0000 46

#__ type_ start__ end____ width___ exp.time_
  8 omega   50.00   76.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -50.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   78.00  142.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   64.0000 -120.0000 64

#__ type_ start__ end____ width___ exp.time_
 10 omega   93.00  119.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  179.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 11 omega   49.00  103.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -112.0000 -180.0000 54

#__ type_ start__ end____ width___ exp.time_
 12 omega   74.00  108.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   25.0000  150.0000 34

#__ type_ start__ end____ width___ exp.time_
 13 omega  108.00  134.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  112.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 14 omega  106.00  157.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  112.0000  120.0000 51

#__ type_ start__ end____ width___ exp.time_
 15 omega   78.00  149.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   64.0000  -60.0000 71

#__ type_ start__ end____ width___ exp.time_
 16 omega   33.00  109.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -64.0000 -180.0000 76

#__ type_ start__ end____ width___ exp.time_
 17 omega   45.00   87.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -50.0000 -150.0000 42

#__ type_ start__ end____ width___ exp.time_
 18 omega   64.00   90.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  179.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega  101.00  158.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  112.0000  -60.0000 57

#__ type_ start__ end____ width___ exp.time_
 20 omega   34.00   92.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -38.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
 21 omega   91.00  116.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -112.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
 22 omega  144.00  170.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   50.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 23 omega   96.00  128.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   50.0000  -30.0000 32

#__ type_ start__ end____ width___ exp.time_
 24 omega  -55.00   35.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.6428   57.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
 25 omega   -4.00   76.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6428  -99.0000  120.0000 80

#__ type_ start__ end____ width___ exp.time_
 26 omega   13.00  102.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6428   57.0000  -90.0000 89

#__ type_ start__ end____ width___ exp.time_
 27 omega   13.00  102.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6428   57.0000   30.0000 89

#__ type_ start__ end____ width___ exp.time_
 28 omega   74.00  172.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   38.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
 29 omega   28.00  116.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -112.0000    0.0000 88

#__ type_ start__ end____ width___ exp.time_
 30 omega   30.00  104.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -50.0000    0.0000 74

#__ type_ start__ end____ width___ exp.time_
 31 omega   74.00  172.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   38.0000   30.0000 98

#__ type_ start__ end____ width___ exp.time_
 32 omega   70.00  170.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   77.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
 33 omega   74.00  172.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   38.0000 -150.0000 98

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            42569
_reflns_number_total             8878
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.0540
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8878 
# Theoretical number of reflections is about 18015 


_diffrn_reflns_theta_min         3.912
_diffrn_reflns_theta_max         67.488
_diffrn_measured_fraction_theta_max 0.986

_diffrn_reflns_theta_full        62.764
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -26
_reflns_limit_h_max              27
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              24


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

_refine_diff_density_min         -0.63
_refine_diff_density_max         0.74


_refine_ls_number_reflns         7634
_refine_ls_number_restraints     0
_refine_ls_number_parameters     586
_refine_ls_wR_factor_ref         0.0408
_refine_ls_goodness_of_fit_ref   0.9571
_refine_ls_shift/su_max          0.0014202
_refine_ls_shift/su_mean         0.0000394

_refine_ls_R_factor_all          0.0487
_refine_ls_wR_factor_all         0.0494


_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7634
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_gt          0.0408



_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: 
 15.5 -22.6 14.2 -8.79 
;


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 0.245140(6) 0.222739(12) 0.497371(6) 0.0218 1.0000 Uani . . . . . .
Cl2 Cl 0.20097(3) 0.06818(5) 0.56005(3) 0.0372 1.0000 Uani . . . . . .
Cl3 Cl 0.28559(2) 0.07144(5) 0.42904(3) 0.0360 1.0000 Uani . . . . . .
P4 P 0.19676(2) 0.36302(4) 0.55870(2) 0.0200 1.0000 Uani . . . . . .
C5 C 0.17815(8) 0.50813(18) 0.51880(9) 0.0226 1.0000 Uani . . . . . .
N6 N 0.12149(8) 0.54231(18) 0.50445(10) 0.0323 1.0000 Uani . . . . . .
N7 N 0.12270(8) 0.64931(18) 0.47464(10) 0.0352 1.0000 Uani . . . . . .
N8 N 0.17953(7) 0.68443(16) 0.46961(9) 0.0260 1.0000 Uani . . . . . .
C9 C 0.21523(8) 0.59938(18) 0.49704(9) 0.0215 1.0000 Uani . . . . . .
C10 C 0.27992(8) 0.60019(18) 0.49784(9) 0.0226 1.0000 Uani . . . . . .
N11 N 0.31534(7) 0.68882(16) 0.52256(9) 0.0275 1.0000 Uani . . . . . .
N12 N 0.37249(8) 0.65589(18) 0.51587(10) 0.0366 1.0000 Uani . . . . . .
N13 N 0.37389(8) 0.54616(18) 0.48850(10) 0.0338 1.0000 Uani . . . . . .
C14 C 0.31721(8) 0.50852(18) 0.47661(10) 0.0236 1.0000 Uani . . . . . .
P15 P 0.29895(2) 0.36056(4) 0.43953(2) 0.0210 1.0000 Uani . . . . . .
C16 C 0.26416(8) 0.39835(19) 0.36237(10) 0.0257 1.0000 Uani . . . . . .
C17 C 0.21355(10) 0.3327(2) 0.34358(12) 0.0377 1.0000 Uani . . . . . .
C18 C 0.18646(12) 0.3591(3) 0.28429(13) 0.0490 1.0000 Uani . . . . . .
C19 C 0.21024(12) 0.4470(3) 0.24345(12) 0.0486 1.0000 Uani . . . . . .
C20 C 0.25950(12) 0.5126(3) 0.26214(13) 0.0503 1.0000 Uani . . . . . .
C21 C 0.28642(10) 0.4902(2) 0.32174(12) 0.0388 1.0000 Uani . . . . . .
H211 H 0.3183 0.5361 0.3348 0.0459 1.0000 Uiso R . . . . .
H201 H 0.2745 0.5717 0.2345 0.0607 1.0000 Uiso R . . . . .
H191 H 0.1924 0.4621 0.2035 0.0574 1.0000 Uiso R . . . . .
H181 H 0.1524 0.3154 0.2720 0.0596 1.0000 Uiso R . . . . .
H171 H 0.1984 0.2694 0.3693 0.0443 1.0000 Uiso R . . . . .
C22 C 0.37304(9) 0.30070(19) 0.42450(11) 0.0260 1.0000 Uani . . . . . .
C23 C 0.39677(10) 0.2887(2) 0.36255(13) 0.0365 1.0000 Uani . . . . . .
C24 C 0.45379(11) 0.2418(3) 0.35575(15) 0.0483 1.0000 Uani . . . . . .
C25 C 0.48668(11) 0.2096(3) 0.40895(16) 0.0511 1.0000 Uani . . . . . .
C26 C 0.46298(12) 0.2212(2) 0.47134(15) 0.0486 1.0000 Uani . . . . . .
C27 C 0.40617(10) 0.2657(2) 0.47895(12) 0.0365 1.0000 Uani . . . . . .
H271 H 0.3906 0.2732 0.5206 0.0434 1.0000 Uiso R . . . . .
H261 H 0.4852 0.1983 0.5083 0.0580 1.0000 Uiso R . . . . .
H251 H 0.5246 0.1799 0.4047 0.0605 1.0000 Uiso R . . . . .
H241 H 0.4701 0.2331 0.3141 0.0573 1.0000 Uiso R . . . . .
H231 H 0.3756 0.3117 0.3258 0.0434 1.0000 Uiso R . . . . .
C28 C 0.29847(10) 0.8089(2) 0.55198(12) 0.0328 1.0000 Uani . . . . . .
C29 C 0.34026(9) 0.8505(2) 0.60498(11) 0.0304 1.0000 Uani . . . . . .
C30 C 0.35620(11) 0.7756(3) 0.65656(14) 0.0450 1.0000 Uani . . . . . .
C31 C 0.39287(13) 0.8228(4) 0.70563(14) 0.0646 1.0000 Uani . . . . . .
C32 C 0.41264(12) 0.9429(4) 0.70251(18) 0.0725 1.0000 Uani . . . . . .
C33 C 0.39690(12) 1.0163(3) 0.65148(19) 0.0691 1.0000 Uani . . . . . .
C34 C 0.36106(10) 0.9711(2) 0.60263(14) 0.0456 1.0000 Uani . . . . . .
H341 H 0.3510 1.0218 0.5672 0.0549 1.0000 Uiso R . . . . .
H331 H 0.4107 1.0988 0.6492 0.0832 1.0000 Uiso R . . . . .
H321 H 0.4365 0.9731 0.7360 0.0875 1.0000 Uiso R . . . . .
H311 H 0.4028 0.7728 0.7398 0.0763 1.0000 Uiso R . . . . .
H301 H 0.3418 0.6964 0.6584 0.0531 1.0000 Uiso R . . . . .
H282 H 0.2971 0.8704 0.5188 0.0385 1.0000 Uiso R . . . . .
H281 H 0.2593 0.8005 0.5702 0.0386 1.0000 Uiso R . . . . .
C35 C 0.19543(10) 0.8036(2) 0.43861(11) 0.0296 1.0000 Uani . . . . . .
C36 C 0.15972(9) 0.8279(2) 0.37799(11) 0.0304 1.0000 Uani . . . . . .
C37 C 0.13543(10) 0.9431(2) 0.36690(14) 0.0429 1.0000 Uani . . . . . .
C38 C 0.10473(12) 0.9657(3) 0.30760(16) 0.0588 1.0000 Uani . . . . . .
C39 C 0.09983(13) 0.8742(4) 0.26234(16) 0.0664 1.0000 Uani . . . . . .
C40 C 0.12338(15) 0.7608(3) 0.27308(15) 0.0624 1.0000 Uani . . . . . .
C41 C 0.15338(12) 0.7372(3) 0.33030(13) 0.0458 1.0000 Uani . . . . . .
H411 H 0.1700 0.6583 0.3374 0.0557 1.0000 Uiso R . . . . .
H401 H 0.1185 0.6980 0.2415 0.0759 1.0000 Uiso R . . . . .
H391 H 0.0787 0.8883 0.2227 0.0804 1.0000 Uiso R . . . . .
H381 H 0.0884 1.0417 0.3017 0.0714 1.0000 Uiso R . . . . .
H371 H 0.1382 1.0024 0.3988 0.0487 1.0000 Uiso R . . . . .
H352 H 0.1896 0.8689 0.4696 0.0363 1.0000 Uiso R . . . . .
H351 H 0.2360 0.7993 0.4287 0.0358 1.0000 Uiso R . . . . .
C42 C 0.23775(8) 0.40481(19) 0.63132(9) 0.0251 1.0000 Uani . . . . . .
C43 C 0.22481(10) 0.5100(2) 0.66720(11) 0.0364 1.0000 Uani . . . . . .
C44 C 0.25480(12) 0.5324(3) 0.72514(12) 0.0471 1.0000 Uani . . . . . .
C45 C 0.29755(12) 0.4514(3) 0.74667(12) 0.0518 1.0000 Uani . . . . . .
C46 C 0.31187(13) 0.3481(3) 0.71073(13) 0.0550 1.0000 Uani . . . . . .
C47 C 0.28188(11) 0.3237(2) 0.65292(12) 0.0382 1.0000 Uani . . . . . .
H471 H 0.2901 0.2522 0.6290 0.0455 1.0000 Uiso R . . . . .
H461 H 0.3411 0.2942 0.7251 0.0659 1.0000 Uiso R . . . . .
H451 H 0.3167 0.4672 0.7864 0.0632 1.0000 Uiso R . . . . .
H441 H 0.2455 0.6027 0.7490 0.0555 1.0000 Uiso R . . . . .
H431 H 0.1967 0.5647 0.6536 0.0435 1.0000 Uiso R . . . . .
C48 C 0.12376(9) 0.3119(2) 0.58404(11) 0.0271 1.0000 Uani . . . . . .
C49 C 0.08403(10) 0.2740(2) 0.53571(13) 0.0349 1.0000 Uani . . . . . .
C50 C 0.02726(11) 0.2397(3) 0.55294(15) 0.0456 1.0000 Uani . . . . . .
C51 C 0.01031(11) 0.2376(3) 0.61779(16) 0.0496 1.0000 Uani . . . . . .
C52 C 0.05018(12) 0.2719(3) 0.66596(14) 0.0464 1.0000 Uani . . . . . .
C53 C 0.10667(10) 0.3102(2) 0.64933(11) 0.0332 1.0000 Uani . . . . . .
H531 H 0.1327 0.3355 0.6822 0.0397 1.0000 Uiso R . . . . .
H521 H 0.0388 0.2679 0.7095 0.0559 1.0000 Uiso R . . . . .
H511 H -0.0269 0.2126 0.6297 0.0588 1.0000 Uiso R . . . . .
H501 H 0.0007 0.2146 0.5200 0.0547 1.0000 Uiso R . . . . .
H491 H 0.0958 0.2718 0.4923 0.0416 1.0000 Uiso R . . . . .
N54 N 0.3369(2) -0.2320(3) 0.3656(2) 0.0984 1.0000 Uani . . . . . .
C55 C 0.37316(17) -0.1657(3) 0.37902(17) 0.0630 1.0000 Uani . . . . . .
C56 C 0.41879(18) -0.0801(4) 0.3953(3) 0.1127 1.0000 Uani . . . . . .
H561 H 0.4547 -0.1068 0.3759 0.1684 1.0000 Uiso R . . . . .
H562 H 0.4236 -0.0759 0.4410 0.1691 1.0000 Uiso R . . . . .
H563 H 0.4087 -0.0005 0.3783 0.1689 1.0000 Uiso R . . . . .
N57 N 0.0456(2) 0.2523(4) 0.3489(2) 0.1066 1.0000 Uani . . . . . .
C58 C 0.02877(14) 0.3404(3) 0.37197(16) 0.0591 1.0000 Uani . . . . . .
C59 C 0.00691(16) 0.4478(4) 0.40265(19) 0.0746 1.0000 Uani . . . . . .
H593 H 0.0299 0.4637 0.4417 0.1120 1.0000 Uiso R . . . . .
H592 H -0.0342 0.4408 0.4126 0.1125 1.0000 Uiso R . . . . .
H591 H 0.0122 0.5132 0.3734 0.1126 1.0000 Uiso R . . . . .
N60 N 0.14264(19) -0.2324(3) 0.61002(17) 0.0858 1.0000 Uani . . . . . .
C61 C 0.10948(17) -0.1554(3) 0.60693(17) 0.0646 1.0000 Uani . . . . . .
C62 C 0.06722(18) -0.0570(4) 0.6052(3) 0.1158 1.0000 Uani . . . . . .
H623 H 0.0602 -0.0322 0.5601 0.1733 1.0000 Uiso R . . . . .
H622 H 0.0308 -0.0849 0.6242 0.1731 1.0000 Uiso R . . . . .
H621 H 0.0823 0.0129 0.6291 0.1727 1.0000 Uiso R . . . . .
N63 N 0.52026(18) -0.2854(3) 0.32410(19) 0.0896 1.0000 Uani . . . . . .
C64 C 0.51703(15) -0.3680(3) 0.35881(18) 0.0639 1.0000 Uani . . . . . .
C65 C 0.51072(18) -0.4685(4) 0.4037(2) 0.0843 1.0000 Uani . . . . . .
H651 H 0.5358 -0.4533 0.4416 0.1258 1.0000 Uiso R . . . . .
H652 H 0.5245 -0.5408 0.3805 0.1262 1.0000 Uiso R . . . . .
H653 H 0.4695 -0.4765 0.4158 0.1261 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.6093(15)
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 . Cl2 . 2.3320(5) yes
Pd1 . Cl3 . 2.3389(5) yes
Pd1 . P4 . 2.2526(5) yes
Pd1 . P15 . 2.2594(5) yes
P4 . C5 . 1.8182(19) yes
P4 . C42 . 1.8063(19) yes
P4 . C48 . 1.816(2) yes
C5 . N6 . 1.364(2) yes
C5 . C9 . 1.370(3) yes
N6 . N7 . 1.309(3) yes
N7 . N8 . 1.343(2) yes
N8 . C9 . 1.346(3) yes
N8 . C35 . 1.481(3) yes
C9 . C10 . 1.462(3) yes
C10 . N11 . 1.347(3) yes
C10 . C14 . 1.372(3) yes
N11 . N12 . 1.347(2) yes
N11 . C28 . 1.482(3) yes
N12 . N13 . 1.313(3) yes
N13 . C14 . 1.365(2) yes
C14 . P15 . 1.818(2) yes
P15 . C16 . 1.808(2) yes
P15 . C22 . 1.822(2) yes
C16 . C17 . 1.399(3) yes
C16 . C21 . 1.390(3) yes
C17 . C18 . 1.387(3) yes
C17 . H171 . 0.930 no
C18 . C19 . 1.376(4) yes
C18 . H181 . 0.937 no
C19 . C20 . 1.374(4) yes
C19 . H191 . 0.925 no
C20 . C21 . 1.383(3) yes
C20 . H201 . 0.919 no
C21 . H211 . 0.915 no
C22 . C23 . 1.382(3) yes
C22 . C27 . 1.393(3) yes
C23 . C24 . 1.392(3) yes
C23 . H231 . 0.925 no
C24 . C25 . 1.362(4) yes
C24 . H241 . 0.933 no
C25 . C26 . 1.390(4) yes
C25 . H251 . 0.920 no
C26 . C27 . 1.380(3) yes
C26 . H261 . 0.939 no
C27 . H271 . 0.926 no
C28 . C29 . 1.505(3) yes
C28 . H282 . 0.950 no
C28 . H281 . 0.966 no
C29 . C30 . 1.378(4) yes
C29 . C34 . 1.387(3) yes
C30 . C31 . 1.397(4) yes
C30 . H301 . 0.917 no
C31 . C32 . 1.376(5) yes
C31 . H311 . 0.910 no
C32 . C33 . 1.358(5) yes
C32 . H321 . 0.931 no
C33 . C34 . 1.375(4) yes
C33 . H331 . 0.946 no
C34 . H341 . 0.936 no
C35 . C36 . 1.501(3) yes
C35 . H352 . 0.958 no
C35 . H351 . 0.941 no
C36 . C37 . 1.380(3) yes
C36 . C41 . 1.390(4) yes
C37 . C38 . 1.417(4) yes
C37 . H371 . 0.917 no
C38 . C39 . 1.359(5) yes
C38 . H381 . 0.910 no
C39 . C40 . 1.355(5) yes
C39 . H391 . 0.952 no
C40 . C41 . 1.375(4) yes
C40 . H401 . 0.943 no
C41 . H411 . 0.944 no
C42 . C43 . 1.386(3) yes
C42 . C47 . 1.399(3) yes
C43 . C44 . 1.385(3) yes
C43 . H431 . 0.912 no
C44 . C45 . 1.376(4) yes
C44 . H441 . 0.928 no
C45 . C46 . 1.376(4) yes
C45 . H451 . 0.935 no
C46 . C47 . 1.387(3) yes
C46 . H461 . 0.928 no
C47 . H471 . 0.934 no
C48 . C49 . 1.396(3) yes
C48 . C53 . 1.390(3) yes
C49 . C50 . 1.382(3) yes
C49 . H491 . 0.926 no
C50 . C51 . 1.381(4) yes
C50 . H501 . 0.941 no
C51 . C52 . 1.385(4) yes
C51 . H511 . 0.917 no
C52 . C53 . 1.385(3) yes
C52 . H521 . 0.928 no
C53 . H531 . 0.935 no
N54 . C55 . 1.122(5) yes
C55 . C56 . 1.425(5) yes
C56 . H561 . 0.949 no
C56 . H562 . 0.940 no
C56 . H563 . 0.956 no
N57 . C58 . 1.130(5) yes
C58 . C59 . 1.411(5) yes
C59 . H593 . 0.967 no
C59 . H592 . 0.955 no
C59 . H591 . 0.935 no
N60 . C61 . 1.122(5) yes
C61 . C62 . 1.430(5) yes
C62 . H623 . 0.972 no
C62 . H622 . 0.960 no
C62 . H621 . 0.963 no
N63 . C64 . 1.144(5) yes
C64 . C65 . 1.430(5) yes
C65 . H651 . 0.973 no
C65 . H652 . 0.967 no
C65 . H653 . 0.969 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
Cl2 . Pd1 . Cl3 . 89.68(2) yes
Cl2 . Pd1 . P4 . 88.205(19) yes
Cl3 . Pd1 . P4 . 173.922(19) yes
Cl2 . Pd1 . P15 . 172.733(19) yes
Cl3 . Pd1 . P15 . 86.448(19) yes
P4 . Pd1 . P15 . 96.245(19) yes
Pd1 . P4 . C5 . 116.37(6) yes
Pd1 . P4 . C42 . 112.18(7) yes
C5 . P4 . C42 . 105.70(9) yes
Pd1 . P4 . C48 . 113.29(7) yes
C5 . P4 . C48 . 100.44(9) yes
C42 . P4 . C48 . 107.86(10) yes
P4 . C5 . N6 . 123.16(15) yes
P4 . C5 . C9 . 128.81(14) yes
N6 . C5 . C9 . 108.02(17) yes
C5 . N6 . N7 . 108.64(17) yes
N6 . N7 . N8 . 107.86(16) yes
N7 . N8 . C9 . 110.33(17) yes
N7 . N8 . C35 . 120.77(16) yes
C9 . N8 . C35 . 128.88(17) yes
C5 . C9 . N8 . 105.15(16) yes
C5 . C9 . C10 . 127.81(17) yes
N8 . C9 . C10 . 126.84(17) yes
C9 . C10 . N11 . 127.02(17) yes
C9 . C10 . C14 . 127.35(17) yes
N11 . C10 . C14 . 105.56(16) yes
C10 . N11 . N12 . 110.05(17) yes
C10 . N11 . C28 . 128.57(17) yes
N12 . N11 . C28 . 121.36(16) yes
N11 . N12 . N13 . 107.83(16) yes
N12 . N13 . C14 . 108.80(17) yes
C10 . C14 . N13 . 107.74(17) yes
C10 . C14 . P15 . 128.97(14) yes
N13 . C14 . P15 . 123.29(15) yes
C14 . P15 . Pd1 . 118.99(7) yes
C14 . P15 . C16 . 105.24(9) yes
Pd1 . P15 . C16 . 111.85(7) yes
C14 . P15 . C22 . 100.09(9) yes
Pd1 . P15 . C22 . 110.44(7) yes
C16 . P15 . C22 . 109.37(10) yes
P15 . C16 . C17 . 118.60(17) yes
P15 . C16 . C21 . 121.72(16) yes
C17 . C16 . C21 . 119.67(19) yes
C16 . C17 . C18 . 119.7(2) yes
C16 . C17 . H171 . 121.4 no
C18 . C17 . H171 . 118.9 no
C17 . C18 . C19 . 120.0(2) yes
C17 . C18 . H181 . 119.5 no
C19 . C18 . H181 . 120.4 no
C18 . C19 . C20 . 120.4(2) yes
C18 . C19 . H191 . 119.2 no
C20 . C19 . H191 . 120.4 no
C19 . C20 . C21 . 120.7(2) yes
C19 . C20 . H201 . 119.2 no
C21 . C20 . H201 . 120.1 no
C16 . C21 . C20 . 119.5(2) yes
C16 . C21 . H211 . 120.0 no
C20 . C21 . H211 . 120.5 no
P15 . C22 . C23 . 123.09(17) yes
P15 . C22 . C27 . 117.05(17) yes
C23 . C22 . C27 . 119.9(2) yes
C22 . C23 . C24 . 119.1(2) yes
C22 . C23 . H231 . 121.3 no
C24 . C23 . H231 . 119.6 no
C23 . C24 . C25 . 121.2(3) yes
C23 . C24 . H241 . 119.7 no
C25 . C24 . H241 . 119.1 no
C24 . C25 . C26 . 120.0(2) yes
C24 . C25 . H251 . 121.5 no
C26 . C25 . H251 . 118.6 no
C25 . C26 . C27 . 119.6(3) yes
C25 . C26 . H261 . 120.6 no
C27 . C26 . H261 . 119.8 no
C22 . C27 . C26 . 120.2(2) yes
C22 . C27 . H271 . 120.5 no
C26 . C27 . H271 . 119.3 no
N11 . C28 . C29 . 113.14(17) yes
N11 . C28 . H282 . 109.5 no
C29 . C28 . H282 . 108.9 no
N11 . C28 . H281 . 108.1 no
C29 . C28 . H281 . 108.9 no
H282 . C28 . H281 . 108.2 no
C28 . C29 . C30 . 122.6(2) yes
C28 . C29 . C34 . 117.9(2) yes
C30 . C29 . C34 . 119.4(2) yes
C29 . C30 . C31 . 119.3(3) yes
C29 . C30 . H301 . 119.2 no
C31 . C30 . H301 . 121.5 no
C30 . C31 . C32 . 120.3(3) yes
C30 . C31 . H311 . 118.6 no
C32 . C31 . H311 . 121.1 no
C31 . C32 . C33 . 120.2(3) yes
C31 . C32 . H321 . 119.0 no
C33 . C32 . H321 . 120.8 no
C32 . C33 . C34 . 120.2(3) yes
C32 . C33 . H331 . 120.2 no
C34 . C33 . H331 . 119.5 no
C29 . C34 . C33 . 120.6(3) yes
C29 . C34 . H341 . 119.7 no
C33 . C34 . H341 . 119.7 no
N8 . C35 . C36 . 112.05(17) yes
N8 . C35 . H352 . 109.0 no
C36 . C35 . H352 . 110.0 no
N8 . C35 . H351 . 106.7 no
C36 . C35 . H351 . 110.7 no
H352 . C35 . H351 . 108.3 no
C35 . C36 . C37 . 120.5(2) yes
C35 . C36 . C41 . 120.7(2) yes
C37 . C36 . C41 . 118.8(2) yes
C36 . C37 . C38 . 119.4(3) yes
C36 . C37 . H371 . 119.2 no
C38 . C37 . H371 . 121.4 no
C37 . C38 . C39 . 119.7(3) yes
C37 . C38 . H381 . 118.0 no
C39 . C38 . H381 . 122.3 no
C38 . C39 . C40 . 121.2(3) yes
C38 . C39 . H391 . 120.2 no
C40 . C39 . H391 . 118.6 no
C39 . C40 . C41 . 119.9(3) yes
C39 . C40 . H401 . 119.7 no
C41 . C40 . H401 . 120.4 no
C36 . C41 . C40 . 121.1(3) yes
C36 . C41 . H411 . 119.3 no
C40 . C41 . H411 . 119.7 no
P4 . C42 . C43 . 122.17(16) yes
P4 . C42 . C47 . 117.83(17) yes
C43 . C42 . C47 . 119.92(19) yes
C42 . C43 . C44 . 119.5(2) yes
C42 . C43 . H431 . 121.3 no
C44 . C43 . H431 . 119.2 no
C43 . C44 . C45 . 120.3(2) yes
C43 . C44 . H441 . 118.8 no
C45 . C44 . H441 . 120.9 no
C44 . C45 . C46 . 120.8(2) yes
C44 . C45 . H451 . 119.1 no
C46 . C45 . H451 . 120.2 no
C45 . C46 . C47 . 119.7(2) yes
C45 . C46 . H461 . 120.6 no
C47 . C46 . H461 . 119.7 no
C42 . C47 . C46 . 119.8(2) yes
C42 . C47 . H471 . 119.7 no
C46 . C47 . H471 . 120.5 no
P4 . C48 . C49 . 118.12(18) yes
P4 . C48 . C53 . 122.12(16) yes
C49 . C48 . C53 . 119.8(2) yes
C48 . C49 . C50 . 119.7(2) yes
C48 . C49 . H491 . 120.0 no
C50 . C49 . H491 . 120.4 no
C49 . C50 . C51 . 120.5(2) yes
C49 . C50 . H501 . 119.0 no
C51 . C50 . H501 . 120.4 no
C50 . C51 . C52 . 119.8(2) yes
C50 . C51 . H511 . 121.0 no
C52 . C51 . H511 . 119.1 no
C51 . C52 . C53 . 120.3(3) yes
C51 . C52 . H521 . 119.2 no
C53 . C52 . H521 . 120.5 no
C48 . C53 . C52 . 119.8(2) yes
C48 . C53 . H531 . 120.8 no
C52 . C53 . H531 . 119.4 no
N54 . C55 . C56 . 179.1(4) yes
C55 . C56 . H561 . 108.8 no
C55 . C56 . H562 . 110.2 no
H561 . C56 . H562 . 109.5 no
C55 . C56 . H563 . 109.1 no
H561 . C56 . H563 . 109.1 no
H562 . C56 . H563 . 110.2 no
N57 . C58 . C59 . 177.9(4) yes
C58 . C59 . H593 . 109.0 no
C58 . C59 . H592 . 111.8 no
H593 . C59 . H592 . 111.1 no
C58 . C59 . H591 . 107.0 no
H593 . C59 . H591 . 109.0 no
H592 . C59 . H591 . 108.8 no
N60 . C61 . C62 . 178.2(5) yes
C61 . C62 . H623 . 109.7 no
C61 . C62 . H622 . 109.2 no
H623 . C62 . H622 . 109.5 no
C61 . C62 . H621 . 109.6 no
H623 . C62 . H621 . 108.7 no
H622 . C62 . H621 . 110.1 no
N63 . C64 . C65 . 177.3(4) yes
C64 . C65 . H651 . 108.9 no
C64 . C65 . H652 . 105.4 no
H651 . C65 . H652 . 109.9 no
C64 . C65 . H653 . 109.2 no
H651 . C65 . H653 . 111.9 no
H652 . C65 . H653 . 111.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C59 . H593 . N6 . 154.03(10) 0.967 2.578 3.473(4) yes
C62 . H622 . N57 2_556 152.61(14) 0.960 2.562 3.442(4) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 03/05/13 at 09:54:58
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S)
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) H   ( 563,X'S) 
RIDE C   (  59,X'S) H   ( 593,X'S) H   ( 592,X'S) H   ( 591,X'S) 
RIDE C   (  62,X'S) H   ( 623,X'S) H   ( 622,X'S) H   ( 621,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) H   ( 653,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 03/05/13 at 09:54:58
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

_vrf_PLAT027_13.11               
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      62.76 Degree
RESPONSE: the data were collected using Cu radiation
;
####################################################################### 
# 
# 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_14
_database_code_depnum_ccdc_archive 'CCDC 1031969'
_audit_update_record             
;
2014-10-31 deposited with the CCDC.
2015-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H68 Cl4 N12 P4 Pt2'
_chemical_formula_weight         1901.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2yc'

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

_cell_length_a                   25.778(5)
_cell_length_b                   17.954(5)
_cell_length_c                   19.364(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 104.467(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     8678(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9977
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      19.72

_exptl_crystal_description       flattened
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3760
_exptl_absorpt_coefficient_mu    3.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5397
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           ?

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            70384
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         19.76
_reflns_number_total             7804
_reflns_number_gt                6507
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0417P)²+22.5205P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7804
_refine_ls_number_parameters     925
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0810
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.09504(2) 0.58986(2) 0.38086(2) 0.02017(12) Uani 1 1 d . . . . .
Cl1 Cl 0.15947(9) 0.49497(11) 0.40451(12) 0.0360(6) Uani 1 1 d . . . . .
Cl2 Cl 0.03051(8) 0.49901(11) 0.33568(10) 0.0301(5) Uani 1 1 d . . . . .
P1 P 0.02730(8) 0.67130(11) 0.36712(10) 0.0196(5) Uani 1 1 d . . . . .
P2 P 0.16096(8) 0.67368(11) 0.41180(10) 0.0202(5) Uani 1 1 d . . . . .
N11 N 0.0198(3) 0.7679(4) 0.4811(3) 0.0256(17) Uani 1 1 d . . . . .
N12 N 0.0406(3) 0.8305(4) 0.5103(3) 0.0303(18) Uani 1 1 d . . . . .
N13 N 0.0739(3) 0.8572(3) 0.4728(3) 0.0230(17) Uani 1 1 d . . . . .
N14 N 0.1666(3) 0.7798(4) 0.3070(3) 0.0250(17) Uani 1 1 d . . . . .
N15 N 0.1437(3) 0.8420(4) 0.2788(3) 0.0286(18) Uani 1 1 d . . . . .
N16 N 0.1087(3) 0.8624(3) 0.3166(3) 0.0179(16) Uani 1 1 d . . . . .
C11 C 0.0407(3) 0.7530(4) 0.4248(4) 0.021(2) Uani 1 1 d . . . . .
C12 C 0.0748(3) 0.8097(4) 0.4180(4) 0.018(2) Uani 1 1 d . . . . .
C13 C 0.1098(3) 0.8136(4) 0.3704(4) 0.017(2) Uani 1 1 d . . . . .
C14 C 0.1467(3) 0.7604(4) 0.3632(4) 0.0170(19) Uani 1 1 d . . . . .
C111 C -0.0309(3) 0.6309(4) 0.3888(4) 0.0174(19) Uani 1 1 d . . . . .
C112 C -0.0256(4) 0.6002(4) 0.4563(4) 0.027(2) Uani 1 1 d . . . . .
H112 H 0.0069 0.6039 0.4902 0.032 Uiso 1 1 calc R U . . .
C113 C -0.0678(4) 0.5646(5) 0.4734(5) 0.034(2) Uani 1 1 d . . . . .
H113 H -0.0642 0.5453 0.5190 0.041 Uiso 1 1 calc R U . . .
C114 C -0.1150(4) 0.5578(5) 0.4233(5) 0.039(2) Uani 1 1 d . . . . .
H114 H -0.1435 0.5335 0.4349 0.046 Uiso 1 1 calc R U . . .
C115 C -0.1214(3) 0.5861(5) 0.3561(5) 0.033(2) Uani 1 1 d . . . . .
H115 H -0.1540 0.5807 0.3225 0.039 Uiso 1 1 calc R U . . .
C116 C -0.0797(3) 0.6223(4) 0.3385(4) 0.028(2) Uani 1 1 d . . . . .
H116 H -0.0840 0.6413 0.2927 0.033 Uiso 1 1 calc R U . . .
C121 C 0.0090(3) 0.7151(4) 0.2800(4) 0.018(2) Uani 1 1 d . . . . .
C122 C -0.0293(3) 0.7713(4) 0.2646(4) 0.020(2) Uani 1 1 d . . . . .
H122 H -0.0486 0.7837 0.2976 0.023 Uiso 1 1 calc R U . . .
C123 C -0.0389(4) 0.8092(5) 0.1994(4) 0.034(2) Uani 1 1 d . . . . .
H123 H -0.0649 0.8462 0.1886 0.041 Uiso 1 1 calc R U . . .
C124 C -0.0095(4) 0.7908(5) 0.1517(4) 0.039(3) Uani 1 1 d . . . . .
H124 H -0.0153 0.8162 0.1086 0.047 Uiso 1 1 calc R U . . .
C125 C 0.0284(4) 0.7358(5) 0.1668(4) 0.036(2) Uani 1 1 d . . . . .
H125 H 0.0486 0.7247 0.1345 0.044 Uiso 1 1 calc R U . . .
C126 C 0.0366(3) 0.6966(5) 0.2303(4) 0.028(2) Uani 1 1 d . . . . .
H126 H 0.0610 0.6575 0.2393 0.034 Uiso 1 1 calc R U . . .
C131 C 0.1075(4) 0.9223(5) 0.4953(4) 0.039(3) Uani 1 1 d . . . . .
H13A H 0.1021 0.9569 0.4558 0.047 Uiso 1 1 calc R U . . .
H13B H 0.1448 0.9069 0.5069 0.047 Uiso 1 1 calc R U . . .
C132 C 0.0966(4) 0.9623(5) 0.5594(4) 0.028(2) Uani 1 1 d . . . . .
C133 C 0.0643(4) 1.0223(5) 0.5510(5) 0.035(2) Uani 1 1 d . . . . .
H133 H 0.0479 1.0388 0.5053 0.042 Uiso 1 1 calc R U . . .
C134 C 0.0550(4) 1.0595(5) 0.6085(6) 0.048(3) Uani 1 1 d . . . . .
H134 H 0.0322 1.1005 0.6014 0.057 Uiso 1 1 calc R U . . .
C135 C 0.0790(4) 1.0369(5) 0.6757(5) 0.041(3) Uani 1 1 d . . . . .
H135 H 0.0723 1.0619 0.7148 0.049 Uiso 1 1 calc R U . . .
C136 C 0.1127(5) 0.9777(6) 0.6856(5) 0.058(3) Uani 1 1 d . . . . .
H136 H 0.1298 0.9624 0.7316 0.069 Uiso 1 1 calc R U . . .
C137 C 0.1214(4) 0.9399(5) 0.6272(5) 0.056(3) Uani 1 1 d . . . . .
H137 H 0.1443 0.8991 0.6341 0.067 Uiso 1 1 calc R U . . .
C161 C 0.0761(3) 0.9293(4) 0.2946(4) 0.023(2) Uani 1 1 d . . . . .
H16A H 0.0433 0.9249 0.3102 0.027 Uiso 1 1 calc R U . . .
H16B H 0.0664 0.9320 0.2429 0.027 Uiso 1 1 calc R U . . .
C162 C 0.1042(4) 1.0004(4) 0.3241(4) 0.027(2) Uani 1 1 d . . . . .
C163 C 0.0742(4) 1.0572(5) 0.3426(4) 0.043(3) Uani 1 1 d . . . . .
H163 H 0.0376 1.0509 0.3377 0.051 Uiso 1 1 calc R U . . .
C164 C 0.0989(5) 1.1236(6) 0.3686(5) 0.055(3) Uani 1 1 d . . . . .
H164 H 0.0790 1.1618 0.3818 0.067 Uiso 1 1 calc R U . . .
C165 C 0.1516(6) 1.1329(6) 0.3748(6) 0.059(3) Uani 1 1 d . . . . .
H165 H 0.1681 1.1775 0.3925 0.071 Uiso 1 1 calc R U . . .
C166 C 0.1811(4) 1.0773(6) 0.3553(5) 0.055(3) Uani 1 1 d . . . . .
H166 H 0.2174 1.0847 0.3590 0.065 Uiso 1 1 calc R U . . .
C167 C 0.1580(4) 1.0109(5) 0.3303(5) 0.046(3) Uani 1 1 d . . . . .
H167 H 0.1785 0.9731 0.3175 0.056 Uiso 1 1 calc R U . . .
C211 C 0.2235(3) 0.6449(4) 0.3921(4) 0.023(2) Uani 1 1 d . . . . .
C212 C 0.2702(4) 0.6363(5) 0.4431(5) 0.036(2) Uani 1 1 d . . . . .
H212 H 0.2715 0.6475 0.4904 0.044 Uiso 1 1 calc R U . . .
C213 C 0.3152(4) 0.6114(5) 0.4251(5) 0.044(3) Uani 1 1 d . . . . .
H213 H 0.3469 0.6051 0.4603 0.053 Uiso 1 1 calc R U . . .
C214 C 0.3139(4) 0.5956(5) 0.3550(6) 0.043(3) Uani 1 1 d . . . . .
H214 H 0.3446 0.5790 0.3428 0.052 Uiso 1 1 calc R U . . .
C215 C 0.2667(4) 0.6044(5) 0.3031(5) 0.041(3) Uani 1 1 d . . . . .
H215 H 0.2655 0.5936 0.2558 0.049 Uiso 1 1 calc R U . . .
C216 C 0.2218(3) 0.6292(4) 0.3214(5) 0.028(2) Uani 1 1 d . . . . .
H216 H 0.1901 0.6356 0.2863 0.033 Uiso 1 1 calc R U . . .
C221 C 0.1769(3) 0.7022(5) 0.5044(4) 0.025(2) Uani 1 1 d . . . . .
C222 C 0.2114(3) 0.7623(5) 0.5283(4) 0.033(2) Uani 1 1 d . . . . .
H222 H 0.2257 0.7895 0.4965 0.039 Uiso 1 1 calc R U . . .
C223 C 0.2241(4) 0.7805(5) 0.6001(5) 0.045(3) Uani 1 1 d . . . . .
H223 H 0.2474 0.8198 0.6168 0.054 Uiso 1 1 calc R U . . .
C224 C 0.2021(4) 0.7402(6) 0.6470(5) 0.050(3) Uani 1 1 d . . . . .
H224 H 0.2107 0.7527 0.6951 0.060 Uiso 1 1 calc R U . . .
C225 C 0.1681(4) 0.6826(6) 0.6232(5) 0.048(3) Uani 1 1 d . . . . .
H225 H 0.1536 0.6561 0.6552 0.058 Uiso 1 1 calc R U . . .
C226 C 0.1548(4) 0.6627(5) 0.5517(4) 0.033(2) Uani 1 1 d . . . . .
H226 H 0.1314 0.6234 0.5356 0.040 Uiso 1 1 calc R U . . .
Pt3 Pt 0.41814(2) 0.26055(2) 0.29398(2) 0.02711(13) Uani 1 1 d . . . . .
Cl3 Cl 0.47838(9) 0.17621(13) 0.26497(11) 0.0403(6) Uani 1 1 d . . . . .
Cl4 Cl 0.39743(10) 0.30072(13) 0.17381(11) 0.0431(6) Uani 1 1 d . . . . .
P3 P 0.36470(9) 0.35148(13) 0.31501(11) 0.0299(6) Uani 1 1 d . . . . .
P4 P 0.43291(9) 0.21130(12) 0.40365(11) 0.0280(6) Uani 1 1 d . . . . .
N31 N 0.3978(3) 0.4546(4) 0.4271(4) 0.0294(18) Uani 1 1 d . . . . .
N32 N 0.4037(3) 0.4599(4) 0.4958(4) 0.0315(18) Uani 1 1 d . . . . .
N33 N 0.3872(3) 0.3959(4) 0.5199(3) 0.0265(17) Uani 1 1 d . . . . .
N34 N 0.3452(4) 0.1488(4) 0.4459(4) 0.054(2) Uani 1 1 d . . . . .
N35 N 0.3091(4) 0.1669(5) 0.4806(5) 0.065(3) Uani 1 1 d . . . . .
N36 N 0.3136(3) 0.2421(4) 0.4922(4) 0.047(2) Uani 1 1 d . . . . .
C21 C 0.3772(3) 0.3863(5) 0.4061(4) 0.024(2) Uani 1 1 d . . . . .
C22 C 0.3702(3) 0.3477(5) 0.4656(5) 0.029(2) Uani 1 1 d . . . . .
C23 C 0.3751(3) 0.2098(5) 0.4396(4) 0.029(2) Uani 1 1 d . . . . .
C24 C 0.3548(4) 0.2705(5) 0.4685(4) 0.033(2) Uani 1 1 d . . . . .
C311 C 0.3741(5) 0.4351(5) 0.2686(5) 0.039(2) Uani 1 1 d . . . . .
C312 C 0.3324(5) 0.4690(6) 0.2203(6) 0.067(4) Uani 1 1 d . . . . .
H312 H 0.2977 0.4503 0.2110 0.081 Uiso 1 1 calc R U . . .
C313 C 0.3455(8) 0.5371(7) 0.1835(7) 0.094(5) Uani 1 1 d . . . . .
H313 H 0.3196 0.5631 0.1502 0.113 Uiso 1 1 calc R U . . .
C314 C 0.3991(8) 0.5594(8) 0.2025(8) 0.089(5) Uani 1 1 d . . . . .
H314 H 0.4080 0.6021 0.1808 0.107 Uiso 1 1 calc R U . . .
C315 C 0.4375(7) 0.5259(8) 0.2473(8) 0.086(4) Uani 1 1 d . . . . .
H315 H 0.4726 0.5432 0.2568 0.103 Uiso 1 1 calc R U . . .
C316 C 0.4246(6) 0.4641(6) 0.2803(6) 0.069(4) Uani 1 1 d . . . . .
H316 H 0.4520 0.4400 0.3130 0.083 Uiso 1 1 calc R U . . .
C321 C 0.2953(4) 0.3270(5) 0.2947(4) 0.031(2) Uani 1 1 d . . . . .
C322 C 0.2775(4) 0.2609(5) 0.2574(5) 0.044(3) Uani 1 1 d . . . . .
H322 H 0.3020 0.2304 0.2430 0.053 Uiso 1 1 calc R U . . .
C323 C 0.2251(5) 0.2411(6) 0.2421(6) 0.066(3) Uani 1 1 d . . . . .
H323 H 0.2139 0.1973 0.2172 0.079 Uiso 1 1 calc R U . . .
C324 C 0.1883(4) 0.2858(8) 0.2634(6) 0.071(4) Uani 1 1 d . . . . .
H324 H 0.1525 0.2714 0.2532 0.085 Uiso 1 1 calc R U . . .
C325 C 0.2037(4) 0.3502(7) 0.2988(6) 0.065(3) Uani 1 1 d . . . . .
H325 H 0.1788 0.3802 0.3129 0.078 Uiso 1 1 calc R U . . .
C326 C 0.2568(4) 0.3707(6) 0.3136(5) 0.047(3) Uani 1 1 d . . . . .
H326 H 0.2672 0.4155 0.3372 0.056 Uiso 1 1 calc R U . . .
C331 C 0.3903(3) 0.3898(5) 0.5961(4) 0.033(2) Uani 1 1 d . . . . .
H33A H 0.4241 0.4109 0.6227 0.040 Uiso 1 1 calc R U . . .
H33B H 0.3902 0.3375 0.6087 0.040 Uiso 1 1 calc R U . . .
C332 C 0.3449(3) 0.4287(4) 0.6181(4) 0.026(2) Uani 1 1 d . . . . .
C333 C 0.3407(4) 0.4195(5) 0.6886(5) 0.042(3) Uani 1 1 d . . . . .
H333 H 0.3656 0.3904 0.7203 0.050 Uiso 1 1 calc R U . . .
C334 C 0.3006(4) 0.4528(6) 0.7106(5) 0.056(3) Uani 1 1 d . . . . .
H334 H 0.2985 0.4463 0.7574 0.067 Uiso 1 1 calc R U . . .
C335 C 0.2627(4) 0.4964(6) 0.6650(6) 0.054(3) Uani 1 1 d . . . . .
H335 H 0.2354 0.5193 0.6807 0.064 Uiso 1 1 calc R U . . .
C336 C 0.2664(4) 0.5050(5) 0.5960(5) 0.044(3) Uani 1 1 d . . . . .
H336 H 0.2412 0.5337 0.5645 0.053 Uiso 1 1 calc R U . . .
C337 C 0.3070(4) 0.4717(5) 0.5730(5) 0.040(3) Uani 1 1 d . . . . .
H337 H 0.3089 0.4783 0.5260 0.048 Uiso 1 1 calc R U . . .
C361 C 0.2844(4) 0.2796(6) 0.5390(6) 0.062(3) Uani 1 1 d . . . . .
H36A H 0.3043 0.2722 0.5881 0.075 Uiso 1 1 calc R U . . .
H36B H 0.2841 0.3327 0.5295 0.075 Uiso 1 1 calc R U . . .
C362 C 0.2287(5) 0.2556(8) 0.5323(7) 0.0853(18) Uani 1 1 d . . . . .
C363 C 0.2208(5) 0.1904(7) 0.5689(7) 0.0853(18) Uani 1 1 d . . . . .
H363 H 0.2502 0.1623 0.5926 0.102 Uiso 1 1 calc R U . . .
C364 C 0.1676(5) 0.1666(8) 0.5702(7) 0.0853(18) Uani 1 1 d . . . . .
H364 H 0.1611 0.1220 0.5909 0.102 Uiso 1 1 calc R U . . .
C365 C 0.1304(5) 0.2115(8) 0.5408(7) 0.0853(18) Uani 1 1 d . . . . .
H365 H 0.0967 0.1995 0.5467 0.102 Uiso 1 1 calc R U . . .
C366 C 0.1319(5) 0.2688(7) 0.5052(7) 0.0853(18) Uani 1 1 d . . . . .
H366 H 0.1008 0.2940 0.4826 0.102 Uiso 1 1 calc R U . . .
C367 C 0.1845(5) 0.2953(8) 0.5002(7) 0.0853(18) Uani 1 1 d . . . . .
H367 H 0.1875 0.3387 0.4754 0.102 Uiso 1 1 calc R U . . .
C411 C 0.4787(3) 0.2651(5) 0.4725(4) 0.029(2) Uani 1 1 d . . . . .
C412 C 0.5044(3) 0.3265(5) 0.4535(5) 0.038(2) Uani 1 1 d . . . . .
H412 H 0.5017 0.3374 0.4057 0.046 Uiso 1 1 calc R U . . .
C413 C 0.5343(4) 0.3717(6) 0.5072(7) 0.058(3) Uani 1 1 d . . . . .
H413 H 0.5520 0.4132 0.4954 0.070 Uiso 1 1 calc R U . . .
C414 C 0.5379(4) 0.3555(7) 0.5769(7) 0.058(3) Uani 1 1 d . . . . .
H414 H 0.5569 0.3873 0.6121 0.069 Uiso 1 1 calc R U . . .
C415 C 0.5139(4) 0.2932(7) 0.5967(5) 0.055(3) Uani 1 1 d . . . . .
H415 H 0.5178 0.2820 0.6446 0.066 Uiso 1 1 calc R U . . .
C416 C 0.4839(4) 0.2471(6) 0.5437(5) 0.044(3) Uani 1 1 d . . . . .
H416 H 0.4674 0.2046 0.5558 0.052 Uiso 1 1 calc R U . . .
C421 C 0.4566(4) 0.1162(5) 0.4095(4) 0.035(2) Uani 1 1 d . . . . .
C422 C 0.4232(5) 0.0589(6) 0.3773(5) 0.055(3) Uani 1 1 d . . . . .
H422 H 0.3868 0.0681 0.3592 0.066 Uiso 1 1 calc R U . . .
C423 C 0.4425(6) -0.0100(6) 0.3720(6) 0.069(4) Uani 1 1 d . . . . .
H423 H 0.4192 -0.0476 0.3506 0.082 Uiso 1 1 calc R U . . .
C424 C 0.4949(7) -0.0253(7) 0.3969(6) 0.076(4) Uani 1 1 d . . . . .
H424 H 0.5075 -0.0731 0.3922 0.091 Uiso 1 1 calc R U . . .
C425 C 0.5301(5) 0.0298(8) 0.4297(6) 0.063(3) Uani 1 1 d . . . . .
H425 H 0.5662 0.0189 0.4477 0.076 Uiso 1 1 calc R U . . .
C426 C 0.5112(4) 0.1014(6) 0.4354(5) 0.046(3) Uani 1 1 d . . . . .
H426 H 0.5346 0.1391 0.4563 0.055 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 P2 2.237(2) . ?
Pt1 P1 2.242(2) . ?
Pt1 Cl2 2.338(2) . ?
Pt1 Cl1 2.343(2) . ?
P1 C111 1.807(8) . ?
P1 C121 1.814(8) . ?
P1 C11 1.823(8) . ?
P2 C14 1.809(8) . ?
P2 C221 1.811(8) . ?
P2 C211 1.820(8) . ?
N11 N12 1.310(9) . ?
N11 C11 1.361(9) . ?
N12 N13 1.345(9) . ?
N13 C12 1.366(9) . ?
N13 C131 1.454(10) . ?
N14 N15 1.315(8) . ?
N14 C14 1.361(9) . ?
N15 N16 1.346(8) . ?
N16 C13 1.355(9) . ?
N16 C161 1.467(9) . ?
C11 C12 1.374(10) . ?
C12 C13 1.442(11) . ?
C13 C14 1.379(10) . ?
C111 C112 1.394(10) . ?
C111 C116 1.394(10) . ?
C112 C113 1.372(11) . ?
C113 C114 1.359(12) . ?
C114 C115 1.367(11) . ?
C115 C116 1.372(11) . ?
C121 C126 1.375(11) . ?
C121 C122 1.390(10) . ?
C122 C123 1.400(11) . ?
C123 C124 1.374(12) . ?
C124 C125 1.368(12) . ?
C125 C126 1.386(11) . ?
C131 C132 1.519(11) . ?
C132 C133 1.347(12) . ?
C132 C137 1.370(12) . ?
C133 C134 1.369(12) . ?
C134 C135 1.356(12) . ?
C135 C136 1.357(13) . ?
C136 C137 1.385(13) . ?
C161 C162 1.508(11) . ?
C162 C167 1.374(12) . ?
C162 C163 1.381(12) . ?
C163 C164 1.386(13) . ?
C164 C165 1.344(14) . ?
C165 C166 1.363(14) . ?
C166 C167 1.368(13) . ?
C211 C212 1.362(11) . ?
C211 C216 1.389(11) . ?
C212 C213 1.369(12) . ?
C213 C214 1.378(12) . ?
C214 C215 1.379(12) . ?
C215 C216 1.366(11) . ?
C221 C226 1.387(11) . ?
C221 C222 1.403(11) . ?
C222 C223 1.384(11) . ?
C223 C224 1.389(13) . ?
C224 C225 1.360(13) . ?
C225 C226 1.387(11) . ?
Pt3 P3 2.238(2) . ?
Pt3 P4 2.243(2) . ?
Pt3 Cl3 2.336(2) . ?
Pt3 Cl4 2.366(2) . ?
P3 C321 1.789(9) . ?
P3 C311 1.798(10) . ?
P3 C21 1.822(8) . ?
P4 C23 1.796(9) . ?
P4 C421 1.807(9) . ?
P4 C411 1.821(9) . ?
N31 N32 1.305(9) . ?
N31 C21 1.358(10) . ?
N32 N33 1.349(9) . ?
N33 C22 1.348(10) . ?
N33 C331 1.461(10) . ?
N34 N35 1.317(10) . ?
N34 C23 1.362(10) . ?
N35 N36 1.369(10) . ?
N36 C24 1.358(10) . ?
N36 C361 1.478(11) . ?
C21 C22 1.394(11) . ?
C22 C24 1.446(12) . ?
C23 C24 1.385(11) . ?
C311 C316 1.365(14) . ?
C311 C312 1.378(13) . ?
C312 C313 1.497(16) . ?
C313 C314 1.397(19) . ?
C314 C315 1.291(17) . ?
C315 C316 1.362(15) . ?
C321 C326 1.384(12) . ?
C321 C322 1.404(12) . ?
C322 C323 1.356(13) . ?
C323 C324 1.383(15) . ?
C324 C325 1.352(14) . ?
C325 C326 1.378(13) . ?
C331 C332 1.514(11) . ?
C332 C337 1.374(12) . ?
C332 C333 1.405(11) . ?
C333 C334 1.351(12) . ?
C334 C335 1.384(13) . ?
C335 C336 1.371(12) . ?
C336 C337 1.373(12) . ?
C361 C362 1.471(15) . ?
C362 C367 1.357(16) . ?
C362 C363 1.411(17) . ?
C363 C364 1.440(16) . ?
C364 C365 1.274(16) . ?
C365 C366 1.245(16) . ?
C366 C367 1.460(16) . ?
C411 C412 1.382(11) . ?
C411 C416 1.390(11) . ?
C412 C413 1.391(13) . ?
C413 C414 1.362(14) . ?
C414 C415 1.377(14) . ?
C415 C416 1.393(13) . ?
C421 C422 1.386(13) . ?
C421 C426 1.397(12) . ?
C422 C423 1.346(14) . ?
C423 C424 1.344(16) . ?
C424 C425 1.385(16) . ?
C425 C426 1.390(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 Pt1 P1 96.32(8) . . ?
P2 Pt1 Cl2 172.56(7) . . ?
P1 Pt1 Cl2 87.15(8) . . ?
P2 Pt1 Cl1 89.02(8) . . ?
P1 Pt1 Cl1 172.07(8) . . ?
Cl2 Pt1 Cl1 88.23(8) . . ?
C111 P1 C121 110.6(4) . . ?
C111 P1 C11 102.9(4) . . ?
C121 P1 C11 100.7(3) . . ?
C111 P1 Pt1 112.2(3) . . ?
C121 P1 Pt1 114.1(3) . . ?
C11 P1 Pt1 115.4(3) . . ?
C14 P2 C221 103.7(4) . . ?
C14 P2 C211 102.2(4) . . ?
C221 P2 C211 107.1(4) . . ?
C14 P2 Pt1 113.4(3) . . ?
C221 P2 Pt1 115.1(3) . . ?
C211 P2 Pt1 113.9(3) . . ?
N12 N11 C11 108.2(6) . . ?
N11 N12 N13 108.8(6) . . ?
N12 N13 C12 109.5(6) . . ?
N12 N13 C131 122.5(6) . . ?
C12 N13 C131 127.6(7) . . ?
N15 N14 C14 109.1(6) . . ?
N14 N15 N16 107.4(6) . . ?
N15 N16 C13 110.8(6) . . ?
N15 N16 C161 118.5(6) . . ?
C13 N16 C161 130.7(7) . . ?
N11 C11 C12 108.8(7) . . ?
N11 C11 P1 126.7(6) . . ?
C12 C11 P1 124.5(6) . . ?
N13 C12 C11 104.7(7) . . ?
N13 C12 C13 126.9(7) . . ?
C11 C12 C13 127.8(7) . . ?
N16 C13 C14 104.6(6) . . ?
N16 C13 C12 128.8(7) . . ?
C14 C13 C12 126.0(7) . . ?
N14 C14 C13 108.2(6) . . ?
N14 C14 P2 124.6(6) . . ?
C13 C14 P2 126.9(6) . . ?
C112 C111 C116 118.0(7) . . ?
C112 C111 P1 119.0(6) . . ?
C116 C111 P1 122.6(6) . . ?
C113 C112 C111 121.0(8) . . ?
C114 C113 C112 119.4(8) . . ?
C113 C114 C115 121.4(8) . . ?
C114 C115 C116 119.8(8) . . ?
C115 C116 C111 120.4(7) . . ?
C126 C121 C122 119.4(7) . . ?
C126 C121 P1 119.1(6) . . ?
C122 C121 P1 121.4(6) . . ?
C121 C122 C123 120.1(7) . . ?
C124 C123 C122 119.2(8) . . ?
C125 C124 C123 120.9(8) . . ?
C124 C125 C126 120.0(8) . . ?
C121 C126 C125 120.4(8) . . ?
N13 C131 C132 114.1(7) . . ?
C133 C132 C137 118.5(8) . . ?
C133 C132 C131 121.1(8) . . ?
C137 C132 C131 120.4(9) . . ?
C132 C133 C134 121.4(8) . . ?
C135 C134 C133 120.3(9) . . ?
C134 C135 C136 119.5(9) . . ?
C135 C136 C137 119.9(9) . . ?
C132 C137 C136 120.5(9) . . ?
N16 C161 C162 113.4(6) . . ?
C167 C162 C163 119.6(8) . . ?
C167 C162 C161 121.9(8) . . ?
C163 C162 C161 118.4(9) . . ?
C162 C163 C164 119.5(10) . . ?
C165 C164 C163 120.2(10) . . ?
C164 C165 C166 120.3(10) . . ?
C165 C166 C167 120.9(10) . . ?
C166 C167 C162 119.5(9) . . ?
C212 C211 C216 119.6(8) . . ?
C212 C211 P2 123.3(7) . . ?
C216 C211 P2 117.0(6) . . ?
C211 C212 C213 120.4(9) . . ?
C212 C213 C214 120.2(9) . . ?
C213 C214 C215 119.7(8) . . ?
C216 C215 C214 119.8(9) . . ?
C215 C216 C211 120.2(8) . . ?
C226 C221 C222 120.5(7) . . ?
C226 C221 P2 118.7(7) . . ?
C222 C221 P2 120.8(6) . . ?
C223 C222 C221 119.0(8) . . ?
C222 C223 C224 120.1(9) . . ?
C225 C224 C223 120.5(9) . . ?
C224 C225 C226 120.8(9) . . ?
C221 C226 C225 119.2(9) . . ?
P3 Pt3 P4 94.70(8) . . ?
P3 Pt3 Cl3 173.24(8) . . ?
P4 Pt3 Cl3 90.36(8) . . ?
P3 Pt3 Cl4 87.63(8) . . ?
P4 Pt3 Cl4 173.87(8) . . ?
Cl3 Pt3 Cl4 87.78(8) . . ?
C321 P3 C311 110.4(5) . . ?
C321 P3 C21 102.8(4) . . ?
C311 P3 C21 100.6(4) . . ?
C321 P3 Pt3 114.1(3) . . ?
C311 P3 Pt3 110.6(3) . . ?
C21 P3 Pt3 117.3(3) . . ?
C23 P4 C421 105.2(4) . . ?
C23 P4 C411 100.0(4) . . ?
C421 P4 C411 108.0(4) . . ?
C23 P4 Pt3 114.3(3) . . ?
C421 P4 Pt3 114.0(3) . . ?
C411 P4 Pt3 114.2(3) . . ?
N32 N31 C21 107.9(6) . . ?
N31 N32 N33 108.9(6) . . ?
C22 N33 N32 110.3(6) . . ?
C22 N33 C331 131.6(7) . . ?
N32 N33 C331 118.1(7) . . ?
N35 N34 C23 109.5(7) . . ?
N34 N35 N36 106.7(7) . . ?
C24 N36 N35 110.8(7) . . ?
C24 N36 C361 126.8(8) . . ?
N35 N36 C361 121.0(8) . . ?
N31 C21 C22 108.9(7) . . ?
N31 C21 P3 124.0(6) . . ?
C22 C21 P3 127.0(7) . . ?
N33 C22 C21 104.0(7) . . ?
N33 C22 C24 128.6(8) . . ?
C21 C22 C24 126.9(8) . . ?
N34 C23 C24 108.6(7) . . ?
N34 C23 P4 126.1(7) . . ?
C24 C23 P4 125.3(7) . . ?
N36 C24 C23 104.3(7) . . ?
N36 C24 C22 128.1(8) . . ?
C23 C24 C22 127.2(8) . . ?
C316 C311 C312 119.6(10) . . ?
C316 C311 P3 118.5(8) . . ?
C312 C311 P3 121.8(9) . . ?
C311 C312 C313 116.9(12) . . ?
C314 C313 C312 115.8(12) . . ?
C315 C314 C313 125.8(15) . . ?
C314 C315 C316 117.3(15) . . ?
C315 C316 C311 124.5(14) . . ?
C326 C321 C322 116.9(8) . . ?
C326 C321 P3 123.1(7) . . ?
C322 C321 P3 120.1(7) . . ?
C323 C322 C321 120.9(9) . . ?
C322 C323 C324 120.2(10) . . ?
C325 C324 C323 120.7(10) . . ?
C324 C325 C326 119.0(10) . . ?
C325 C326 C321 122.3(9) . . ?
N33 C331 C332 113.5(7) . . ?
C337 C332 C333 118.0(8) . . ?
C337 C332 C331 123.8(8) . . ?
C333 C332 C331 118.2(8) . . ?
C334 C333 C332 120.3(9) . . ?
C333 C334 C335 121.5(9) . . ?
C336 C335 C334 118.3(9) . . ?
C335 C336 C337 120.8(9) . . ?
C336 C337 C332 121.1(8) . . ?
C362 C361 N36 116.6(8) . . ?
C367 C362 C363 117.0(13) . . ?
C367 C362 C361 125.2(14) . . ?
C363 C362 C361 117.4(13) . . ?
C362 C363 C364 120.9(13) . . ?
C365 C364 C363 114.8(15) . . ?
C366 C365 C364 130.2(16) . . ?
C365 C366 C367 117.7(15) . . ?
C362 C367 C366 119.1(14) . . ?
C412 C411 C416 121.1(8) . . ?
C412 C411 P4 119.6(6) . . ?
C416 C411 P4 119.1(7) . . ?
C411 C412 C413 118.6(9) . . ?
C414 C413 C412 120.3(10) . . ?
C413 C414 C415 121.7(10) . . ?
C414 C415 C416 118.9(9) . . ?
C411 C416 C415 119.3(9) . . ?
C422 C421 C426 118.5(9) . . ?
C422 C421 P4 120.8(8) . . ?
C426 C421 P4 119.8(8) . . ?
C423 C422 C421 121.1(11) . . ?
C424 C423 C422 121.2(12) . . ?
C423 C424 C425 120.3(11) . . ?
C424 C425 C426 119.6(11) . . ?
C425 C426 C421 119.3(10) . . ?

_refine_diff_density_max         1.218
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.098

#====END
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.341 -0.250 0.364 801 312 ' '
2 0.659 0.250 0.453 801 312 ' '

_platon_squeeze_details          
;
;
_vrf_THETM01_14                  
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: inherently weak scatterer, no data above \Q = 19.6\%
;
_vrf_PLAT023_14                  
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda 
RESPONSE: inherently weak scatterer, no data above \Q = 19.6\%
;
####################################################################### 
# 
# 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_16
_database_code_depnum_ccdc_archive 'CCDC 1031970'
_audit_update_record             
;
2014-10-31 deposited with the CCDC.
2015-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H46 Cl Ir N6 P2, (C H Cl3)3'
_chemical_formula_sum            'C53 H49 Cl10 Ir N6 P2'
_chemical_formula_weight         1378.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_cell_length_a                   14.3765(3)
_cell_length_b                   14.3894(3)
_cell_length_c                   16.3672(3)
_cell_angle_alpha                113.044(2)
_cell_angle_beta                 95.930(2)
_cell_angle_gamma                111.798(2)
_cell_volume                     2767.68(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    36496
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      30.83

_exptl_crystal_description       'flattened prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1372
_exptl_absorpt_coefficient_mu    2.996
_exptl_absorpt_correction_T_min  0.82523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. 
CrysAlisPro (Agilent Technologies,2012)
;

_exptl_special_details           ?

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            73416
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         30.03
_reflns_number_total             15709
_reflns_number_gt                14139
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2012)'
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0273P)²+3.0511P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15709
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0629
_refine_ls_wR_factor_gt          0.0598
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.264050(6) 0.187601(7) 0.720099(6) 0.01686(3) Uani 1 1 d . . .
Cl1 Cl 0.45122(4) 0.29850(5) 0.76923(4) 0.02577(11) Uani 1 1 d . . .
P1 P 0.28329(4) 0.06321(5) 0.58573(4) 0.01703(10) Uani 1 1 d . . .
P2 P 0.29693(4) 0.10829(5) 0.81791(4) 0.01750(10) Uani 1 1 d . . .
N2 N 0.57706(16) 0.12511(18) 0.61339(15) 0.0248(4) Uani 1 1 d . . .
N1 N 0.55675(14) 0.08009(16) 0.67134(14) 0.0212(4) Uani 1 1 d . . .
N3 N 0.48960(15) 0.11797(17) 0.57245(14) 0.0222(4) Uani 1 1 d . . .
N4 N 0.41829(16) -0.10540(16) 0.71793(14) 0.0229(4) Uani 1 1 d . . .
N5 N 0.37125(17) -0.14011(17) 0.77457(15) 0.0267(4) Uani 1 1 d . . .
N6 N 0.32742(16) -0.07501(17) 0.81207(14) 0.0241(4) Uani 1 1 d . . .
C1 C 0.2598(2) 0.3436(2) 0.80171(19) 0.0277(5) Uani 1 1 d . . .
H1 H 0.3282 0.4039 0.8489 0.033 Uiso 1 1 calc R . .
C2 C 0.1667(2) 0.3308(2) 0.8400(2) 0.0402(7) Uani 1 1 d . . .
H2A H 0.1470 0.3911 0.8439 0.048 Uiso 1 1 calc R . .
H2B H 0.1870 0.3407 0.9036 0.048 Uiso 1 1 calc R . .
C3 C 0.0727(2) 0.2165(2) 0.78065(19) 0.0322(6) Uani 1 1 d . . .
H3A H 0.0229 0.2251 0.7411 0.039 Uiso 1 1 calc R . .
H3B H 0.0369 0.1907 0.8217 0.039 Uiso 1 1 calc R . .
C4 C 0.10114(17) 0.1259(2) 0.71848(17) 0.0238(5) Uani 1 1 d . . .
H4 H 0.0727 0.0547 0.7243 0.029 Uiso 1 1 calc R . .
C5 C 0.10551(17) 0.10892(19) 0.62811(16) 0.0218(4) Uani 1 1 d . . .
H5 H 0.0803 0.0279 0.5822 0.026 Uiso 1 1 calc R . .
C6 C 0.08818(19) 0.1797(2) 0.58597(18) 0.0275(5) Uani 1 1 d . . .
H6A H 0.1019 0.1561 0.5248 0.033 Uiso 1 1 calc R . .
H6B H 0.0139 0.1649 0.5754 0.033 Uiso 1 1 calc R . .
C7 C 0.1565(2) 0.3047(3) 0.6453(2) 0.0436(7) Uani 1 1 d . . .
H7A H 0.1172 0.3386 0.6831 0.052 Uiso 1 1 calc R . .
H7B H 0.1752 0.3407 0.6049 0.052 Uiso 1 1 calc R . .
C8 C 0.2568(2) 0.3278(2) 0.7096(2) 0.0308(6) Uani 1 1 d . . .
H8 H 0.3228 0.3797 0.7047 0.037 Uiso 1 1 calc R . .
C11 C 0.45379(16) 0.04259(18) 0.66770(15) 0.0179(4) Uani 1 1 d . . .
C12 C 0.41184(17) 0.06832(18) 0.60468(15) 0.0190(4) Uani 1 1 d . . .
C13 C 0.64418(19) 0.0907(2) 0.73530(18) 0.0274(5) Uani 1 1 d . . .
H13A H 0.6850 0.0575 0.6992 0.033 Uiso 1 1 calc R . .
H13B H 0.6160 0.0476 0.7690 0.033 Uiso 1 1 calc R . .
C21 C 0.40627(17) -0.01476(18) 0.71967(16) 0.0189(4) Uani 1 1 d . . .
C22 C 0.34582(17) 0.00285(18) 0.77932(15) 0.0190(4) Uani 1 1 d . . .
C23 C 0.4677(2) -0.1694(2) 0.6603(2) 0.0306(5) Uani 1 1 d . . .
H23A H 0.5319 -0.1572 0.7006 0.037 Uiso 1 1 calc R . .
H23B H 0.4884 -0.1409 0.6157 0.037 Uiso 1 1 calc R . .
C111 C 0.27529(18) 0.10107(19) 0.49202(16) 0.0209(4) Uani 1 1 d . . .
C112 C 0.3514(2) 0.2066(2) 0.50760(19) 0.0281(5) Uani 1 1 d . . .
H112 H 0.4082 0.2521 0.5629 0.034 Uiso 1 1 calc R . .
C113 C 0.3439(2) 0.2447(2) 0.4425(2) 0.0353(6) Uani 1 1 d . . .
H113 H 0.3966 0.3152 0.4526 0.042 Uiso 1 1 calc R . .
C114 C 0.2598(3) 0.1804(3) 0.3630(2) 0.0383(6) Uani 1 1 d . . .
H114 H 0.2543 0.2075 0.3192 0.046 Uiso 1 1 calc R . .
C115 C 0.1837(2) 0.0766(3) 0.34695(19) 0.0363(6) Uani 1 1 d . . .
H115 H 0.1261 0.0325 0.2922 0.044 Uiso 1 1 calc R . .
C116 C 0.1918(2) 0.0370(2) 0.41113(17) 0.0270(5) Uani 1 1 d . . .
H116 H 0.1398 -0.0346 0.3996 0.032 Uiso 1 1 calc R . .
C121 C 0.19786(17) -0.08894(18) 0.53216(16) 0.0198(4) Uani 1 1 d . . .
C122 C 0.20239(19) -0.1644(2) 0.44913(18) 0.0261(5) Uani 1 1 d . . .
H122 H 0.2514 -0.1370 0.4194 0.031 Uiso 1 1 calc R . .
C123 C 0.1356(2) -0.2792(2) 0.4097(2) 0.0324(6) Uani 1 1 d . . .
H123 H 0.1377 -0.3299 0.3523 0.039 Uiso 1 1 calc R . .
C124 C 0.0657(2) -0.3201(2) 0.4542(2) 0.0338(6) Uani 1 1 d . . .
H124 H 0.0201 -0.3987 0.4271 0.041 Uiso 1 1 calc R . .
C125 C 0.0628(2) -0.2464(2) 0.5377(2) 0.0305(5) Uani 1 1 d . . .
H125 H 0.0161 -0.2743 0.5689 0.037 Uiso 1 1 calc R . .
C126 C 0.12829(19) -0.1313(2) 0.57599(17) 0.0239(5) Uani 1 1 d . . .
H126 H 0.1254 -0.0808 0.6331 0.029 Uiso 1 1 calc R . .
C161 C 0.71562(19) 0.2126(2) 0.80457(18) 0.0277(5) Uani 1 1 d . . .
C162 C 0.8199(2) 0.2613(3) 0.8073(2) 0.0392(7) Uani 1 1 d . . .
H162 H 0.8465 0.2182 0.7651 0.047 Uiso 1 1 calc R . .
C163 C 0.8856(3) 0.3731(3) 0.8718(3) 0.0572(10) Uani 1 1 d . . .
H163 H 0.9569 0.4066 0.8733 0.069 Uiso 1 1 calc R . .
C164 C 0.8477(3) 0.4350(3) 0.9333(3) 0.0620(11) Uani 1 1 d . . .
H164 H 0.8930 0.5113 0.9775 0.074 Uiso 1 1 calc R . .
C165 C 0.7447(3) 0.3875(3) 0.9313(2) 0.0534(9) Uani 1 1 d . . .
H165 H 0.7188 0.4310 0.9742 0.064 Uiso 1 1 calc R . .
C166 C 0.6781(2) 0.2761(3) 0.8669(2) 0.0378(6) Uani 1 1 d . . .
H166 H 0.6068 0.2435 0.8655 0.045 Uiso 1 1 calc R . .
C211 C 0.18066(18) 0.0347(2) 0.84633(17) 0.0248(5) Uani 1 1 d . . .
C212 C 0.1478(2) 0.1012(3) 0.91279(19) 0.0345(6) Uani 1 1 d . . .
H212 H 0.1929 0.1795 0.9508 0.041 Uiso 1 1 calc R . .
C213 C 0.0494(3) 0.0531(4) 0.9235(2) 0.0498(9) Uani 1 1 d . . .
H213 H 0.0271 0.0992 0.9682 0.060 Uiso 1 1 calc R . .
C214 C -0.0159(2) -0.0601(4) 0.8703(3) 0.0555(10) Uani 1 1 d . . .
H214 H -0.0835 -0.0918 0.8775 0.067 Uiso 1 1 calc R . .
C215 C 0.0161(2) -0.1280(3) 0.8066(2) 0.0441(8) Uani 1 1 d . . .
H215 H -0.0288 -0.2067 0.7708 0.053 Uiso 1 1 calc R . .
C216 C 0.1146(2) -0.0813(2) 0.79434(19) 0.0308(5) Uani 1 1 d . . .
H216 H 0.1367 -0.1285 0.7505 0.037 Uiso 1 1 calc R . .
C221 C 0.39088(18) 0.2092(2) 0.93340(16) 0.0224(4) Uani 1 1 d . . .
C222 C 0.4052(2) 0.3201(2) 0.97405(18) 0.0289(5) Uani 1 1 d . . .
H222 H 0.3684 0.3432 0.9406 0.035 Uiso 1 1 calc R . .
C223 C 0.4722(2) 0.3976(2) 1.06268(18) 0.0337(6) Uani 1 1 d . . .
H223 H 0.4811 0.4731 1.0896 0.040 Uiso 1 1 calc R . .
C224 C 0.5260(2) 0.3649(3) 1.1118(2) 0.0401(7) Uani 1 1 d . . .
H224 H 0.5720 0.4179 1.1725 0.048 Uiso 1 1 calc R . .
C225 C 0.5131(3) 0.2552(3) 1.0727(2) 0.0440(7) Uani 1 1 d . . .
H225 H 0.5499 0.2326 1.1065 0.053 Uiso 1 1 calc R . .
C226 C 0.4457(2) 0.1776(2) 0.98352(19) 0.0339(6) Uani 1 1 d . . .
H226 H 0.4373 0.1022 0.9568 0.041 Uiso 1 1 calc R . .
C261 C 0.3945(2) -0.2940(2) 0.60804(19) 0.0277(5) Uani 1 1 d . . .
C262 C 0.4101(2) -0.3683(2) 0.6352(2) 0.0376(6) Uani 1 1 d . . .
H262 H 0.4660 -0.3404 0.6881 0.045 Uiso 1 1 calc R . .
C263 C 0.3440(3) -0.4835(3) 0.5849(3) 0.0460(8) Uani 1 1 d . . .
H263 H 0.3560 -0.5346 0.6025 0.055 Uiso 1 1 calc R . .
C264 C 0.2618(3) -0.5237(3) 0.5102(2) 0.0455(8) Uani 1 1 d . . .
H264 H 0.2158 -0.6024 0.4769 0.055 Uiso 1 1 calc R . .
C265 C 0.2455(3) -0.4506(3) 0.4832(2) 0.0493(8) Uani 1 1 d . . .
H265 H 0.1883 -0.4787 0.4312 0.059 Uiso 1 1 calc R . .
C266 C 0.3123(3) -0.3361(3) 0.5315(2) 0.0423(7) Uani 1 1 d . . .
H266 H 0.3015 -0.2860 0.5118 0.051 Uiso 1 1 calc R . .
C100 C 0.1373(3) 0.6539(3) 0.7783(2) 0.0469(8) Uani 1 1 d . . .
H100 H 0.1696 0.7375 0.8190 0.056 Uiso 1 1 calc R . .
Cl11 Cl 0.21095(12) 0.60133(13) 0.81755(13) 0.1121(6) Uani 1 1 d . . .
Cl12 Cl 0.00795(9) 0.59437(11) 0.78296(10) 0.0864(4) Uani 1 1 d . . .
Cl13 Cl 0.13552(10) 0.62901(9) 0.66495(8) 0.0772(3) Uani 1 1 d . . .
C200 C -0.2739(3) 0.0312(4) 0.9681(2) 0.0537(9) Uani 1 1 d . . .
H200 H -0.2665 0.0177 1.0233 0.064 Uiso 1 1 calc R . .
Cl21 Cl -0.38333(8) 0.05578(11) 0.95506(8) 0.0684(3) Uani 1 1 d . . .
Cl22 Cl -0.16037(10) 0.14988(13) 0.98803(10) 0.0869(4) Uani 1 1 d . . .
Cl23 Cl -0.29020(11) -0.08879(15) 0.87094(9) 0.1099(6) Uani 1 1 d . . .
C300 C 0.6664(3) 0.5197(3) 0.7662(3) 0.0550(9) Uani 1 1 d . . .
H300 H 0.6174 0.4958 0.8011 0.066 Uiso 1 1 calc R . .
Cl31 Cl 0.70365(9) 0.41433(9) 0.71515(7) 0.0609(2) Uani 1 1 d . . .
Cl32 Cl 0.77475(14) 0.64537(12) 0.84569(15) 0.1397(8) Uani 1 1 d . . .
Cl33 Cl 0.59923(15) 0.53709(17) 0.68238(14) 0.1188(6) Uani 1 1 d . . .


_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
Ir1 C8 2.130(2) . ?
Ir1 C1 2.144(2) . ?
Ir1 C4 2.168(2) . ?
Ir1 C5 2.187(2) . ?
Ir1 P1 2.3512(6) . ?
Ir1 P2 2.4007(6) . ?
Ir1 Cl1 2.4069(6) . ?
P1 C12 1.811(2) . ?
P1 C111 1.824(2) . ?
P1 C121 1.830(2) . ?
P2 C22 1.824(2) . ?
P2 C211 1.834(2) . ?
P2 C221 1.837(2) . ?
N2 N3 1.310(3) . ?
N2 N1 1.343(3) . ?
N1 C11 1.360(3) . ?
N1 C13 1.469(3) . ?
N3 C12 1.364(3) . ?
N4 N5 1.344(3) . ?
N4 C21 1.368(3) . ?
N4 C23 1.479(3) . ?
N5 N6 1.311(3) . ?
N6 C22 1.375(3) . ?
C1 C8 1.428(4) . ?
C1 C2 1.517(4) . ?
C2 C3 1.517(4) . ?
C3 C4 1.532(3) . ?
C4 C5 1.414(3) . ?
C5 C6 1.510(3) . ?
C6 C7 1.505(4) . ?
C7 C8 1.534(4) . ?
C11 C12 1.379(3) . ?
C11 C21 1.457(3) . ?
C13 C161 1.510(4) . ?
C21 C22 1.385(3) . ?
C23 C261 1.505(4) . ?
C111 C116 1.392(3) . ?
C111 C112 1.405(3) . ?
C112 C113 1.387(4) . ?
C113 C114 1.383(4) . ?
C114 C115 1.385(4) . ?
C115 C116 1.391(4) . ?
C121 C126 1.387(3) . ?
C121 C122 1.395(3) . ?
C122 C123 1.388(4) . ?
C123 C124 1.390(4) . ?
C124 C125 1.380(4) . ?
C125 C126 1.390(3) . ?
C161 C166 1.384(4) . ?
C161 C162 1.387(4) . ?
C162 C163 1.389(5) . ?
C163 C164 1.370(6) . ?
C164 C165 1.373(6) . ?
C165 C166 1.388(4) . ?
C211 C212 1.396(4) . ?
C211 C216 1.398(4) . ?
C212 C213 1.390(4) . ?
C213 C214 1.371(6) . ?
C214 C215 1.373(5) . ?
C215 C216 1.398(4) . ?
C221 C226 1.388(3) . ?
C221 C222 1.388(3) . ?
C222 C223 1.387(4) . ?
C223 C224 1.379(4) . ?
C224 C225 1.379(4) . ?
C225 C226 1.394(4) . ?
C261 C266 1.379(4) . ?
C261 C262 1.386(4) . ?
C262 C263 1.389(4) . ?
C263 C264 1.366(5) . ?
C264 C265 1.372(5) . ?
C265 C266 1.382(4) . ?
C100 Cl11 1.716(4) . ?
C100 Cl13 1.742(4) . ?
C100 Cl12 1.759(4) . ?
C200 Cl23 1.743(4) . ?
C200 Cl21 1.746(3) . ?
C200 Cl22 1.752(4) . ?
C300 Cl31 1.729(4) . ?
C300 Cl32 1.742(4) . ?
C300 Cl33 1.746(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
C8 Ir1 C1 39.03(11) . . ?
C8 Ir1 C4 88.81(10) . . ?
C1 Ir1 C4 79.38(9) . . ?
C8 Ir1 C5 78.46(9) . . ?
C1 Ir1 C5 93.91(9) . . ?
C4 Ir1 C5 37.89(9) . . ?
C8 Ir1 P1 112.80(8) . . ?
C1 Ir1 P1 151.42(8) . . ?
C4 Ir1 P1 110.44(7) . . ?
C5 Ir1 P1 81.00(6) . . ?
C8 Ir1 P2 148.12(8) . . ?
C1 Ir1 P2 109.72(8) . . ?
C4 Ir1 P2 90.44(7) . . ?
C5 Ir1 P2 118.13(7) . . ?
P1 Ir1 P2 97.277(19) . . ?
C8 Ir1 Cl1 85.79(7) . . ?
C1 Ir1 Cl1 85.79(7) . . ?
C4 Ir1 Cl1 162.19(7) . . ?
C5 Ir1 Cl1 154.82(7) . . ?
P1 Ir1 Cl1 87.27(2) . . ?
P2 Ir1 Cl1 85.30(2) . . ?
C12 P1 C111 103.02(10) . . ?
C12 P1 C121 101.64(10) . . ?
C111 P1 C121 105.36(11) . . ?
C12 P1 Ir1 112.22(7) . . ?
C111 P1 Ir1 112.57(8) . . ?
C121 P1 Ir1 120.18(8) . . ?
C22 P2 C211 101.29(11) . . ?
C22 P2 C221 100.90(10) . . ?
C211 P2 C221 102.05(11) . . ?
C22 P2 Ir1 120.15(7) . . ?
C211 P2 Ir1 113.65(8) . . ?
C221 P2 Ir1 116.15(8) . . ?
N3 N2 N1 108.02(18) . . ?
N2 N1 C11 110.49(19) . . ?
N2 N1 C13 119.22(19) . . ?
C11 N1 C13 129.7(2) . . ?
N2 N3 C12 108.7(2) . . ?
N5 N4 C21 111.10(19) . . ?
N5 N4 C23 119.5(2) . . ?
C21 N4 C23 129.3(2) . . ?
N6 N5 N4 107.46(19) . . ?
N5 N6 C22 109.4(2) . . ?
C8 C1 C2 124.3(3) . . ?
C8 C1 Ir1 69.94(14) . . ?
C2 C1 Ir1 114.55(18) . . ?
C1 C2 C3 112.5(2) . . ?
C2 C3 C4 113.4(2) . . ?
C5 C4 C3 121.6(2) . . ?
C5 C4 Ir1 71.80(13) . . ?
C3 C4 Ir1 114.64(17) . . ?
C4 C5 C6 124.2(2) . . ?
C4 C5 Ir1 70.31(13) . . ?
C6 C5 Ir1 113.26(16) . . ?
C7 C6 C5 113.5(2) . . ?
C6 C7 C8 111.2(2) . . ?
C1 C8 C7 119.5(3) . . ?
C1 C8 Ir1 71.02(14) . . ?
C7 C8 Ir1 117.31(18) . . ?
N1 C11 C12 104.41(19) . . ?
N1 C11 C21 123.8(2) . . ?
C12 C11 C21 131.8(2) . . ?
N3 C12 C11 108.34(19) . . ?
N3 C12 P1 125.29(17) . . ?
C11 C12 P1 125.32(17) . . ?
N1 C13 C161 111.8(2) . . ?
N4 C21 C22 104.2(2) . . ?
N4 C21 C11 122.3(2) . . ?
C22 C21 C11 133.5(2) . . ?
N6 C22 C21 107.80(19) . . ?
N6 C22 P2 121.31(17) . . ?
C21 C22 P2 130.86(17) . . ?
N4 C23 C261 111.4(2) . . ?
C116 C111 C112 118.7(2) . . ?
C116 C111 P1 123.25(18) . . ?
C112 C111 P1 117.62(18) . . ?
C113 C112 C111 120.3(3) . . ?
C114 C113 C112 120.1(3) . . ?
C113 C114 C115 120.3(3) . . ?
C114 C115 C116 119.8(3) . . ?
C115 C116 C111 120.7(2) . . ?
C126 C121 C122 118.8(2) . . ?
C126 C121 P1 119.47(18) . . ?
C122 C121 P1 121.72(18) . . ?
C123 C122 C121 120.3(2) . . ?
C122 C123 C124 120.1(2) . . ?
C125 C124 C123 120.0(2) . . ?
C124 C125 C126 119.7(2) . . ?
C121 C126 C125 121.1(2) . . ?
C166 C161 C162 119.4(3) . . ?
C166 C161 C13 120.4(2) . . ?
C162 C161 C13 120.2(3) . . ?
C161 C162 C163 120.0(3) . . ?
C164 C163 C162 120.1(3) . . ?
C163 C164 C165 120.4(3) . . ?
C164 C165 C166 120.1(3) . . ?
C161 C166 C165 120.1(3) . . ?
C212 C211 C216 118.6(2) . . ?
C212 C211 P2 117.4(2) . . ?
C216 C211 P2 123.10(19) . . ?
C213 C212 C211 120.2(3) . . ?
C214 C213 C212 120.6(3) . . ?
C213 C214 C215 120.2(3) . . ?
C214 C215 C216 120.1(3) . . ?
C211 C216 C215 120.2(3) . . ?
C226 C221 C222 118.4(2) . . ?
C226 C221 P2 122.23(19) . . ?
C222 C221 P2 119.35(19) . . ?
C223 C222 C221 121.0(2) . . ?
C224 C223 C222 120.0(3) . . ?
C225 C224 C223 120.0(3) . . ?
C224 C225 C226 119.9(3) . . ?
C221 C226 C225 120.7(3) . . ?
C266 C261 C262 119.1(3) . . ?
C266 C261 C23 120.6(2) . . ?
C262 C261 C23 120.3(3) . . ?
C261 C262 C263 120.0(3) . . ?
C264 C263 C262 120.3(3) . . ?
C263 C264 C265 120.1(3) . . ?
C264 C265 C266 120.0(3) . . ?
C261 C266 C265 120.5(3) . . ?
Cl11 C100 Cl13 110.9(2) . . ?
Cl11 C100 Cl12 111.5(2) . . ?
Cl13 C100 Cl12 109.3(2) . . ?
Cl23 C200 Cl21 110.5(2) . . ?
Cl23 C200 Cl22 111.0(2) . . ?
Cl21 C200 Cl22 110.3(2) . . ?
Cl31 C300 Cl32 110.4(2) . . ?
Cl31 C300 Cl33 111.0(2) . . ?
Cl32 C300 Cl33 112.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.266
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.091

#====END







