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

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

data_ad1ck
_database_code_depnum_ccdc_archive 'CCDC 1572769'
_audit_update_record             
;
2017-09-05 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H60 Cl N4 P2 1+, 3(C H2 Cl2), Cl 1-'
_chemical_formula_sum            'C51 H66 Cl8 N4 P2'
_chemical_formula_weight         1080.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2720(8)
_cell_length_b                   15.0620(10)
_cell_length_c                   16.43380(10)
_cell_angle_alpha                94.872(5)
_cell_angle_beta                 91.976(5)
_cell_angle_gamma                93.136(5)
_cell_volume                     2773.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17941
_cell_measurement_theta_min      3.79
_cell_measurement_theta_max      76.13

_exptl_crystal_description       flake
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    4.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 The crystal was mounted at rt with perfluoroether oil on top of a human hair
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 41 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.3 deg in ω.
 Each frame was exposured for 10 s (low 2θ angles) or 30 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;



_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            64014
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.823
_diffrn_reflns_theta_max         76.318
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11513
_reflns_number_gt                9141
_reflns_threshold_expression     'I > 2σ(I)'


_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;



_computing_data_collection       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_molecular_graphics    
;

;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;





_refine_special_details          
;
 A disordered molecule of dichloromethane was refined using a
 split atom model (0.535(7) SOF of main component).

 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond but not tip.


 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 > 2sigma(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)+(0.0801P)²+2.5541P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         11513
_refine_ls_number_parameters     628
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1595
_refine_ls_wR_factor_gt          0.1472
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_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
C1 C 0.6376(2) 0.65836(16) 0.26127(15) 0.0220(5) Uani 1 1 d . . . . .
C2 C 0.5817(2) 0.52371(17) 0.19922(17) 0.0248(5) Uani 1 1 d . . . . .
H2 H 0.5606 0.4775 0.1574 0.030 Uiso 1 1 calc R U . . .
C3 C 0.5849(2) 0.51535(17) 0.28014(16) 0.0251(5) Uani 1 1 d . . . . .
H3 H 0.5672 0.4625 0.3061 0.030 Uiso 1 1 calc R U . . .
C4 C 0.6342(3) 0.64346(17) 0.10752(16) 0.0249(5) Uani 1 1 d . . . . .
C5 C 0.5346(3) 0.65771(17) 0.05781(17) 0.0280(6) Uani 1 1 d . . . . .
C6 C 0.5567(3) 0.68291(19) -0.02074(18) 0.0349(7) Uani 1 1 d . . . . .
H6 H 0.4916 0.6930 -0.0564 0.042 Uiso 1 1 calc R U . . .
C7 C 0.6701(3) 0.6932(2) -0.04702(19) 0.0411(7) Uani 1 1 d . . . . .
H7 H 0.6828 0.7106 -0.1004 0.049 Uiso 1 1 calc R U . . .
C8 C 0.7671(3) 0.6786(2) 0.00387(19) 0.0393(7) Uani 1 1 d . . . . .
H8 H 0.8453 0.6861 -0.0152 0.047 Uiso 1 1 calc R U . . .
C9 C 0.7509(3) 0.6529(2) 0.08269(17) 0.0310(6) Uani 1 1 d . . . . .
C10 C 0.4084(3) 0.64574(19) 0.08454(18) 0.0320(6) Uani 1 1 d . . . . .
H10 H 0.4108 0.6375 0.1443 0.038 Uiso 1 1 calc R U . . .
C11 C 0.3373(3) 0.7278(2) 0.0710(2) 0.0446(8) Uani 1 1 d . . . . .
H11A H 0.3805 0.7815 0.0972 0.067 Uiso 1 1 calc R U . . .
H11B H 0.2592 0.7208 0.0949 0.067 Uiso 1 1 calc R U . . .
H11C H 0.3268 0.7335 0.0122 0.067 Uiso 1 1 calc R U . . .
C12 C 0.3449(3) 0.5624(2) 0.0391(2) 0.0388(7) Uani 1 1 d . . . . .
H12A H 0.3375 0.5707 -0.0194 0.058 Uiso 1 1 calc R U . . .
H12B H 0.2656 0.5531 0.0605 0.058 Uiso 1 1 calc R U . . .
H12C H 0.3910 0.5103 0.0470 0.058 Uiso 1 1 calc R U . . .
C13 C 0.8594(3) 0.6343(2) 0.13499(19) 0.0362(7) Uani 1 1 d . . . . .
H13 H 0.8319 0.6226 0.1905 0.043 Uiso 1 1 calc R U . . .
C14 C 0.9504(3) 0.7137(3) 0.1450(3) 0.0569(10) Uani 1 1 d . . . . .
H14A H 0.9792 0.7263 0.0914 0.085 Uiso 1 1 calc R U . . .
H14B H 1.0174 0.6997 0.1804 0.085 Uiso 1 1 calc R U . . .
H14C H 0.9131 0.7662 0.1698 0.085 Uiso 1 1 calc R U . . .
C15 C 0.9164(4) 0.5514(3) 0.0993(3) 0.0680(13) Uani 1 1 d . . . . .
H15A H 0.8585 0.5002 0.0967 0.102 Uiso 1 1 calc R U . . .
H15B H 0.9853 0.5398 0.1341 0.102 Uiso 1 1 calc R U . . .
H15C H 0.9423 0.5606 0.0442 0.102 Uiso 1 1 calc R U . . .
C16 C 0.6474(3) 0.62120(16) 0.40470(16) 0.0265(5) Uani 1 1 d . . . . .
C17 C 0.7650(3) 0.61500(18) 0.43196(17) 0.0307(6) Uani 1 1 d . . . . .
C18 C 0.7928(3) 0.6408(2) 0.51469(19) 0.0380(7) Uani 1 1 d . . . . .
H18 H 0.8720 0.6378 0.5356 0.046 Uiso 1 1 calc R U . . .
C19 C 0.7060(4) 0.6705(2) 0.56616(18) 0.0410(8) Uani 1 1 d . . . . .
H19 H 0.7264 0.6885 0.6219 0.049 Uiso 1 1 calc R U . . .
C20 C 0.5896(3) 0.6741(2) 0.53719(18) 0.0372(7) Uani 1 1 d . . . . .
H20 H 0.5309 0.6934 0.5738 0.045 Uiso 1 1 calc R U . . .
C21 C 0.5572(3) 0.65006(18) 0.45544(17) 0.0308(6) Uani 1 1 d . . . . .
C22 C 0.8601(3) 0.5797(2) 0.3767(2) 0.0356(6) Uani 1 1 d . . . . .
H22 H 0.8278 0.5764 0.3190 0.043 Uiso 1 1 calc R U . . .
C23 C 0.9725(3) 0.6401(3) 0.3828(3) 0.0531(9) Uani 1 1 d . . . . .
H23A H 0.9533 0.7002 0.3700 0.080 Uiso 1 1 calc R U . . .
H23B H 1.0294 0.6164 0.3439 0.080 Uiso 1 1 calc R U . . .
H23C H 1.0076 0.6427 0.4384 0.080 Uiso 1 1 calc R U . . .
C24 C 0.8863(4) 0.4850(3) 0.3964(3) 0.0561(10) Uani 1 1 d . . . . .
H24A H 0.9116 0.4857 0.4541 0.084 Uiso 1 1 calc R U . . .
H24B H 0.9496 0.4630 0.3621 0.084 Uiso 1 1 calc R U . . .
H24C H 0.8143 0.4457 0.3857 0.084 Uiso 1 1 calc R U . . .
C25 C 0.4292(3) 0.6498(2) 0.4251(2) 0.0362(7) Uani 1 1 d . . . . .
H25 H 0.4282 0.6517 0.3644 0.043 Uiso 1 1 calc R U . . .
C26 C 0.3637(4) 0.7301(3) 0.4615(3) 0.0588(10) Uani 1 1 d . . . . .
H26A H 0.3529 0.7247 0.5198 0.088 Uiso 1 1 calc R U . . .
H26B H 0.2859 0.7312 0.4333 0.088 Uiso 1 1 calc R U . . .
H26C H 0.4107 0.7854 0.4545 0.088 Uiso 1 1 calc R U . . .
C27 C 0.3623(4) 0.5639(3) 0.4436(3) 0.0597(11) Uani 1 1 d . . . . .
H27A H 0.4024 0.5127 0.4192 0.090 Uiso 1 1 calc R U . . .
H27B H 0.2807 0.5627 0.4207 0.090 Uiso 1 1 calc R U . . .
H27C H 0.3607 0.5611 0.5029 0.090 Uiso 1 1 calc R U . . .
C28 C 0.5920(2) 0.94691(17) 0.26987(16) 0.0241(5) Uani 1 1 d . . . . .
C29 C 0.5289(3) 1.08436(18) 0.30038(18) 0.0321(6) Uani 1 1 d . . . . .
H29 H 0.4830 1.1354 0.3000 0.039 Uiso 1 1 calc R U . . .
C30 C 0.6287(3) 1.07606(18) 0.34650(19) 0.0312(6) Uani 1 1 d . . . . .
H30 H 0.6659 1.1203 0.3852 0.037 Uiso 1 1 calc R U . . .
C31 C 0.4055(3) 0.9827(2) 0.19729(18) 0.0329(6) Uani 1 1 d . . . . .
C32 C 0.3106(3) 0.9282(2) 0.2216(2) 0.0387(7) Uani 1 1 d . . . . .
C33 C 0.2142(3) 0.9086(2) 0.1664(2) 0.0436(8) Uani 1 1 d . . . . .
H33 H 0.1483 0.8725 0.1817 0.052 Uiso 1 1 calc R U . . .
C34 C 0.2126(3) 0.9400(2) 0.0910(2) 0.0469(8) Uani 1 1 d . . . . .
C35 C 0.3049(4) 0.9951(2) 0.0691(2) 0.0473(9) Uani 1 1 d . . . . .
H35 H 0.3013 1.0178 0.0170 0.057 Uiso 1 1 calc R U . . .
C36 C 0.4063(3) 1.0193(2) 0.12240(19) 0.0401(7) Uani 1 1 d . . . . .
C37 C 0.3109(3) 0.8912(3) 0.3034(2) 0.0478(8) Uani 1 1 d . . . . .
H37A H 0.3769 0.8519 0.3078 0.072 Uiso 1 1 calc R U . . .
H37B H 0.2355 0.8571 0.3092 0.072 Uiso 1 1 calc R U . . .
H37C H 0.3205 0.9403 0.3466 0.072 Uiso 1 1 calc R U . . .
C38 C 0.1091(4) 0.9141(3) 0.0299(3) 0.0632(12) Uani 1 1 d . . . . .
H38A H 0.1134 0.8515 0.0088 0.095 Uiso 1 1 calc R U . . .
H38B H 0.1135 0.9522 -0.0154 0.095 Uiso 1 1 calc R U . . .
H38C H 0.0339 0.9217 0.0572 0.095 Uiso 1 1 calc R U . . .
C39 C 0.5048(4) 1.0823(2) 0.1011(2) 0.0490(9) Uani 1 1 d . . . . .
H39A H 0.4982 1.1404 0.1319 0.074 Uiso 1 1 calc R U . . .
H39B H 0.4995 1.0894 0.0424 0.074 Uiso 1 1 calc R U . . .
H39C H 0.5814 1.0585 0.1151 0.074 Uiso 1 1 calc R U . . .
C40 C 0.7705(2) 0.95816(17) 0.36643(17) 0.0251(5) Uani 1 1 d . . . . .
C41 C 0.8778(3) 0.96251(18) 0.32769(18) 0.0291(6) Uani 1 1 d . . . . .
C42 C 0.9759(3) 0.93052(19) 0.3685(2) 0.0336(6) Uani 1 1 d . . . . .
H42 H 1.0509 0.9326 0.3439 0.040 Uiso 1 1 calc R U . . .
C43 C 0.9665(3) 0.89591(19) 0.44389(19) 0.0342(6) Uani 1 1 d . . . . .
C44 C 0.8572(3) 0.89306(19) 0.47937(18) 0.0321(6) Uani 1 1 d . . . . .
H44 H 0.8501 0.8687 0.5306 0.039 Uiso 1 1 calc R U . . .
C45 C 0.7570(3) 0.92492(18) 0.44216(17) 0.0295(6) Uani 1 1 d . . . . .
C46 C 0.8904(3) 0.9996(2) 0.2462(2) 0.0403(7) Uani 1 1 d . . . . .
H46A H 0.8369 0.9651 0.2055 0.060 Uiso 1 1 calc R U . . .
H46B H 0.9727 0.9956 0.2295 0.060 Uiso 1 1 calc R U . . .
H46C H 0.8699 1.0621 0.2505 0.060 Uiso 1 1 calc R U . . .
C47 C 1.0734(3) 0.8623(2) 0.4872(2) 0.0454(8) Uani 1 1 d . . . . .
H47A H 1.1383 0.8566 0.4493 0.068 Uiso 1 1 calc R U . . .
H47B H 1.0522 0.8039 0.5065 0.068 Uiso 1 1 calc R U . . .
H47C H 1.0990 0.9046 0.5340 0.068 Uiso 1 1 calc R U . . .
C48 C 0.6394(3) 0.9205(2) 0.4819(2) 0.0394(7) Uani 1 1 d . . . . .
H48A H 0.6157 0.9812 0.4971 0.059 Uiso 1 1 calc R U . . .
H48B H 0.6462 0.8882 0.5310 0.059 Uiso 1 1 calc R U . . .
H48C H 0.5794 0.8893 0.4436 0.059 Uiso 1 1 calc R U . . .
C49 C 0.2544(4) 0.4596(3) 0.2311(3) 0.0592(10) Uani 1 1 d . . . . .
H49A H 0.2938 0.4464 0.1789 0.071 Uiso 1 1 calc R U . . .
H49B H 0.3084 0.4440 0.2759 0.071 Uiso 1 1 calc R U . . .
C50 C 0.1999(3) 0.1660(2) 0.2080(2) 0.0407(7) Uani 1 1 d . . . . .
H50A H 0.2333 0.2283 0.2174 0.049 Uiso 1 1 calc R U . . .
H50B H 0.2609 0.1301 0.1813 0.049 Uiso 1 1 calc R U . . .
N1 N 0.6191(2) 0.59867(14) 0.31809(13) 0.0234(4) Uani 1 1 d . . . . .
N2 N 0.6146(2) 0.61173(14) 0.18757(13) 0.0225(4) Uani 1 1 d . . . . .
N3 N 0.5068(2) 1.00385(15) 0.25384(14) 0.0274(5) Uani 1 1 d . . . . .
N4 N 0.6671(2) 0.99109(14) 0.32707(14) 0.0247(4) Uani 1 1 d . . . . .
P1 P 0.70015(7) 0.77024(4) 0.29273(4) 0.02928(16) Uani 1 1 d . . . . .
P2 P 0.58635(7) 0.83419(5) 0.21495(4) 0.02901(16) Uani 1 1 d . . . . .
Cl1 Cl 0.67327(9) 0.87949(5) 0.10992(5) 0.0472(2) Uani 1 1 d . . . . .
Cl2 Cl 0.46585(6) 0.29795(4) 0.25041(4) 0.02899(15) Uani 1 1 d . . . . .
Cl3 Cl 0.23077(8) 0.57487(6) 0.24418(6) 0.0503(2) Uani 1 1 d . . . . .
Cl4 Cl 0.12335(9) 0.39433(7) 0.23071(10) 0.0741(4) Uani 1 1 d . . . . .
Cl5 Cl 0.07534(8) 0.16344(6) 0.14152(5) 0.0485(2) Uani 1 1 d . . . . .
Cl6 Cl 0.17132(9) 0.12574(6) 0.30272(5) 0.0526(2) Uani 1 1 d . . . . .
C51 C 0.7638(6) 0.2482(5) 0.2222(5) 0.0412(16) Uani 0.535(7) 1 d . . P A 1
H51A H 0.7743 0.1907 0.1900 0.049 Uiso 0.535(7) 1 calc R U P A 1
H51B H 0.6782 0.2524 0.2325 0.049 Uiso 0.535(7) 1 calc R U P A 1
Cl7 Cl 0.81452(17) 0.33764(19) 0.16759(19) 0.0617(10) Uani 0.535(7) 1 d . . P A
1
Cl8 Cl 0.8480(7) 0.2536(5) 0.3171(5) 0.080(2) Uani 0.535(7) 1 d . . P A 1
C51' C 0.7742(9) 0.3050(10) 0.2410(7) 0.065(3) Uani 0.465(7) 1 d . . P A 2
H51C H 0.6884 0.3004 0.2520 0.078 Uiso 0.465(7) 1 calc R U P A 2
H51D H 0.8007 0.3690 0.2476 0.078 Uiso 0.465(7) 1 calc R U P A 2
Cl7' Cl 0.7925(5) 0.2653(8) 0.1425(2) 0.171(4) Uani 0.465(7) 1 d . . P A 2
Cl8' Cl 0.8517(4) 0.2494(4) 0.3151(3) 0.0381(12) Uani 0.465(7) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.357(3) . ?
C1 N1 1.363(3) . ?
C1 P1 1.817(3) . ?
C2 C3 1.346(4) . ?
C2 N2 1.388(3) . ?
C3 N1 1.382(3) . ?
C4 C9 1.394(4) . ?
C4 C5 1.403(4) . ?
C4 N2 1.457(3) . ?
C5 C6 1.403(4) . ?
C5 C10 1.509(4) . ?
C6 C7 1.369(5) . ?
C7 C8 1.392(5) . ?
C8 C9 1.398(4) . ?
C9 C13 1.522(4) . ?
C10 C12 1.533(4) . ?
C10 C11 1.537(4) . ?
C13 C15 1.519(5) . ?
C13 C14 1.527(5) . ?
C16 C17 1.396(4) . ?
C16 C21 1.401(4) . ?
C16 N1 1.455(3) . ?
C17 C18 1.402(4) . ?
C17 C22 1.518(4) . ?
C18 C19 1.383(5) . ?
C19 C20 1.386(5) . ?
C20 C21 1.392(4) . ?
C21 C25 1.511(5) . ?
C22 C23 1.514(5) . ?
C22 C24 1.532(5) . ?
C25 C27 1.520(5) . ?
C25 C26 1.540(5) . ?
C28 N4 1.349(3) . ?
C28 N3 1.356(3) . ?
C28 P2 1.851(3) . ?
C29 C30 1.353(4) . ?
C29 N3 1.383(4) . ?
C30 N4 1.388(3) . ?
C31 C36 1.391(4) . ?
C31 C32 1.402(5) . ?
C31 N3 1.451(4) . ?
C32 C33 1.394(5) . ?
C32 C37 1.498(5) . ?
C33 C34 1.365(5) . ?
C34 C35 1.372(6) . ?
C34 C38 1.524(5) . ?
C35 C36 1.427(5) . ?
C36 C39 1.491(6) . ?
C40 C41 1.387(4) . ?
C40 C45 1.390(4) . ?
C40 N4 1.446(3) . ?
C41 C42 1.402(4) . ?
C41 C46 1.502(4) . ?
C42 C43 1.390(5) . ?
C43 C44 1.382(5) . ?
C43 C47 1.511(4) . ?
C44 C45 1.393(4) . ?
C45 C48 1.498(4) . ?
C49 Cl4 1.729(4) . ?
C49 Cl3 1.767(4) . ?
C50 Cl5 1.745(3) . ?
C50 Cl6 1.751(3) . ?
P1 P2 2.1067(10) . ?
P2 Cl1 2.1560(11) . ?
C51 Cl7 1.762(7) . ?
C51 Cl8 1.792(10) . ?
C51' Cl7' 1.702(13) . ?
C51' Cl8' 1.767(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 N1 105.8(2) . . ?
N2 C1 P1 133.69(19) . . ?
N1 C1 P1 119.99(19) . . ?
C3 C2 N2 108.0(2) . . ?
C2 C3 N1 106.6(2) . . ?
C9 C4 C5 123.6(3) . . ?
C9 C4 N2 118.1(2) . . ?
C5 C4 N2 118.3(2) . . ?
C6 C5 C4 116.7(3) . . ?
C6 C5 C10 120.0(3) . . ?
C4 C5 C10 123.3(3) . . ?
C7 C6 C5 121.3(3) . . ?
C6 C7 C8 120.6(3) . . ?
C7 C8 C9 120.9(3) . . ?
C4 C9 C8 117.0(3) . . ?
C4 C9 C13 124.0(3) . . ?
C8 C9 C13 119.0(3) . . ?
C5 C10 C12 110.8(2) . . ?
C5 C10 C11 111.7(3) . . ?
C12 C10 C11 109.6(2) . . ?
C15 C13 C9 110.5(3) . . ?
C15 C13 C14 110.4(3) . . ?
C9 C13 C14 112.1(3) . . ?
C17 C16 C21 123.7(3) . . ?
C17 C16 N1 117.4(3) . . ?
C21 C16 N1 118.9(3) . . ?
C16 C17 C18 117.1(3) . . ?
C16 C17 C22 122.8(3) . . ?
C18 C17 C22 120.1(3) . . ?
C19 C18 C17 120.6(3) . . ?
C18 C19 C20 120.7(3) . . ?
C19 C20 C21 121.1(3) . . ?
C20 C21 C16 116.8(3) . . ?
C20 C21 C25 120.9(3) . . ?
C16 C21 C25 122.1(3) . . ?
C23 C22 C17 112.4(3) . . ?
C23 C22 C24 111.1(3) . . ?
C17 C22 C24 109.4(3) . . ?
C21 C25 C27 110.0(3) . . ?
C21 C25 C26 113.4(3) . . ?
C27 C25 C26 109.2(3) . . ?
N4 C28 N3 106.2(2) . . ?
N4 C28 P2 134.0(2) . . ?
N3 C28 P2 119.8(2) . . ?
C30 C29 N3 106.4(2) . . ?
C29 C30 N4 107.5(2) . . ?
C36 C31 C32 123.3(3) . . ?
C36 C31 N3 118.2(3) . . ?
C32 C31 N3 118.4(3) . . ?
C33 C32 C31 117.6(3) . . ?
C33 C32 C37 120.1(3) . . ?
C31 C32 C37 122.3(3) . . ?
C34 C33 C32 121.4(4) . . ?
C33 C34 C35 120.1(3) . . ?
C33 C34 C38 120.6(4) . . ?
C35 C34 C38 119.3(4) . . ?
C34 C35 C36 122.0(3) . . ?
C31 C36 C35 115.6(3) . . ?
C31 C36 C39 121.8(3) . . ?
C35 C36 C39 122.6(3) . . ?
C41 C40 C45 123.5(3) . . ?
C41 C40 N4 118.7(2) . . ?
C45 C40 N4 117.8(2) . . ?
C40 C41 C42 116.7(3) . . ?
C40 C41 C46 122.6(3) . . ?
C42 C41 C46 120.8(3) . . ?
C43 C42 C41 121.9(3) . . ?
C44 C43 C42 118.8(3) . . ?
C44 C43 C47 120.0(3) . . ?
C42 C43 C47 121.2(3) . . ?
C43 C44 C45 121.8(3) . . ?
C40 C45 C44 117.3(3) . . ?
C40 C45 C48 122.1(3) . . ?
C44 C45 C48 120.6(3) . . ?
Cl4 C49 Cl3 112.3(2) . . ?
Cl5 C50 Cl6 114.36(19) . . ?
C1 N1 C3 110.3(2) . . ?
C1 N1 C16 122.3(2) . . ?
C3 N1 C16 127.0(2) . . ?
C1 N2 C2 109.3(2) . . ?
C1 N2 C4 126.8(2) . . ?
C2 N2 C4 123.5(2) . . ?
C28 N3 C29 110.3(2) . . ?
C28 N3 C31 124.8(2) . . ?
C29 N3 C31 124.9(2) . . ?
C28 N4 C30 109.6(2) . . ?
C28 N4 C40 127.7(2) . . ?
C30 N4 C40 122.7(2) . . ?
C1 P1 P2 94.99(9) . . ?
C28 P2 P1 99.89(9) . . ?
C28 P2 Cl1 93.75(9) . . ?
P1 P2 Cl1 113.14(5) . . ?
Cl7 C51 Cl8 108.3(5) . . ?
Cl7' C51' Cl8' 114.9(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C2 C3 N1 0.4(3) . . . . ?
C9 C4 C5 C6 -0.1(4) . . . . ?
N2 C4 C5 C6 -176.2(2) . . . . ?
C9 C4 C5 C10 178.9(3) . . . . ?
N2 C4 C5 C10 2.8(4) . . . . ?
C4 C5 C6 C7 -0.2(4) . . . . ?
C10 C5 C6 C7 -179.2(3) . . . . ?
C5 C6 C7 C8 0.2(5) . . . . ?
C6 C7 C8 C9 0.1(5) . . . . ?
C5 C4 C9 C8 0.4(4) . . . . ?
N2 C4 C9 C8 176.5(2) . . . . ?
C5 C4 C9 C13 -177.7(3) . . . . ?
N2 C4 C9 C13 -1.6(4) . . . . ?
C7 C8 C9 C4 -0.4(5) . . . . ?
C7 C8 C9 C13 177.8(3) . . . . ?
C6 C5 C10 C12 70.4(3) . . . . ?
C4 C5 C10 C12 -108.6(3) . . . . ?
C6 C5 C10 C11 -52.1(4) . . . . ?
C4 C5 C10 C11 129.0(3) . . . . ?
C4 C9 C13 C15 110.6(4) . . . . ?
C8 C9 C13 C15 -67.5(4) . . . . ?
C4 C9 C13 C14 -125.8(3) . . . . ?
C8 C9 C13 C14 56.2(4) . . . . ?
C21 C16 C17 C18 -1.0(4) . . . . ?
N1 C16 C17 C18 177.1(2) . . . . ?
C21 C16 C17 C22 177.2(3) . . . . ?
N1 C16 C17 C22 -4.6(4) . . . . ?
C16 C17 C18 C19 0.3(4) . . . . ?
C22 C17 C18 C19 -178.0(3) . . . . ?
C17 C18 C19 C20 0.9(5) . . . . ?
C18 C19 C20 C21 -1.4(5) . . . . ?
C19 C20 C21 C16 0.7(4) . . . . ?
C19 C20 C21 C25 176.9(3) . . . . ?
C17 C16 C21 C20 0.5(4) . . . . ?
N1 C16 C21 C20 -177.6(2) . . . . ?
C17 C16 C21 C25 -175.6(3) . . . . ?
N1 C16 C21 C25 6.3(4) . . . . ?
C16 C17 C22 C23 131.4(3) . . . . ?
C18 C17 C22 C23 -50.4(4) . . . . ?
C16 C17 C22 C24 -104.6(3) . . . . ?
C18 C17 C22 C24 73.7(4) . . . . ?
C20 C21 C25 C27 -81.6(4) . . . . ?
C16 C21 C25 C27 94.4(4) . . . . ?
C20 C21 C25 C26 41.0(4) . . . . ?
C16 C21 C25 C26 -143.0(3) . . . . ?
N3 C29 C30 N4 0.6(3) . . . . ?
C36 C31 C32 C33 1.7(5) . . . . ?
N3 C31 C32 C33 -179.9(3) . . . . ?
C36 C31 C32 C37 -178.7(3) . . . . ?
N3 C31 C32 C37 -0.3(4) . . . . ?
C31 C32 C33 C34 0.8(5) . . . . ?
C37 C32 C33 C34 -178.8(3) . . . . ?
C32 C33 C34 C35 -2.6(5) . . . . ?
C32 C33 C34 C38 177.0(3) . . . . ?
C33 C34 C35 C36 1.8(5) . . . . ?
C38 C34 C35 C36 -177.7(3) . . . . ?
C32 C31 C36 C35 -2.3(4) . . . . ?
N3 C31 C36 C35 179.3(3) . . . . ?
C32 C31 C36 C39 175.4(3) . . . . ?
N3 C31 C36 C39 -3.0(4) . . . . ?
C34 C35 C36 C31 0.6(5) . . . . ?
C34 C35 C36 C39 -177.1(3) . . . . ?
C45 C40 C41 C42 0.5(4) . . . . ?
N4 C40 C41 C42 179.5(2) . . . . ?
C45 C40 C41 C46 -179.4(3) . . . . ?
N4 C40 C41 C46 -0.4(4) . . . . ?
C40 C41 C42 C43 0.2(4) . . . . ?
C46 C41 C42 C43 -180.0(3) . . . . ?
C41 C42 C43 C44 0.0(4) . . . . ?
C41 C42 C43 C47 -179.6(3) . . . . ?
C42 C43 C44 C45 -0.9(4) . . . . ?
C47 C43 C44 C45 178.8(3) . . . . ?
C41 C40 C45 C44 -1.2(4) . . . . ?
N4 C40 C45 C44 179.8(2) . . . . ?
C41 C40 C45 C48 -179.5(3) . . . . ?
N4 C40 C45 C48 1.5(4) . . . . ?
C43 C44 C45 C40 1.4(4) . . . . ?
C43 C44 C45 C48 179.7(3) . . . . ?
N2 C1 N1 C3 0.0(3) . . . . ?
P1 C1 N1 C3 -172.75(19) . . . . ?
N2 C1 N1 C16 173.1(2) . . . . ?
P1 C1 N1 C16 0.4(3) . . . . ?
C2 C3 N1 C1 -0.3(3) . . . . ?
C2 C3 N1 C16 -172.9(3) . . . . ?
C17 C16 N1 C1 -83.0(3) . . . . ?
C21 C16 N1 C1 95.2(3) . . . . ?
C17 C16 N1 C3 88.9(3) . . . . ?
C21 C16 N1 C3 -92.9(3) . . . . ?
N1 C1 N2 C2 0.2(3) . . . . ?
P1 C1 N2 C2 171.5(2) . . . . ?
N1 C1 N2 C4 -172.7(2) . . . . ?
P1 C1 N2 C4 -1.4(4) . . . . ?
C3 C2 N2 C1 -0.4(3) . . . . ?
C3 C2 N2 C4 172.8(2) . . . . ?
C9 C4 N2 C1 73.3(4) . . . . ?
C5 C4 N2 C1 -110.5(3) . . . . ?
C9 C4 N2 C2 -98.7(3) . . . . ?
C5 C4 N2 C2 77.5(3) . . . . ?
N4 C28 N3 C29 0.6(3) . . . . ?
P2 C28 N3 C29 -179.1(2) . . . . ?
N4 C28 N3 C31 -178.1(3) . . . . ?
P2 C28 N3 C31 2.2(4) . . . . ?
C30 C29 N3 C28 -0.7(3) . . . . ?
C30 C29 N3 C31 178.0(3) . . . . ?
C36 C31 N3 C28 -105.7(3) . . . . ?
C32 C31 N3 C28 75.9(4) . . . . ?
C36 C31 N3 C29 75.7(4) . . . . ?
C32 C31 N3 C29 -102.7(3) . . . . ?
N3 C28 N4 C30 -0.2(3) . . . . ?
P2 C28 N4 C30 179.4(2) . . . . ?
N3 C28 N4 C40 177.9(3) . . . . ?
P2 C28 N4 C40 -2.6(5) . . . . ?
C29 C30 N4 C28 -0.2(3) . . . . ?
C29 C30 N4 C40 -178.4(3) . . . . ?
C41 C40 N4 C28 84.8(3) . . . . ?
C45 C40 N4 C28 -96.1(3) . . . . ?
C41 C40 N4 C30 -97.3(3) . . . . ?
C45 C40 N4 C30 81.7(3) . . . . ?
N2 C1 P1 P2 50.9(3) . . . . ?
N1 C1 P1 P2 -138.7(2) . . . . ?
N4 C28 P2 P1 18.4(3) . . . . ?
N3 C28 P2 P1 -162.0(2) . . . . ?
N4 C28 P2 Cl1 -95.8(3) . . . . ?
N3 C28 P2 Cl1 83.7(2) . . . . ?

_refine_diff_density_max         1.249
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.073

####################################################################### 
# 
# 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_ad031db
_database_code_depnum_ccdc_archive 'CCDC 1572771'
_audit_update_record             
;
2017-09-05 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H60 N4 P2, P F6, 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H64 Cl4 F6 N4 P3'
_chemical_formula_weight         1069.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9228(4)
_cell_length_b                   14.9659(8)
_cell_length_c                   18.5836(8)
_cell_angle_alpha                67.890(4)
_cell_angle_beta                 79.842(4)
_cell_angle_gamma                84.588(4)
_cell_volume                     2769.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    20897
_cell_measurement_theta_min      3.2670
_cell_measurement_theta_max      75.6940

_exptl_crystal_description       irregular
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             1118
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.237
_shelx_estimated_absorpt_T_min   0.523
_shelx_estimated_absorpt_T_max   0.642
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 5 -2 0.0844
-4 0 -11 0.1160
-6 -4 -7 0.1115
-6 -5 1 0.0737
-2 -4 8 0.0411
2 -1 11 0.0378
-2 6 -5 0.0997
2 -7 -9 0.0801
-1 0 -11 0.1273
3 -8 0 0.0586
0 9 8 0.1248
1 -9 -1 0.0411
0 -8 -9 0.0757
4 8 2 0.1037
-5 4 -5 0.0847
-5 5 4 0.0788
-4 3 9 0.0594
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.0039 4.9911 -1.9771 -0.4610 0.7274 0.4478
-3.9876 0.0110 -11.0051 0.2940 -0.3140 0.9806
-5.9948 -3.9868 -7.0208 0.4539 -0.7561 0.4053
-6.0020 -4.9887 0.9758 0.5694 -0.7962 -0.3570
-2.0099 -3.9986 7.9842 0.2398 -0.4199 -0.9279
1.9883 -1.0069 10.9992 -0.0813 0.1031 -1.0322
-1.9837 6.0076 -4.9830 0.4222 0.3526 0.7883
1.9915 -7.0053 -9.0201 -0.7460 -0.5147 0.3889
-0.9913 0.0043 -11.0012 -0.0913 -0.1243 0.9725
2.9824 -8.0096 -0.0222 -0.7389 -0.4860 -0.4643
0.0102 9.0018 8.0293 0.5577 0.8046 -0.1921
0.9838 -9.0053 -1.0281 -0.5463 -0.7025 -0.4277
-0.0078 -8.0012 -9.0260 -0.5334 -0.7257 0.3373
4.0077 7.9937 2.0313 -0.1201 0.9398 0.2690
-4.9835 4.0135 -4.9934 0.7191 -0.0061 0.6824
-4.9879 5.0122 4.0097 0.9430 0.1284 -0.0540
-3.9960 3.0082 9.0044 0.8260 0.0504 -0.6115
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.596
_oxdiff_exptl_absorpt_empirical_full_max 1.648
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxfrord Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            114993
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.189
_diffrn_reflns_theta_max         76.345
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11541
_reflns_number_gt                8328
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
;
 SHELXT-2014/7 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_molecular_graphics    ?
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;


_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as a rigid bodies and allowed to 
 rotate about the E-CH3 bond.

 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 > 2sigma(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)+(0.1007P)²+1.2267P] 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         11541
_refine_ls_number_parameters     682
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1895
_refine_ls_wR_factor_gt          0.1676
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_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
Cl96 Cl 0.27277(18) 0.4221(2) 0.6386(2) 0.0966(12) Uani 0.739(7) 1 d D . P A 3
Cl97 Cl 0.20285(19) 0.2608(2) 0.6079(3) 0.1240(14) Uani 0.739(7) 1 d D . P A 3
C98 C 0.1530(6) 0.3557(6) 0.6389(6) 0.091(2) Uani 0.739(7) 1 d D . P A 3
H98A H 0.0954 0.3986 0.6042 0.110 Uiso 0.739(7) 1 calc R U P A 3
H98B H 0.1062 0.3297 0.6928 0.110 Uiso 0.739(7) 1 calc R U P A 3
Cl95 Cl 0.153(2) 0.3456(19) 0.5586(13) 0.249(11) Uiso 0.169(5) 1 d D . P B 4
Cl94 Cl 0.2674(12) 0.3889(8) 0.6706(6) 0.093(3) Uiso 0.169(5) 1 d D . P B 4
C97 C 0.180(6) 0.310(3) 0.6551(19) 0.18(3) Uiso 0.169(5) 1 d D . P B 4
H97A H 0.0986 0.3030 0.6899 0.219 Uiso 0.169(5) 1 calc R U P B 4
H97B H 0.2228 0.2457 0.6700 0.219 Uiso 0.169(5) 1 calc R U P B 4
Cl92 Cl 0.2206(14) 0.4517(8) 0.6005(8) 0.075(4) Uiso 0.092(5) 1 d . . P C 5
Cl93 Cl 0.2254(10) 0.2508(8) 0.6414(6) 0.053(3) Uiso 0.092(5) 1 d . . P C 5
C96 C 0.179(4) 0.339(3) 0.673(3) 0.056(11) Uiso 0.092(5) 1 d . . P C 5
H96A H 0.2169 0.3296 0.7202 0.067 Uiso 0.092(5) 1 calc R U P C 5
H96B H 0.0874 0.3382 0.6885 0.067 Uiso 0.092(5) 1 calc R U P C 5
Cl98 Cl 0.90443(19) 0.36510(18) 0.52685(12) 0.1674(9) Uani 1 1 d . . . . .
Cl99 Cl 0.8732(3) 0.1746(2) 0.53252(18) 0.2197(14) Uani 1 1 d . . . . .
C99 C 0.8789(6) 0.2465(5) 0.5871(3) 0.1168(18) Uani 1 1 d . . . . .
H99A H 0.7994 0.2426 0.6231 0.140 Uiso 1 1 calc R U . . .
H99B H 0.9465 0.2219 0.6194 0.140 Uiso 1 1 calc R U . . .
C1 C 0.5969(2) 0.87334(17) 0.80223(15) 0.0382(5) Uani 1 1 d . . . . .
C2 C 0.7277(2) 0.9586(2) 0.83088(19) 0.0524(7) Uani 1 1 d . . . . .
H2 H 0.7573 1.0043 0.8476 0.063 Uiso 1 1 calc R U . . .
C3 C 0.7976(2) 0.8966(2) 0.80326(19) 0.0526(7) Uani 1 1 d . . . . .
H3 H 0.8858 0.8899 0.7968 0.063 Uiso 1 1 calc R U . . .
C4 C 0.3347(2) 0.70006(16) 0.74872(14) 0.0334(4) Uani 1 1 d . . . . .
C5 C 0.1334(2) 0.68158(19) 0.74539(17) 0.0441(6) Uani 1 1 d . . . . .
H5 H 0.0455 0.6904 0.7507 0.053 Uiso 1 1 calc R U . . .
C6 C 0.2012(2) 0.61805(19) 0.71837(16) 0.0421(5) Uani 1 1 d . . . . .
H6 H 0.1702 0.5735 0.7011 0.051 Uiso 1 1 calc R U . . .
C11 C 0.4979(2) 0.99138(18) 0.86086(16) 0.0402(5) Uani 1 1 d . . . . .
C12 C 0.4407(2) 0.94442(19) 0.93783(16) 0.0430(5) Uani 1 1 d . . . . .
C13 C 0.3362(2) 0.9896(2) 0.96526(17) 0.0482(6) Uani 1 1 d . . . . .
H13 H 0.2956 0.9594 1.0176 0.058 Uiso 1 1 calc R U . . .
C14 C 0.2894(2) 1.0778(2) 0.91823(19) 0.0510(6) Uani 1 1 d . . . . .
C15 C 0.3498(3) 1.1220(2) 0.84210(19) 0.0524(6) Uani 1 1 d . . . . .
H15 H 0.3185 1.1826 0.8099 0.063 Uiso 1 1 calc R U . . .
C16 C 0.4545(3) 1.0801(2) 0.81156(17) 0.0475(6) Uani 1 1 d . . . . .
C17 C 0.4883(3) 0.8483(2) 0.98930(18) 0.0548(7) Uani 1 1 d . . . . .
H17A H 0.4399 0.8298 1.0422 0.082 Uiso 1 1 calc R U . . .
H17B H 0.5761 0.8527 0.9922 0.082 Uiso 1 1 calc R U . . .
H17C H 0.4800 0.7997 0.9671 0.082 Uiso 1 1 calc R U . . .
C18 C 0.1751(3) 1.1242(3) 0.9505(2) 0.0695(9) Uani 1 1 d . . . . .
H18A H 0.1495 1.1820 0.9084 0.104 Uiso 1 1 calc R U . . .
H18B H 0.1942 1.1422 0.9927 0.104 Uiso 1 1 calc R U . . .
H18C H 0.1074 1.0784 0.9712 0.104 Uiso 1 1 calc R U . . .
C19 C 0.5171(3) 1.1292(3) 0.72855(19) 0.0655(8) Uani 1 1 d . . . . .
H19A H 0.6012 1.1466 0.7289 0.098 Uiso 1 1 calc R U . . .
H19B H 0.4689 1.1877 0.7026 0.098 Uiso 1 1 calc R U . . .
H19C H 0.5220 1.0854 0.7000 0.098 Uiso 1 1 calc R U . . .
C21 C 0.7596(2) 0.76662(18) 0.75792(16) 0.0404(5) Uani 1 1 d . . . . .
C22 C 0.7719(2) 0.6740(2) 0.81338(17) 0.0467(6) Uani 1 1 d . . . . .
C23 C 0.8160(2) 0.6007(2) 0.7860(2) 0.0564(7) Uani 1 1 d . . . . .
H23 H 0.8244 0.5368 0.8228 0.068 Uiso 1 1 calc R U . . .
C24 C 0.8480(2) 0.6182(2) 0.7068(2) 0.0587(8) Uani 1 1 d . . . . .
C25 C 0.8321(3) 0.7109(3) 0.6537(2) 0.0585(8) Uani 1 1 d . . . . .
H25 H 0.8521 0.7229 0.5991 0.070 Uiso 1 1 calc R U . . .
C26 C 0.7877(2) 0.7872(2) 0.67753(17) 0.0468(6) Uani 1 1 d . . . . .
C27 C 0.7321(3) 0.6539(3) 0.89968(19) 0.0652(8) Uani 1 1 d . . . . .
H27A H 0.6410 0.6554 0.9113 0.098 Uiso 1 1 calc R U . . .
H27B H 0.7648 0.7031 0.9135 0.098 Uiso 1 1 calc R U . . .
H27C H 0.7646 0.5901 0.9304 0.098 Uiso 1 1 calc R U . . .
C28 C 0.8992(3) 0.5378(3) 0.6778(3) 0.0880(14) Uani 1 1 d . . . . .
H28A H 0.9873 0.5483 0.6555 0.132 Uiso 1 1 calc R U . . .
H28B H 0.8527 0.5377 0.6373 0.132 Uiso 1 1 calc R U . . .
H28C H 0.8907 0.4757 0.7218 0.132 Uiso 1 1 calc R U . . .
C29 C 0.7647(3) 0.8864(2) 0.6190(2) 0.0639(8) Uani 1 1 d . . . . .
H29A H 0.6751 0.8983 0.6183 0.096 Uiso 1 1 calc R U . . .
H29B H 0.8066 0.8911 0.5667 0.096 Uiso 1 1 calc R U . . .
H29C H 0.7974 0.9346 0.6341 0.096 Uiso 1 1 calc R U . . .
C31 C 0.1744(2) 0.80665(17) 0.79503(15) 0.0365(5) Uani 1 1 d . . . . .
C32 C 0.1689(2) 0.90157(18) 0.74128(17) 0.0446(6) Uani 1 1 d . . . . .
C33 C 0.1283(3) 0.9724(2) 0.7729(2) 0.0551(7) Uani 1 1 d . . . . .
H33 H 0.1218 1.0378 0.7386 0.066 Uiso 1 1 calc R U . . .
C34 C 0.0977(3) 0.9488(2) 0.8527(2) 0.0597(8) Uani 1 1 d . . . . .
H34 H 0.0715 0.9983 0.8728 0.072 Uiso 1 1 calc R U . . .
C35 C 0.1045(3) 0.8544(2) 0.90385(19) 0.0549(7) Uani 1 1 d . . . . .
H35 H 0.0833 0.8399 0.9588 0.066 Uiso 1 1 calc R U . . .
C36 C 0.1419(2) 0.7798(2) 0.87626(17) 0.0443(6) Uani 1 1 d . . . . .
C41 C 0.4269(2) 0.57155(17) 0.69818(15) 0.0373(5) Uani 1 1 d . . . . .
C42 C 0.4787(2) 0.5994(2) 0.61869(16) 0.0453(6) Uani 1 1 d . . . . .
C43 C 0.5737(3) 0.5392(3) 0.59961(19) 0.0583(7) Uani 1 1 d . . . . .
H43 H 0.6111 0.5548 0.5463 0.070 Uiso 1 1 calc R U . . .
C44 C 0.6140(3) 0.4577(3) 0.6562(2) 0.0622(8) Uani 1 1 d . . . . .
H44 H 0.6794 0.4185 0.6416 0.075 Uiso 1 1 calc R U . . .
C45 C 0.5614(3) 0.4321(2) 0.7338(2) 0.0559(7) Uani 1 1 d . . . . .
H45 H 0.5901 0.3750 0.7720 0.067 Uiso 1 1 calc R U . . .
C46 C 0.4656(2) 0.48944(19) 0.75709(17) 0.0441(5) Uani 1 1 d . . . . .
C321 C 0.2044(3) 0.9263(2) 0.65335(19) 0.0576(7) Uani 1 1 d . . . . .
H321 H 0.2515 0.8691 0.6457 0.069 Uiso 1 1 calc R U . . .
C322 C 0.2891(5) 1.0120(4) 0.6135(3) 0.0985(15) Uani 1 1 d . . . . .
H32A H 0.2424 1.0711 0.6138 0.148 Uiso 1 1 calc R U . . .
H32B H 0.3198 1.0178 0.5592 0.148 Uiso 1 1 calc R U . . .
H32C H 0.3597 1.0022 0.6420 0.148 Uiso 1 1 calc R U . . .
C323 C 0.0893(4) 0.9421(4) 0.6145(3) 0.1015(16) Uani 1 1 d . . . . .
H32D H 0.0367 0.8858 0.6407 0.152 Uiso 1 1 calc R U . . .
H32E H 0.1140 0.9510 0.5589 0.152 Uiso 1 1 calc R U . . .
H32F H 0.0427 0.9997 0.6186 0.152 Uiso 1 1 calc R U . . .
C361 C 0.1488(3) 0.6759(2) 0.93257(18) 0.0555(7) Uani 1 1 d . . . . .
H361 H 0.1585 0.6335 0.9011 0.067 Uiso 1 1 calc R U . . .
C362 C 0.2594(4) 0.6557(3) 0.9762(3) 0.0847(12) Uani 1 1 d . . . . .
H36A H 0.3360 0.6735 0.9383 0.127 Uiso 1 1 calc R U . . .
H36B H 0.2641 0.5868 1.0086 0.127 Uiso 1 1 calc R U . . .
H36C H 0.2496 0.6936 1.0100 0.127 Uiso 1 1 calc R U . . .
C363 C 0.0304(4) 0.6476(4) 0.9928(3) 0.1092(18) Uani 1 1 d . . . . .
H36D H 0.0185 0.6885 1.0242 0.164 Uiso 1 1 calc R U . . .
H36E H 0.0381 0.5799 1.0273 0.164 Uiso 1 1 calc R U . . .
H36F H -0.0413 0.6564 0.9653 0.164 Uiso 1 1 calc R U . . .
C421 C 0.4349(3) 0.6900(2) 0.55599(17) 0.0573(7) Uani 1 1 d . . . . .
H421 H 0.3492 0.7076 0.5771 0.069 Uiso 1 1 calc R U . . .
C422 C 0.5170(5) 0.7744(3) 0.5378(3) 0.0967(15) Uani 1 1 d . . . . .
H42A H 0.5147 0.7884 0.5855 0.145 Uiso 1 1 calc R U . . .
H42B H 0.4866 0.8312 0.4969 0.145 Uiso 1 1 calc R U . . .
H42C H 0.6027 0.7580 0.5194 0.145 Uiso 1 1 calc R U . . .
C423 C 0.4270(4) 0.6736(3) 0.4808(2) 0.0779(10) Uani 1 1 d . . . . .
H42D H 0.5106 0.6598 0.4571 0.117 Uiso 1 1 calc R U . . .
H42E H 0.3913 0.7315 0.4437 0.117 Uiso 1 1 calc R U . . .
H42F H 0.3741 0.6188 0.4932 0.117 Uiso 1 1 calc R U . . .
C461 C 0.4077(3) 0.4602(2) 0.84303(17) 0.0508(6) Uani 1 1 d . . . . .
H461 H 0.3508 0.5143 0.8486 0.061 Uiso 1 1 calc R U . . .
C462 C 0.5073(3) 0.4444(3) 0.8957(2) 0.0689(9) Uani 1 1 d . . . . .
H46A H 0.5617 0.3892 0.8936 0.103 Uiso 1 1 calc R U . . .
H46B H 0.4671 0.4316 0.9499 0.103 Uiso 1 1 calc R U . . .
H46C H 0.5569 0.5023 0.8772 0.103 Uiso 1 1 calc R U . . .
C463 C 0.3300(4) 0.3705(3) 0.8695(2) 0.0777(10) Uani 1 1 d . . . . .
H46D H 0.2649 0.3831 0.8364 0.117 Uiso 1 1 calc R U . . .
H46E H 0.2916 0.3547 0.9244 0.117 Uiso 1 1 calc R U . . .
H46F H 0.3837 0.3162 0.8645 0.117 Uiso 1 1 calc R U . . .
N1 N 0.60501(19) 0.94411(15) 0.83065(13) 0.0420(5) Uani 1 1 d . . . . .
N2 N 0.71722(18) 0.84374(16) 0.78584(13) 0.0410(5) Uani 1 1 d . . . . .
N3 N 0.21515(17) 0.73182(14) 0.76407(12) 0.0365(4) Uani 1 1 d . . . . .
N4 N 0.32479(17) 0.62945(14) 0.72026(12) 0.0358(4) Uani 1 1 d . . . . .
P1 P 0.44560(6) 0.84509(5) 0.79379(5) 0.04900(19) Uani 1 1 d . . . . .
P2 P 0.48713(5) 0.72635(5) 0.75801(4) 0.04351(17) Uani 1 1 d . . . . .
F1 F 0.2465(11) 0.8217(7) 1.1909(8) 0.152(5) Uani 0.588(17) 1 d D . P D 1
F2 F 0.2238(7) 0.7057(7) 1.1488(5) 0.128(3) Uani 0.588(17) 1 d D . P D 1
F3 F 0.0205(9) 0.7178(8) 1.1810(8) 0.111(3) Uani 0.588(17) 1 d D . P D 1
F4 F 0.0421(12) 0.8290(7) 1.2271(6) 0.122(4) Uani 0.588(17) 1 d D . P D 1
F1' F 0.2715(7) 0.8072(10) 1.1757(7) 0.095(3) Uani 0.412(17) 1 d D . P D 2
F2' F 0.176(2) 0.7037(11) 1.1488(9) 0.191(8) Uani 0.412(17) 1 d D . P D 2
F3' F -0.0038(14) 0.7516(19) 1.2004(11) 0.214(12) Uani 0.412(17) 1 d D . P D 2
F4' F 0.0945(16) 0.8565(9) 1.2241(12) 0.151(6) Uani 0.412(17) 1 d D . P D 2
F5 F 0.1453(2) 0.69422(15) 1.27128(14) 0.0843(6) Uani 1 1 d . . . . .
F6 F 0.1199(3) 0.8521(3) 1.10314(18) 0.1372(15) Uani 1 1 d . . . . .
P3 P 0.13431(8) 0.77253(7) 1.18619(6) 0.0636(2) 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
Cl96 C98 1.713(6) . ?
Cl97 C98 1.734(6) . ?
Cl95 C97 1.738(17) . ?
Cl94 C97 1.723(17) . ?
Cl92 C96 1.75(5) . ?
Cl93 C96 1.65(5) . ?
Cl98 C99 1.723(7) . ?
Cl99 C99 1.745(6) . ?
C1 N1 1.365(3) . ?
C1 N2 1.366(3) . ?
C1 P1 1.791(2) . ?
C2 C3 1.340(4) . ?
C2 N1 1.379(3) . ?
C3 N2 1.388(3) . ?
C4 N3 1.366(3) . ?
C4 N4 1.368(3) . ?
C4 P2 1.798(2) . ?
C5 C6 1.342(4) . ?
C5 N3 1.384(3) . ?
C6 N4 1.384(3) . ?
C11 C12 1.393(4) . ?
C11 C16 1.395(4) . ?
C11 N1 1.447(3) . ?
C12 C13 1.389(4) . ?
C12 C17 1.501(4) . ?
C13 C14 1.389(4) . ?
C14 C15 1.387(4) . ?
C14 C18 1.512(4) . ?
C15 C16 1.388(4) . ?
C16 C19 1.502(4) . ?
C21 C26 1.390(4) . ?
C21 C22 1.393(4) . ?
C21 N2 1.442(3) . ?
C22 C23 1.389(4) . ?
C22 C27 1.506(4) . ?
C23 C24 1.380(5) . ?
C24 C25 1.383(5) . ?
C24 C28 1.518(4) . ?
C25 C26 1.391(4) . ?
C26 C29 1.504(4) . ?
C31 C36 1.396(4) . ?
C31 C32 1.399(4) . ?
C31 N3 1.444(3) . ?
C32 C33 1.397(4) . ?
C32 C321 1.518(4) . ?
C33 C34 1.374(5) . ?
C34 C35 1.378(5) . ?
C35 C36 1.396(4) . ?
C36 C361 1.517(4) . ?
C41 C46 1.392(4) . ?
C41 C42 1.401(4) . ?
C41 N4 1.445(3) . ?
C42 C43 1.396(4) . ?
C42 C421 1.520(4) . ?
C43 C44 1.372(5) . ?
C44 C45 1.374(5) . ?
C45 C46 1.404(4) . ?
C46 C461 1.520(4) . ?
C321 C323 1.515(5) . ?
C321 C322 1.522(5) . ?
C361 C362 1.517(5) . ?
C361 C363 1.529(5) . ?
C421 C422 1.515(5) . ?
C421 C423 1.525(5) . ?
C461 C463 1.528(4) . ?
C461 C462 1.533(4) . ?
P1 P2 2.1065(9) . ?
F1 P3 1.518(7) . ?
F2 P3 1.593(6) . ?
F3 P3 1.588(8) . ?
F4 P3 1.537(7) . ?
F1' P3 1.587(9) . ?
F2' P3 1.446(12) . ?
F3' P3 1.527(12) . ?
F4' P3 1.648(16) . ?
F5 P3 1.592(2) . ?
F6 P3 1.578(3) . ?

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
Cl96 C98 Cl97 113.1(3) . . ?
Cl94 C97 Cl95 113.7(17) . . ?
Cl93 C96 Cl92 111(3) . . ?
Cl98 C99 Cl99 111.3(4) . . ?
N1 C1 N2 104.8(2) . . ?
N1 C1 P1 118.02(17) . . ?
N2 C1 P1 137.12(18) . . ?
C3 C2 N1 107.4(2) . . ?
C2 C3 N2 107.3(2) . . ?
N3 C4 N4 104.82(18) . . ?
N3 C4 P2 136.94(17) . . ?
N4 C4 P2 118.22(16) . . ?
C6 C5 N3 107.4(2) . . ?
C5 C6 N4 107.3(2) . . ?
C12 C11 C16 122.9(2) . . ?
C12 C11 N1 118.0(2) . . ?
C16 C11 N1 119.0(2) . . ?
C13 C12 C11 117.3(3) . . ?
C13 C12 C17 120.9(3) . . ?
C11 C12 C17 121.8(2) . . ?
C12 C13 C14 121.8(3) . . ?
C15 C14 C13 118.8(3) . . ?
C15 C14 C18 121.2(3) . . ?
C13 C14 C18 120.0(3) . . ?
C14 C15 C16 121.9(3) . . ?
C15 C16 C11 117.3(3) . . ?
C15 C16 C19 120.7(3) . . ?
C11 C16 C19 122.0(3) . . ?
C26 C21 C22 122.6(2) . . ?
C26 C21 N2 119.3(2) . . ?
C22 C21 N2 118.1(2) . . ?
C23 C22 C21 117.7(3) . . ?
C23 C22 C27 121.5(3) . . ?
C21 C22 C27 120.7(3) . . ?
C24 C23 C22 121.7(3) . . ?
C23 C24 C25 118.7(3) . . ?
C23 C24 C28 121.1(3) . . ?
C25 C24 C28 120.2(4) . . ?
C24 C25 C26 122.3(3) . . ?
C21 C26 C25 117.1(3) . . ?
C21 C26 C29 121.3(3) . . ?
C25 C26 C29 121.6(3) . . ?
C36 C31 C32 124.2(2) . . ?
C36 C31 N3 118.2(2) . . ?
C32 C31 N3 117.6(2) . . ?
C33 C32 C31 116.4(3) . . ?
C33 C32 C321 121.8(3) . . ?
C31 C32 C321 121.9(2) . . ?
C34 C33 C32 121.0(3) . . ?
C33 C34 C35 121.0(3) . . ?
C34 C35 C36 121.1(3) . . ?
C31 C36 C35 116.4(3) . . ?
C31 C36 C361 122.6(2) . . ?
C35 C36 C361 121.1(3) . . ?
C46 C41 C42 123.8(2) . . ?
C46 C41 N4 117.9(2) . . ?
C42 C41 N4 118.3(2) . . ?
C43 C42 C41 116.3(3) . . ?
C43 C42 C421 121.3(3) . . ?
C41 C42 C421 122.4(2) . . ?
C44 C43 C42 121.3(3) . . ?
C43 C44 C45 121.1(3) . . ?
C44 C45 C46 120.6(3) . . ?
C41 C46 C45 116.9(3) . . ?
C41 C46 C461 123.0(2) . . ?
C45 C46 C461 120.1(3) . . ?
C323 C321 C32 110.7(3) . . ?
C323 C321 C322 111.0(3) . . ?
C32 C321 C322 113.3(3) . . ?
C36 C361 C362 112.2(3) . . ?
C36 C361 C363 112.1(3) . . ?
C362 C361 C363 108.6(3) . . ?
C422 C421 C42 111.7(3) . . ?
C422 C421 C423 110.2(3) . . ?
C42 C421 C423 111.9(3) . . ?
C46 C461 C463 111.3(3) . . ?
C46 C461 C462 111.2(3) . . ?
C463 C461 C462 110.9(3) . . ?
C1 N1 C2 110.4(2) . . ?
C1 N1 C11 123.7(2) . . ?
C2 N1 C11 125.8(2) . . ?
C1 N2 C3 110.1(2) . . ?
C1 N2 C21 127.11(19) . . ?
C3 N2 C21 122.8(2) . . ?
C4 N3 C5 110.26(19) . . ?
C4 N3 C31 127.02(18) . . ?
C5 N3 C31 122.73(19) . . ?
C4 N4 C6 110.26(19) . . ?
C4 N4 C41 125.54(19) . . ?
C6 N4 C41 124.15(19) . . ?
C1 P1 P2 101.57(8) . . ?
C4 P2 P1 100.90(7) . . ?
F2' P3 F3' 96.1(7) . . ?
F1 P3 F4 93.2(5) . . ?
F2' P3 F6 89.5(8) . . ?
F1 P3 F6 91.1(5) . . ?
F3' P3 F6 90.1(7) . . ?
F4 P3 F6 90.7(4) . . ?
F2' P3 F1' 92.4(8) . . ?
F3' P3 F1' 171.5(11) . . ?
F6 P3 F1' 88.8(4) . . ?
F1 P3 F3 177.8(6) . . ?
F4 P3 F3 88.8(5) . . ?
F6 P3 F3 89.7(5) . . ?
F2' P3 F5 92.3(8) . . ?
F1 P3 F5 89.1(5) . . ?
F3' P3 F5 88.9(7) . . ?
F4 P3 F5 87.3(4) . . ?
F6 P3 F5 178.05(19) . . ?
F1' P3 F5 92.0(4) . . ?
F3 P3 F5 90.2(5) . . ?
F1 P3 F2 90.2(5) . . ?
F4 P3 F2 175.0(5) . . ?
F6 P3 F2 92.8(4) . . ?
F3 P3 F2 87.7(4) . . ?
F5 P3 F2 89.1(4) . . ?
F2' P3 F4' 175.7(8) . . ?
F3' P3 F4' 87.4(8) . . ?
F6 P3 F4' 87.9(7) . . ?
F1' P3 F4' 84.2(6) . . ?
F5 P3 F4' 90.4(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.1(4) . . . . ?
N3 C5 C6 N4 -0.1(3) . . . . ?
C16 C11 C12 C13 -0.1(4) . . . . ?
N1 C11 C12 C13 -178.4(2) . . . . ?
C16 C11 C12 C17 179.2(2) . . . . ?
N1 C11 C12 C17 0.9(4) . . . . ?
C11 C12 C13 C14 0.4(4) . . . . ?
C17 C12 C13 C14 -179.0(3) . . . . ?
C12 C13 C14 C15 -0.6(4) . . . . ?
C12 C13 C14 C18 179.8(3) . . . . ?
C13 C14 C15 C16 0.6(4) . . . . ?
C18 C14 C15 C16 -179.7(3) . . . . ?
C14 C15 C16 C11 -0.4(4) . . . . ?
C14 C15 C16 C19 179.3(3) . . . . ?
C12 C11 C16 C15 0.2(4) . . . . ?
N1 C11 C16 C15 178.4(2) . . . . ?
C12 C11 C16 C19 -179.6(3) . . . . ?
N1 C11 C16 C19 -1.3(4) . . . . ?
C26 C21 C22 C23 1.0(4) . . . . ?
N2 C21 C22 C23 -178.3(2) . . . . ?
C26 C21 C22 C27 -175.8(2) . . . . ?
N2 C21 C22 C27 4.9(3) . . . . ?
C21 C22 C23 C24 0.6(4) . . . . ?
C27 C22 C23 C24 177.4(3) . . . . ?
C22 C23 C24 C25 -1.8(4) . . . . ?
C22 C23 C24 C28 178.4(3) . . . . ?
C23 C24 C25 C26 1.4(4) . . . . ?
C28 C24 C25 C26 -178.7(3) . . . . ?
C22 C21 C26 C25 -1.4(4) . . . . ?
N2 C21 C26 C25 177.9(2) . . . . ?
C22 C21 C26 C29 175.5(2) . . . . ?
N2 C21 C26 C29 -5.2(4) . . . . ?
C24 C25 C26 C21 0.1(4) . . . . ?
C24 C25 C26 C29 -176.8(3) . . . . ?
C36 C31 C32 C33 0.4(4) . . . . ?
N3 C31 C32 C33 179.6(2) . . . . ?
C36 C31 C32 C321 -179.4(2) . . . . ?
N3 C31 C32 C321 -0.2(3) . . . . ?
C31 C32 C33 C34 0.9(4) . . . . ?
C321 C32 C33 C34 -179.3(3) . . . . ?
C32 C33 C34 C35 -0.9(4) . . . . ?
C33 C34 C35 C36 -0.4(4) . . . . ?
C32 C31 C36 C35 -1.5(4) . . . . ?
N3 C31 C36 C35 179.3(2) . . . . ?
C32 C31 C36 C361 179.7(2) . . . . ?
N3 C31 C36 C361 0.5(3) . . . . ?
C34 C35 C36 C31 1.5(4) . . . . ?
C34 C35 C36 C361 -179.7(3) . . . . ?
C46 C41 C42 C43 0.5(4) . . . . ?
N4 C41 C42 C43 -177.4(2) . . . . ?
C46 C41 C42 C421 -179.5(3) . . . . ?
N4 C41 C42 C421 2.6(4) . . . . ?
C41 C42 C43 C44 -0.6(4) . . . . ?
C421 C42 C43 C44 179.5(3) . . . . ?
C42 C43 C44 C45 0.7(5) . . . . ?
C43 C44 C45 C46 -0.7(5) . . . . ?
C42 C41 C46 C45 -0.6(4) . . . . ?
N4 C41 C46 C45 177.4(2) . . . . ?
C42 C41 C46 C461 -179.7(2) . . . . ?
N4 C41 C46 C461 -1.8(4) . . . . ?
C44 C45 C46 C41 0.6(4) . . . . ?
C44 C45 C46 C461 179.8(3) . . . . ?
C33 C32 C321 C323 -78.7(4) . . . . ?
C31 C32 C321 C323 101.1(4) . . . . ?
C33 C32 C321 C322 46.7(4) . . . . ?
C31 C32 C321 C322 -133.5(3) . . . . ?
C31 C36 C361 C362 104.9(3) . . . . ?
C35 C36 C361 C362 -73.7(4) . . . . ?
C31 C36 C361 C363 -132.5(3) . . . . ?
C35 C36 C361 C363 48.8(4) . . . . ?
C43 C42 C421 C422 -83.4(4) . . . . ?
C41 C42 C421 C422 96.6(4) . . . . ?
C43 C42 C421 C423 40.6(4) . . . . ?
C41 C42 C421 C423 -139.3(3) . . . . ?
C41 C46 C461 C463 109.2(3) . . . . ?
C45 C46 C461 C463 -70.0(4) . . . . ?
C41 C46 C461 C462 -126.7(3) . . . . ?
C45 C46 C461 C462 54.1(4) . . . . ?
N2 C1 N1 C2 0.7(3) . . . . ?
P1 C1 N1 C2 -178.1(2) . . . . ?
N2 C1 N1 C11 -175.4(2) . . . . ?
P1 C1 N1 C11 5.8(3) . . . . ?
C3 C2 N1 C1 -0.5(4) . . . . ?
C3 C2 N1 C11 175.5(3) . . . . ?
C12 C11 N1 C1 81.2(3) . . . . ?
C16 C11 N1 C1 -97.1(3) . . . . ?
C12 C11 N1 C2 -94.4(3) . . . . ?
C16 C11 N1 C2 87.3(3) . . . . ?
N1 C1 N2 C3 -0.6(3) . . . . ?
P1 C1 N2 C3 177.8(2) . . . . ?
N1 C1 N2 C21 176.7(2) . . . . ?
P1 C1 N2 C21 -4.9(5) . . . . ?
C2 C3 N2 C1 0.3(4) . . . . ?
C2 C3 N2 C21 -177.1(3) . . . . ?
C26 C21 N2 C1 91.6(3) . . . . ?
C22 C21 N2 C1 -89.0(3) . . . . ?
C26 C21 N2 C3 -91.3(3) . . . . ?
C22 C21 N2 C3 88.0(3) . . . . ?
N4 C4 N3 C5 0.0(3) . . . . ?
P2 C4 N3 C5 -178.9(2) . . . . ?
N4 C4 N3 C31 -179.8(2) . . . . ?
P2 C4 N3 C31 1.3(4) . . . . ?
C6 C5 N3 C4 0.1(3) . . . . ?
C6 C5 N3 C31 180.0(2) . . . . ?
C36 C31 N3 C4 -92.5(3) . . . . ?
C32 C31 N3 C4 88.3(3) . . . . ?
C36 C31 N3 C5 87.7(3) . . . . ?
C32 C31 N3 C5 -91.5(3) . . . . ?
N3 C4 N4 C6 -0.1(3) . . . . ?
P2 C4 N4 C6 179.03(18) . . . . ?
N3 C4 N4 C41 -177.7(2) . . . . ?
P2 C4 N4 C41 1.4(3) . . . . ?
C5 C6 N4 C4 0.2(3) . . . . ?
C5 C6 N4 C41 177.8(2) . . . . ?
C46 C41 N4 C4 84.8(3) . . . . ?
C42 C41 N4 C4 -97.1(3) . . . . ?
C46 C41 N4 C6 -92.4(3) . . . . ?
C42 C41 N4 C6 85.6(3) . . . . ?
N1 C1 P1 P2 -175.15(19) . . . . ?
N2 C1 P1 P2 6.6(3) . . . . ?
N3 C4 P2 P1 -5.9(3) . . . . ?
N4 C4 P2 P1 175.32(17) . . . . ?

_refine_diff_density_max         0.654
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.056

####################################################################### 
# 
# 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_ad031db2
_database_code_depnum_ccdc_archive 'CCDC 1572772'
_audit_update_record             
;
2017-09-05 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H60 N4 P2, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H64 Cl4 F6 N4 P3'
_chemical_formula_weight         1069.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   18.8778(10)
_cell_length_b                   16.6879(8)
_cell_length_c                   17.4336(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.902(4)
_cell_angle_gamma                90
_cell_volume                     5463.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15655
_cell_measurement_theta_min      3.5200
_cell_measurement_theta_max      75.8950

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_F_000             2236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.281
_shelx_estimated_absorpt_T_min   0.675
_shelx_estimated_absorpt_T_max   0.779
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -9 -7 0.0413
0 8 7 0.0480
12 1 0 0.0505
1 6 -9 0.0664
-12 -1 0 0.0614
0 -6 9 0.0571
-4 -6 9 0.0633
10 -3 5 0.0623
9 -7 1 0.0588
0 -3 -11 0.0528
9 -6 -5 0.0577
-2 4 10 0.0608
0 11 -2 0.0487
10 6 3 0.0498
0 10 4 0.0295
1 -8 7 0.0453
0 -5 -10 0.0420
4 -7 -8 0.0426
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0335 -8.9606 -6.9894 -0.0616 1.0262 -0.1127
-0.0285 7.9649 6.9907 0.1013 -0.9471 0.1376
11.9974 1.0086 -0.0215 -0.5605 -0.0777 0.8105
0.9558 5.9761 -9.0118 -0.8192 -0.0711 -0.5126
-11.9974 -1.0086 0.0215 0.5605 0.0777 -0.8105
0.0444 -5.9750 9.0101 0.7758 0.0712 0.5823
-3.9564 -5.9793 9.0168 0.9494 0.0707 0.3038
10.0250 -2.9768 4.9884 -0.0162 0.0144 1.0113
9.0382 -6.9603 0.9946 -0.0534 0.5102 0.8488
-0.0029 -2.9860 -10.9984 -0.5385 0.7308 -0.4545
9.0235 -5.9640 -5.0081 -0.4516 0.7002 0.5353
-2.0041 3.9797 10.0002 0.5259 -0.7653 0.2423
-0.0580 10.9528 -2.0153 -0.5556 -0.7808 -0.3700
9.9770 5.9847 2.9758 -0.4925 -0.6082 0.6911
-0.0433 9.9566 3.9873 -0.1573 -0.9708 -0.0565
1.0513 -7.9651 7.0107 0.6921 0.3193 0.6054
0.0087 -4.9775 -9.9955 -0.3995 0.8442 -0.3566
4.0227 -6.9648 -7.9990 -0.3743 0.9133 0.0678
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.739
_oxdiff_exptl_absorpt_empirical_full_max 1.657
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            72990
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.543
_diffrn_reflns_theta_max         76.350
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11369
_reflns_number_gt                8718
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
;
 SHELXT-2014/7 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_molecular_graphics    ?
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;


_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as a rigid bodies and allowed to 
 rotate about the E-CH3 bond.

 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 > 2sigma(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)+(0.0517P)²+2.4465P] 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         11369
_refine_ls_number_parameters     618
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1260
_refine_ls_wR_factor_gt          0.1127
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_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
C1 C 0.24180(11) 0.61117(12) 0.48225(11) 0.0206(4) Uani 1 1 d . . . . .
C2 C 0.23374(12) 0.74469(13) 0.46194(13) 0.0269(4) Uani 1 1 d . . . . .
H2 H 0.2249 0.7947 0.4368 0.032 Uiso 1 1 calc R U . . .
C3 C 0.25868(12) 0.73326(13) 0.53644(13) 0.0272(4) Uani 1 1 d . . . . .
H3 H 0.2707 0.7740 0.5736 0.033 Uiso 1 1 calc R U . . .
C4 C 0.26923(11) 0.34644(13) 0.52385(12) 0.0219(4) Uani 1 1 d . . . . .
C5 C 0.27566(12) 0.21417(13) 0.55111(13) 0.0263(4) Uani 1 1 d . . . . .
H5 H 0.2855 0.1654 0.5782 0.032 Uiso 1 1 calc R U . . .
C6 C 0.24314(12) 0.22221(13) 0.47880(13) 0.0261(4) Uani 1 1 d . . . . .
H6 H 0.2258 0.1799 0.4455 0.031 Uiso 1 1 calc R U . . .
C11 C 0.19596(11) 0.65425(12) 0.35051(11) 0.0217(4) Uani 1 1 d . . . . .
C12 C 0.24489(11) 0.64380(13) 0.29611(12) 0.0236(4) Uani 1 1 d . . . . .
C13 C 0.21678(13) 0.62826(15) 0.22004(13) 0.0296(5) Uani 1 1 d . . . . .
H13 H 0.2480 0.6205 0.1813 0.036 Uiso 1 1 calc R U . . .
C14 C 0.14343(13) 0.62412(16) 0.20058(13) 0.0335(5) Uani 1 1 d . . . . .
H14 H 0.1252 0.6141 0.1486 0.040 Uiso 1 1 calc R U . . .
C15 C 0.09701(12) 0.63441(16) 0.25594(14) 0.0317(5) Uani 1 1 d . . . . .
H15 H 0.0472 0.6311 0.2416 0.038 Uiso 1 1 calc R U . . .
C16 C 0.12221(12) 0.64957(13) 0.33266(13) 0.0260(4) Uani 1 1 d . . . . .
C21 C 0.28563(11) 0.61681(12) 0.62372(11) 0.0208(4) Uani 1 1 d . . . . .
C22 C 0.35820(11) 0.59981(13) 0.64291(12) 0.0233(4) Uani 1 1 d . . . . .
C23 C 0.37723(12) 0.56705(14) 0.71558(13) 0.0265(4) Uani 1 1 d . . . . .
H23 H 0.4258 0.5553 0.7310 0.032 Uiso 1 1 calc R U . . .
C24 C 0.32654(13) 0.55121(14) 0.76589(12) 0.0288(5) Uani 1 1 d . . . . .
H24 H 0.3407 0.5281 0.8149 0.035 Uiso 1 1 calc R U . . .
C25 C 0.25542(12) 0.56886(14) 0.74514(12) 0.0262(4) Uani 1 1 d . . . . .
H25 H 0.2212 0.5573 0.7799 0.031 Uiso 1 1 calc R U . . .
C26 C 0.23348(11) 0.60342(13) 0.67369(12) 0.0229(4) Uani 1 1 d . . . . .
C31 C 0.32732(12) 0.31040(13) 0.65304(12) 0.0237(4) Uani 1 1 d . . . . .
C32 C 0.40136(12) 0.31570(14) 0.66058(13) 0.0265(4) Uani 1 1 d . . . . .
C33 C 0.43479(12) 0.33487(14) 0.73339(13) 0.0281(4) Uani 1 1 d . . . . .
H33 H 0.4853 0.3381 0.7406 0.034 Uiso 1 1 calc R U . . .
C34 C 0.39618(13) 0.34941(13) 0.79570(13) 0.0273(4) Uani 1 1 d . . . . .
C35 C 0.32233(12) 0.34440(14) 0.78506(13) 0.0280(4) Uani 1 1 d . . . . .
H35 H 0.2957 0.3546 0.8274 0.034 Uiso 1 1 calc R U . . .
C36 C 0.28640(12) 0.32472(13) 0.71354(13) 0.0257(4) Uani 1 1 d . . . . .
C37 C 0.44384(13) 0.30380(16) 0.59292(14) 0.0329(5) Uani 1 1 d . . . . .
H37A H 0.4311 0.2523 0.5682 0.049 Uiso 1 1 calc R U . . .
H37B H 0.4948 0.3041 0.6109 0.049 Uiso 1 1 calc R U . . .
H37C H 0.4333 0.3472 0.5557 0.049 Uiso 1 1 calc R U . . .
C38 C 0.43363(14) 0.37064(16) 0.87389(14) 0.0363(5) Uani 1 1 d . . . . .
H38A H 0.4234 0.4266 0.8860 0.054 Uiso 1 1 calc R U . . .
H38B H 0.4851 0.3636 0.8732 0.054 Uiso 1 1 calc R U . . .
H38C H 0.4166 0.3355 0.9132 0.054 Uiso 1 1 calc R U . . .
C39 C 0.20586(12) 0.32183(16) 0.70223(14) 0.0335(5) Uani 1 1 d . . . . .
H39A H 0.1873 0.3748 0.6863 0.050 Uiso 1 1 calc R U . . .
H39B H 0.1876 0.3065 0.7508 0.050 Uiso 1 1 calc R U . . .
H39C H 0.1905 0.2823 0.6623 0.050 Uiso 1 1 calc R U . . .
C41 C 0.21158(11) 0.33448(12) 0.38778(12) 0.0221(4) Uani 1 1 d . . . . .
C42 C 0.25895(11) 0.35477(13) 0.33484(12) 0.0234(4) Uani 1 1 d . . . . .
C43 C 0.23033(12) 0.38121(14) 0.26216(12) 0.0271(4) Uani 1 1 d . . . . .
H43 H 0.2614 0.3959 0.2250 0.033 Uiso 1 1 calc R U . . .
C44 C 0.15674(13) 0.38636(14) 0.24314(13) 0.0297(5) Uani 1 1 d . . . . .
C45 C 0.11170(12) 0.36627(15) 0.29837(14) 0.0302(5) Uani 1 1 d . . . . .
H45 H 0.0617 0.3704 0.2857 0.036 Uiso 1 1 calc R U . . .
C46 C 0.13778(12) 0.34021(14) 0.37182(13) 0.0268(4) Uani 1 1 d . . . . .
C47 C 0.33858(12) 0.34989(15) 0.35540(13) 0.0291(4) Uani 1 1 d . . . . .
H47A H 0.3544 0.3952 0.3886 0.044 Uiso 1 1 calc R U . . .
H47B H 0.3626 0.3518 0.3082 0.044 Uiso 1 1 calc R U . . .
H47C H 0.3504 0.2996 0.3827 0.044 Uiso 1 1 calc R U . . .
C48 C 0.12720(15) 0.41114(18) 0.16276(15) 0.0397(6) Uani 1 1 d . . . . .
H48A H 0.0759 0.4209 0.1617 0.060 Uiso 1 1 calc R U . . .
H48B H 0.1356 0.3683 0.1263 0.060 Uiso 1 1 calc R U . . .
H48C H 0.1510 0.4602 0.1482 0.060 Uiso 1 1 calc R U . . .
C49 C 0.08870(13) 0.32142(18) 0.43220(15) 0.0375(5) Uani 1 1 d . . . . .
H49A H 0.0393 0.3312 0.4111 0.056 Uiso 1 1 calc R U . . .
H49B H 0.1005 0.3558 0.4773 0.056 Uiso 1 1 calc R U . . .
H49C H 0.0943 0.2651 0.4475 0.056 Uiso 1 1 calc R U . . .
C98 C 0.44868(14) 0.06373(18) 0.58635(16) 0.0405(6) Uani 1 1 d . . . . .
H98A H 0.4453 0.0045 0.5872 0.049 Uiso 1 1 calc R U . . .
H98B H 0.4117 0.0839 0.5466 0.049 Uiso 1 1 calc R U . . .
C99 C 0.05307(18) 0.0398(3) 0.4056(2) 0.0646(10) Uani 1 1 d . . . . .
H99A H 0.0178 0.0020 0.3799 0.078 Uiso 1 1 calc R U . . .
H99B H 0.0889 0.0082 0.4383 0.078 Uiso 1 1 calc R U . . .
C121 C 0.32468(12) 0.64967(14) 0.31649(13) 0.0275(4) Uani 1 1 d . . . . .
H121 H 0.3340 0.6493 0.3740 0.033 Uiso 1 1 calc R U . . .
C122 C 0.36390(15) 0.57903(19) 0.2861(2) 0.0509(8) Uani 1 1 d . . . . .
H12A H 0.3425 0.5290 0.3021 0.076 Uiso 1 1 calc R U . . .
H12B H 0.4141 0.5810 0.3070 0.076 Uiso 1 1 calc R U . . .
H12C H 0.3604 0.5815 0.2297 0.076 Uiso 1 1 calc R U . . .
C123 C 0.35236(14) 0.72847(18) 0.2880(2) 0.0500(8) Uani 1 1 d . . . . .
H12D H 0.3445 0.7303 0.2316 0.075 Uiso 1 1 calc R U . . .
H12E H 0.4034 0.7330 0.3044 0.075 Uiso 1 1 calc R U . . .
H12F H 0.3271 0.7730 0.3097 0.075 Uiso 1 1 calc R U . . .
C161 C 0.07043(12) 0.65965(15) 0.39330(14) 0.0308(5) Uani 1 1 d . . . . .
H161 H 0.0989 0.6662 0.4445 0.037 Uiso 1 1 calc R U . . .
C162 C 0.02416(15) 0.5847(2) 0.39701(17) 0.0454(7) Uani 1 1 d . . . . .
H16A H -0.0057 0.5781 0.3480 0.068 Uiso 1 1 calc R U . . .
H16B H -0.0063 0.5904 0.4390 0.068 Uiso 1 1 calc R U . . .
H16C H 0.0548 0.5376 0.4065 0.068 Uiso 1 1 calc R U . . .
C163 C 0.02456(19) 0.7346(2) 0.3780(2) 0.0570(8) Uani 1 1 d . . . . .
H16D H 0.0553 0.7818 0.3777 0.085 Uiso 1 1 calc R U . . .
H16E H -0.0074 0.7403 0.4186 0.085 Uiso 1 1 calc R U . . .
H16F H -0.0037 0.7296 0.3278 0.085 Uiso 1 1 calc R U . . .
C221 C 0.41382(12) 0.61594(15) 0.58759(13) 0.0295(5) Uani 1 1 d . . . . .
H221 H 0.3893 0.6147 0.5340 0.035 Uiso 1 1 calc R U . . .
C222 C 0.47255(14) 0.55235(18) 0.59288(17) 0.0409(6) Uani 1 1 d . . . . .
H22A H 0.5007 0.5560 0.6432 0.061 Uiso 1 1 calc R U . . .
H22B H 0.5035 0.5613 0.5519 0.061 Uiso 1 1 calc R U . . .
H22C H 0.4510 0.4990 0.5869 0.061 Uiso 1 1 calc R U . . .
C223 C 0.44640(15) 0.69931(18) 0.60123(18) 0.0424(6) Uani 1 1 d . . . . .
H22D H 0.4090 0.7400 0.5922 0.064 Uiso 1 1 calc R U . . .
H22E H 0.4827 0.7081 0.5657 0.064 Uiso 1 1 calc R U . . .
H22F H 0.4684 0.7033 0.6545 0.064 Uiso 1 1 calc R U . . .
C261 C 0.15540(11) 0.62484(14) 0.65287(13) 0.0276(4) Uani 1 1 d . . . . .
H261 H 0.1528 0.6661 0.6111 0.033 Uiso 1 1 calc R U . . .
C262 C 0.11253(13) 0.55215(18) 0.62237(18) 0.0424(6) Uani 1 1 d . . . . .
H26A H 0.1326 0.5310 0.5769 0.064 Uiso 1 1 calc R U . . .
H26B H 0.0629 0.5680 0.6082 0.064 Uiso 1 1 calc R U . . .
H26C H 0.1145 0.5107 0.6624 0.064 Uiso 1 1 calc R U . . .
C263 C 0.12186(14) 0.66029(19) 0.72115(18) 0.0435(6) Uani 1 1 d . . . . .
H26D H 0.0752 0.6829 0.7033 0.065 Uiso 1 1 calc R U . . .
H26E H 0.1527 0.7026 0.7450 0.065 Uiso 1 1 calc R U . . .
H26F H 0.1161 0.6181 0.7591 0.065 Uiso 1 1 calc R U . . .
N1 N 0.22363(9) 0.66976(11) 0.42934(10) 0.0218(3) Uani 1 1 d . . . . .
N2 N 0.26365(9) 0.65136(10) 0.54891(10) 0.0218(3) Uani 1 1 d . . . . .
N3 N 0.29184(10) 0.29054(11) 0.57795(10) 0.0238(4) Uani 1 1 d . . . . .
N4 N 0.23968(9) 0.30359(11) 0.46201(10) 0.0222(3) Uani 1 1 d . . . . .
F1 F 0.20574(8) -0.07946(10) 0.54416(8) 0.0371(3) Uani 1 1 d . . . . .
F2 F 0.28914(9) 0.01392(10) 0.58452(9) 0.0423(4) Uani 1 1 d . . . . .
F3 F 0.31072(10) 0.03387(11) 0.46108(11) 0.0520(4) Uani 1 1 d . . . . .
F4 F 0.22595(11) -0.05893(11) 0.42167(9) 0.0503(4) Uani 1 1 d . . . . .
F5 F 0.19938(9) 0.04620(10) 0.49552(10) 0.0451(4) Uani 1 1 d . . . . .
F6 F 0.31727(10) -0.09124(11) 0.51147(14) 0.0581(5) Uani 1 1 d . . . . .
P1 P 0.23068(3) 0.50808(3) 0.45192(3) 0.02541(12) Uani 1 1 d . . . . .
P2 P 0.28432(3) 0.45004(3) 0.54849(3) 0.02921(13) Uani 1 1 d . . . . .
P3 P 0.25838(3) -0.02295(3) 0.50286(3) 0.02679(13) Uani 1 1 d . . . . .
Cl96 Cl 0.53343(3) 0.09192(4) 0.56165(3) 0.03561(13) Uani 1 1 d . . . . .
Cl97 Cl 0.43242(3) 0.10219(4) 0.67771(3) 0.04067(15) Uani 1 1 d . . . . .
Cl98 Cl 0.09577(5) 0.09210(9) 0.33476(5) 0.0811(4) Uani 1 1 d . . . . .
Cl99 Cl 0.00972(5) 0.10612(7) 0.46384(5) 0.0666(2) 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
C1 N1 1.364(3) . ?
C1 N2 1.368(3) . ?
C1 P1 1.806(2) . ?
C2 C3 1.349(3) . ?
C2 N1 1.379(3) . ?
C3 N2 1.386(3) . ?
C4 N3 1.364(3) . ?
C4 N4 1.364(3) . ?
C4 P2 1.797(2) . ?
C5 C6 1.351(3) . ?
C5 N3 1.381(3) . ?
C6 N4 1.389(3) . ?
C11 C16 1.397(3) . ?
C11 C12 1.401(3) . ?
C11 N1 1.443(3) . ?
C12 C13 1.401(3) . ?
C12 C121 1.515(3) . ?
C13 C14 1.393(3) . ?
C14 C15 1.379(4) . ?
C15 C16 1.396(3) . ?
C16 C161 1.521(3) . ?
C21 C26 1.398(3) . ?
C21 C22 1.405(3) . ?
C21 N2 1.447(3) . ?
C22 C23 1.393(3) . ?
C22 C221 1.521(3) . ?
C23 C24 1.388(3) . ?
C24 C25 1.386(3) . ?
C25 C26 1.396(3) . ?
C26 C261 1.524(3) . ?
C31 C36 1.391(3) . ?
C31 C32 1.393(3) . ?
C31 N3 1.446(3) . ?
C32 C33 1.395(3) . ?
C32 C37 1.506(3) . ?
C33 C34 1.390(3) . ?
C34 C35 1.390(3) . ?
C34 C38 1.512(3) . ?
C35 C36 1.396(3) . ?
C36 C39 1.514(3) . ?
C41 C42 1.391(3) . ?
C41 C46 1.396(3) . ?
C41 N4 1.442(3) . ?
C42 C43 1.397(3) . ?
C42 C47 1.511(3) . ?
C43 C44 1.397(3) . ?
C44 C45 1.390(4) . ?
C44 C48 1.512(3) . ?
C45 C46 1.393(3) . ?
C46 C49 1.505(3) . ?
C98 Cl96 1.763(3) . ?
C98 Cl97 1.773(3) . ?
C99 Cl99 1.760(5) . ?
C99 Cl98 1.772(4) . ?
C121 C122 1.516(4) . ?
C121 C123 1.517(3) . ?
C161 C163 1.529(4) . ?
C161 C162 1.531(4) . ?
C221 C223 1.530(4) . ?
C221 C222 1.531(4) . ?
C261 C262 1.523(3) . ?
C261 C263 1.524(3) . ?
F1 P3 1.5945(15) . ?
F2 P3 1.6039(15) . ?
F3 P3 1.5981(17) . ?
F4 P3 1.6001(16) . ?
F5 P3 1.5999(17) . ?
F6 P3 1.5883(18) . ?
P1 P2 2.1088(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 104.83(17) . . ?
N1 C1 P1 118.13(14) . . ?
N2 C1 P1 137.02(16) . . ?
C3 C2 N1 106.77(19) . . ?
C2 C3 N2 107.57(19) . . ?
N3 C4 N4 105.16(18) . . ?
N3 C4 P2 117.53(15) . . ?
N4 C4 P2 137.31(16) . . ?
C6 C5 N3 106.73(19) . . ?
C5 C6 N4 107.51(19) . . ?
C16 C11 C12 123.61(19) . . ?
C16 C11 N1 118.49(19) . . ?
C12 C11 N1 117.90(18) . . ?
C13 C12 C11 116.9(2) . . ?
C13 C12 C121 120.3(2) . . ?
C11 C12 C121 122.82(19) . . ?
C14 C13 C12 120.7(2) . . ?
C15 C14 C13 120.7(2) . . ?
C14 C15 C16 121.0(2) . . ?
C15 C16 C11 117.2(2) . . ?
C15 C16 C161 120.4(2) . . ?
C11 C16 C161 122.40(19) . . ?
C26 C21 C22 123.44(19) . . ?
C26 C21 N2 118.06(18) . . ?
C22 C21 N2 118.50(19) . . ?
C23 C22 C21 116.7(2) . . ?
C23 C22 C221 121.1(2) . . ?
C21 C22 C221 122.21(19) . . ?
C24 C23 C22 121.3(2) . . ?
C25 C24 C23 120.5(2) . . ?
C24 C25 C26 120.7(2) . . ?
C25 C26 C21 117.30(19) . . ?
C25 C26 C261 120.0(2) . . ?
C21 C26 C261 122.68(19) . . ?
C36 C31 C32 123.2(2) . . ?
C36 C31 N3 118.96(19) . . ?
C32 C31 N3 117.8(2) . . ?
C31 C32 C33 117.1(2) . . ?
C31 C32 C37 121.8(2) . . ?
C33 C32 C37 121.0(2) . . ?
C34 C33 C32 121.8(2) . . ?
C35 C34 C33 119.0(2) . . ?
C35 C34 C38 120.3(2) . . ?
C33 C34 C38 120.8(2) . . ?
C34 C35 C36 121.5(2) . . ?
C31 C36 C35 117.5(2) . . ?
C31 C36 C39 121.6(2) . . ?
C35 C36 C39 120.9(2) . . ?
C42 C41 C46 123.20(19) . . ?
C42 C41 N4 118.68(18) . . ?
C46 C41 N4 118.09(19) . . ?
C41 C42 C43 117.6(2) . . ?
C41 C42 C47 121.40(19) . . ?
C43 C42 C47 121.0(2) . . ?
C42 C43 C44 121.1(2) . . ?
C45 C44 C43 119.0(2) . . ?
C45 C44 C48 121.0(2) . . ?
C43 C44 C48 120.0(2) . . ?
C44 C45 C46 121.9(2) . . ?
C45 C46 C41 117.1(2) . . ?
C45 C46 C49 121.5(2) . . ?
C41 C46 C49 121.3(2) . . ?
Cl96 C98 Cl97 111.59(15) . . ?
Cl99 C99 Cl98 111.3(3) . . ?
C12 C121 C122 112.2(2) . . ?
C12 C121 C123 110.30(19) . . ?
C122 C121 C123 111.3(2) . . ?
C16 C161 C163 111.2(2) . . ?
C16 C161 C162 110.4(2) . . ?
C163 C161 C162 111.1(2) . . ?
C22 C221 C223 110.8(2) . . ?
C22 C221 C222 112.5(2) . . ?
C223 C221 C222 110.1(2) . . ?
C262 C261 C26 111.3(2) . . ?
C262 C261 C263 109.5(2) . . ?
C26 C261 C263 111.98(19) . . ?
C1 N1 C2 110.91(17) . . ?
C1 N1 C11 123.85(18) . . ?
C2 N1 C11 125.22(18) . . ?
C1 N2 C3 109.91(17) . . ?
C1 N2 C21 127.13(17) . . ?
C3 N2 C21 122.89(17) . . ?
C4 N3 C5 110.76(18) . . ?
C4 N3 C31 123.52(18) . . ?
C5 N3 C31 125.72(18) . . ?
C4 N4 C6 109.83(17) . . ?
C4 N4 C41 127.19(18) . . ?
C6 N4 C41 122.92(17) . . ?
C1 P1 P2 99.90(7) . . ?
C4 P2 P1 101.52(7) . . ?
F6 P3 F1 89.75(10) . . ?
F6 P3 F3 90.53(11) . . ?
F1 P3 F3 179.63(11) . . ?
F6 P3 F5 179.13(12) . . ?
F1 P3 F5 90.09(9) . . ?
F3 P3 F5 89.63(11) . . ?
F6 P3 F4 90.85(11) . . ?
F1 P3 F4 88.74(9) . . ?
F3 P3 F4 91.02(10) . . ?
F5 P3 F4 90.00(10) . . ?
F6 P3 F2 90.31(11) . . ?
F1 P3 F2 90.67(8) . . ?
F3 P3 F2 89.57(9) . . ?
F5 P3 F2 88.84(9) . . ?
F4 P3 F2 178.69(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.0(3) . . . . ?
N3 C5 C6 N4 0.0(3) . . . . ?
C16 C11 C12 C13 0.3(3) . . . . ?
N1 C11 C12 C13 179.6(2) . . . . ?
C16 C11 C12 C121 179.6(2) . . . . ?
N1 C11 C12 C121 -1.2(3) . . . . ?
C11 C12 C13 C14 0.4(3) . . . . ?
C121 C12 C13 C14 -178.9(2) . . . . ?
C12 C13 C14 C15 -0.7(4) . . . . ?
C13 C14 C15 C16 0.3(4) . . . . ?
C14 C15 C16 C11 0.3(4) . . . . ?
C14 C15 C16 C161 -179.2(2) . . . . ?
C12 C11 C16 C15 -0.7(3) . . . . ?
N1 C11 C16 C15 -179.9(2) . . . . ?
C12 C11 C16 C161 178.8(2) . . . . ?
N1 C11 C16 C161 -0.4(3) . . . . ?
C26 C21 C22 C23 0.8(3) . . . . ?
N2 C21 C22 C23 179.63(18) . . . . ?
C26 C21 C22 C221 -179.3(2) . . . . ?
N2 C21 C22 C221 -0.5(3) . . . . ?
C21 C22 C23 C24 0.8(3) . . . . ?
C221 C22 C23 C24 -179.1(2) . . . . ?
C22 C23 C24 C25 -0.9(3) . . . . ?
C23 C24 C25 C26 -0.5(3) . . . . ?
C24 C25 C26 C21 2.0(3) . . . . ?
C24 C25 C26 C261 -178.1(2) . . . . ?
C22 C21 C26 C25 -2.2(3) . . . . ?
N2 C21 C26 C25 179.00(18) . . . . ?
C22 C21 C26 C261 177.9(2) . . . . ?
N2 C21 C26 C261 -0.9(3) . . . . ?
C36 C31 C32 C33 1.3(3) . . . . ?
N3 C31 C32 C33 -180.0(2) . . . . ?
C36 C31 C32 C37 -176.9(2) . . . . ?
N3 C31 C32 C37 1.8(3) . . . . ?
C31 C32 C33 C34 -1.0(3) . . . . ?
C37 C32 C33 C34 177.2(2) . . . . ?
C32 C33 C34 C35 0.2(4) . . . . ?
C32 C33 C34 C38 -179.6(2) . . . . ?
C33 C34 C35 C36 0.4(3) . . . . ?
C38 C34 C35 C36 -179.8(2) . . . . ?
C32 C31 C36 C35 -0.7(3) . . . . ?
N3 C31 C36 C35 -179.47(19) . . . . ?
C32 C31 C36 C39 177.3(2) . . . . ?
N3 C31 C36 C39 -1.4(3) . . . . ?
C34 C35 C36 C31 -0.1(3) . . . . ?
C34 C35 C36 C39 -178.2(2) . . . . ?
C46 C41 C42 C43 -0.7(3) . . . . ?
N4 C41 C42 C43 177.24(19) . . . . ?
C46 C41 C42 C47 178.2(2) . . . . ?
N4 C41 C42 C47 -3.8(3) . . . . ?
C41 C42 C43 C44 -0.6(3) . . . . ?
C47 C42 C43 C44 -179.5(2) . . . . ?
C42 C43 C44 C45 1.3(3) . . . . ?
C42 C43 C44 C48 -176.9(2) . . . . ?
C43 C44 C45 C46 -0.8(4) . . . . ?
C48 C44 C45 C46 177.4(2) . . . . ?
C44 C45 C46 C41 -0.4(4) . . . . ?
C44 C45 C46 C49 177.8(2) . . . . ?
C42 C41 C46 C45 1.2(3) . . . . ?
N4 C41 C46 C45 -176.8(2) . . . . ?
C42 C41 C46 C49 -177.0(2) . . . . ?
N4 C41 C46 C49 5.0(3) . . . . ?
C13 C12 C121 C122 -50.0(3) . . . . ?
C11 C12 C121 C122 130.8(3) . . . . ?
C13 C12 C121 C123 74.6(3) . . . . ?
C11 C12 C121 C123 -104.6(3) . . . . ?
C15 C16 C161 C163 -65.5(3) . . . . ?
C11 C16 C161 C163 115.0(3) . . . . ?
C15 C16 C161 C162 58.4(3) . . . . ?
C11 C16 C161 C162 -121.1(2) . . . . ?
C23 C22 C221 C223 -87.9(3) . . . . ?
C21 C22 C221 C223 92.2(3) . . . . ?
C23 C22 C221 C222 35.9(3) . . . . ?
C21 C22 C221 C222 -144.1(2) . . . . ?
C25 C26 C261 C262 -82.8(3) . . . . ?
C21 C26 C261 C262 97.1(3) . . . . ?
C25 C26 C261 C263 40.0(3) . . . . ?
C21 C26 C261 C263 -140.0(2) . . . . ?
N2 C1 N1 C2 -0.1(2) . . . . ?
P1 C1 N1 C2 178.66(16) . . . . ?
N2 C1 N1 C11 -178.66(19) . . . . ?
P1 C1 N1 C11 0.1(3) . . . . ?
C3 C2 N1 C1 0.0(3) . . . . ?
C3 C2 N1 C11 178.6(2) . . . . ?
C16 C11 N1 C1 91.6(3) . . . . ?
C12 C11 N1 C1 -87.7(3) . . . . ?
C16 C11 N1 C2 -86.8(3) . . . . ?
C12 C11 N1 C2 93.9(3) . . . . ?
N1 C1 N2 C3 0.1(2) . . . . ?
P1 C1 N2 C3 -178.29(19) . . . . ?
N1 C1 N2 C21 177.03(19) . . . . ?
P1 C1 N2 C21 -1.3(4) . . . . ?
C2 C3 N2 C1 0.0(3) . . . . ?
C2 C3 N2 C21 -177.2(2) . . . . ?
C26 C21 N2 C1 -89.7(3) . . . . ?
C22 C21 N2 C1 91.4(3) . . . . ?
C26 C21 N2 C3 86.9(3) . . . . ?
C22 C21 N2 C3 -92.0(3) . . . . ?
N4 C4 N3 C5 -1.0(2) . . . . ?
P2 C4 N3 C5 179.15(16) . . . . ?
N4 C4 N3 C31 179.41(19) . . . . ?
P2 C4 N3 C31 -0.4(3) . . . . ?
C6 C5 N3 C4 0.7(3) . . . . ?
C6 C5 N3 C31 -179.8(2) . . . . ?
C36 C31 N3 C4 88.5(3) . . . . ?
C32 C31 N3 C4 -90.3(3) . . . . ?
C36 C31 N3 C5 -91.0(3) . . . . ?
C32 C31 N3 C5 90.2(3) . . . . ?
N3 C4 N4 C6 1.0(2) . . . . ?
P2 C4 N4 C6 -179.23(19) . . . . ?
N3 C4 N4 C41 -176.04(19) . . . . ?
P2 C4 N4 C41 3.7(4) . . . . ?
C5 C6 N4 C4 -0.6(3) . . . . ?
C5 C6 N4 C41 176.6(2) . . . . ?
C42 C41 N4 C4 79.1(3) . . . . ?
C46 C41 N4 C4 -102.8(3) . . . . ?
C42 C41 N4 C6 -97.6(2) . . . . ?
C46 C41 N4 C6 80.5(3) . . . . ?
N1 C1 P1 P2 169.79(15) . . . . ?
N2 C1 P1 P2 -12.0(2) . . . . ?
N3 C4 P2 P1 -174.28(15) . . . . ?
N4 C4 P2 P1 6.0(3) . . . . ?

_refine_diff_density_max         0.985
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_ad017db
_database_code_depnum_ccdc_archive 'CCDC 1572770'
_audit_update_record             
;
2017-09-05 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H60 N4 P2'
_chemical_formula_sum            'C48 H60 N4 P2'
_chemical_formula_weight         754.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7604(2)
_cell_length_b                   12.9388(4)
_cell_length_c                   18.3755(6)
_cell_angle_alpha                100.342(2)
_cell_angle_beta                 104.409(2)
_cell_angle_gamma                110.565(2)
_cell_volume                     2217.19(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    57404
_cell_measurement_theta_min      3.8070
_cell_measurement_theta_max      76.0060

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_F_000             812
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.155
_shelx_estimated_absorpt_T_min   0.769
_shelx_estimated_absorpt_T_max   0.855
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -7 0 0.0723
0 7 0 0.0678
6 0 -3 0.1175
-6 -1 3 0.0691
0 -3 12 0.1135
1 3 -12 0.0876
5 0 2 0.1078
6 2 -4 0.1106
-6 -1 1 0.0518
-2 2 -10 0.0767
-7 1 3 0.0695
0 -7 8 0.0786
0 7 -8 0.0718
-6 4 -2 0.0535
5 -1 -10 0.1449
5 2 2 0.0902
0 3 9 0.1140
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0026 -7.0073 0.0225 -0.7209 0.3441 -0.4801
0.0026 7.0073 -0.0225 0.7209 -0.3441 0.4801
5.9987 0.0102 -3.0315 -0.1479 0.0693 0.9048
-5.9990 -1.0112 3.0347 0.0449 -0.0202 -0.9734
0.0133 -2.9912 11.9944 0.4070 0.9554 -0.0806
0.9871 2.9934 -12.0003 -0.4019 -0.9102 0.2366
5.0043 0.0129 1.9680 0.1452 0.3607 0.8009
5.9982 2.0113 -4.0367 -0.0016 -0.0963 1.0316
-6.0014 -1.0132 1.0373 -0.0744 -0.1548 -0.9943
-2.0120 1.9878 -9.9819 -0.4011 -0.8620 -0.2791
-6.9987 0.9887 3.0342 0.2457 -0.1637 -0.9922
0.0070 -6.9994 8.0123 -0.2436 0.8827 -0.3967
-0.0070 6.9994 -8.0123 0.2436 -0.8827 0.3967
-6.0032 3.9890 -1.9750 0.2615 -0.6026 -0.6826
4.9895 -1.0000 -10.0135 -0.6738 -0.3980 0.6072
5.0050 2.0150 1.9616 0.3512 0.2624 0.9381
0.0119 3.0120 8.9789 0.8460 0.4585 0.2996
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.749
_oxdiff_exptl_absorpt_empirical_full_max 1.494
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            94739
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.818
_diffrn_reflns_theta_max         76.107
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9240
_reflns_number_gt                8583
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
;
 SHELXS-2014/7 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112--122)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_molecular_graphics    ?
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;


_refine_special_details          
;
 The hydrogen atoms of the methyl group on C27 were refined over two positions
 (HFIX127). All other H atoms were placed in idealised positions and refined 
 using a riding model, with a common U restrained to be 1.2 (1.5 for methyl
 groups) times the equivalent isotropic displacement parameter of the parent
 atom. Not-disordered methyl groups were treated as a rigid bodies and allowed
 to rotate about the E-CH3 bond.

 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 > 2sigma(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)+(0.0542P)²+0.6620P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9240
_refine_ls_number_parameters     501
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0948
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_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
C1 C 0.31018(11) 0.38222(9) 0.21936(6) 0.0181(2) Uani 1 1 d . . . . .
C2 C 0.07353(12) 0.26681(10) 0.16095(7) 0.0233(2) Uani 1 1 d . . . . .
H2 H -0.0122 0.2011 0.1315 0.028 Uiso 1 1 calc R U . . .
C3 C 0.08645(12) 0.37122(10) 0.19794(7) 0.0248(2) Uani 1 1 d . . . . .
H3 H 0.0112 0.3929 0.1992 0.030 Uiso 1 1 calc R U . . .
C4 C 0.76516(11) 0.62903(9) 0.31794(6) 0.0197(2) Uani 1 1 d . . . . .
C5 C 0.99250(12) 0.75956(10) 0.34843(7) 0.0262(2) Uani 1 1 d . . . . .
H5 H 1.0742 0.8305 0.3675 0.031 Uiso 1 1 calc R U . . .
C6 C 0.98404(12) 0.65601(10) 0.31299(7) 0.0265(2) Uani 1 1 d . . . . .
H6 H 1.0586 0.6403 0.3022 0.032 Uiso 1 1 calc R U . . .
C11 C 0.27914(11) 0.56510(9) 0.26814(6) 0.0204(2) Uani 1 1 d . . . . .
C12 C 0.32341(11) 0.61077(9) 0.35003(7) 0.0217(2) Uani 1 1 d . . . . .
C13 C 0.36733(13) 0.72954(10) 0.38030(7) 0.0274(2) Uani 1 1 d . . . . .
H13 H 0.3985 0.7633 0.4356 0.033 Uiso 1 1 calc R U . . .
C14 C 0.36620(14) 0.79889(10) 0.33124(8) 0.0334(3) Uani 1 1 d . . . . .
H14 H 0.3962 0.8795 0.3530 0.040 Uiso 1 1 calc R U . . .
C15 C 0.32167(15) 0.75156(11) 0.25063(8) 0.0331(3) Uani 1 1 d . . . . .
H15 H 0.3215 0.8003 0.2176 0.040 Uiso 1 1 calc R U . . .
C16 C 0.27706(12) 0.63348(10) 0.21697(7) 0.0253(2) Uani 1 1 d . . . . .
C21 C 0.24086(11) 0.17977(9) 0.14115(6) 0.0205(2) Uani 1 1 d . . . . .
C22 C 0.25910(12) 0.10583(10) 0.18585(7) 0.0254(2) Uani 1 1 d . . . . .
C23 C 0.28322(15) 0.01286(11) 0.15104(8) 0.0346(3) Uani 1 1 d . . . . .
H23 H 0.2953 -0.0394 0.1795 0.042 Uiso 1 1 calc R U . . .
C24 C 0.28983(15) -0.00456(11) 0.07586(9) 0.0373(3) Uani 1 1 d . . . . .
H24 H 0.3047 -0.0691 0.0530 0.045 Uiso 1 1 calc R U . . .
C25 C 0.27490(14) 0.07132(11) 0.03387(8) 0.0328(3) Uani 1 1 d . . . . .
H25 H 0.2811 0.0590 -0.0174 0.039 Uiso 1 1 calc R U . . .
C26 C 0.25082(12) 0.16609(10) 0.06581(7) 0.0247(2) Uani 1 1 d . . . . .
C31 C 0.81960(11) 0.83385(9) 0.37976(7) 0.0218(2) Uani 1 1 d . . . . .
C32 C 0.82692(12) 0.86285(9) 0.45800(7) 0.0243(2) Uani 1 1 d . . . . .
C33 C 0.78330(13) 0.94855(10) 0.48245(7) 0.0269(2) Uani 1 1 d . . . . .
H33 H 0.7869 0.9695 0.5355 0.032 Uiso 1 1 calc R U . . .
C34 C 0.73466(13) 1.00422(10) 0.43150(7) 0.0278(2) Uani 1 1 d . . . . .
C35 C 0.72807(13) 0.97192(10) 0.35365(7) 0.0277(2) Uani 1 1 d . . . . .
H35 H 0.6950 1.0096 0.3184 0.033 Uiso 1 1 calc R U . . .
C36 C 0.76874(12) 0.88588(9) 0.32616(7) 0.0247(2) Uani 1 1 d . . . . .
C37 C 0.87715(15) 0.80220(11) 0.51362(7) 0.0326(3) Uani 1 1 d . . . . .
H37A H 0.9280 0.7624 0.4918 0.049 Uiso 0.5 1 calc R U P . .
H37B H 0.7959 0.7458 0.5209 0.049 Uiso 0.5 1 calc R U P . .
H37C H 0.9403 0.8590 0.5644 0.049 Uiso 0.5 1 calc R U P . .
H37D H 0.8481 0.8157 0.5596 0.049 Uiso 0.5 1 calc R U P . .
H37E H 0.9802 0.8323 0.5305 0.049 Uiso 0.5 1 calc R U P . .
H37F H 0.8359 0.7191 0.4870 0.049 Uiso 0.5 1 calc R U P . .
C38 C 0.68879(16) 1.09711(12) 0.45996(9) 0.0382(3) Uani 1 1 d . . . . .
H38A H 0.6240 1.0693 0.4884 0.057 Uiso 1 1 calc R U . . .
H38B H 0.6409 1.1159 0.4148 0.057 Uiso 1 1 calc R U . . .
H38C H 0.7717 1.1664 0.4952 0.057 Uiso 1 1 calc R U . . .
C39 C 0.75234(15) 0.84549(11) 0.24084(7) 0.0321(3) Uani 1 1 d . . . . .
H39A H 0.6793 0.7663 0.2172 0.048 Uiso 1 1 calc R U . . .
H39B H 0.8421 0.8474 0.2366 0.048 Uiso 1 1 calc R U . . .
H39C H 0.7250 0.8964 0.2132 0.048 Uiso 1 1 calc R U . . .
C41 C 0.79902(11) 0.45516(9) 0.25694(6) 0.0191(2) Uani 1 1 d . . . . .
C42 C 0.79104(12) 0.37869(10) 0.30223(7) 0.0225(2) Uani 1 1 d . . . . .
C43 C 0.74896(13) 0.26286(10) 0.26334(8) 0.0282(2) Uani 1 1 d . . . . .
H43 H 0.7437 0.2094 0.2930 0.034 Uiso 1 1 calc R U . . .
C44 C 0.71444(13) 0.22323(10) 0.18248(8) 0.0300(3) Uani 1 1 d . . . . .
C45 C 0.72139(12) 0.30159(11) 0.13931(7) 0.0282(2) Uani 1 1 d . . . . .
H45 H 0.6965 0.2749 0.0838 0.034 Uiso 1 1 calc R U . . .
C46 C 0.76415(12) 0.41870(10) 0.17553(6) 0.0233(2) Uani 1 1 d . . . . .
C47 C 0.81895(14) 0.41885(11) 0.38898(7) 0.0301(3) Uani 1 1 d . . . . .
H47A H 0.9030 0.4921 0.4127 0.045 Uiso 1 1 calc R U . . .
H47B H 0.8344 0.3608 0.4131 0.045 Uiso 1 1 calc R U . . .
H47C H 0.7376 0.4299 0.3977 0.045 Uiso 1 1 calc R U . . .
C48 C 0.67122(17) 0.09687(12) 0.14271(10) 0.0451(4) Uani 1 1 d . . . . .
H48A H 0.6285 0.0800 0.0858 0.068 Uiso 1 1 calc R U . . .
H48B H 0.6026 0.0491 0.1628 0.068 Uiso 1 1 calc R U . . .
H48C H 0.7545 0.0797 0.1537 0.068 Uiso 1 1 calc R U . . .
C49 C 0.76605(15) 0.50304(12) 0.12893(8) 0.0355(3) Uani 1 1 d . . . . .
H49A H 0.6953 0.5326 0.1339 0.053 Uiso 1 1 calc R U . . .
H49B H 0.7443 0.4642 0.0735 0.053 Uiso 1 1 calc R U . . .
H49C H 0.8597 0.5674 0.1490 0.053 Uiso 1 1 calc R U . . .
C121 C 0.32332(13) 0.53438(10) 0.40403(7) 0.0252(2) Uani 1 1 d . . . . .
H121 H 0.3516 0.4733 0.3816 0.030 Uiso 1 1 calc R U . . .
C122 C 0.42696(14) 0.60062(12) 0.48760(7) 0.0338(3) Uani 1 1 d . . . . .
H12A H 0.5219 0.6395 0.4858 0.051 Uiso 1 1 calc R U . . .
H12B H 0.4271 0.5466 0.5187 0.051 Uiso 1 1 calc R U . . .
H12C H 0.3983 0.6582 0.5118 0.051 Uiso 1 1 calc R U . . .
C123 C 0.17439(14) 0.47445(12) 0.40656(8) 0.0347(3) Uani 1 1 d . . . . .
H12D H 0.1436 0.5328 0.4273 0.052 Uiso 1 1 calc R U . . .
H12E H 0.1750 0.4243 0.4407 0.052 Uiso 1 1 calc R U . . .
H12F H 0.1093 0.4279 0.3534 0.052 Uiso 1 1 calc R U . . .
C161 C 0.23921(14) 0.58386(11) 0.12889(7) 0.0305(3) Uani 1 1 d . . . . .
H161 H 0.1802 0.4990 0.1144 0.037 Uiso 1 1 calc R U . . .
C162 C 0.37350(17) 0.59972(16) 0.10946(8) 0.0451(4) Uani 1 1 d . . . . .
H16A H 0.4297 0.6821 0.1190 0.068 Uiso 1 1 calc R U . . .
H16B H 0.3484 0.5584 0.0541 0.068 Uiso 1 1 calc R U . . .
H16C H 0.4286 0.5689 0.1429 0.068 Uiso 1 1 calc R U . . .
C163 C 0.15355(18) 0.63573(16) 0.08036(9) 0.0474(4) Uani 1 1 d . . . . .
H16D H 0.0709 0.6286 0.0960 0.071 Uiso 1 1 calc R U . . .
H16E H 0.1225 0.5944 0.0244 0.071 Uiso 1 1 calc R U . . .
H16F H 0.2123 0.7175 0.0895 0.071 Uiso 1 1 calc R U . . .
C221 C 0.25028(14) 0.12381(10) 0.26794(7) 0.0302(3) Uani 1 1 d . . . . .
H221 H 0.2473 0.2006 0.2845 0.036 Uiso 1 1 calc R U . . .
C222 C 0.37991(18) 0.12572(13) 0.32698(9) 0.0454(4) Uani 1 1 d . . . . .
H22A H 0.3829 0.0500 0.3134 0.068 Uiso 1 1 calc R U . . .
H22B H 0.3746 0.1434 0.3800 0.068 Uiso 1 1 calc R U . . .
H22C H 0.4654 0.1850 0.3254 0.068 Uiso 1 1 calc R U . . .
C223 C 0.11347(17) 0.03124(13) 0.26696(8) 0.0448(4) Uani 1 1 d . . . . .
H22D H 0.0327 0.0341 0.2297 0.067 Uiso 1 1 calc R U . . .
H22E H 0.1065 0.0455 0.3197 0.067 Uiso 1 1 calc R U . . .
H22F H 0.1137 -0.0451 0.2508 0.067 Uiso 1 1 calc R U . . .
C261 C 0.23734(14) 0.24976(11) 0.01934(7) 0.0297(3) Uani 1 1 d . . . . .
H261 H 0.2291 0.3145 0.0538 0.036 Uiso 1 1 calc R U . . .
C262 C 0.36807(16) 0.30119(14) -0.00328(9) 0.0421(3) Uani 1 1 d . . . . .
H26A H 0.4522 0.3369 0.0441 0.063 Uiso 1 1 calc R U . . .
H26B H 0.3602 0.3597 -0.0291 0.063 Uiso 1 1 calc R U . . .
H26C H 0.3758 0.2399 -0.0394 0.063 Uiso 1 1 calc R U . . .
C263 C 0.10418(18) 0.19173(17) -0.05351(10) 0.0526(4) Uani 1 1 d . . . . .
H26D H 0.1084 0.1265 -0.0877 0.079 Uiso 1 1 calc R U . . .
H26E H 0.0977 0.2477 -0.0822 0.079 Uiso 1 1 calc R U . . .
H26F H 0.0211 0.1639 -0.0374 0.079 Uiso 1 1 calc R U . . .
N1 N 0.23031(10) 0.44255(8) 0.23431(5) 0.02003(18) Uani 1 1 d . . . . .
N2 N 0.20869(9) 0.27254(7) 0.17375(5) 0.01940(18) Uani 1 1 d . . . . .
N3 N 0.86039(10) 0.74408(8) 0.35207(6) 0.02271(19) Uani 1 1 d . . . . .
N4 N 0.84562(10) 0.57542(8) 0.29477(5) 0.02075(18) Uani 1 1 d . . . . .
P1 P 0.48845(3) 0.40754(2) 0.24463(2) 0.02155(8) Uani 1 1 d . . . . .
P2 P 0.59115(3) 0.58865(2) 0.31627(2) 0.02354(8) 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
C1 N1 1.3912(13) . ?
C1 N2 1.3919(13) . ?
C1 P1 1.7502(11) . ?
C2 C3 1.3409(16) . ?
C2 N2 1.3870(14) . ?
C3 N1 1.3981(14) . ?
C4 N4 1.3826(13) . ?
C4 N3 1.3902(13) . ?
C4 P2 1.7488(11) . ?
C5 C6 1.3412(16) . ?
C5 N3 1.3848(15) . ?
C6 N4 1.3976(14) . ?
C11 C12 1.4024(15) . ?
C11 C16 1.4034(16) . ?
C11 N1 1.4405(13) . ?
C12 C13 1.3951(15) . ?
C12 C121 1.5211(15) . ?
C13 C14 1.3822(18) . ?
C14 C15 1.3835(19) . ?
C15 C16 1.3945(17) . ?
C16 C161 1.5208(16) . ?
C21 C26 1.3996(16) . ?
C21 C22 1.4009(16) . ?
C21 N2 1.4341(13) . ?
C22 C23 1.3961(17) . ?
C22 C221 1.5162(17) . ?
C23 C24 1.383(2) . ?
C24 C25 1.381(2) . ?
C25 C26 1.3985(16) . ?
C26 C261 1.5174(16) . ?
C31 C32 1.3939(16) . ?
C31 C36 1.3969(16) . ?
C31 N3 1.4345(13) . ?
C32 C33 1.3941(16) . ?
C32 C37 1.5045(16) . ?
C33 C34 1.3902(17) . ?
C34 C35 1.3929(17) . ?
C34 C38 1.5103(16) . ?
C35 C36 1.3915(16) . ?
C36 C39 1.5053(16) . ?
C41 C46 1.3943(15) . ?
C41 C42 1.3967(15) . ?
C41 N4 1.4302(13) . ?
C42 C43 1.3927(16) . ?
C42 C47 1.5019(16) . ?
C43 C44 1.3881(18) . ?
C44 C45 1.3885(19) . ?
C44 C48 1.5135(16) . ?
C45 C46 1.3952(16) . ?
C46 C49 1.5010(16) . ?
C121 C122 1.5298(17) . ?
C121 C123 1.5325(17) . ?
C161 C162 1.5273(19) . ?
C161 C163 1.5282(18) . ?
C221 C222 1.5285(19) . ?
C221 C223 1.5305(19) . ?
C261 C262 1.5255(19) . ?
C261 C263 1.5289(19) . ?
P1 P2 2.1897(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 103.30(9) . . ?
N1 C1 P1 137.86(8) . . ?
N2 C1 P1 118.79(7) . . ?
C3 C2 N2 107.26(10) . . ?
C2 C3 N1 107.93(10) . . ?
N4 C4 N3 103.55(9) . . ?
N4 C4 P2 137.36(8) . . ?
N3 C4 P2 119.08(8) . . ?
C6 C5 N3 107.47(10) . . ?
C5 C6 N4 107.55(10) . . ?
C12 C11 C16 122.78(10) . . ?
C12 C11 N1 119.14(9) . . ?
C16 C11 N1 118.07(10) . . ?
C13 C12 C11 117.32(10) . . ?
C13 C12 C121 121.05(10) . . ?
C11 C12 C121 121.63(10) . . ?
C14 C13 C12 121.10(11) . . ?
C13 C14 C15 120.40(11) . . ?
C14 C15 C16 121.10(11) . . ?
C15 C16 C11 117.30(11) . . ?
C15 C16 C161 120.59(11) . . ?
C11 C16 C161 121.93(10) . . ?
C26 C21 C22 122.89(10) . . ?
C26 C21 N2 118.69(10) . . ?
C22 C21 N2 118.42(10) . . ?
C23 C22 C21 117.14(11) . . ?
C23 C22 C221 121.02(11) . . ?
C21 C22 C221 121.83(10) . . ?
C24 C23 C22 121.20(12) . . ?
C25 C24 C23 120.42(11) . . ?
C24 C25 C26 120.89(12) . . ?
C25 C26 C21 117.41(11) . . ?
C25 C26 C261 120.12(11) . . ?
C21 C26 C261 122.46(10) . . ?
C32 C31 C36 122.46(10) . . ?
C32 C31 N3 119.06(10) . . ?
C36 C31 N3 118.42(10) . . ?
C31 C32 C33 117.55(11) . . ?
C31 C32 C37 121.27(10) . . ?
C33 C32 C37 121.17(11) . . ?
C34 C33 C32 121.89(11) . . ?
C33 C34 C35 118.65(10) . . ?
C33 C34 C38 120.57(11) . . ?
C35 C34 C38 120.78(11) . . ?
C36 C35 C34 121.62(11) . . ?
C35 C36 C31 117.80(11) . . ?
C35 C36 C39 121.54(11) . . ?
C31 C36 C39 120.60(10) . . ?
C46 C41 C42 122.29(10) . . ?
C46 C41 N4 118.30(10) . . ?
C42 C41 N4 119.41(9) . . ?
C43 C42 C41 117.56(10) . . ?
C43 C42 C47 121.23(10) . . ?
C41 C42 C47 121.12(10) . . ?
C44 C43 C42 121.93(11) . . ?
C43 C44 C45 118.80(11) . . ?
C43 C44 C48 120.21(12) . . ?
C45 C44 C48 120.99(12) . . ?
C44 C45 C46 121.50(11) . . ?
C41 C46 C45 117.91(10) . . ?
C41 C46 C49 120.24(10) . . ?
C45 C46 C49 121.78(11) . . ?
C12 C121 C122 112.96(10) . . ?
C12 C121 C123 110.06(10) . . ?
C122 C121 C123 109.64(10) . . ?
C16 C161 C162 109.55(11) . . ?
C16 C161 C163 112.96(11) . . ?
C162 C161 C163 110.97(12) . . ?
C22 C221 C222 111.43(12) . . ?
C22 C221 C223 109.94(10) . . ?
C222 C221 C223 111.72(12) . . ?
C26 C261 C262 111.19(11) . . ?
C26 C261 C263 111.15(11) . . ?
C262 C261 C263 110.81(12) . . ?
C1 N1 C3 110.28(9) . . ?
C1 N1 C11 127.63(9) . . ?
C3 N1 C11 121.07(9) . . ?
C2 N2 C1 111.23(9) . . ?
C2 N2 C21 124.72(9) . . ?
C1 N2 C21 123.98(9) . . ?
C5 N3 C4 110.94(9) . . ?
C5 N3 C31 125.95(9) . . ?
C4 N3 C31 122.85(9) . . ?
C4 N4 C6 110.49(9) . . ?
C4 N4 C41 126.75(9) . . ?
C6 N4 C41 122.75(9) . . ?
C1 P1 P2 101.50(4) . . ?
C4 P2 P1 102.54(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C2 C3 N1 -0.22(13) . . . . ?
N3 C5 C6 N4 -0.25(14) . . . . ?
C16 C11 C12 C13 -0.32(16) . . . . ?
N1 C11 C12 C13 -178.79(10) . . . . ?
C16 C11 C12 C121 179.45(10) . . . . ?
N1 C11 C12 C121 0.98(15) . . . . ?
C11 C12 C13 C14 0.39(17) . . . . ?
C121 C12 C13 C14 -179.38(11) . . . . ?
C12 C13 C14 C15 -0.2(2) . . . . ?
C13 C14 C15 C16 0.0(2) . . . . ?
C14 C15 C16 C11 0.06(19) . . . . ?
C14 C15 C16 C161 -175.22(12) . . . . ?
C12 C11 C16 C15 0.10(17) . . . . ?
N1 C11 C16 C15 178.58(10) . . . . ?
C12 C11 C16 C161 175.32(11) . . . . ?
N1 C11 C16 C161 -6.20(16) . . . . ?
C26 C21 C22 C23 -2.30(17) . . . . ?
N2 C21 C22 C23 176.83(10) . . . . ?
C26 C21 C22 C221 178.92(11) . . . . ?
N2 C21 C22 C221 -1.96(16) . . . . ?
C21 C22 C23 C24 0.50(19) . . . . ?
C221 C22 C23 C24 179.29(12) . . . . ?
C22 C23 C24 C25 1.1(2) . . . . ?
C23 C24 C25 C26 -0.9(2) . . . . ?
C24 C25 C26 C21 -0.76(19) . . . . ?
C24 C25 C26 C261 178.89(12) . . . . ?
C22 C21 C26 C25 2.43(17) . . . . ?
N2 C21 C26 C25 -176.69(10) . . . . ?
C22 C21 C26 C261 -177.21(11) . . . . ?
N2 C21 C26 C261 3.67(16) . . . . ?
C36 C31 C32 C33 -1.04(17) . . . . ?
N3 C31 C32 C33 -178.50(10) . . . . ?
C36 C31 C32 C37 177.70(11) . . . . ?
N3 C31 C32 C37 0.24(17) . . . . ?
C31 C32 C33 C34 -0.29(18) . . . . ?
C37 C32 C33 C34 -179.04(12) . . . . ?
C32 C33 C34 C35 0.78(18) . . . . ?
C32 C33 C34 C38 -179.72(12) . . . . ?
C33 C34 C35 C36 0.03(18) . . . . ?
C38 C34 C35 C36 -179.46(12) . . . . ?
C34 C35 C36 C31 -1.28(18) . . . . ?
C34 C35 C36 C39 175.79(11) . . . . ?
C32 C31 C36 C35 1.81(17) . . . . ?
N3 C31 C36 C35 179.29(10) . . . . ?
C32 C31 C36 C39 -175.29(11) . . . . ?
N3 C31 C36 C39 2.18(16) . . . . ?
C46 C41 C42 C43 1.19(16) . . . . ?
N4 C41 C42 C43 -178.24(10) . . . . ?
C46 C41 C42 C47 -175.45(10) . . . . ?
N4 C41 C42 C47 5.12(16) . . . . ?
C41 C42 C43 C44 -0.65(17) . . . . ?
C47 C42 C43 C44 175.99(11) . . . . ?
C42 C43 C44 C45 -0.41(18) . . . . ?
C42 C43 C44 C48 179.12(12) . . . . ?
C43 C44 C45 C46 1.00(18) . . . . ?
C48 C44 C45 C46 -178.53(12) . . . . ?
C42 C41 C46 C45 -0.64(16) . . . . ?
N4 C41 C46 C45 178.79(10) . . . . ?
C42 C41 C46 C49 176.29(11) . . . . ?
N4 C41 C46 C49 -4.27(16) . . . . ?
C44 C45 C46 C41 -0.48(17) . . . . ?
C44 C45 C46 C49 -177.37(11) . . . . ?
C13 C12 C121 C122 -23.88(15) . . . . ?
C11 C12 C121 C122 156.35(10) . . . . ?
C13 C12 C121 C123 99.03(13) . . . . ?
C11 C12 C121 C123 -80.73(13) . . . . ?
C15 C16 C161 C162 82.20(15) . . . . ?
C11 C16 C161 C162 -92.86(14) . . . . ?
C15 C16 C161 C163 -42.06(17) . . . . ?
C11 C16 C161 C163 142.88(13) . . . . ?
C23 C22 C221 C222 53.35(16) . . . . ?
C21 C22 C221 C222 -127.91(12) . . . . ?
C23 C22 C221 C223 -71.07(16) . . . . ?
C21 C22 C221 C223 107.67(14) . . . . ?
C25 C26 C261 C262 -57.05(16) . . . . ?
C21 C26 C261 C262 122.58(13) . . . . ?
C25 C26 C261 C263 66.90(16) . . . . ?
C21 C26 C261 C263 -113.47(14) . . . . ?
N2 C1 N1 C3 -0.68(11) . . . . ?
P1 C1 N1 C3 -177.98(10) . . . . ?
N2 C1 N1 C11 -169.11(10) . . . . ?
P1 C1 N1 C11 13.60(18) . . . . ?
C2 C3 N1 C1 0.59(13) . . . . ?
C2 C3 N1 C11 169.89(10) . . . . ?
C12 C11 N1 C1 -89.25(13) . . . . ?
C16 C11 N1 C1 92.21(13) . . . . ?
C12 C11 N1 C3 103.44(12) . . . . ?
C16 C11 N1 C3 -75.10(13) . . . . ?
C3 C2 N2 C1 -0.22(13) . . . . ?
C3 C2 N2 C21 -177.25(10) . . . . ?
N1 C1 N2 C2 0.55(11) . . . . ?
P1 C1 N2 C2 178.48(8) . . . . ?
N1 C1 N2 C21 177.61(9) . . . . ?
P1 C1 N2 C21 -4.46(14) . . . . ?
C26 C21 N2 C2 85.68(14) . . . . ?
C22 C21 N2 C2 -93.48(13) . . . . ?
C26 C21 N2 C1 -90.98(13) . . . . ?
C22 C21 N2 C1 89.86(13) . . . . ?
C6 C5 N3 C4 -0.46(14) . . . . ?
C6 C5 N3 C31 -174.70(11) . . . . ?
N4 C4 N3 C5 0.97(12) . . . . ?
P2 C4 N3 C5 179.62(8) . . . . ?
N4 C4 N3 C31 175.42(10) . . . . ?
P2 C4 N3 C31 -5.93(14) . . . . ?
C32 C31 N3 C5 -94.45(14) . . . . ?
C36 C31 N3 C5 87.99(14) . . . . ?
C32 C31 N3 C4 91.96(13) . . . . ?
C36 C31 N3 C4 -85.61(14) . . . . ?
N3 C4 N4 C6 -1.12(12) . . . . ?
P2 C4 N4 C6 -179.38(10) . . . . ?
N3 C4 N4 C41 179.21(10) . . . . ?
P2 C4 N4 C41 0.95(19) . . . . ?
C5 C6 N4 C4 0.89(14) . . . . ?
C5 C6 N4 C41 -179.42(10) . . . . ?
C46 C41 N4 C4 98.66(13) . . . . ?
C42 C41 N4 C4 -81.88(14) . . . . ?
C46 C41 N4 C6 -80.97(14) . . . . ?
C42 C41 N4 C6 98.48(13) . . . . ?
N1 C1 P1 P2 -1.83(12) . . . . ?
N2 C1 P1 P2 -178.82(7) . . . . ?
N4 C4 P2 P1 -8.49(13) . . . . ?
N3 C4 P2 P1 173.44(8) . . . . ?

_refine_diff_density_max         0.209
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.045

####################################################################### 
# 
# 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_ad032db2
_database_code_depnum_ccdc_archive 'CCDC 1572773'
_audit_update_record             
;
2017-09-05 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H60 N4 P2, B F4, 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H64 B Cl4 F4 N4 P2'
_chemical_formula_weight         1011.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   18.6443(2)
_cell_length_b                   16.6256(2)
_cell_length_c                   17.2750(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.787(2)
_cell_angle_gamma                90
_cell_volume                     5317.25(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    58045
_cell_measurement_theta_min      3.5550
_cell_measurement_theta_max      75.9700

_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_F_000             2124
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    3.008
_shelx_estimated_absorpt_T_min   0.456
_shelx_estimated_absorpt_T_max   0.585
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 0 0 0.0918
12 0 1 0.1115
0 -7 -8 0.1269
0 7 8 0.1352
-2 -8 8 0.1574
1 8 -7 0.1394
9 0 7 0.1379
10 -3 4 0.1496
3 -8 -7 0.1363
-2 -8 -7 0.1385
11 4 -4 0.1655
11 -4 -5 0.1569
-12 1 -1 0.0770
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.0160 0.0020 0.0269 0.5594 0.8283 0.0075
12.0192 0.0002 0.9736 -0.5146 -0.8709 -0.0727
-0.0300 -7.0135 -7.9839 0.0328 0.0727 0.9646
0.0300 7.0135 7.9839 -0.0328 -0.0727 -0.9646
-1.9828 -7.9761 8.0315 0.8986 -0.5082 -0.0150
0.9847 7.9786 -7.0287 -0.8072 0.5347 -0.0497
9.0341 0.0144 6.9833 -0.1060 -0.9191 -0.4624
10.0239 -2.9906 3.9882 -0.1194 -0.9752 -0.0776
2.9765 -8.0111 -6.9873 -0.0064 -0.2152 0.9607
-2.0302 -8.0102 -6.9761 0.2267 0.1299 0.9638
11.0047 3.9864 -4.0382 -0.9154 -0.4362 0.0013
10.9962 -4.0106 -5.0157 -0.5132 -0.6996 0.5723
-12.0185 0.9991 -0.9764 0.4587 0.9091 0.0095
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            107023
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.573
_diffrn_reflns_theta_max         76.361
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11089
_reflns_number_gt                10125
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
;
 SHELXT-2014/7 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_molecular_graphics    ?
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;


_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as a rigid bodies and allowed to 
 rotate about the E-CH3 bond.

 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 > 2sigma(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.

 One BF4 anion and one dichloromethane molecule were refined with a discrete
 disorder model over two positions. SADI restraints were applied.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0692P)²+2.0070P] 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         11089
_refine_ls_number_parameters     659
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.1091
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_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
C1 C 0.24355(7) 0.61201(8) 0.47457(8) 0.0169(2) Uani 1 1 d . . . . .
C2 C 0.23622(8) 0.74574(8) 0.45125(9) 0.0230(3) Uani 1 1 d . . . . .
H2 H 0.2275 0.7955 0.4247 0.028 Uiso 1 1 calc R U . . .
C3 C 0.26160(8) 0.73562(8) 0.52702(9) 0.0233(3) Uani 1 1 d . . . . .
H3 H 0.2741 0.7772 0.5639 0.028 Uiso 1 1 calc R U . . .
C4 C 0.26640(7) 0.34633(8) 0.52078(7) 0.0167(2) Uani 1 1 d . . . . .
C5 C 0.27228(8) 0.21346(8) 0.54909(8) 0.0210(3) Uani 1 1 d . . . . .
H5 H 0.2820 0.1646 0.5769 0.025 Uiso 1 1 calc R U . . .
C6 C 0.24056(8) 0.22124(8) 0.47526(8) 0.0212(3) Uani 1 1 d . . . . .
H6 H 0.2236 0.1787 0.4412 0.025 Uiso 1 1 calc R U . . .
C11 C 0.19788(7) 0.65241(8) 0.33975(8) 0.0186(3) Uani 1 1 d . . . . .
C12 C 0.24767(8) 0.64172(8) 0.28594(8) 0.0206(3) Uani 1 1 d . . . . .
C13 C 0.21981(9) 0.62433(9) 0.20917(9) 0.0263(3) Uani 1 1 d . . . . .
H13 H 0.2518 0.6165 0.1709 0.032 Uiso 1 1 calc R U . . .
C14 C 0.14579(9) 0.61845(10) 0.18825(9) 0.0306(3) Uani 1 1 d . . . . .
H14 H 0.1277 0.6074 0.1356 0.037 Uiso 1 1 calc R U . . .
C15 C 0.09797(8) 0.62844(10) 0.24305(9) 0.0284(3) Uani 1 1 d . . . . .
H15 H 0.0475 0.6236 0.2277 0.034 Uiso 1 1 calc R U . . .
C16 C 0.12307(8) 0.64547(8) 0.32064(8) 0.0223(3) Uani 1 1 d . . . . .
C21 C 0.28874(7) 0.62021(8) 0.61761(8) 0.0172(2) Uani 1 1 d . . . . .
C22 C 0.36231(8) 0.60302(8) 0.63789(8) 0.0201(3) Uani 1 1 d . . . . .
C23 C 0.38226(8) 0.57130(9) 0.71190(9) 0.0241(3) Uani 1 1 d . . . . .
H23 H 0.4316 0.5596 0.7280 0.029 Uiso 1 1 calc R U . . .
C24 C 0.33134(8) 0.55656(9) 0.76245(8) 0.0251(3) Uani 1 1 d . . . . .
H24 H 0.3460 0.5340 0.8123 0.030 Uiso 1 1 calc R U . . .
C25 C 0.25922(8) 0.57446(9) 0.74081(8) 0.0231(3) Uani 1 1 d . . . . .
H25 H 0.2249 0.5639 0.7761 0.028 Uiso 1 1 calc R U . . .
C26 C 0.23624(7) 0.60778(8) 0.66801(8) 0.0192(3) Uani 1 1 d . . . . .
C31 C 0.32134(8) 0.31097(8) 0.65339(8) 0.0192(3) Uani 1 1 d . . . . .
C32 C 0.39633(8) 0.31686(9) 0.66569(8) 0.0236(3) Uani 1 1 d . . . . .
C33 C 0.42745(9) 0.33736(9) 0.74042(9) 0.0291(3) Uani 1 1 d . . . . .
H33 H 0.4786 0.3404 0.7510 0.035 Uiso 1 1 calc R U . . .
C34 C 0.38530(10) 0.35349(9) 0.79996(9) 0.0310(3) Uani 1 1 d . . . . .
C35 C 0.31060(10) 0.34881(9) 0.78426(9) 0.0290(3) Uani 1 1 d . . . . .
H35 H 0.2818 0.3608 0.8246 0.035 Uiso 1 1 calc R U . . .
C36 C 0.27675(8) 0.32697(8) 0.71110(8) 0.0231(3) Uani 1 1 d . . . . .
C37 C 0.44178(9) 0.30361(10) 0.60016(10) 0.0307(3) Uani 1 1 d . . . . .
H37A H 0.4927 0.3133 0.6191 0.046 Uiso 1 1 calc R U . . .
H37B H 0.4264 0.3408 0.5574 0.046 Uiso 1 1 calc R U . . .
H37C H 0.4357 0.2481 0.5814 0.046 Uiso 1 1 calc R U . . .
C38 C 0.42033(14) 0.37555(11) 0.88033(10) 0.0469(5) Uani 1 1 d . . . . .
H38A H 0.4727 0.3800 0.8798 0.070 Uiso 1 1 calc R U . . .
H38B H 0.4100 0.3338 0.9175 0.070 Uiso 1 1 calc R U . . .
H38C H 0.4011 0.4272 0.8959 0.070 Uiso 1 1 calc R U . . .
C39 C 0.19581(9) 0.32342(10) 0.69428(10) 0.0307(3) Uani 1 1 d . . . . .
H39A H 0.1748 0.3156 0.7431 0.046 Uiso 1 1 calc R U . . .
H39B H 0.1820 0.2785 0.6589 0.046 Uiso 1 1 calc R U . . .
H39C H 0.1779 0.3739 0.6698 0.046 Uiso 1 1 calc R U . . .
C41 C 0.20756(7) 0.33365(8) 0.38311(8) 0.0180(3) Uani 1 1 d . . . . .
C42 C 0.25450(8) 0.35334(8) 0.32881(8) 0.0205(3) Uani 1 1 d . . . . .
C43 C 0.22355(9) 0.38129(9) 0.25637(8) 0.0274(3) Uani 1 1 d . . . . .
H43 H 0.2541 0.3958 0.2184 0.033 Uiso 1 1 calc R U . . .
C44 C 0.14925(10) 0.38842(9) 0.23822(9) 0.0316(3) Uani 1 1 d . . . . .
C45 C 0.10460(9) 0.36917(10) 0.29469(10) 0.0314(3) Uani 1 1 d . . . . .
H45 H 0.0538 0.3749 0.2828 0.038 Uiso 1 1 calc R U . . .
C46 C 0.13258(8) 0.34176(9) 0.36813(9) 0.0242(3) Uani 1 1 d . . . . .
C47 C 0.33495(8) 0.34716(9) 0.34864(9) 0.0260(3) Uani 1 1 d . . . . .
H47A H 0.3530 0.3953 0.3774 0.039 Uiso 1 1 calc R U . . .
H47B H 0.3578 0.3427 0.3005 0.039 Uiso 1 1 calc R U . . .
H47C H 0.3466 0.2994 0.3810 0.039 Uiso 1 1 calc R U . . .
C48 C 0.11704(14) 0.41391(12) 0.15758(11) 0.0496(5) Uani 1 1 d . . . . .
H48A H 0.1527 0.4451 0.1329 0.074 Uiso 1 1 calc R U . . .
H48B H 0.0742 0.4471 0.1615 0.074 Uiso 1 1 calc R U . . .
H48C H 0.1034 0.3661 0.1261 0.074 Uiso 1 1 calc R U . . .
C49 C 0.08461(9) 0.32451(12) 0.43044(11) 0.0367(4) Uani 1 1 d . . . . .
H49A H 0.0339 0.3292 0.4083 0.055 Uiso 1 1 calc R U . . .
H49B H 0.0948 0.3632 0.4731 0.055 Uiso 1 1 calc R U . . .
H49C H 0.0939 0.2699 0.4504 0.055 Uiso 1 1 calc R U . . .
C99 C 0.44259(9) 0.05811(11) 0.58390(10) 0.0346(4) Uani 1 1 d . . . . .
H99A H 0.4425 -0.0014 0.5866 0.042 Uiso 1 1 calc R U . . .
H99B H 0.4052 0.0748 0.5414 0.042 Uiso 1 1 calc R U . . .
C121 C 0.32858(8) 0.64945(9) 0.30858(9) 0.0235(3) Uani 1 1 d . . . . .
H121 H 0.3378 0.6527 0.3667 0.028 Uiso 1 1 calc R U . . .
C122 C 0.36831(11) 0.57606(12) 0.28226(17) 0.0558(6) Uani 1 1 d . . . . .
H12D H 0.3655 0.5758 0.2252 0.084 Uiso 1 1 calc R U . . .
H12E H 0.3459 0.5270 0.2998 0.084 Uiso 1 1 calc R U . . .
H12F H 0.4191 0.5782 0.3048 0.084 Uiso 1 1 calc R U . . .
C123 C 0.35655(10) 0.72545(13) 0.27529(17) 0.0591(7) Uani 1 1 d . . . . .
H12A H 0.3502 0.7223 0.2182 0.089 Uiso 1 1 calc R U . . .
H12B H 0.4080 0.7317 0.2939 0.089 Uiso 1 1 calc R U . . .
H12C H 0.3297 0.7717 0.2920 0.089 Uiso 1 1 calc R U . . .
C161 C 0.07053(8) 0.65610(10) 0.38081(9) 0.0274(3) Uani 1 1 d . . . . .
H161 H 0.0995 0.6613 0.4331 0.033 Uiso 1 1 calc R U . . .
C162 C 0.02210(11) 0.58231(13) 0.38317(12) 0.0429(4) Uani 1 1 d . . . . .
H16A H -0.0090 0.5775 0.3335 0.064 Uiso 1 1 calc R U . . .
H16B H -0.0079 0.5881 0.4257 0.064 Uiso 1 1 calc R U . . .
H16C H 0.0521 0.5340 0.3918 0.064 Uiso 1 1 calc R U . . .
C163 C 0.02558(13) 0.73269(14) 0.36618(15) 0.0552(6) Uani 1 1 d . . . . .
H16D H 0.0578 0.7794 0.3680 0.083 Uiso 1 1 calc R U . . .
H16E H -0.0070 0.7381 0.4064 0.083 Uiso 1 1 calc R U . . .
H16F H -0.0028 0.7296 0.3148 0.083 Uiso 1 1 calc R U . . .
C221 C 0.41819(8) 0.61844(10) 0.58209(9) 0.0269(3) Uani 1 1 d . . . . .
H221 H 0.3930 0.6159 0.5277 0.032 Uiso 1 1 calc R U . . .
C222 C 0.47812(9) 0.55493(11) 0.58970(12) 0.0383(4) Uani 1 1 d . . . . .
H22A H 0.5075 0.5608 0.6403 0.057 Uiso 1 1 calc R U . . .
H22B H 0.5087 0.5623 0.5478 0.057 Uiso 1 1 calc R U . . .
H22C H 0.4565 0.5011 0.5858 0.057 Uiso 1 1 calc R U . . .
C223 C 0.45123(10) 0.70265(11) 0.59467(12) 0.0395(4) Uani 1 1 d . . . . .
H22D H 0.4131 0.7432 0.5854 0.059 Uiso 1 1 calc R U . . .
H22E H 0.4871 0.7111 0.5583 0.059 Uiso 1 1 calc R U . . .
H22F H 0.4746 0.7074 0.6483 0.059 Uiso 1 1 calc R U . . .
C261 C 0.15718(8) 0.62876(9) 0.64550(9) 0.0238(3) Uani 1 1 d . . . . .
H261 H 0.1542 0.6693 0.6025 0.029 Uiso 1 1 calc R U . . .
C262 C 0.11385(9) 0.55508(11) 0.61587(12) 0.0383(4) Uani 1 1 d . . . . .
H26D H 0.1342 0.5327 0.5707 0.057 Uiso 1 1 calc R U . . .
H26E H 0.0634 0.5705 0.6006 0.057 Uiso 1 1 calc R U . . .
H26F H 0.1161 0.5145 0.6573 0.057 Uiso 1 1 calc R U . . .
C263 C 0.12364(9) 0.66571(12) 0.71397(12) 0.0388(4) Uani 1 1 d . . . . .
H26A H 0.1192 0.6243 0.7535 0.058 Uiso 1 1 calc R U . . .
H26B H 0.0757 0.6871 0.6954 0.058 Uiso 1 1 calc R U . . .
H26C H 0.1546 0.7093 0.7368 0.058 Uiso 1 1 calc R U . . .
N1 N 0.22535(6) 0.66959(7) 0.41967(7) 0.0182(2) Uani 1 1 d . . . . .
N2 N 0.26617(6) 0.65336(7) 0.54128(7) 0.0183(2) Uani 1 1 d . . . . .
N3 N 0.28790(6) 0.29041(7) 0.57652(6) 0.0181(2) Uani 1 1 d . . . . .
N4 N 0.23714(6) 0.30290(7) 0.45797(6) 0.0172(2) Uani 1 1 d . . . . .
B1 B 0.2683(4) -0.0286(6) 0.5045(5) 0.034(3) Uani 0.525(4) 1 d D . P A 1
F1 F 0.29890(16) 0.0162(2) 0.45031(15) 0.0682(11) Uani 0.525(4) 1 d D . P A 1
F2 F 0.2433(2) 0.0249(2) 0.5563(2) 0.0716(10) Uani 0.525(4) 1 d D . P A 1
F3 F 0.21158(18) -0.07310(18) 0.4680(4) 0.096(2) Uani 0.525(4) 1 d D . P A 1
F4 F 0.3191(4) -0.0804(4) 0.5432(5) 0.0555(18) Uani 0.525(4) 1 d D . P A 1
B1' B 0.2693(5) -0.0426(6) 0.5069(5) 0.027(2) Uani 0.475(4) 1 d D . P A 2
F1' F 0.26702(17) 0.03901(14) 0.5184(2) 0.0582(11) Uani 0.475(4) 1 d D . P A 2
F2' F 0.28425(19) -0.0598(2) 0.43274(15) 0.0654(11) Uani 0.475(4) 1 d D . P A 2
F3' F 0.20438(16) -0.07628(18) 0.51757(17) 0.0397(7) Uani 0.475(4) 1 d D . P A
2
F4' F 0.3230(3) -0.0764(4) 0.5594(4) 0.0387(13) Uani 0.475(4) 1 d D . P A 2
P1 P 0.23140(2) 0.50818(2) 0.44531(2) 0.02206(9) Uani 1 1 d . . . . .
P2 P 0.28271(2) 0.45028(2) 0.54547(2) 0.02326(9) Uani 1 1 d . . . . .
Cl98 Cl 0.52795(2) 0.09148(2) 0.56261(2) 0.03063(10) Uani 1 1 d . . . . .
Cl99 Cl 0.42112(2) 0.09785(3) 0.67329(2) 0.03604(10) Uani 1 1 d . . . . .
C98 C 0.0860(3) 0.0410(4) 0.4359(2) 0.0542(18) Uani 0.905(4) 1 d D . P B 3
H98A H 0.0690 -0.0155 0.4336 0.065 Uiso 0.905(4) 1 calc R U P B 3
H98B H 0.1279 0.0447 0.4766 0.065 Uiso 0.905(4) 1 calc R U P B 3
Cl96 Cl 0.01666(4) 0.10382(4) 0.46052(3) 0.03808(19) Uani 0.905(4) 1 d D . P B
3
Cl97 Cl 0.11320(4) 0.06827(7) 0.34476(3) 0.0556(3) Uani 0.905(4) 1 d D . P B 3
C98' C 0.0943(17) 0.0449(19) 0.4376(10) 0.013(6) Uiso 0.095(4) 1 d D . P B 4
H98C H 0.0896 -0.0077 0.4635 0.016 Uiso 0.095(4) 1 calc R U P B 4
H98D H 0.1407 0.0695 0.4593 0.016 Uiso 0.095(4) 1 calc R U P B 4
Cl95 Cl 0.0928(5) 0.0307(6) 0.3352(4) 0.056(2) Uiso 0.095(4) 1 d D . P B 4
Cl94 Cl 0.0217(12) 0.1085(15) 0.4553(12) 0.158(10) Uiso 0.095(4) 1 d D . P B 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3620(17) . ?
C1 N2 1.3652(17) . ?
C1 P1 1.8054(13) . ?
C2 C3 1.349(2) . ?
C2 N1 1.3840(18) . ?
C3 N2 1.3905(17) . ?
C4 N4 1.3626(17) . ?
C4 N3 1.3642(17) . ?
C4 P2 1.7973(13) . ?
C5 C6 1.347(2) . ?
C5 N3 1.3833(18) . ?
C6 N4 1.3899(17) . ?
C11 C16 1.3995(19) . ?
C11 C12 1.4004(19) . ?
C11 N1 1.4431(17) . ?
C12 C13 1.396(2) . ?
C12 C121 1.5185(19) . ?
C13 C14 1.388(2) . ?
C14 C15 1.385(2) . ?
C15 C16 1.396(2) . ?
C16 C161 1.521(2) . ?
C21 C26 1.4001(19) . ?
C21 C22 1.4045(19) . ?
C21 N2 1.4451(17) . ?
C22 C23 1.392(2) . ?
C22 C221 1.522(2) . ?
C23 C24 1.386(2) . ?
C24 C25 1.385(2) . ?
C25 C26 1.394(2) . ?
C26 C261 1.5200(19) . ?
C31 C32 1.393(2) . ?
C31 C36 1.397(2) . ?
C31 N3 1.4399(17) . ?
C32 C33 1.394(2) . ?
C32 C37 1.508(2) . ?
C33 C34 1.392(2) . ?
C34 C35 1.389(3) . ?
C34 C38 1.508(2) . ?
C35 C36 1.392(2) . ?
C36 C39 1.504(2) . ?
C41 C42 1.3954(19) . ?
C41 C46 1.398(2) . ?
C41 N4 1.4386(17) . ?
C42 C43 1.394(2) . ?
C42 C47 1.502(2) . ?
C43 C44 1.389(3) . ?
C44 C45 1.393(3) . ?
C44 C48 1.511(2) . ?
C45 C46 1.390(2) . ?
C46 C49 1.506(2) . ?
C99 Cl98 1.7647(18) . ?
C99 Cl99 1.7684(17) . ?
C121 C123 1.507(2) . ?
C121 C122 1.524(2) . ?
C161 C162 1.527(2) . ?
C161 C163 1.529(2) . ?
C221 C222 1.532(2) . ?
C221 C223 1.535(2) . ?
C261 C262 1.522(2) . ?
C261 C263 1.530(2) . ?
B1 F1 1.373(9) . ?
B1 F3 1.381(9) . ?
B1 F2 1.381(9) . ?
B1 F4 1.392(9) . ?
B1' F3' 1.366(10) . ?
B1' F1' 1.373(10) . ?
B1' F2' 1.374(8) . ?
B1' F4' 1.386(10) . ?
P1 P2 2.1083(5) . ?
C98 Cl96 1.754(4) . ?
C98 Cl97 1.769(4) . ?
C98' Cl94 1.773(15) . ?
C98' Cl95 1.783(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 105.10(11) . . ?
N1 C1 P1 117.67(10) . . ?
N2 C1 P1 137.22(10) . . ?
C3 C2 N1 106.67(12) . . ?
C2 C3 N2 107.56(12) . . ?
N4 C4 N3 104.92(11) . . ?
N4 C4 P2 137.66(10) . . ?
N3 C4 P2 117.42(10) . . ?
C6 C5 N3 106.65(12) . . ?
C5 C6 N4 107.53(12) . . ?
C16 C11 C12 123.58(13) . . ?
C16 C11 N1 118.24(12) . . ?
C12 C11 N1 118.16(12) . . ?
C13 C12 C11 117.09(13) . . ?
C13 C12 C121 120.59(13) . . ?
C11 C12 C121 122.31(13) . . ?
C14 C13 C12 120.57(14) . . ?
C15 C14 C13 120.94(14) . . ?
C14 C15 C16 120.72(14) . . ?
C15 C16 C11 117.07(13) . . ?
C15 C16 C161 120.67(13) . . ?
C11 C16 C161 122.26(13) . . ?
C26 C21 C22 123.28(13) . . ?
C26 C21 N2 118.31(12) . . ?
C22 C21 N2 118.41(12) . . ?
C23 C22 C21 116.95(13) . . ?
C23 C22 C221 121.11(13) . . ?
C21 C22 C221 121.94(13) . . ?
C24 C23 C22 121.14(13) . . ?
C25 C24 C23 120.51(14) . . ?
C24 C25 C26 120.91(14) . . ?
C25 C26 C21 117.18(13) . . ?
C25 C26 C261 120.47(13) . . ?
C21 C26 C261 122.35(12) . . ?
C32 C31 C36 123.31(13) . . ?
C32 C31 N3 118.34(12) . . ?
C36 C31 N3 118.30(13) . . ?
C31 C32 C33 117.32(14) . . ?
C31 C32 C37 121.21(13) . . ?
C33 C32 C37 121.45(14) . . ?
C34 C33 C32 121.46(15) . . ?
C35 C34 C33 119.03(14) . . ?
C35 C34 C38 120.55(17) . . ?
C33 C34 C38 120.42(17) . . ?
C34 C35 C36 121.88(15) . . ?
C35 C36 C31 116.95(14) . . ?
C35 C36 C39 121.49(14) . . ?
C31 C36 C39 121.53(13) . . ?
C42 C41 C46 123.09(13) . . ?
C42 C41 N4 118.90(12) . . ?
C46 C41 N4 118.00(12) . . ?
C43 C42 C41 117.09(14) . . ?
C43 C42 C47 121.58(13) . . ?
C41 C42 C47 121.30(12) . . ?
C44 C43 C42 121.81(14) . . ?
C43 C44 C45 119.02(14) . . ?
C43 C44 C48 120.62(17) . . ?
C45 C44 C48 120.33(18) . . ?
C46 C45 C44 121.57(15) . . ?
C45 C46 C41 117.38(14) . . ?
C45 C46 C49 121.60(14) . . ?
C41 C46 C49 120.98(13) . . ?
Cl98 C99 Cl99 111.55(10) . . ?
C123 C121 C12 110.53(12) . . ?
C123 C121 C122 110.80(17) . . ?
C12 C121 C122 111.00(14) . . ?
C16 C161 C162 110.84(14) . . ?
C16 C161 C163 111.63(13) . . ?
C162 C161 C163 111.06(16) . . ?
C22 C221 C222 112.12(14) . . ?
C22 C221 C223 110.93(12) . . ?
C222 C221 C223 109.89(14) . . ?
C26 C261 C262 111.18(12) . . ?
C26 C261 C263 111.52(13) . . ?
C262 C261 C263 109.51(13) . . ?
C1 N1 C2 110.83(11) . . ?
C1 N1 C11 123.92(11) . . ?
C2 N1 C11 125.25(11) . . ?
C1 N2 C3 109.84(11) . . ?
C1 N2 C21 127.28(11) . . ?
C3 N2 C21 122.82(11) . . ?
C4 N3 C5 110.86(11) . . ?
C4 N3 C31 123.24(11) . . ?
C5 N3 C31 125.89(11) . . ?
C4 N4 C6 110.03(11) . . ?
C4 N4 C41 127.04(11) . . ?
C6 N4 C41 122.91(11) . . ?
F1 B1 F3 109.7(7) . . ?
F1 B1 F2 107.0(7) . . ?
F3 B1 F2 110.0(6) . . ?
F1 B1 F4 110.5(6) . . ?
F3 B1 F4 109.2(7) . . ?
F2 B1 F4 110.5(7) . . ?
F3' B1' F1' 110.0(7) . . ?
F3' B1' F2' 108.7(7) . . ?
F1' B1' F2' 110.6(7) . . ?
F3' B1' F4' 109.2(7) . . ?
F1' B1' F4' 109.9(7) . . ?
F2' B1' F4' 108.4(7) . . ?
C1 P1 P2 100.19(4) . . ?
C4 P2 P1 101.34(4) . . ?
Cl96 C98 Cl97 111.1(3) . . ?
Cl94 C98' Cl95 109.1(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.06(16) . . . . ?
N3 C5 C6 N4 0.14(16) . . . . ?
C16 C11 C12 C13 0.9(2) . . . . ?
N1 C11 C12 C13 179.35(12) . . . . ?
C16 C11 C12 C121 -179.83(13) . . . . ?
N1 C11 C12 C121 -1.39(19) . . . . ?
C11 C12 C13 C14 0.2(2) . . . . ?
C121 C12 C13 C14 -179.04(14) . . . . ?
C12 C13 C14 C15 -1.0(2) . . . . ?
C13 C14 C15 C16 0.6(3) . . . . ?
C14 C15 C16 C11 0.5(2) . . . . ?
C14 C15 C16 C161 -179.76(15) . . . . ?
C12 C11 C16 C15 -1.2(2) . . . . ?
N1 C11 C16 C15 -179.69(12) . . . . ?
C12 C11 C16 C161 178.97(13) . . . . ?
N1 C11 C16 C161 0.5(2) . . . . ?
C26 C21 C22 C23 0.7(2) . . . . ?
N2 C21 C22 C23 179.87(12) . . . . ?
C26 C21 C22 C221 -179.06(13) . . . . ?
N2 C21 C22 C221 0.10(19) . . . . ?
C21 C22 C23 C24 0.8(2) . . . . ?
C221 C22 C23 C24 -179.41(13) . . . . ?
C22 C23 C24 C25 -1.1(2) . . . . ?
C23 C24 C25 C26 -0.2(2) . . . . ?
C24 C25 C26 C21 1.6(2) . . . . ?
C24 C25 C26 C261 -178.75(13) . . . . ?
C22 C21 C26 C25 -1.9(2) . . . . ?
N2 C21 C26 C25 178.95(12) . . . . ?
C22 C21 C26 C261 178.46(12) . . . . ?
N2 C21 C26 C261 -0.71(19) . . . . ?
C36 C31 C32 C33 2.1(2) . . . . ?
N3 C31 C32 C33 179.58(12) . . . . ?
C36 C31 C32 C37 -176.41(13) . . . . ?
N3 C31 C32 C37 1.1(2) . . . . ?
C31 C32 C33 C34 -1.7(2) . . . . ?
C37 C32 C33 C34 176.77(14) . . . . ?
C32 C33 C34 C35 0.1(2) . . . . ?
C32 C33 C34 C38 180.00(14) . . . . ?
C33 C34 C35 C36 1.2(2) . . . . ?
C38 C34 C35 C36 -178.64(14) . . . . ?
C34 C35 C36 C31 -0.9(2) . . . . ?
C34 C35 C36 C39 -178.95(14) . . . . ?
C32 C31 C36 C35 -0.8(2) . . . . ?
N3 C31 C36 C35 -178.31(12) . . . . ?
C32 C31 C36 C39 177.24(13) . . . . ?
N3 C31 C36 C39 -0.25(19) . . . . ?
C46 C41 C42 C43 -0.8(2) . . . . ?
N4 C41 C42 C43 178.64(12) . . . . ?
C46 C41 C42 C47 177.24(13) . . . . ?
N4 C41 C42 C47 -3.28(19) . . . . ?
C41 C42 C43 C44 -0.8(2) . . . . ?
C47 C42 C43 C44 -178.88(14) . . . . ?
C42 C43 C44 C45 1.8(2) . . . . ?
C42 C43 C44 C48 -176.15(15) . . . . ?
C43 C44 C45 C46 -1.1(2) . . . . ?
C48 C44 C45 C46 176.80(16) . . . . ?
C44 C45 C46 C41 -0.4(2) . . . . ?
C44 C45 C46 C49 177.18(15) . . . . ?
C42 C41 C46 C45 1.4(2) . . . . ?
N4 C41 C46 C45 -178.04(13) . . . . ?
C42 C41 C46 C49 -176.19(14) . . . . ?
N4 C41 C46 C49 4.3(2) . . . . ?
C13 C12 C121 C123 71.1(2) . . . . ?
C11 C12 C121 C123 -108.11(19) . . . . ?
C13 C12 C121 C122 -52.2(2) . . . . ?
C11 C12 C121 C122 128.53(17) . . . . ?
C15 C16 C161 C162 55.9(2) . . . . ?
C11 C16 C161 C162 -124.37(16) . . . . ?
C15 C16 C161 C163 -68.5(2) . . . . ?
C11 C16 C161 C163 111.26(19) . . . . ?
C23 C22 C221 C222 35.29(19) . . . . ?
C21 C22 C221 C222 -144.95(14) . . . . ?
C23 C22 C221 C223 -87.98(18) . . . . ?
C21 C22 C221 C223 91.78(17) . . . . ?
C25 C26 C261 C262 -82.47(17) . . . . ?
C21 C26 C261 C262 97.18(17) . . . . ?
C25 C26 C261 C263 40.07(19) . . . . ?
C21 C26 C261 C263 -140.29(14) . . . . ?
N2 C1 N1 C2 -0.08(15) . . . . ?
P1 C1 N1 C2 178.72(10) . . . . ?
N2 C1 N1 C11 -179.54(12) . . . . ?
P1 C1 N1 C11 -0.75(17) . . . . ?
C3 C2 N1 C1 0.01(16) . . . . ?
C3 C2 N1 C11 179.47(13) . . . . ?
C16 C11 N1 C1 90.13(16) . . . . ?
C12 C11 N1 C1 -88.40(16) . . . . ?
C16 C11 N1 C2 -89.26(17) . . . . ?
C12 C11 N1 C2 92.21(17) . . . . ?
N1 C1 N2 C3 0.11(15) . . . . ?
P1 C1 N2 C3 -178.32(12) . . . . ?
N1 C1 N2 C21 177.34(12) . . . . ?
P1 C1 N2 C21 -1.1(2) . . . . ?
C2 C3 N2 C1 -0.11(17) . . . . ?
C2 C3 N2 C21 -177.48(12) . . . . ?
C26 C21 N2 C1 -89.55(17) . . . . ?
C22 C21 N2 C1 91.24(16) . . . . ?
C26 C21 N2 C3 87.34(16) . . . . ?
C22 C21 N2 C3 -91.87(16) . . . . ?
N4 C4 N3 C5 -0.08(15) . . . . ?
P2 C4 N3 C5 -179.63(9) . . . . ?
N4 C4 N3 C31 -179.30(12) . . . . ?
P2 C4 N3 C31 1.16(17) . . . . ?
C6 C5 N3 C4 -0.03(16) . . . . ?
C6 C5 N3 C31 179.15(13) . . . . ?
C32 C31 N3 C4 -90.43(16) . . . . ?
C36 C31 N3 C4 87.19(16) . . . . ?
C32 C31 N3 C5 90.47(17) . . . . ?
C36 C31 N3 C5 -91.90(17) . . . . ?
N3 C4 N4 C6 0.17(15) . . . . ?
P2 C4 N4 C6 179.57(12) . . . . ?
N3 C4 N4 C41 -178.77(12) . . . . ?
P2 C4 N4 C41 0.6(2) . . . . ?
C5 C6 N4 C4 -0.19(16) . . . . ?
C5 C6 N4 C41 178.80(12) . . . . ?
C42 C41 N4 C4 81.43(17) . . . . ?
C46 C41 N4 C4 -99.06(16) . . . . ?
C42 C41 N4 C6 -97.39(16) . . . . ?
C46 C41 N4 C6 82.12(17) . . . . ?
N1 C1 P1 P2 171.38(10) . . . . ?
N2 C1 P1 P2 -10.33(15) . . . . ?
N4 C4 P2 P1 5.72(15) . . . . ?
N3 C4 P2 P1 -174.93(9) . . . . ?

_refine_diff_density_max         0.590
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.062

####################################################################### 
# 
# 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_ad2ck
_database_code_depnum_ccdc_archive 'CCDC 1572775'
_audit_update_record             
;
2017-09-05 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H60 N4 P2 2+, 2(C32 H12 B F24 1-)'
_chemical_formula_sum            'C112 H84 B2 F48 N4 P2'
_chemical_formula_weight         2481.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.1731(7)
_cell_length_b                   19.4127(10)
_cell_length_c                   20.26550(10)
_cell_angle_alpha                80.996(4)
_cell_angle_beta                 76.569(4)
_cell_angle_gamma                69.481(4)
_cell_volume                     5776.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    43942
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      75.80

_exptl_crystal_description       'fragment of plate'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_recrystallization_method 
;
 ADF-631 from a solution in DCM/n-hexane.
;


_exptl_special_details           
;
 The crystal was mounted on top of a human hair with perfluorether oil
 and placed in a cold nitrogen gas stream on the diffractometer.

 The collected data cover more than a hemisphere of the reciprocal space.
 A combination of 106 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 1.5 deg in ω.
 Each frame was exposed for 5 s (low 2θ angles) or 15 s (high 2θ angles).
 Nominal crystal to detector distance 53 mm.
;



_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            274849
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.367
_diffrn_reflns_theta_max         65.996
_diffrn_reflns_theta_full        65.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             20102
_reflns_number_gt                16591
_reflns_threshold_expression     'I > 2σ(I)'


_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
;


_computing_data_collection       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_molecular_graphics    
;
 K. Brandenburg, 1999, Diamond 3.2i, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;




_refine_special_details          
;No appropriate model could be established for co-crystallised solvent 
 molecules, presumably DCM; the data were processed using the 
 SQUEEZE/PLATON program (A. L. Spek, J. Appl. Crystallogr. 2003, 36, 7-13.).
 
 A P2 moiety is disordered over two sites. It was refined applying a
 split atom model. The SOF refined to 0.866(2),
 a common ADP was refined for each disordered atom pair.

 Six disordered CF3 groups were refined using a split atom models (0.64(1),
 0.596(9), 0.70(1), 0.81(2), 0.73(2), 0.887(8) SOF
 of main components). Similarity restraints were applied (SAME); the ADPs
 were restrained to approximate isotropic behaviour (ISOR).


 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as rigid bodies and allowed to rotate about
 the E-CH3 bond but not to tip.


 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 > 2sigma(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.,SQUEEZE
;





_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1102P)²+4.6446P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         20102
_refine_ls_number_parameters     1697
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1997
_refine_ls_wR_factor_gt          0.1888
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.007
_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
C1 C 0.2900(2) 0.62533(17) 0.23132(18) 0.0445(7) Uani 1 1 d . . . . .
C2 C 0.2788(3) 0.5219(2) 0.2903(2) 0.0608(10) Uani 1 1 d . . . . .
H2 H 0.2551 0.4880 0.3209 0.073 Uiso 1 1 calc R U . . .
C3 C 0.3630(2) 0.50697(19) 0.2540(2) 0.0586(10) Uani 1 1 d . . . . .
H3 H 0.4095 0.4605 0.2537 0.070 Uiso 1 1 calc R U . . .
C4 C 0.4501(2) 0.57901(17) 0.17151(18) 0.0437(7) Uani 1 1 d . . . . .
C5 C 0.4581(2) 0.57406(19) 0.10264(19) 0.0508(8) Uani 1 1 d . . . . .
C6 C 0.5361(3) 0.5824(2) 0.05984(19) 0.0564(9) Uani 1 1 d . . . . .
H6 H 0.5430 0.5810 0.0122 0.068 Uiso 1 1 calc R U . . .
C7 C 0.6034(2) 0.5926(2) 0.0846(2) 0.0532(8) Uani 1 1 d . . . . .
C8 C 0.5926(2) 0.5948(2) 0.1538(2) 0.0534(8) Uani 1 1 d . . . . .
H8 H 0.6393 0.6006 0.1710 0.064 Uiso 1 1 calc R U . . .
C9 C 0.5166(2) 0.58872(18) 0.19913(18) 0.0466(7) Uani 1 1 d . . . . .
C10 C 0.3867(3) 0.5610(3) 0.0754(2) 0.0701(12) Uani 1 1 d . . . . .
H10A H 0.3744 0.5168 0.0996 0.105 Uiso 1 1 calc R U . . .
H10B H 0.4074 0.5540 0.0267 0.105 Uiso 1 1 calc R U . . .
H10C H 0.3315 0.6037 0.0820 0.105 Uiso 1 1 calc R U . . .
C11 C 0.6854(3) 0.6030(3) 0.0362(2) 0.0720(12) Uani 1 1 d . . . . .
H11A H 0.6950 0.5797 -0.0057 0.108 Uiso 1 1 calc R U . . .
H11B H 0.7383 0.5803 0.0576 0.108 Uiso 1 1 calc R U . . .
H11C H 0.6762 0.6559 0.0253 0.108 Uiso 1 1 calc R U . . .
C12 C 0.5056(3) 0.5941(3) 0.2745(2) 0.0627(10) Uani 1 1 d . . . . .
H12A H 0.5641 0.5876 0.2852 0.094 Uiso 1 1 calc R U . . .
H12B H 0.4824 0.5554 0.3002 0.094 Uiso 1 1 calc R U . . .
H12C H 0.4633 0.6426 0.2868 0.094 Uiso 1 1 calc R U . . .
C13 C 0.1410(2) 0.63090(18) 0.30665(18) 0.0458(7) Uani 1 1 d . . . . .
C14 C 0.1254(3) 0.6589(2) 0.36864(19) 0.0564(9) Uani 1 1 d . . . . .
C15 C 0.0360(3) 0.6912(2) 0.3995(2) 0.0608(10) Uani 1 1 d . . . . .
H15 H 0.0231 0.7107 0.4423 0.073 Uiso 1 1 calc R U . . .
C16 C -0.0343(3) 0.6956(2) 0.36963(19) 0.0553(9) Uani 1 1 d . . . . .
C17 C -0.0145(3) 0.6671(2) 0.3068(2) 0.0544(8) Uani 1 1 d . . . . .
H17 H -0.0626 0.6704 0.2857 0.065 Uiso 1 1 calc R U . . .
C18 C 0.0738(2) 0.63361(19) 0.27375(17) 0.0465(7) Uani 1 1 d . . . . .
C19 C 0.2015(4) 0.6552(3) 0.4014(3) 0.0814(14) Uani 1 1 d . . . . .
H19A H 0.2427 0.6043 0.4036 0.122 Uiso 1 1 calc R U . . .
H19B H 0.1774 0.6713 0.4475 0.122 Uiso 1 1 calc R U . . .
H19C H 0.2340 0.6875 0.3744 0.122 Uiso 1 1 calc R U . . .
C20 C -0.1300(3) 0.7282(3) 0.4050(2) 0.0745(12) Uani 1 1 d . . . . .
H20A H -0.1520 0.6886 0.4301 0.112 Uiso 1 1 calc R U . . .
H20B H -0.1673 0.7545 0.3712 0.112 Uiso 1 1 calc R U . . .
H20C H -0.1333 0.7627 0.4368 0.112 Uiso 1 1 calc R U . . .
C21 C 0.0935(3) 0.6006(2) 0.2069(2) 0.0632(10) Uani 1 1 d . . . . .
H21A H 0.1196 0.6308 0.1704 0.095 Uiso 1 1 calc R U . . .
H21B H 0.0376 0.5992 0.1971 0.095 Uiso 1 1 calc R U . . .
H21C H 0.1362 0.5503 0.2097 0.095 Uiso 1 1 calc R U . . .
C22 C 0.15758(19) 0.87131(15) 0.20284(15) 0.0346(6) Uani 1 1 d . . . . .
C23 C 0.1777(2) 0.97831(16) 0.16012(17) 0.0404(7) Uani 1 1 d . . . . .
H23 H 0.2057 1.0136 0.1379 0.048 Uiso 1 1 calc R U . . .
C24 C 0.0899(2) 0.99230(17) 0.18906(17) 0.0418(7) Uani 1 1 d . . . . .
H24 H 0.0445 1.0393 0.1909 0.050 Uiso 1 1 calc R U . . .
C25 C 0.31382(19) 0.86479(15) 0.14673(17) 0.0376(6) Uani 1 1 d . . . . .
C26 C 0.3684(2) 0.84627(17) 0.19509(18) 0.0441(7) Uani 1 1 d . . . . .
C27 C 0.4588(2) 0.8047(2) 0.1728(2) 0.0545(9) Uani 1 1 d . . . . .
H27 H 0.4993 0.7896 0.2036 0.065 Uiso 1 1 calc R U . . .
C28 C 0.4892(2) 0.7856(2) 0.1064(2) 0.0549(9) Uani 1 1 d . . . . .
H28 H 0.5505 0.7572 0.0926 0.066 Uiso 1 1 calc R U . . .
C29 C 0.4343(2) 0.8063(2) 0.0603(2) 0.0519(8) Uani 1 1 d . . . . .
H29 H 0.4578 0.7924 0.0150 0.062 Uiso 1 1 calc R U . . .
C30 C 0.3432(2) 0.84784(17) 0.07873(18) 0.0435(7) Uani 1 1 d . . . . .
C31 C 0.3335(2) 0.8704(2) 0.26695(19) 0.0506(8) Uani 1 1 d . . . . .
H31 H 0.2667 0.8829 0.2760 0.061 Uiso 1 1 calc R U . . .
C32 C 0.3685(3) 0.8098(3) 0.3218(2) 0.0721(11) Uani 1 1 d . . . . .
H32A H 0.3559 0.7653 0.3167 0.108 Uiso 1 1 calc R U . . .
H32B H 0.3384 0.8270 0.3670 0.108 Uiso 1 1 calc R U . . .
H32C H 0.4336 0.7985 0.3167 0.108 Uiso 1 1 calc R U . . .
C33 C 0.3526(3) 0.9413(2) 0.2713(2) 0.0666(11) Uani 1 1 d . . . . .
H33A H 0.4177 0.9317 0.2612 0.100 Uiso 1 1 calc R U . . .
H33B H 0.3277 0.9577 0.3173 0.100 Uiso 1 1 calc R U . . .
H33C H 0.3246 0.9797 0.2382 0.100 Uiso 1 1 calc R U . . .
C34 C 0.2812(3) 0.8714(2) 0.02729(19) 0.0533(8) Uani 1 1 d . . . . .
H34 H 0.2286 0.9145 0.0445 0.064 Uiso 1 1 calc R U . . .
C35 C 0.2449(4) 0.8118(3) 0.0195(2) 0.0790(14) Uani 1 1 d . . . . .
H35A H 0.2950 0.7669 0.0071 0.118 Uiso 1 1 calc R U . . .
H35B H 0.2088 0.8286 -0.0163 0.118 Uiso 1 1 calc R U . . .
H35C H 0.2071 0.8013 0.0626 0.118 Uiso 1 1 calc R U . . .
C36 C 0.3268(4) 0.8970(3) -0.0440(2) 0.0751(12) Uani 1 1 d . . . . .
H36A H 0.3464 0.9383 -0.0398 0.113 Uiso 1 1 calc R U . . .
H36B H 0.2837 0.9130 -0.0748 0.113 Uiso 1 1 calc R U . . .
H36C H 0.3790 0.8560 -0.0622 0.113 Uiso 1 1 calc R U . . .
C37 C -0.00705(19) 0.91816(17) 0.25070(17) 0.0403(7) Uani 1 1 d . . . . .
C38 C -0.0608(2) 0.9061(2) 0.2121(2) 0.0493(8) Uani 1 1 d . . . . .
C39 C -0.1444(2) 0.9026(2) 0.2472(3) 0.0662(11) Uani 1 1 d . . . . .
H39 H -0.1840 0.8951 0.2230 0.079 Uiso 1 1 calc R U . . .
C40 C -0.1708(3) 0.9098(2) 0.3159(3) 0.0698(12) Uani 1 1 d . . . . .
H40 H -0.2281 0.9071 0.3386 0.084 Uiso 1 1 calc R U . . .
C41 C -0.1152(3) 0.9208(2) 0.3521(2) 0.0628(10) Uani 1 1 d . . . . .
H41 H -0.1348 0.9256 0.3997 0.075 Uiso 1 1 calc R U . . .
C42 C -0.0303(2) 0.92525(18) 0.32059(18) 0.0476(8) Uani 1 1 d . . . . .
C43 C -0.0327(3) 0.8985(3) 0.1361(2) 0.0635(11) Uani 1 1 d . . . . .
H43 H 0.0306 0.8991 0.1220 0.076 Uiso 1 1 calc R U . . .
C44 C -0.0333(4) 0.8245(3) 0.1205(3) 0.0881(16) Uani 1 1 d . . . . .
H44A H -0.0006 0.7850 0.1507 0.132 Uiso 1 1 calc R U . . .
H44B H -0.0041 0.8158 0.0730 0.132 Uiso 1 1 calc R U . . .
H44C H -0.0955 0.8250 0.1276 0.132 Uiso 1 1 calc R U . . .
C45 C -0.0913(4) 0.9628(3) 0.0959(3) 0.0867(15) Uani 1 1 d . . . . .
H45A H -0.1545 0.9663 0.1118 0.130 Uiso 1 1 calc R U . . .
H45B H -0.0735 0.9545 0.0474 0.130 Uiso 1 1 calc R U . . .
H45C H -0.0833 1.0088 0.1027 0.130 Uiso 1 1 calc R U . . .
C46 C 0.0301(3) 0.9388(2) 0.36016(19) 0.0556(9) Uani 1 1 d . . . . .
H46 H 0.0896 0.9325 0.3288 0.067 Uiso 1 1 calc R U . . .
C47 C 0.0474(6) 0.8840(3) 0.4204(3) 0.114(2) Uani 1 1 d . . . . .
H47A H -0.0098 0.8863 0.4513 0.171 Uiso 1 1 calc R U . . .
H47B H 0.0864 0.8956 0.4444 0.171 Uiso 1 1 calc R U . . .
H47C H 0.0770 0.8342 0.4050 0.171 Uiso 1 1 calc R U . . .
C48 C -0.0049(4) 1.0173(3) 0.3802(3) 0.0902(16) Uani 1 1 d . . . . .
H48A H -0.0130 1.0516 0.3394 0.135 Uiso 1 1 calc R U . . .
H48B H 0.0383 1.0255 0.4023 0.135 Uiso 1 1 calc R U . . .
H48C H -0.0628 1.0255 0.4118 0.135 Uiso 1 1 calc R U . . .
C49 C 0.85396(19) 0.50575(16) 0.21104(16) 0.0372(6) Uani 1 1 d . . . . .
C50 C 0.8843(2) 0.54105(18) 0.14949(18) 0.0430(7) Uani 1 1 d . . . . .
H50 H 0.9269 0.5120 0.1152 0.052 Uiso 1 1 calc R U . . .
C51 C 0.8539(2) 0.61726(19) 0.13690(19) 0.0498(8) Uani 1 1 d . . . . .
C52 C 0.7925(3) 0.66175(19) 0.1852(2) 0.0538(9) Uani 1 1 d . . . . .
H52 H 0.7718 0.7139 0.1763 0.065 Uiso 1 1 calc R U . . .
C53 C 0.7619(2) 0.62868(19) 0.24673(19) 0.0490(8) Uani 1 1 d . . . . .
C54 C 0.7915(2) 0.55166(17) 0.25957(17) 0.0405(7) Uani 1 1 d . . . . .
H54 H 0.7687 0.5301 0.3021 0.049 Uiso 1 1 calc R U . . .
C55 C 0.8904(3) 0.6528(2) 0.0712(2) 0.0683(11) Uani 1 1 d . . . . .
C56 C 0.6969(3) 0.6767(2) 0.2992(2) 0.0611(10) Uani 1 1 d . . . . .
C57 C 0.8351(2) 0.37999(16) 0.28512(16) 0.0374(6) Uani 1 1 d . . . . .
C58 C 0.7448(2) 0.39498(17) 0.28179(17) 0.0406(7) Uani 1 1 d . . . . .
H58 H 0.7195 0.4318 0.2486 0.049 Uiso 1 1 calc R U . . .
C59 C 0.6908(2) 0.35814(19) 0.32514(18) 0.0467(7) Uani 1 1 d . . . . .
C60 C 0.7242(3) 0.3048(2) 0.3746(2) 0.0556(9) Uani 1 1 d . . . . .
H60 H 0.6872 0.2797 0.4044 0.067 Uiso 1 1 calc R U . . .
C61 C 0.8127(3) 0.2889(2) 0.3798(2) 0.0543(9) Uani 1 1 d . . . . .
C62 C 0.8670(2) 0.32545(18) 0.33562(18) 0.0467(7) Uani 1 1 d . . . . .
H62 H 0.9279 0.3128 0.3400 0.056 Uiso 1 1 calc R U . . .
C63 C 0.5949(3) 0.3756(2) 0.3190(2) 0.0589(10) Uani 1 1 d . . . . .
C64 C 0.8521(4) 0.2314(3) 0.4313(3) 0.0764(13) Uani 1 1 d . . . . .
C65 C 0.91922(19) 0.37052(16) 0.16124(16) 0.0360(6) Uani 1 1 d . . . . .
C66 C 0.86650(19) 0.39489(17) 0.11104(16) 0.0376(6) Uani 1 1 d . . . . .
H66 H 0.8218 0.4423 0.1127 0.045 Uiso 1 1 calc R U . . .
C67 C 0.8773(2) 0.35195(17) 0.05863(16) 0.0400(7) Uani 1 1 d . . . . .
C68 C 0.9424(2) 0.28264(18) 0.05419(16) 0.0418(7) Uani 1 1 d . . . . .
H68 H 0.9504 0.2535 0.0182 0.050 Uiso 1 1 calc R U . . .
C69 C 0.9954(2) 0.25702(17) 0.10323(16) 0.0388(6) Uani 1 1 d . . . . .
C70 C 0.9832(2) 0.29966(16) 0.15589(16) 0.0379(6) Uani 1 1 d . . . . .
H70 H 1.0196 0.2802 0.1895 0.045 Uiso 1 1 calc R U . . .
C71 C 0.8219(2) 0.3831(2) 0.00504(19) 0.0517(8) Uani 1 1 d . . . . .
C72 C 1.0685(2) 0.18423(19) 0.09833(18) 0.0477(8) Uani 1 1 d . . . . .
C73 C 0.9924(2) 0.40949(16) 0.25236(16) 0.0377(6) Uani 1 1 d . . . . .
C74 C 1.0791(2) 0.38660(16) 0.21258(16) 0.0384(6) Uani 1 1 d . . . . .
H74 H 1.0862 0.3746 0.1675 0.046 Uiso 1 1 calc R U . . .
C75 C 1.1550(2) 0.38084(17) 0.23689(17) 0.0414(7) Uani 1 1 d . . . . .
C76 C 1.1472(2) 0.39984(17) 0.30187(17) 0.0414(7) Uani 1 1 d . . . . .
H76 H 1.1991 0.3944 0.3191 0.050 Uiso 1 1 calc R U . . .
C77 C 1.0617(2) 0.42690(17) 0.34115(16) 0.0396(7) Uani 1 1 d . . . . .
C78 C 0.9864(2) 0.43092(17) 0.31673(17) 0.0392(6) Uani 1 1 d . . . . .
H78 H 0.9286 0.4489 0.3447 0.047 Uiso 1 1 calc R U . . .
C79 C 1.2465(2) 0.3550(2) 0.1927(2) 0.0517(8) Uani 1 1 d . . . . .
C80 C 1.0508(2) 0.44844(19) 0.41083(18) 0.0460(7) Uani 1 1 d . . . . .
C81 C 0.52041(18) 0.05683(16) 0.22600(14) 0.0342(6) Uani 1 1 d . . . . .
C82 C 0.45222(19) 0.08569(18) 0.18734(15) 0.0381(6) Uani 1 1 d . . . . .
H82 H 0.4053 0.1304 0.1988 0.046 Uiso 1 1 calc R U . . .
C83 C 0.4513(2) 0.05046(19) 0.13235(15) 0.0411(7) Uani 1 1 d . . . . .
C84 C 0.5189(2) -0.01450(19) 0.11293(15) 0.0417(7) Uani 1 1 d . . . . .
H84 H 0.5174 -0.0389 0.0763 0.050 Uiso 1 1 calc R U . . .
C85 C 0.5885(2) -0.04257(17) 0.14875(15) 0.0370(6) Uani 1 1 d . . . . .
C86 C 0.58935(19) -0.00762(17) 0.20364(15) 0.0354(6) Uani 1 1 d . . . . .
H86 H 0.6384 -0.0282 0.2268 0.042 Uiso 1 1 calc R U . . .
C87 C 0.3753(2) 0.0841(2) 0.09436(17) 0.0507(8) Uani 1 1 d . . . . .
C88 C 0.6651(2) -0.11026(19) 0.12711(17) 0.0443(7) Uani 1 1 d . . . . .
C89 C 0.56946(17) 0.04129(17) 0.34899(14) 0.0343(6) Uani 1 1 d . . . . .
C90 C 0.55974(18) -0.02818(16) 0.36467(14) 0.0338(6) Uani 1 1 d . . . . .
H90 H 0.5322 -0.0446 0.3364 0.041 Uiso 1 1 calc R U . . .
C91 C 0.58906(19) -0.07475(17) 0.42069(14) 0.0370(6) Uani 1 1 d . . . . .
C92 C 0.62886(19) -0.05212(18) 0.46350(15) 0.0412(7) Uani 1 1 d . . . . .
H92 H 0.6486 -0.0833 0.5018 0.049 Uiso 1 1 calc R U . . .
C93 C 0.63888(19) 0.01631(18) 0.44900(15) 0.0392(7) Uani 1 1 d . . . . .
C94 C 0.60968(18) 0.06274(17) 0.39310(15) 0.0364(6) Uani 1 1 d . . . . .
H94 H 0.6172 0.1099 0.3847 0.044 Uiso 1 1 calc R U . . .
C95 C 0.5790(2) -0.14949(17) 0.43506(15) 0.0415(7) Uani 1 1 d . . . . .
C96 C 0.6818(2) 0.0411(2) 0.49507(17) 0.0485(8) Uani 1 1 d . . . . .
C97 C 0.58887(19) 0.15046(17) 0.24818(15) 0.0353(6) Uani 1 1 d . . . . .
C98 C 0.68092(19) 0.13126(16) 0.24721(15) 0.0357(6) Uani 1 1 d . . . . .
H98 H 0.7103 0.0866 0.2713 0.043 Uiso 1 1 calc R U . . .
C99 C 0.7307(2) 0.17597(17) 0.21177(17) 0.0415(7) Uani 1 1 d . . . . .
C100 C 0.6913(2) 0.24059(19) 0.17426(18) 0.0475(8) Uani 1 1 d . . . . .
H100 H 0.7254 0.2710 0.1501 0.057 Uiso 1 1 calc R U . . .
C101 C 0.6009(2) 0.25926(18) 0.17319(17) 0.0459(7) Uani 1 1 d . . . . .
C102 C 0.5507(2) 0.21549(18) 0.20941(15) 0.0404(7) Uani 1 1 d . . . . .
H102 H 0.4886 0.2301 0.2078 0.049 Uiso 1 1 calc R U . . .
C103 C 0.8285(2) 0.15469(19) 0.2138(2) 0.0556(9) Uani 1 1 d . . . . .
C104 C 0.5551(3) 0.3268(2) 0.1308(2) 0.0632(10) Uani 1 1 d . . . . .
C105 C 0.42875(18) 0.15172(16) 0.32574(14) 0.0344(6) Uani 1 1 d . . . . .
C106 C 0.42267(19) 0.21378(16) 0.35553(15) 0.0355(6) Uani 1 1 d . . . . .
H106 H 0.4753 0.2269 0.3501 0.043 Uiso 1 1 calc R U . . .
C107 C 0.34282(19) 0.25723(16) 0.39280(15) 0.0367(6) Uani 1 1 d . . . . .
C108 C 0.2641(2) 0.24029(17) 0.40085(16) 0.0406(7) Uani 1 1 d . . . . .
H108 H 0.2090 0.2701 0.4256 0.049 Uiso 1 1 calc R U . . .
C109 C 0.26821(19) 0.17907(18) 0.37201(16) 0.0397(7) Uani 1 1 d . . . . .
C110 C 0.34929(19) 0.13474(17) 0.33567(15) 0.0367(6) Uani 1 1 d . . . . .
H110 H 0.3504 0.0922 0.3174 0.044 Uiso 1 1 calc R U . . .
C111 C 0.3421(2) 0.32363(17) 0.42177(17) 0.0428(7) Uani 1 1 d . . . . .
C112 C 0.1824(2) 0.1625(2) 0.3786(2) 0.0522(8) Uani 1 1 d . . . . .
B1 B 0.9003(2) 0.41646(19) 0.22731(18) 0.0368(7) Uani 1 1 d . . . . .
B2 B 0.5268(2) 0.09923(19) 0.28746(17) 0.0336(7) Uani 1 1 d . . . . .
N1 N 0.23352(19) 0.59456(15) 0.27553(16) 0.0472(6) Uani 1 1 d . . . . .
N2 N 0.36932(18) 0.57098(14) 0.21759(15) 0.0441(6) Uani 1 1 d . . . . .
N3 N 0.21882(16) 0.90322(13) 0.16896(13) 0.0356(5) Uani 1 1 d . . . . .
N4 N 0.07862(16) 0.92621(13) 0.21518(13) 0.0364(5) Uani 1 1 d . . . . .
F1 F 0.9233(2) 0.61057(16) 0.02117(13) 0.0921(9) Uani 1 1 d . . . . .
F2 F 0.9549(3) 0.6773(2) 0.07858(18) 0.1269(15) Uani 1 1 d . . . . .
F3 F 0.8305(3) 0.7120(2) 0.0504(2) 0.161(2) Uani 1 1 d . . . . .
F4 F 0.6973(8) 0.6489(3) 0.3604(3) 0.104(3) Uani 0.645(16) 1 d D U P A 3
F5 F 0.7217(3) 0.7402(3) 0.2985(3) 0.0654(16) Uani 0.645(16) 1 d D U P A 3
F6 F 0.6158(7) 0.7041(7) 0.2883(7) 0.100(3) Uani 0.645(16) 1 d D U P A 3
F4' F 0.6524(9) 0.6344(6) 0.3534(5) 0.082(3) Uani 0.355(16) 1 d D U P A 4
F5' F 0.7269(7) 0.7063(11) 0.3312(10) 0.109(5) Uani 0.355(16) 1 d D U P A 4
F6' F 0.6240(11) 0.7200(8) 0.2743(8) 0.067(4) Uani 0.355(16) 1 d D U P A 4
F7 F 0.57780(15) 0.40920(15) 0.25840(14) 0.0724(7) Uani 1 1 d . . . . .
F8 F 0.57093(17) 0.31502(15) 0.32804(15) 0.0774(7) Uani 1 1 d . . . . .
F9 F 0.53740(16) 0.42057(16) 0.36602(16) 0.0836(8) Uani 1 1 d . . . . .
F10 F 0.7844(3) 0.2302(3) 0.49179(19) 0.0634(15) Uani 0.596(9) 1 d D U P B 5
F11 F 0.8716(7) 0.1669(3) 0.4146(3) 0.113(3) Uani 0.596(9) 1 d D U P B 5
F12 F 0.9179(5) 0.2370(6) 0.4530(5) 0.092(3) Uani 0.596(9) 1 d D U P B 5
F10' F 0.8231(7) 0.1819(7) 0.4520(7) 0.123(5) Uani 0.404(9) 1 d D U P B 6
F11' F 0.9447(7) 0.1784(5) 0.3935(5) 0.107(3) Uani 0.404(9) 1 d D U P B 6
F12' F 0.8944(10) 0.2550(7) 0.4654(7) 0.087(4) Uani 0.404(9) 1 d D U P B 6
F13 F 0.8232(2) 0.33238(14) -0.03307(15) 0.0839(8) Uani 1 1 d . . . . .
F14 F 0.73659(15) 0.42158(18) 0.03021(13) 0.0801(8) Uani 1 1 d . . . . .
F15 F 0.84955(18) 0.43292(14) -0.03958(12) 0.0707(6) Uani 1 1 d . . . . .
F16 F 1.05299(18) 0.13675(12) 0.06615(13) 0.0720(7) Uani 1 1 d . . . . .
F17 F 1.08275(15) 0.14974(10) 0.15938(11) 0.0576(5) Uani 1 1 d . . . . .
F18 F 1.14787(15) 0.19006(13) 0.06569(14) 0.0771(7) Uani 1 1 d . . . . .
F19 F 1.2522(3) 0.3177(5) 0.1416(4) 0.085(2) Uani 0.701(15) 1 d D U P C 7
F20 F 1.3108(4) 0.3162(5) 0.2239(3) 0.089(2) Uani 0.701(15) 1 d D U P C 7
F21 F 1.2714(4) 0.4143(3) 0.1580(4) 0.0802(17) Uani 0.701(15) 1 d D U P C 7
F19' F 1.2642(7) 0.2840(7) 0.1828(11) 0.089(4) Uani 0.299(15) 1 d D U P C 8
F20' F 1.3088(9) 0.3479(10) 0.2299(7) 0.067(4) Uani 0.299(15) 1 d D U P C 8
F21' F 1.2546(10) 0.3904(11) 0.1417(7) 0.095(5) Uani 0.299(15) 1 d D U P C 8
F22 F 1.05807(17) 0.39164(13) 0.45785(11) 0.0644(6) Uani 1 1 d . . . . .
F23 F 1.11385(17) 0.47695(16) 0.41525(12) 0.0718(7) Uani 1 1 d . . . . .
F24 F 0.97216(16) 0.49936(14) 0.43093(13) 0.0734(7) Uani 1 1 d . . . . .
F25 F 0.3805(5) 0.1432(4) 0.0553(5) 0.0795(19) Uani 0.81(2) 1 d D U P D 9
F26 F 0.29583(19) 0.1026(5) 0.13687(18) 0.0597(16) Uani 0.81(2) 1 d D U P D 9
F27 F 0.3696(5) 0.0357(3) 0.0550(4) 0.0738(16) Uani 0.81(2) 1 d D U P D 9
F25' F 0.3050(13) 0.1403(17) 0.1266(10) 0.065(6) Uani 0.19(2) 1 d D U P D 10
F26' F 0.3472(16) 0.0403(12) 0.0753(13) 0.055(5) Uani 0.19(2) 1 d D U P D 10
F27' F 0.4055(14) 0.1230(12) 0.0351(9) 0.051(5) Uani 0.19(2) 1 d D U P D 10
F28 F 0.6452(3) -0.1583(4) 0.0998(4) 0.0651(17) Uani 0.726(16) 1 d D U P E 11
F29 F 0.7101(5) -0.14796(19) 0.1760(2) 0.0620(16) Uani 0.726(16) 1 d D U P E 11
F30 F 0.7306(3) -0.0935(2) 0.0770(4) 0.0734(18) Uani 0.726(16) 1 d D U P E 11
F28' F 0.6489(11) -0.1342(9) 0.0791(6) 0.060(4) Uani 0.274(16) 1 d D U P E 12
F29' F 0.6625(13) -0.1593(7) 0.1822(5) 0.076(5) Uani 0.274(16) 1 d D U P E 12
F30' F 0.7372(7) -0.0987(8) 0.1134(10) 0.065(4) Uani 0.274(16) 1 d D U P E 12
F31 F 0.52266(14) -0.15649(11) 0.49393(10) 0.0553(5) Uani 1 1 d . . . . .
F32 F 0.65774(13) -0.20289(11) 0.44114(11) 0.0564(5) Uani 1 1 d . . . . .
F33 F 0.54788(16) -0.16812(11) 0.38733(11) 0.0565(5) Uani 1 1 d . . . . .
F34 F 0.63827(15) 0.04103(14) 0.55978(10) 0.0638(6) Uani 1 1 d . . . . .
F35 F 0.6848(2) 0.10869(19) 0.47864(14) 0.0934(10) Uani 1 1 d . . . . .
F36 F 0.76522(16) -0.0030(2) 0.49701(15) 0.1042(12) Uani 1 1 d . . . . .
F37 F 0.85863(17) 0.09568(17) 0.2527(2) 0.1172(14) Uani 1 1 d . . . . .
F38 F 0.85089(14) 0.20853(14) 0.22882(15) 0.0719(7) Uani 1 1 d . . . . .
F39 F 0.88072(16) 0.13813(18) 0.15137(17) 0.0937(10) Uani 1 1 d . . . . .
F40 F 0.6039(2) 0.3697(2) 0.1075(2) 0.1393(18) Uani 1 1 d . . . . .
F41 F 0.48044(15) 0.36960(13) 0.16560(14) 0.0733(7) Uani 1 1 d . . . . .
F42 F 0.5330(4) 0.31005(19) 0.07869(18) 0.158(2) Uani 1 1 d . . . . .
F43 F 0.41273(14) 0.31178(10) 0.45042(11) 0.0522(5) Uani 1 1 d . . . . .
F44 F 0.34517(15) 0.37907(11) 0.37226(11) 0.0569(5) Uani 1 1 d . . . . .
F45 F 0.26908(15) 0.35091(12) 0.46844(13) 0.0669(6) Uani 1 1 d . . . . .
F46 F 0.12638(18) 0.21297(18) 0.3422(2) 0.0823(13) Uani 0.887(8) 1 d D U P F 13
F47 F 0.1360(2) 0.1642(2) 0.44251(15) 0.0784(12) Uani 0.887(8) 1 d D U P F 13
F48 F 0.19391(18) 0.09686(19) 0.3599(2) 0.0653(9) Uani 0.887(8) 1 d D U P F 13
F46' F 0.1128(15) 0.2173(11) 0.3905(14) 0.071(8) Uiso 0.113(8) 1 d D . P F 13
F47' F 0.175(2) 0.1173(16) 0.4401(12) 0.089(9) Uani 0.113(8) 1 d D U P F 13
F48' F 0.1875(18) 0.1231(16) 0.3330(12) 0.067(8) Uani 0.113(8) 1 d D U P F 13
P1 P 0.28445(7) 0.71799(5) 0.19043(5) 0.0450(3) Uani 0.8657(18) 1 d . . P G 1
P2 P 0.15951(7) 0.77833(5) 0.23836(6) 0.0426(3) Uani 0.8657(18) 1 d . . P G 1
P1' P 0.2372(5) 0.7080(3) 0.1746(4) 0.0450(3) Uani 0.1343(18) 1 d . . P G 2
P2' P 0.1864(5) 0.7782(4) 0.2643(4) 0.0426(3) Uani 0.1343(18) 1 d . . P G 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.346(4) . ?
C1 N1 1.352(4) . ?
C1 P1 1.840(3) . ?
C1 P1' 1.883(7) . ?
C2 C3 1.343(6) . ?
C2 N1 1.364(4) . ?
C3 N2 1.366(5) . ?
C4 C5 1.387(5) . ?
C4 C9 1.401(5) . ?
C4 N2 1.460(4) . ?
C5 C6 1.400(6) . ?
C5 C10 1.500(5) . ?
C6 C7 1.384(6) . ?
C7 C8 1.376(6) . ?
C7 C11 1.512(6) . ?
C8 C9 1.383(5) . ?
C9 C12 1.511(5) . ?
C13 C14 1.381(5) . ?
C13 C18 1.383(5) . ?
C13 N1 1.448(4) . ?
C14 C15 1.394(6) . ?
C14 C19 1.504(6) . ?
C15 C16 1.378(6) . ?
C16 C17 1.392(6) . ?
C16 C20 1.500(5) . ?
C17 C18 1.397(5) . ?
C18 C21 1.509(5) . ?
C22 N4 1.345(4) . ?
C22 N3 1.348(4) . ?
C22 P2 1.828(3) . ?
C22 P2' 2.003(8) . ?
C23 C24 1.351(4) . ?
C23 N3 1.376(4) . ?
C24 N4 1.366(4) . ?
C25 C26 1.392(5) . ?
C25 C30 1.400(5) . ?
C25 N3 1.449(4) . ?
C26 C27 1.405(5) . ?
C26 C31 1.518(5) . ?
C27 C28 1.383(6) . ?
C28 C29 1.357(6) . ?
C29 C30 1.402(5) . ?
C30 C34 1.523(5) . ?
C31 C33 1.530(5) . ?
C31 C32 1.534(6) . ?
C34 C35 1.511(6) . ?
C34 C36 1.554(6) . ?
C37 C38 1.392(5) . ?
C37 C42 1.394(5) . ?
C37 N4 1.455(4) . ?
C38 C39 1.393(5) . ?
C38 C43 1.516(5) . ?
C39 C40 1.373(7) . ?
C40 C41 1.371(6) . ?
C41 C42 1.401(5) . ?
C42 C46 1.509(5) . ?
C43 C44 1.523(6) . ?
C43 C45 1.527(7) . ?
C46 C47 1.499(7) . ?
C46 C48 1.512(6) . ?
C49 C50 1.396(5) . ?
C49 C54 1.401(4) . ?
C49 B1 1.643(4) . ?
C50 C51 1.388(5) . ?
C51 C52 1.380(5) . ?
C51 C55 1.492(6) . ?
C52 C53 1.377(6) . ?
C53 C54 1.403(5) . ?
C53 C56 1.486(5) . ?
C55 F1 1.299(5) . ?
C55 F3 1.302(6) . ?
C55 F2 1.335(6) . ?
C56 F5' 1.200(10) . ?
C56 F4 1.272(7) . ?
C56 F6 1.290(10) . ?
C56 F6' 1.342(12) . ?
C56 F5 1.421(6) . ?
C56 F4' 1.470(14) . ?
C57 C62 1.399(5) . ?
C57 C58 1.401(4) . ?
C57 B1 1.636(5) . ?
C58 C59 1.390(5) . ?
C59 C60 1.380(5) . ?
C59 C63 1.498(5) . ?
C60 C61 1.382(6) . ?
C61 C62 1.395(5) . ?
C61 C64 1.479(6) . ?
C63 F8 1.336(5) . ?
C63 F7 1.338(5) . ?
C63 F9 1.347(5) . ?
C64 F10' 1.189(10) . ?
C64 F11 1.260(7) . ?
C64 F12 1.285(10) . ?
C64 F12' 1.302(12) . ?
C64 F10 1.444(7) . ?
C64 F11' 1.588(11) . ?
C65 C66 1.398(4) . ?
C65 C70 1.404(4) . ?
C65 B1 1.635(4) . ?
C66 C67 1.393(4) . ?
C67 C68 1.388(5) . ?
C67 C71 1.489(5) . ?
C68 C69 1.383(5) . ?
C69 C70 1.388(4) . ?
C69 C72 1.491(5) . ?
C71 F13 1.335(4) . ?
C71 F14 1.338(4) . ?
C71 F15 1.340(5) . ?
C72 F16 1.328(4) . ?
C72 F18 1.335(4) . ?
C72 F17 1.341(4) . ?
C73 C74 1.401(4) . ?
C73 C78 1.402(4) . ?
C73 B1 1.638(4) . ?
C74 C75 1.389(4) . ?
C75 C76 1.389(5) . ?
C75 C79 1.499(5) . ?
C76 C77 1.389(5) . ?
C77 C78 1.392(4) . ?
C77 C80 1.489(5) . ?
C79 F21' 1.157(12) . ?
C79 F20 1.286(7) . ?
C79 F19 1.323(5) . ?
C79 F19' 1.343(11) . ?
C79 F20' 1.350(12) . ?
C79 F21 1.387(6) . ?
C80 F24 1.328(4) . ?
C80 F22 1.330(4) . ?
C80 F23 1.345(4) . ?
C81 C82 1.405(4) . ?
C81 C86 1.407(4) . ?
C81 B2 1.637(4) . ?
C82 C83 1.401(4) . ?
C83 C84 1.389(5) . ?
C83 C87 1.501(4) . ?
C84 C85 1.384(4) . ?
C85 C86 1.395(4) . ?
C85 C88 1.497(4) . ?
C87 F26' 1.24(2) . ?
C87 F25 1.305(6) . ?
C87 F26 1.334(5) . ?
C87 F27 1.362(7) . ?
C87 F25' 1.385(14) . ?
C87 F27' 1.397(17) . ?
C88 F30' 1.226(11) . ?
C88 F28' 1.255(13) . ?
C88 F28 1.317(6) . ?
C88 F29 1.335(5) . ?
C88 F29' 1.351(11) . ?
C88 F30 1.378(5) . ?
C89 C90 1.391(4) . ?
C89 C94 1.404(4) . ?
C89 B2 1.647(4) . ?
C90 C91 1.400(4) . ?
C91 C92 1.392(5) . ?
C91 C95 1.493(5) . ?
C92 C93 1.373(5) . ?
C93 C94 1.396(4) . ?
C93 C96 1.504(4) . ?
C95 F33 1.335(4) . ?
C95 F31 1.343(4) . ?
C95 F32 1.349(4) . ?
C96 F35 1.318(5) . ?
C96 F36 1.326(4) . ?
C96 F34 1.337(4) . ?
C97 C98 1.398(4) . ?
C97 C102 1.400(4) . ?
C97 B2 1.647(4) . ?
C98 C99 1.394(4) . ?
C99 C100 1.387(5) . ?
C99 C103 1.497(5) . ?
C100 C101 1.382(5) . ?
C101 C102 1.391(5) . ?
C101 C104 1.505(5) . ?
C103 F37 1.294(5) . ?
C103 F38 1.316(4) . ?
C103 F39 1.363(5) . ?
C104 F40 1.306(5) . ?
C104 F42 1.308(6) . ?
C104 F41 1.316(5) . ?
C105 C106 1.394(4) . ?
C105 C110 1.399(4) . ?
C105 B2 1.642(4) . ?
C106 C107 1.390(4) . ?
C107 C108 1.391(4) . ?
C107 C111 1.493(5) . ?
C108 C109 1.379(5) . ?
C109 C110 1.400(4) . ?
C109 C112 1.503(4) . ?
C111 F45 1.330(4) . ?
C111 F43 1.333(4) . ?
C111 F44 1.358(4) . ?
C112 F46' 1.25(2) . ?
C112 F48' 1.26(2) . ?
C112 F48 1.326(5) . ?
C112 F46 1.336(5) . ?
C112 F47 1.337(5) . ?
C112 F47' 1.41(2) . ?
F46 F46' 0.96(3) . ?
F46 F48' 1.69(3) . ?
F47 F47' 0.91(3) . ?
F47 F46' 1.37(3) . ?
F48 F48' 0.68(3) . ?
F48 F47' 1.67(3) . ?
P1 P2 2.0453(13) . ?
P1' P2' 2.266(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 N1 106.5(3) . . ?
N2 C1 P1 117.0(2) . . ?
N1 C1 P1 136.5(3) . . ?
N2 C1 P1' 129.1(3) . . ?
N1 C1 P1' 116.7(3) . . ?
C3 C2 N1 107.7(3) . . ?
C2 C3 N2 107.2(3) . . ?
C5 C4 C9 123.4(3) . . ?
C5 C4 N2 117.9(3) . . ?
C9 C4 N2 118.6(3) . . ?
C4 C5 C6 116.5(3) . . ?
C4 C5 C10 121.8(4) . . ?
C6 C5 C10 121.8(4) . . ?
C7 C6 C5 122.2(3) . . ?
C8 C7 C6 118.4(4) . . ?
C8 C7 C11 121.3(4) . . ?
C6 C7 C11 120.2(4) . . ?
C7 C8 C9 122.8(3) . . ?
C8 C9 C4 116.7(3) . . ?
C8 C9 C12 121.3(3) . . ?
C4 C9 C12 122.1(3) . . ?
C14 C13 C18 124.1(3) . . ?
C14 C13 N1 117.5(3) . . ?
C18 C13 N1 118.3(3) . . ?
C13 C14 C15 117.1(4) . . ?
C13 C14 C19 121.6(4) . . ?
C15 C14 C19 121.3(4) . . ?
C16 C15 C14 121.9(4) . . ?
C15 C16 C17 118.5(4) . . ?
C15 C16 C20 120.8(4) . . ?
C17 C16 C20 120.6(4) . . ?
C16 C17 C18 122.2(4) . . ?
C13 C18 C17 116.3(3) . . ?
C13 C18 C21 122.5(3) . . ?
C17 C18 C21 121.2(3) . . ?
N4 C22 N3 106.4(2) . . ?
N4 C22 P2 117.3(2) . . ?
N3 C22 P2 136.1(2) . . ?
N4 C22 P2' 122.1(3) . . ?
N3 C22 P2' 124.1(3) . . ?
C24 C23 N3 106.9(3) . . ?
C23 C24 N4 107.2(3) . . ?
C26 C25 C30 125.1(3) . . ?
C26 C25 N3 117.3(3) . . ?
C30 C25 N3 117.5(3) . . ?
C25 C26 C27 115.7(3) . . ?
C25 C26 C31 122.6(3) . . ?
C27 C26 C31 121.7(3) . . ?
C28 C27 C26 120.4(3) . . ?
C29 C28 C27 122.1(3) . . ?
C28 C29 C30 120.7(3) . . ?
C25 C30 C29 115.9(3) . . ?
C25 C30 C34 123.0(3) . . ?
C29 C30 C34 121.1(3) . . ?
C26 C31 C33 109.9(3) . . ?
C26 C31 C32 113.6(3) . . ?
C33 C31 C32 112.2(3) . . ?
C35 C34 C30 112.9(3) . . ?
C35 C34 C36 109.0(3) . . ?
C30 C34 C36 112.6(3) . . ?
C38 C37 C42 124.9(3) . . ?
C38 C37 N4 117.6(3) . . ?
C42 C37 N4 117.4(3) . . ?
C37 C38 C39 116.1(3) . . ?
C37 C38 C43 123.1(3) . . ?
C39 C38 C43 120.8(3) . . ?
C40 C39 C38 121.2(4) . . ?
C41 C40 C39 120.8(3) . . ?
C40 C41 C42 121.5(4) . . ?
C37 C42 C41 115.5(3) . . ?
C37 C42 C46 123.0(3) . . ?
C41 C42 C46 121.5(3) . . ?
C38 C43 C44 110.1(4) . . ?
C38 C43 C45 111.8(4) . . ?
C44 C43 C45 111.6(4) . . ?
C47 C46 C42 112.9(4) . . ?
C47 C46 C48 111.6(4) . . ?
C42 C46 C48 111.5(4) . . ?
C50 C49 C54 116.2(3) . . ?
C50 C49 B1 120.2(3) . . ?
C54 C49 B1 123.1(3) . . ?
C51 C50 C49 121.9(3) . . ?
C52 C51 C50 121.2(3) . . ?
C52 C51 C55 118.7(3) . . ?
C50 C51 C55 120.1(3) . . ?
C53 C52 C51 118.3(3) . . ?
C52 C53 C54 120.9(3) . . ?
C52 C53 C56 118.3(3) . . ?
C54 C53 C56 120.8(4) . . ?
C49 C54 C53 121.5(3) . . ?
F1 C55 F3 106.8(5) . . ?
F1 C55 F2 107.4(4) . . ?
F3 C55 F2 103.5(4) . . ?
F1 C55 C51 114.9(3) . . ?
F3 C55 C51 112.5(4) . . ?
F2 C55 C51 110.9(4) . . ?
F4 C56 F6 110.6(7) . . ?
F5' C56 F6' 115.9(10) . . ?
F4 C56 F5 102.7(5) . . ?
F6 C56 F5 103.2(6) . . ?
F5' C56 F4' 101.8(10) . . ?
F6' C56 F4' 98.1(8) . . ?
F5' C56 C53 117.1(6) . . ?
F4 C56 C53 115.1(4) . . ?
F6 C56 C53 114.8(6) . . ?
F6' C56 C53 110.2(9) . . ?
F5 C56 C53 109.2(4) . . ?
F4' C56 C53 111.7(5) . . ?
C62 C57 C58 115.2(3) . . ?
C62 C57 B1 123.1(3) . . ?
C58 C57 B1 121.3(3) . . ?
C59 C58 C57 122.6(3) . . ?
C60 C59 C58 120.8(3) . . ?
C60 C59 C63 118.6(3) . . ?
C58 C59 C63 120.5(3) . . ?
C59 C60 C61 118.2(3) . . ?
C60 C61 C62 120.7(3) . . ?
C60 C61 C64 120.3(4) . . ?
C62 C61 C64 119.0(4) . . ?
C61 C62 C57 122.4(3) . . ?
F8 C63 F7 106.8(3) . . ?
F8 C63 F9 106.2(3) . . ?
F7 C63 F9 106.4(3) . . ?
F8 C63 C59 112.0(3) . . ?
F7 C63 C59 113.1(3) . . ?
F9 C63 C59 111.9(3) . . ?
F11 C64 F12 109.8(7) . . ?
F10' C64 F12' 123.6(9) . . ?
F11 C64 F10 100.1(5) . . ?
F12 C64 F10 104.6(5) . . ?
F10' C64 C61 120.8(7) . . ?
F11 C64 C61 112.9(5) . . ?
F12 C64 C61 117.7(5) . . ?
F12' C64 C61 111.3(7) . . ?
F10 C64 C61 110.0(4) . . ?
F10' C64 F11' 92.8(8) . . ?
F12' C64 F11' 90.9(8) . . ?
C61 C64 F11' 107.4(5) . . ?
C66 C65 C70 115.7(3) . . ?
C66 C65 B1 122.6(3) . . ?
C70 C65 B1 121.2(3) . . ?
C67 C66 C65 122.2(3) . . ?
C68 C67 C66 120.6(3) . . ?
C68 C67 C71 120.2(3) . . ?
C66 C67 C71 119.1(3) . . ?
C69 C68 C67 118.5(3) . . ?
C68 C69 C70 120.6(3) . . ?
C68 C69 C72 119.9(3) . . ?
C70 C69 C72 119.5(3) . . ?
C69 C70 C65 122.4(3) . . ?
F13 C71 F14 109.5(3) . . ?
F13 C71 F15 104.7(3) . . ?
F14 C71 F15 102.7(3) . . ?
F13 C71 C67 113.3(3) . . ?
F14 C71 C67 112.8(3) . . ?
F15 C71 C67 113.1(3) . . ?
F16 C72 F18 106.1(3) . . ?
F16 C72 F17 105.6(3) . . ?
F18 C72 F17 105.1(3) . . ?
F16 C72 C69 113.8(3) . . ?
F18 C72 C69 112.7(3) . . ?
F17 C72 C69 112.8(3) . . ?
C74 C73 C78 115.8(3) . . ?
C74 C73 B1 124.8(3) . . ?
C78 C73 B1 119.4(3) . . ?
C75 C74 C73 122.2(3) . . ?
C76 C75 C74 120.6(3) . . ?
C76 C75 C79 119.1(3) . . ?
C74 C75 C79 120.3(3) . . ?
C75 C76 C77 118.6(3) . . ?
C76 C77 C78 120.2(3) . . ?
C76 C77 C80 120.0(3) . . ?
C78 C77 C80 119.8(3) . . ?
C77 C78 C73 122.5(3) . . ?
F20 C79 F19 106.6(5) . . ?
F21' C79 F19' 111.5(10) . . ?
F21' C79 F20' 113.4(11) . . ?
F19' C79 F20' 100.4(8) . . ?
F20 C79 F21 106.1(5) . . ?
F19 C79 F21 101.0(5) . . ?
F21' C79 C75 114.2(7) . . ?
F20 C79 C75 115.7(4) . . ?
F19 C79 C75 115.2(3) . . ?
F19' C79 C75 107.6(6) . . ?
F20' C79 C75 108.7(7) . . ?
F21 C79 C75 110.9(4) . . ?
F24 C80 F22 106.9(3) . . ?
F24 C80 F23 105.8(3) . . ?
F22 C80 F23 105.6(3) . . ?
F24 C80 C77 113.1(3) . . ?
F22 C80 C77 112.8(3) . . ?
F23 C80 C77 112.0(3) . . ?
C82 C81 C86 115.3(3) . . ?
C82 C81 B2 123.1(3) . . ?
C86 C81 B2 121.2(2) . . ?
C83 C82 C81 121.9(3) . . ?
C84 C83 C82 121.3(3) . . ?
C84 C83 C87 120.0(3) . . ?
C82 C83 C87 118.7(3) . . ?
C85 C84 C83 117.8(3) . . ?
C84 C85 C86 121.0(3) . . ?
C84 C85 C88 119.5(3) . . ?
C86 C85 C88 119.6(3) . . ?
C85 C86 C81 122.6(3) . . ?
F25 C87 F26 107.4(4) . . ?
F25 C87 F27 107.8(4) . . ?
F26 C87 F27 104.3(4) . . ?
F26' C87 F25' 111.1(11) . . ?
F26' C87 F27' 105.7(11) . . ?
F25' C87 F27' 100.9(11) . . ?
F26' C87 C83 116.1(11) . . ?
F25 C87 C83 113.2(4) . . ?
F26 C87 C83 111.4(3) . . ?
F27 C87 C83 112.2(4) . . ?
F25' C87 C83 113.6(6) . . ?
F27' C87 C83 107.9(9) . . ?
F30' C88 F28' 113.3(9) . . ?
F28 C88 F29 106.7(4) . . ?
F30' C88 F29' 110.5(8) . . ?
F28' C88 F29' 108.4(9) . . ?
F28 C88 F30 102.9(4) . . ?
F29 C88 F30 103.3(4) . . ?
F30' C88 C85 111.6(6) . . ?
F28' C88 C85 109.0(8) . . ?
F28 C88 C85 116.0(3) . . ?
F29 C88 C85 114.6(3) . . ?
F29' C88 C85 103.6(5) . . ?
F30 C88 C85 111.9(3) . . ?
C90 C89 C94 116.2(3) . . ?
C90 C89 B2 122.4(3) . . ?
C94 C89 B2 121.1(3) . . ?
C89 C90 C91 122.3(3) . . ?
C92 C91 C90 120.3(3) . . ?
C92 C91 C95 119.0(3) . . ?
C90 C91 C95 120.7(3) . . ?
C93 C92 C91 118.3(3) . . ?
C92 C93 C94 121.4(3) . . ?
C92 C93 C96 118.6(3) . . ?
C94 C93 C96 120.1(3) . . ?
C93 C94 C89 121.5(3) . . ?
F33 C95 F31 105.8(3) . . ?
F33 C95 F32 106.6(3) . . ?
F31 C95 F32 105.1(2) . . ?
F33 C95 C91 113.9(3) . . ?
F31 C95 C91 112.9(3) . . ?
F32 C95 C91 111.9(3) . . ?
F35 C96 F36 107.2(3) . . ?
F35 C96 F34 105.0(3) . . ?
F36 C96 F34 105.0(3) . . ?
F35 C96 C93 114.0(3) . . ?
F36 C96 C93 112.3(3) . . ?
F34 C96 C93 112.6(3) . . ?
C98 C97 C102 116.1(3) . . ?
C98 C97 B2 124.1(3) . . ?
C102 C97 B2 119.7(2) . . ?
C99 C98 C97 121.7(3) . . ?
C100 C99 C98 121.2(3) . . ?
C100 C99 C103 118.7(3) . . ?
C98 C99 C103 120.1(3) . . ?
C101 C100 C99 117.8(3) . . ?
C100 C101 C102 121.2(3) . . ?
C100 C101 C104 120.4(3) . . ?
C102 C101 C104 118.3(3) . . ?
C101 C102 C97 122.0(3) . . ?
F37 C103 F38 109.7(4) . . ?
F37 C103 F39 103.6(3) . . ?
F38 C103 F39 103.4(3) . . ?
F37 C103 C99 114.6(3) . . ?
F38 C103 C99 113.4(3) . . ?
F39 C103 C99 111.2(3) . . ?
F40 C104 F42 107.5(4) . . ?
F40 C104 F41 104.2(4) . . ?
F42 C104 F41 106.4(4) . . ?
F40 C104 C101 113.3(4) . . ?
F42 C104 C101 112.3(4) . . ?
F41 C104 C101 112.6(3) . . ?
C106 C105 C110 116.1(3) . . ?
C106 C105 B2 120.2(2) . . ?
C110 C105 B2 123.5(3) . . ?
C107 C106 C105 122.8(3) . . ?
C106 C107 C108 120.2(3) . . ?
C106 C107 C111 119.1(3) . . ?
C108 C107 C111 120.6(3) . . ?
C109 C108 C107 118.3(3) . . ?
C108 C109 C110 121.2(3) . . ?
C108 C109 C112 118.1(3) . . ?
C110 C109 C112 120.7(3) . . ?
C105 C110 C109 121.4(3) . . ?
F45 C111 F43 106.7(3) . . ?
F45 C111 F44 106.5(3) . . ?
F43 C111 F44 105.1(3) . . ?
F45 C111 C107 113.5(3) . . ?
F43 C111 C107 113.6(3) . . ?
F44 C111 C107 110.9(3) . . ?
F46' C112 F48' 117.7(16) . . ?
F46' C112 F48 130.8(11) . . ?
F48' C112 F48 30.6(13) . . ?
F46' C112 F46 43.5(12) . . ?
F48' C112 F46 81.3(13) . . ?
F48 C112 F46 107.4(4) . . ?
F46' C112 F47 63.9(12) . . ?
F48' C112 F47 128.7(14) . . ?
F48 C112 F47 105.5(3) . . ?
F46 C112 F47 104.9(3) . . ?
F46' C112 F47' 101.7(14) . . ?
F48' C112 F47' 104.8(15) . . ?
F48 C112 F47' 74.9(12) . . ?
F46 C112 F47' 137.2(13) . . ?
F47 C112 F47' 38.6(13) . . ?
F46' C112 C109 113.8(11) . . ?
F48' C112 C109 111.7(13) . . ?
F48 C112 C109 114.3(3) . . ?
F46 C112 C109 111.6(3) . . ?
F47 C112 C109 112.5(3) . . ?
F47' C112 C109 105.3(12) . . ?
C65 B1 C57 103.2(2) . . ?
C65 B1 C73 113.2(2) . . ?
C57 B1 C73 111.9(3) . . ?
C65 B1 C49 112.3(3) . . ?
C57 B1 C49 112.9(2) . . ?
C73 B1 C49 103.7(2) . . ?
C81 B2 C105 113.7(2) . . ?
C81 B2 C97 103.3(2) . . ?
C105 B2 C97 109.9(2) . . ?
C81 B2 C89 112.4(2) . . ?
C105 B2 C89 104.4(2) . . ?
C97 B2 C89 113.4(2) . . ?
C1 N1 C2 109.1(3) . . ?
C1 N1 C13 127.5(3) . . ?
C2 N1 C13 123.3(3) . . ?
C1 N2 C3 109.5(3) . . ?
C1 N2 C4 125.5(3) . . ?
C3 N2 C4 125.0(3) . . ?
C22 N3 C23 109.5(2) . . ?
C22 N3 C25 125.4(2) . . ?
C23 N3 C25 125.1(2) . . ?
C22 N4 C24 109.9(2) . . ?
C22 N4 C37 126.2(2) . . ?
C24 N4 C37 123.9(2) . . ?
F46' F46 C112 63.6(12) . . ?
F46' F46 F48' 104.9(14) . . ?
C112 F46 F48' 47.4(9) . . ?
F47' F47 C112 75.3(15) . . ?
F47' F47 F46' 128.9(18) . . ?
C112 F47 F46' 55.1(9) . . ?
F48' F48 C112 69.5(19) . . ?
F48' F48 F47' 123(2) . . ?
C112 F48 F47' 55.0(9) . . ?
F46 F46' C112 72.9(14) . . ?
F46 F46' F47 129.5(17) . . ?
C112 F46' F47 61.0(10) . . ?
F47 F47' C112 66.1(13) . . ?
F47 F47' F48 106.7(16) . . ?
C112 F47' F48 50.1(8) . . ?
F48 F48' C112 80.0(19) . . ?
F48 F48' F46 123(2) . . ?
C112 F48' F46 51.3(9) . . ?
C1 P1 P2 100.15(12) . . ?
C22 P2 P1 100.17(10) . . ?
C1 P1' P2' 89.9(4) . . ?
C22 P2' P1' 91.6(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.8(5) . . . . ?
C9 C4 C5 C6 -2.6(5) . . . . ?
N2 C4 C5 C6 179.7(3) . . . . ?
C9 C4 C5 C10 177.8(3) . . . . ?
N2 C4 C5 C10 0.1(5) . . . . ?
C4 C5 C6 C7 2.1(5) . . . . ?
C10 C5 C6 C7 -178.4(4) . . . . ?
C5 C6 C7 C8 -0.1(5) . . . . ?
C5 C6 C7 C11 -178.7(3) . . . . ?
C6 C7 C8 C9 -1.4(6) . . . . ?
C11 C7 C8 C9 177.1(4) . . . . ?
C7 C8 C9 C4 1.0(5) . . . . ?
C7 C8 C9 C12 -177.8(4) . . . . ?
C5 C4 C9 C8 1.2(5) . . . . ?
N2 C4 C9 C8 178.9(3) . . . . ?
C5 C4 C9 C12 179.9(3) . . . . ?
N2 C4 C9 C12 -2.4(5) . . . . ?
C18 C13 C14 C15 0.5(6) . . . . ?
N1 C13 C14 C15 -177.5(3) . . . . ?
C18 C13 C14 C19 -179.2(4) . . . . ?
N1 C13 C14 C19 2.8(5) . . . . ?
C13 C14 C15 C16 -0.4(6) . . . . ?
C19 C14 C15 C16 179.3(4) . . . . ?
C14 C15 C16 C17 -0.2(6) . . . . ?
C14 C15 C16 C20 177.8(4) . . . . ?
C15 C16 C17 C18 0.7(6) . . . . ?
C20 C16 C17 C18 -177.3(4) . . . . ?
C14 C13 C18 C17 -0.1(5) . . . . ?
N1 C13 C18 C17 178.0(3) . . . . ?
C14 C13 C18 C21 -178.3(4) . . . . ?
N1 C13 C18 C21 -0.3(5) . . . . ?
C16 C17 C18 C13 -0.6(5) . . . . ?
C16 C17 C18 C21 177.8(4) . . . . ?
N3 C23 C24 N4 0.2(4) . . . . ?
C30 C25 C26 C27 -2.7(5) . . . . ?
N3 C25 C26 C27 175.8(3) . . . . ?
C30 C25 C26 C31 176.1(3) . . . . ?
N3 C25 C26 C31 -5.3(4) . . . . ?
C25 C26 C27 C28 1.0(5) . . . . ?
C31 C26 C27 C28 -177.8(3) . . . . ?
C26 C27 C28 C29 0.5(6) . . . . ?
C27 C28 C29 C30 -0.5(6) . . . . ?
C26 C25 C30 C29 2.8(5) . . . . ?
N3 C25 C30 C29 -175.8(3) . . . . ?
C26 C25 C30 C34 -178.2(3) . . . . ?
N3 C25 C30 C34 3.2(4) . . . . ?
C28 C29 C30 C25 -1.1(5) . . . . ?
C28 C29 C30 C34 179.9(3) . . . . ?
C25 C26 C31 C33 -95.2(4) . . . . ?
C27 C26 C31 C33 83.5(4) . . . . ?
C25 C26 C31 C32 138.2(4) . . . . ?
C27 C26 C31 C32 -43.1(5) . . . . ?
C25 C30 C34 C35 -96.1(4) . . . . ?
C29 C30 C34 C35 82.9(4) . . . . ?
C25 C30 C34 C36 140.0(3) . . . . ?
C29 C30 C34 C36 -41.0(5) . . . . ?
C42 C37 C38 C39 1.3(5) . . . . ?
N4 C37 C38 C39 -176.7(3) . . . . ?
C42 C37 C38 C43 -179.8(3) . . . . ?
N4 C37 C38 C43 2.2(5) . . . . ?
C37 C38 C39 C40 -0.8(6) . . . . ?
C43 C38 C39 C40 -179.7(4) . . . . ?
C38 C39 C40 C41 0.1(7) . . . . ?
C39 C40 C41 C42 0.1(7) . . . . ?
C38 C37 C42 C41 -1.1(5) . . . . ?
N4 C37 C42 C41 176.9(3) . . . . ?
C38 C37 C42 C46 -179.6(3) . . . . ?
N4 C37 C42 C46 -1.5(5) . . . . ?
C40 C41 C42 C37 0.4(6) . . . . ?
C40 C41 C42 C46 178.8(4) . . . . ?
C37 C38 C43 C44 122.2(4) . . . . ?
C39 C38 C43 C44 -59.0(5) . . . . ?
C37 C38 C43 C45 -113.2(4) . . . . ?
C39 C38 C43 C45 65.7(5) . . . . ?
C37 C42 C46 C47 -126.7(5) . . . . ?
C41 C42 C46 C47 54.9(6) . . . . ?
C37 C42 C46 C48 106.7(4) . . . . ?
C41 C42 C46 C48 -71.6(5) . . . . ?
C54 C49 C50 C51 -0.3(5) . . . . ?
B1 C49 C50 C51 -172.7(3) . . . . ?
C49 C50 C51 C52 0.4(5) . . . . ?
C49 C50 C51 C55 178.0(3) . . . . ?
C50 C51 C52 C53 0.2(5) . . . . ?
C55 C51 C52 C53 -177.5(4) . . . . ?
C51 C52 C53 C54 -0.9(5) . . . . ?
C51 C52 C53 C56 179.0(3) . . . . ?
C50 C49 C54 C53 -0.4(4) . . . . ?
B1 C49 C54 C53 171.8(3) . . . . ?
C52 C53 C54 C49 1.0(5) . . . . ?
C56 C53 C54 C49 -178.9(3) . . . . ?
C52 C51 C55 F1 -158.7(4) . . . . ?
C50 C51 C55 F1 23.6(6) . . . . ?
C52 C51 C55 F3 -36.2(6) . . . . ?
C50 C51 C55 F3 146.1(5) . . . . ?
C52 C51 C55 F2 79.2(5) . . . . ?
C50 C51 C55 F2 -98.5(5) . . . . ?
C52 C53 C56 F5' -78.7(15) . . . . ?
C54 C53 C56 F5' 101.3(14) . . . . ?
C52 C53 C56 F4 -154.2(8) . . . . ?
C54 C53 C56 F4 25.7(9) . . . . ?
C52 C53 C56 F6 75.8(8) . . . . ?
C54 C53 C56 F6 -104.3(8) . . . . ?
C52 C53 C56 F6' 56.7(9) . . . . ?
C54 C53 C56 F6' -123.4(8) . . . . ?
C52 C53 C56 F5 -39.4(5) . . . . ?
C54 C53 C56 F5 140.5(4) . . . . ?
C52 C53 C56 F4' 164.5(7) . . . . ?
C54 C53 C56 F4' -15.5(8) . . . . ?
C62 C57 C58 C59 -0.4(4) . . . . ?
B1 C57 C58 C59 172.0(3) . . . . ?
C57 C58 C59 C60 0.7(5) . . . . ?
C57 C58 C59 C63 -179.3(3) . . . . ?
C58 C59 C60 C61 -0.2(5) . . . . ?
C63 C59 C60 C61 179.9(3) . . . . ?
C59 C60 C61 C62 -0.7(6) . . . . ?
C59 C60 C61 C64 -179.0(4) . . . . ?
C60 C61 C62 C57 1.0(6) . . . . ?
C64 C61 C62 C57 179.3(4) . . . . ?
C58 C57 C62 C61 -0.4(5) . . . . ?
B1 C57 C62 C61 -172.7(3) . . . . ?
C60 C59 C63 F8 -39.4(5) . . . . ?
C58 C59 C63 F8 140.6(3) . . . . ?
C60 C59 C63 F7 -160.2(3) . . . . ?
C58 C59 C63 F7 19.8(5) . . . . ?
C60 C59 C63 F9 79.7(4) . . . . ?
C58 C59 C63 F9 -100.3(4) . . . . ?
C60 C61 C64 F10' 26.2(12) . . . . ?
C62 C61 C64 F10' -152.2(10) . . . . ?
C60 C61 C64 F11 77.0(8) . . . . ?
C62 C61 C64 F11 -101.3(7) . . . . ?
C60 C61 C64 F12 -153.4(6) . . . . ?
C62 C61 C64 F12 28.3(8) . . . . ?
C60 C61 C64 F12' -131.5(8) . . . . ?
C62 C61 C64 F12' 50.1(9) . . . . ?
C60 C61 C64 F10 -33.8(6) . . . . ?
C62 C61 C64 F10 147.9(4) . . . . ?
C60 C61 C64 F11' 130.5(6) . . . . ?
C62 C61 C64 F11' -47.9(6) . . . . ?
C70 C65 C66 C67 -0.6(4) . . . . ?
B1 C65 C66 C67 -173.4(3) . . . . ?
C65 C66 C67 C68 -0.5(5) . . . . ?
C65 C66 C67 C71 -176.9(3) . . . . ?
C66 C67 C68 C69 0.7(5) . . . . ?
C71 C67 C68 C69 177.0(3) . . . . ?
C67 C68 C69 C70 0.4(5) . . . . ?
C67 C68 C69 C72 -177.4(3) . . . . ?
C68 C69 C70 C65 -1.6(5) . . . . ?
C72 C69 C70 C65 176.2(3) . . . . ?
C66 C65 C70 C69 1.7(4) . . . . ?
B1 C65 C70 C69 174.6(3) . . . . ?
C68 C67 C71 F13 17.7(5) . . . . ?
C66 C67 C71 F13 -165.9(3) . . . . ?
C68 C67 C71 F14 142.8(3) . . . . ?
C66 C67 C71 F14 -40.8(5) . . . . ?
C68 C67 C71 F15 -101.3(4) . . . . ?
C66 C67 C71 F15 75.1(4) . . . . ?
C68 C69 C72 F16 -27.9(4) . . . . ?
C70 C69 C72 F16 154.3(3) . . . . ?
C68 C69 C72 F18 92.9(4) . . . . ?
C70 C69 C72 F18 -84.8(4) . . . . ?
C68 C69 C72 F17 -148.2(3) . . . . ?
C70 C69 C72 F17 34.0(4) . . . . ?
C78 C73 C74 C75 4.1(4) . . . . ?
B1 C73 C74 C75 -179.2(3) . . . . ?
C73 C74 C75 C76 -1.8(5) . . . . ?
C73 C74 C75 C79 179.1(3) . . . . ?
C74 C75 C76 C77 -2.0(5) . . . . ?
C79 C75 C76 C77 177.1(3) . . . . ?
C75 C76 C77 C78 3.4(5) . . . . ?
C75 C76 C77 C80 -179.5(3) . . . . ?
C76 C77 C78 C73 -1.0(5) . . . . ?
C80 C77 C78 C73 -178.2(3) . . . . ?
C74 C73 C78 C77 -2.7(4) . . . . ?
B1 C73 C78 C77 -179.6(3) . . . . ?
C76 C75 C79 F21' -121.4(14) . . . . ?
C74 C75 C79 F21' 57.7(14) . . . . ?
C76 C75 C79 F20 35.3(7) . . . . ?
C74 C75 C79 F20 -145.5(6) . . . . ?
C76 C75 C79 F19 160.6(6) . . . . ?
C74 C75 C79 F19 -20.3(7) . . . . ?
C76 C75 C79 F19' 114.2(11) . . . . ?
C74 C75 C79 F19' -66.6(11) . . . . ?
C76 C75 C79 F20' 6.3(9) . . . . ?
C74 C75 C79 F20' -174.5(8) . . . . ?
C76 C75 C79 F21 -85.5(5) . . . . ?
C74 C75 C79 F21 93.6(5) . . . . ?
C76 C77 C80 F24 153.6(3) . . . . ?
C78 C77 C80 F24 -29.2(4) . . . . ?
C76 C77 C80 F22 -85.0(4) . . . . ?
C78 C77 C80 F22 92.2(4) . . . . ?
C76 C77 C80 F23 34.0(4) . . . . ?
C78 C77 C80 F23 -148.8(3) . . . . ?
C86 C81 C82 C83 2.8(4) . . . . ?
B2 C81 C82 C83 176.1(3) . . . . ?
C81 C82 C83 C84 -0.9(5) . . . . ?
C81 C82 C83 C87 178.9(3) . . . . ?
C82 C83 C84 C85 -1.4(5) . . . . ?
C87 C83 C84 C85 178.8(3) . . . . ?
C83 C84 C85 C86 1.6(5) . . . . ?
C83 C84 C85 C88 -176.8(3) . . . . ?
C84 C85 C86 C81 0.5(5) . . . . ?
C88 C85 C86 C81 178.9(3) . . . . ?
C82 C81 C86 C85 -2.7(4) . . . . ?
B2 C81 C86 C85 -176.1(3) . . . . ?
C84 C83 C87 F26' 38.0(14) . . . . ?
C82 C83 C87 F26' -141.8(14) . . . . ?
C84 C83 C87 F25 -106.4(7) . . . . ?
C82 C83 C87 F25 73.8(7) . . . . ?
C84 C83 C87 F26 132.4(5) . . . . ?
C82 C83 C87 F26 -47.4(6) . . . . ?
C84 C83 C87 F27 15.9(6) . . . . ?
C82 C83 C87 F27 -163.9(5) . . . . ?
C84 C83 C87 F25' 168.6(18) . . . . ?
C82 C83 C87 F25' -11.1(18) . . . . ?
C84 C83 C87 F27' -80.4(11) . . . . ?
C82 C83 C87 F27' 99.8(10) . . . . ?
C84 C85 C88 F30' 121.6(11) . . . . ?
C86 C85 C88 F30' -56.8(11) . . . . ?
C84 C85 C88 F28' -4.3(9) . . . . ?
C86 C85 C88 F28' 177.3(9) . . . . ?
C84 C85 C88 F28 -31.7(6) . . . . ?
C86 C85 C88 F28 149.9(5) . . . . ?
C84 C85 C88 F29 -156.9(4) . . . . ?
C86 C85 C88 F29 24.7(5) . . . . ?
C84 C85 C88 F29' -119.5(11) . . . . ?
C86 C85 C88 F29' 62.1(12) . . . . ?
C84 C85 C88 F30 86.0(6) . . . . ?
C86 C85 C88 F30 -92.4(5) . . . . ?
C94 C89 C90 C91 -0.7(4) . . . . ?
B2 C89 C90 C91 -174.2(2) . . . . ?
C89 C90 C91 C92 0.6(4) . . . . ?
C89 C90 C91 C95 -178.8(3) . . . . ?
C90 C91 C92 C93 -0.4(4) . . . . ?
C95 C91 C92 C93 179.0(3) . . . . ?
C91 C92 C93 C94 0.4(4) . . . . ?
C91 C92 C93 C96 180.0(3) . . . . ?
C92 C93 C94 C89 -0.5(4) . . . . ?
C96 C93 C94 C89 179.9(3) . . . . ?
C90 C89 C94 C93 0.6(4) . . . . ?
B2 C89 C94 C93 174.3(2) . . . . ?
C92 C91 C95 F33 -174.0(3) . . . . ?
C90 C91 C95 F33 5.4(4) . . . . ?
C92 C91 C95 F31 65.3(4) . . . . ?
C90 C91 C95 F31 -115.3(3) . . . . ?
C92 C91 C95 F32 -53.0(4) . . . . ?
C90 C91 C95 F32 126.4(3) . . . . ?
C92 C93 C96 F35 -177.2(3) . . . . ?
C94 C93 C96 F35 2.4(4) . . . . ?
C92 C93 C96 F36 60.7(4) . . . . ?
C94 C93 C96 F36 -119.7(4) . . . . ?
C92 C93 C96 F34 -57.6(4) . . . . ?
C94 C93 C96 F34 122.0(3) . . . . ?
C102 C97 C98 C99 2.4(4) . . . . ?
B2 C97 C98 C99 178.5(3) . . . . ?
C97 C98 C99 C100 -1.8(5) . . . . ?
C97 C98 C99 C103 178.0(3) . . . . ?
C98 C99 C100 C101 0.0(5) . . . . ?
C103 C99 C100 C101 -179.9(3) . . . . ?
C99 C100 C101 C102 1.1(5) . . . . ?
C99 C100 C101 C104 -177.1(3) . . . . ?
C100 C101 C102 C97 -0.5(5) . . . . ?
C104 C101 C102 C97 177.8(3) . . . . ?
C98 C97 C102 C101 -1.3(5) . . . . ?
B2 C97 C102 C101 -177.5(3) . . . . ?
C100 C99 C103 F37 176.7(4) . . . . ?
C98 C99 C103 F37 -3.2(5) . . . . ?
C100 C99 C103 F38 49.7(5) . . . . ?
C98 C99 C103 F38 -130.2(4) . . . . ?
C100 C99 C103 F39 -66.4(4) . . . . ?
C98 C99 C103 F39 113.8(4) . . . . ?
C100 C101 C104 F40 -11.6(6) . . . . ?
C102 C101 C104 F40 170.1(4) . . . . ?
C100 C101 C104 F42 110.4(5) . . . . ?
C102 C101 C104 F42 -67.8(5) . . . . ?
C100 C101 C104 F41 -129.6(4) . . . . ?
C102 C101 C104 F41 52.2(5) . . . . ?
C110 C105 C106 C107 -0.4(4) . . . . ?
B2 C105 C106 C107 -175.2(3) . . . . ?
C105 C106 C107 C108 -1.0(4) . . . . ?
C105 C106 C107 C111 -178.8(3) . . . . ?
C106 C107 C108 C109 1.1(4) . . . . ?
C111 C107 C108 C109 178.8(3) . . . . ?
C107 C108 C109 C110 0.2(5) . . . . ?
C107 C108 C109 C112 -177.8(3) . . . . ?
C106 C105 C110 C109 1.6(4) . . . . ?
B2 C105 C110 C109 176.3(3) . . . . ?
C108 C109 C110 C105 -1.6(5) . . . . ?
C112 C109 C110 C105 176.3(3) . . . . ?
C106 C107 C111 F45 -165.7(3) . . . . ?
C108 C107 C111 F45 16.6(4) . . . . ?
C106 C107 C111 F43 -43.5(4) . . . . ?
C108 C107 C111 F43 138.7(3) . . . . ?
C106 C107 C111 F44 74.6(3) . . . . ?
C108 C107 C111 F44 -103.2(3) . . . . ?
C108 C109 C112 F46' 21.3(15) . . . . ?
C110 C109 C112 F46' -156.7(14) . . . . ?
C108 C109 C112 F48' 157.6(15) . . . . ?
C110 C109 C112 F48' -20.4(16) . . . . ?
C108 C109 C112 F48 -169.3(4) . . . . ?
C110 C109 C112 F48 12.8(5) . . . . ?
C108 C109 C112 F46 68.6(4) . . . . ?
C110 C109 C112 F46 -109.4(4) . . . . ?
C108 C109 C112 F47 -49.0(5) . . . . ?
C110 C109 C112 F47 133.0(4) . . . . ?
C108 C109 C112 F47' -89.2(14) . . . . ?
C110 C109 C112 F47' 92.8(14) . . . . ?
C66 C65 B1 C57 92.8(3) . . . . ?
C70 C65 B1 C57 -79.6(3) . . . . ?
C66 C65 B1 C73 -146.0(3) . . . . ?
C70 C65 B1 C73 41.6(4) . . . . ?
C66 C65 B1 C49 -29.0(4) . . . . ?
C70 C65 B1 C49 158.5(3) . . . . ?
C62 C57 B1 C65 98.2(3) . . . . ?
C58 C57 B1 C65 -73.5(3) . . . . ?
C62 C57 B1 C73 -23.7(4) . . . . ?
C58 C57 B1 C73 164.5(3) . . . . ?
C62 C57 B1 C49 -140.3(3) . . . . ?
C58 C57 B1 C49 48.0(4) . . . . ?
C74 C73 B1 C65 18.1(4) . . . . ?
C78 C73 B1 C65 -165.2(3) . . . . ?
C74 C73 B1 C57 134.2(3) . . . . ?
C78 C73 B1 C57 -49.1(4) . . . . ?
C74 C73 B1 C49 -103.8(3) . . . . ?
C78 C73 B1 C49 72.8(3) . . . . ?
C50 C49 B1 C65 -42.0(4) . . . . ?
C54 C49 B1 C65 146.1(3) . . . . ?
C50 C49 B1 C57 -158.2(3) . . . . ?
C54 C49 B1 C57 29.9(4) . . . . ?
C50 C49 B1 C73 80.5(3) . . . . ?
C54 C49 B1 C73 -91.4(3) . . . . ?
C82 C81 B2 C105 29.3(4) . . . . ?
C86 C81 B2 C105 -157.9(3) . . . . ?
C82 C81 B2 C97 -89.8(3) . . . . ?
C86 C81 B2 C97 83.0(3) . . . . ?
C82 C81 B2 C89 147.6(3) . . . . ?
C86 C81 B2 C89 -39.5(4) . . . . ?
C106 C105 B2 C81 -151.5(3) . . . . ?
C110 C105 B2 C81 34.1(4) . . . . ?
C106 C105 B2 C97 -36.3(4) . . . . ?
C110 C105 B2 C97 149.3(3) . . . . ?
C106 C105 B2 C89 85.7(3) . . . . ?
C110 C105 B2 C89 -88.8(3) . . . . ?
C98 C97 B2 C81 -99.3(3) . . . . ?
C102 C97 B2 C81 76.6(3) . . . . ?
C98 C97 B2 C105 139.0(3) . . . . ?
C102 C97 B2 C105 -45.0(4) . . . . ?
C98 C97 B2 C89 22.6(4) . . . . ?
C102 C97 B2 C89 -161.5(3) . . . . ?
C90 C89 B2 C81 -29.4(4) . . . . ?
C94 C89 B2 C81 157.3(2) . . . . ?
C90 C89 B2 C105 94.3(3) . . . . ?
C94 C89 B2 C105 -79.0(3) . . . . ?
C90 C89 B2 C97 -146.1(3) . . . . ?
C94 C89 B2 C97 40.7(4) . . . . ?
N2 C1 N1 C2 1.7(4) . . . . ?
P1 C1 N1 C2 -176.6(3) . . . . ?
P1' C1 N1 C2 154.0(4) . . . . ?
N2 C1 N1 C13 178.5(3) . . . . ?
P1 C1 N1 C13 0.3(6) . . . . ?
P1' C1 N1 C13 -29.2(5) . . . . ?
C3 C2 N1 C1 -1.5(5) . . . . ?
C3 C2 N1 C13 -178.5(3) . . . . ?
C14 C13 N1 C1 -91.0(4) . . . . ?
C18 C13 N1 C1 90.8(4) . . . . ?
C14 C13 N1 C2 85.4(5) . . . . ?
C18 C13 N1 C2 -92.8(4) . . . . ?
N1 C1 N2 C3 -1.2(4) . . . . ?
P1 C1 N2 C3 177.4(3) . . . . ?
P1' C1 N2 C3 -148.9(4) . . . . ?
N1 C1 N2 C4 179.4(3) . . . . ?
P1 C1 N2 C4 -2.0(5) . . . . ?
P1' C1 N2 C4 31.7(6) . . . . ?
C2 C3 N2 C1 0.3(5) . . . . ?
C2 C3 N2 C4 179.7(3) . . . . ?
C5 C4 N2 C1 -84.3(4) . . . . ?
C9 C4 N2 C1 97.9(4) . . . . ?
C5 C4 N2 C3 96.4(4) . . . . ?
C9 C4 N2 C3 -81.5(4) . . . . ?
N4 C22 N3 C23 -0.1(3) . . . . ?
P2 C22 N3 C23 -174.9(3) . . . . ?
P2' C22 N3 C23 -150.4(4) . . . . ?
N4 C22 N3 C25 178.4(3) . . . . ?
P2 C22 N3 C25 3.7(5) . . . . ?
P2' C22 N3 C25 28.2(5) . . . . ?
C24 C23 N3 C22 -0.1(4) . . . . ?
C24 C23 N3 C25 -178.6(3) . . . . ?
C26 C25 N3 C22 -80.0(4) . . . . ?
C30 C25 N3 C22 98.7(4) . . . . ?
C26 C25 N3 C23 98.3(4) . . . . ?
C30 C25 N3 C23 -83.0(4) . . . . ?
N3 C22 N4 C24 0.2(3) . . . . ?
P2 C22 N4 C24 176.1(2) . . . . ?
P2' C22 N4 C24 151.2(4) . . . . ?
N3 C22 N4 C37 -179.9(3) . . . . ?
P2 C22 N4 C37 -4.0(4) . . . . ?
P2' C22 N4 C37 -28.9(5) . . . . ?
C23 C24 N4 C22 -0.2(4) . . . . ?
C23 C24 N4 C37 179.9(3) . . . . ?
C38 C37 N4 C22 -88.9(4) . . . . ?
C42 C37 N4 C22 92.9(4) . . . . ?
C38 C37 N4 C24 90.9(4) . . . . ?
C42 C37 N4 C24 -87.3(4) . . . . ?
F48' C112 F46 F46' 148(2) . . . . ?
F48 C112 F46 F46' 131.6(16) . . . . ?
F47 C112 F46 F46' 19.7(16) . . . . ?
F47' C112 F46 F46' 45(2) . . . . ?
C109 C112 F46 F46' -102.4(16) . . . . ?
F46' C112 F46 F48' -148(2) . . . . ?
F48 C112 F46 F48' -16.0(13) . . . . ?
F47 C112 F46 F48' -127.9(13) . . . . ?
F47' C112 F46 F48' -102(2) . . . . ?
C109 C112 F46 F48' 110.0(13) . . . . ?
F46' C112 F47 F47' 167(2) . . . . ?
F48' C112 F47 F47' 61(2) . . . . ?
F48 C112 F47 F47' 38.8(19) . . . . ?
F46 C112 F47 F47' 152.1(19) . . . . ?
C109 C112 F47 F47' -86.5(19) . . . . ?
F48' C112 F47 F46' -105.7(19) . . . . ?
F48 C112 F47 F46' -128.3(13) . . . . ?
F46 C112 F47 F46' -15.0(12) . . . . ?
F47' C112 F47 F46' -167(2) . . . . ?
C109 C112 F47 F46' 106.5(13) . . . . ?
F46' C112 F48 F48' 75(3) . . . . ?
F46 C112 F48 F48' 32(3) . . . . ?
F47 C112 F48 F48' 144(3) . . . . ?
F47' C112 F48 F48' 168(3) . . . . ?
C109 C112 F48 F48' -92(3) . . . . ?
F46' C112 F48 F47' -92.5(18) . . . . ?
F48' C112 F48 F47' -168(3) . . . . ?
F46 C112 F48 F47' -135.4(13) . . . . ?
F47 C112 F48 F47' -23.9(13) . . . . ?
C109 C112 F48 F47' 100.2(13) . . . . ?
F48' F46 F46' C112 24.1(15) . . . . ?
C112 F46 F46' F47 -24.3(19) . . . . ?
F48' F46 F46' F47 0(3) . . . . ?
F48' C112 F46' F46 -37(2) . . . . ?
F48 C112 F46' F46 -70.5(19) . . . . ?
F47 C112 F46' F46 -158.7(17) . . . . ?
F47' C112 F46' F46 -150.5(15) . . . . ?
C109 C112 F46' F46 96.8(13) . . . . ?
F48' C112 F46' F47 122.0(16) . . . . ?
F48 C112 F46' F47 88.3(13) . . . . ?
F46 C112 F46' F47 158.7(17) . . . . ?
F47' C112 F46' F47 8.2(14) . . . . ?
C109 C112 F46' F47 -104.5(7) . . . . ?
F47' F47 F46' F46 11(4) . . . . ?
C112 F47 F46' F46 27(2) . . . . ?
F47' F47 F46' C112 -16(3) . . . . ?
F46' F47 F47' C112 14(2) . . . . ?
C112 F47 F47' F48 -30.1(12) . . . . ?
F46' F47 F47' F48 -16(3) . . . . ?
F46' C112 F47' F47 -12(2) . . . . ?
F48' C112 F47' F47 -134.9(18) . . . . ?
F48 C112 F47' F47 -141.3(18) . . . . ?
F46 C112 F47' F47 -42(3) . . . . ?
C109 C112 F47' F47 107.1(15) . . . . ?
F46' C112 F47' F48 129.5(12) . . . . ?
F48' C112 F47' F48 6.4(15) . . . . ?
F46 C112 F47' F48 99.6(15) . . . . ?
F47 C112 F47' F48 141.3(18) . . . . ?
C109 C112 F47' F48 -111.6(5) . . . . ?
F48' F48 F47' F47 23(4) . . . . ?
C112 F48 F47' F47 36.6(17) . . . . ?
F48' F48 F47' C112 -14(3) . . . . ?
F47' F48 F48' C112 12(3) . . . . ?
C112 F48 F48' F46 -29(2) . . . . ?
F47' F48 F48' F46 -17(5) . . . . ?
F46' C112 F48' F48 -124(2) . . . . ?
F46 C112 F48' F48 -149(2) . . . . ?
F47 C112 F48' F48 -47(3) . . . . ?
F47' C112 F48' F48 -12(3) . . . . ?
C109 C112 F48' F48 101(2) . . . . ?
F46' C112 F48' F46 24.6(15) . . . . ?
F48 C112 F48' F46 149(2) . . . . ?
F47 C112 F48' F46 102.2(11) . . . . ?
F47' C112 F48' F46 136.7(13) . . . . ?
C109 C112 F48' F46 -109.8(6) . . . . ?
F46' F46 F48' F48 8(4) . . . . ?
C112 F46 F48' F48 38(3) . . . . ?
F46' F46 F48' C112 -29.8(19) . . . . ?
N2 C1 P1 P2 -172.4(2) . . . . ?
N1 C1 P1 P2 5.6(4) . . . . ?
N4 C22 P2 P1 170.1(2) . . . . ?
N3 C22 P2 P1 -15.5(3) . . . . ?
N2 C1 P1' P2' -141.2(4) . . . . ?
N1 C1 P1' P2' 73.8(4) . . . . ?

_refine_diff_density_max         0.851
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.062



#=============================================================================
# end of cif data for "ad2ck" ([6][BArF]2)
#=============================================================================
#=============================================================================
# end of combined cif file
#=============================================================================
####################################################################### 
# 
# 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_ad022db
_database_code_depnum_ccdc_archive 'CCDC 1572774'
_audit_update_record             
;
2017-09-05 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_ad022db             
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
 calculated from the _atom_site* data lies outside
 the range 0.90 <> 1.10
RESPONSE:  Three dichloromethane
 molecules as well as one agglomeration of residual density of unknown 
 composition have been treated with the program SQUEEZE (part of the PLATON 
 suite: A. L. Spek, University of Utrecht, Netherlands) to remove mathematically 
 the residual electron density. The empirical formula and derived parameters are 
 based on three dichloromethane molecules per asymmetric unit. Since an
 unidentified moiety has been removed this structure is only confirming the 
 connectivity of the NHC diphosphorus adduct.  
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H60 N4 P2, 2(Cl4 Ga)'
_chemical_formula_sum            'C51 H66 Cl14 Ga2 N4 P2'
_chemical_formula_weight         1432.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   21.5044(8)
_cell_length_b                   13.6283(4)
_cell_length_c                   46.5389(14)
_cell_angle_alpha                90
_cell_angle_beta                 95.086(4)
_cell_angle_gamma                90
_cell_volume                     13585.4(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    31310
_cell_measurement_theta_min      3.8030
_cell_measurement_theta_max      74.8250

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_F_000             5840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    6.761
_shelx_estimated_absorpt_T_min   0.376
_shelx_estimated_absorpt_T_max   0.581
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 30 0.0396
7 -8 0 0.0823
14 0 -1 0.0462
-14 0 2 0.0383
2 9 -7 0.0525
-2 -9 6 0.1038
0 -1 -30 0.0466
-9 -1 -20 0.0431
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0089 -0.0222 30.0032 0.8848 -0.1211 0.4436
7.0362 -8.0022 -0.0715 -0.4044 -0.5987 0.7431
14.0124 0.0114 -1.0234 -0.0103 -0.9974 -0.1264
-14.0121 -0.0121 2.0235 0.0398 0.9934 0.1412
1.9661 9.0152 -6.9368 0.2621 -0.0046 -1.0182
-1.9664 -9.0144 5.9367 -0.2916 0.0086 1.0034
-0.0052 -0.9787 -30.0107 -0.9365 0.1089 -0.3437
-9.0103 -0.9930 -19.9946 -0.6540 0.7123 -0.1241
_exptl_absorpt_correction_T_min  0.64316
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.579
_oxdiff_exptl_absorpt_empirical_full_max 1.926
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_reflns_number            147972
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_theta_min         3.814
_diffrn_reflns_theta_max         76.497
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14127
_reflns_number_gt                11828
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
;
 SHELXT-2014/7 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_molecular_graphics    ?
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;


_refine_special_details          
;All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Not-disordered methyl groups were treated as a rigid bodies and allowed to 
 rotate about the E-CH3 bond.

 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 > 2sigma(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.
 
 The structure suffers from severe disorder. The two gallium tetrachloride 
 (GaCl4) anions were refined over two positions. Three dichloromethane
 molecules as well as one agglomeration of residual density of unknown 
 composition have been treated with the program SQUEEZE (part of the PLATON 
 suite: A. L. Spek, University of Utrecht, Netherlands) to remove mathematically 
 the residual electron density. The empirical formula and derived parameters are 
 based on three dichloromethane molecules per asymmetric unit. Since an
 unidentified moiety has been removed this structure is only confirming the 
 connectivity of the NHC diphosphorus adduct.,SQUEEZE
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0427P)²+35.6022P] 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         14127
_refine_ls_number_parameters     633
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1226
_refine_ls_wR_factor_gt          0.1167
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_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
C1 C 0.22822(13) 0.6206(2) 0.13364(6) 0.0325(6) Uani 1 1 d . . . . .
C2 C 0.18137(15) 0.7647(2) 0.12557(6) 0.0390(7) Uani 1 1 d . . . . .
H2 H 0.1535 0.8136 0.1176 0.047 Uiso 1 1 calc R U . . .
C3 C 0.22764(15) 0.7777(2) 0.14707(6) 0.0388(6) Uani 1 1 d . . . . .
H3 H 0.2383 0.8373 0.1569 0.047 Uiso 1 1 calc R U . . .
C4 C 0.22745(13) 0.3027(2) 0.10868(6) 0.0325(6) Uani 1 1 d . . . . .
C5 C 0.22533(15) 0.1440(2) 0.09605(7) 0.0404(7) Uani 1 1 d . . . . .
H5 H 0.2149 0.0848 0.0860 0.048 Uiso 1 1 calc R U . . .
C6 C 0.26584(16) 0.1542(2) 0.11989(7) 0.0457(8) Uani 1 1 d . . . . .
H6 H 0.2894 0.1031 0.1296 0.055 Uiso 1 1 calc R U . . .
C11 C 0.13926(15) 0.6220(2) 0.09568(7) 0.0400(7) Uani 1 1 d . . . . .
C12 C 0.08717(16) 0.5746(2) 0.10507(8) 0.0490(8) Uani 1 1 d . . . . .
C13 C 0.04976(18) 0.5241(3) 0.08386(10) 0.0602(10) Uani 1 1 d . . . . .
H13 H 0.0137 0.4904 0.0890 0.072 Uiso 1 1 calc R U . . .
C14 C 0.0641(2) 0.5221(3) 0.05567(10) 0.0685(13) Uani 1 1 d . . . . .
H14 H 0.0380 0.4868 0.0417 0.082 Uiso 1 1 calc R U . . .
C15 C 0.1148(2) 0.5697(3) 0.04744(8) 0.0625(11) Uani 1 1 d . . . . .
H15 H 0.1237 0.5667 0.0278 0.075 Uiso 1 1 calc R U . . .
C16 C 0.15496(19) 0.6236(2) 0.06721(7) 0.0500(9) Uani 1 1 d . . . . .
C21 C 0.30651(15) 0.6685(2) 0.17348(7) 0.0421(7) Uani 1 1 d . . . . .
C22 C 0.29071(17) 0.6454(3) 0.20129(7) 0.0540(9) Uani 1 1 d . . . . .
C23 C 0.3403(2) 0.6255(4) 0.22179(9) 0.0773(14) Uani 1 1 d . . . . .
H23 H 0.3322 0.6094 0.2410 0.093 Uiso 1 1 calc R U . . .
C24 C 0.4012(2) 0.6290(4) 0.21455(10) 0.0823(15) Uani 1 1 d . . . . .
H24 H 0.4343 0.6154 0.2289 0.099 Uiso 1 1 calc R U . . .
C25 C 0.41496(18) 0.6519(4) 0.18684(10) 0.0682(11) Uani 1 1 d . . . . .
H25 H 0.4572 0.6537 0.1824 0.082 Uiso 1 1 calc R U . . .
C26 C 0.36738(16) 0.6723(3) 0.16530(8) 0.0490(8) Uani 1 1 d . . . . .
C31 C 0.15771(13) 0.25782(19) 0.06481(6) 0.0319(6) Uani 1 1 d . . . . .
C32 C 0.09476(14) 0.2452(2) 0.06810(7) 0.0384(6) Uani 1 1 d . . . . .
C33 C 0.05320(15) 0.2634(2) 0.04394(7) 0.0432(7) Uani 1 1 d . . . . .
H33 H 0.0097 0.2546 0.0453 0.052 Uiso 1 1 calc R U . . .
C34 C 0.07372(16) 0.2941(2) 0.01787(7) 0.0448(7) Uani 1 1 d . . . . .
C35 C 0.13709(15) 0.3064(2) 0.01601(6) 0.0386(6) Uani 1 1 d . . . . .
H35 H 0.1512 0.3274 -0.0018 0.046 Uiso 1 1 calc R U . . .
C36 C 0.18087(14) 0.2890(2) 0.03925(6) 0.0343(6) Uani 1 1 d . . . . .
C37 C 0.07161(16) 0.2165(3) 0.09657(8) 0.0509(8) Uani 1 1 d . . . . .
H37A H 0.0930 0.1566 0.1037 0.076 Uiso 1 1 calc R U . . .
H37B H 0.0265 0.2046 0.0939 0.076 Uiso 1 1 calc R U . . .
H37C H 0.0803 0.2696 0.1106 0.076 Uiso 1 1 calc R U . . .
C38 C 0.02700(18) 0.3158(3) -0.00755(8) 0.0619(10) Uani 1 1 d . . . . .
H38A H 0.0448 0.2975 -0.0255 0.093 Uiso 1 1 calc R U . . .
H38B H 0.0171 0.3860 -0.0079 0.093 Uiso 1 1 calc R U . . .
H38C H -0.0112 0.2779 -0.0057 0.093 Uiso 1 1 calc R U . . .
C39 C 0.24927(14) 0.3044(2) 0.03724(6) 0.0391(6) Uani 1 1 d . . . . .
H39A H 0.2565 0.3227 0.0174 0.059 Uiso 1 1 calc R U . . .
H39B H 0.2718 0.2437 0.0425 0.059 Uiso 1 1 calc R U . . .
H39C H 0.2642 0.3570 0.0505 0.059 Uiso 1 1 calc R U . . .
C41 C 0.30486(16) 0.2910(2) 0.15226(7) 0.0431(7) Uani 1 1 d . . . . .
C42 C 0.27851(19) 0.2937(3) 0.17872(7) 0.0532(9) Uani 1 1 d . . . . .
C43 C 0.3176(2) 0.3292(3) 0.20227(8) 0.0650(11) Uani 1 1 d . . . . .
H43 H 0.3015 0.3340 0.2206 0.078 Uiso 1 1 calc R U . . .
C44 C 0.3788(2) 0.3574(3) 0.19974(9) 0.0696(12) Uani 1 1 d . . . . .
C45 C 0.40168(18) 0.3542(3) 0.17266(9) 0.0593(10) Uani 1 1 d . . . . .
H45 H 0.4434 0.3743 0.1708 0.071 Uiso 1 1 calc R U . . .
C46 C 0.36481(16) 0.3220(2) 0.14824(8) 0.0482(8) Uani 1 1 d . . . . .
C47 C 0.2132(2) 0.2605(3) 0.18160(8) 0.0648(11) Uani 1 1 d . . . . .
H47A H 0.1842 0.2992 0.1687 0.097 Uiso 1 1 calc R U . . .
H47B H 0.2032 0.2694 0.2016 0.097 Uiso 1 1 calc R U . . .
H47C H 0.2092 0.1909 0.1764 0.097 Uiso 1 1 calc R U . . .
C48 C 0.4210(3) 0.3859(4) 0.22635(11) 0.0997(19) Uani 1 1 d . . . . .
H48A H 0.3973 0.4248 0.2393 0.150 Uiso 1 1 calc R U . . .
H48B H 0.4562 0.4247 0.2205 0.150 Uiso 1 1 calc R U . . .
H48C H 0.4369 0.3264 0.2363 0.150 Uiso 1 1 calc R U . . .
C49 C 0.38912(17) 0.3221(3) 0.11896(9) 0.0577(9) Uani 1 1 d . . . . .
H49A H 0.4316 0.3487 0.1205 0.087 Uiso 1 1 calc R U . . .
H49B H 0.3621 0.3629 0.1058 0.087 Uiso 1 1 calc R U . . .
H49C H 0.3895 0.2549 0.1115 0.087 Uiso 1 1 calc R U . . .
C121 C 0.07036(17) 0.5788(3) 0.13592(9) 0.0551(9) Uani 1 1 d . . . . .
H121 H 0.1074 0.6052 0.1480 0.066 Uiso 1 1 calc R U . . .
C122 C 0.0547(2) 0.4791(3) 0.14828(12) 0.0837(15) Uani 1 1 d . . . . .
H12A H 0.0184 0.4513 0.1369 0.126 Uiso 1 1 calc R U . . .
H12B H 0.0453 0.4870 0.1684 0.126 Uiso 1 1 calc R U . . .
H12C H 0.0905 0.4350 0.1475 0.126 Uiso 1 1 calc R U . . .
C123 C 0.0161(2) 0.6510(4) 0.13841(11) 0.0779(13) Uani 1 1 d . . . . .
H12D H 0.0262 0.7141 0.1299 0.117 Uiso 1 1 calc R U . . .
H12E H 0.0095 0.6605 0.1588 0.117 Uiso 1 1 calc R U . . .
H12F H -0.0220 0.6244 0.1282 0.117 Uiso 1 1 calc R U . . .
C161 C 0.2104(2) 0.6793(3) 0.05788(7) 0.0595(10) Uani 1 1 d . . . . .
H161 H 0.2259 0.7225 0.0743 0.071 Uiso 1 1 calc R U . . .
C162 C 0.2643(3) 0.6125(4) 0.05140(13) 0.0956(18) Uani 1 1 d . . . . .
H16A H 0.2790 0.5761 0.0689 0.143 Uiso 1 1 calc R U . . .
H16B H 0.2985 0.6524 0.0451 0.143 Uiso 1 1 calc R U . . .
H16C H 0.2500 0.5662 0.0361 0.143 Uiso 1 1 calc R U . . .
C163 C 0.1929(3) 0.7459(3) 0.03199(10) 0.0929(17) Uani 1 1 d . . . . .
H16D H 0.1774 0.7059 0.0154 0.139 Uiso 1 1 calc R U . . .
H16E H 0.2298 0.7827 0.0273 0.139 Uiso 1 1 calc R U . . .
H16F H 0.1603 0.7919 0.0367 0.139 Uiso 1 1 calc R U . . .
C221 C 0.22347(18) 0.6393(3) 0.20890(7) 0.0602(10) Uani 1 1 d . . . . .
H221 H 0.1964 0.6704 0.1929 0.072 Uiso 1 1 calc R U . . .
C222 C 0.2022(2) 0.5340(4) 0.21171(9) 0.0767(13) Uani 1 1 d . . . . .
H22A H 0.2047 0.4999 0.1933 0.115 Uiso 1 1 calc R U . . .
H22B H 0.1590 0.5331 0.2168 0.115 Uiso 1 1 calc R U . . .
H22C H 0.2292 0.5010 0.2268 0.115 Uiso 1 1 calc R U . . .
C223 C 0.2141(2) 0.6952(3) 0.23650(8) 0.0647(11) Uani 1 1 d . . . . .
H22D H 0.1696 0.6964 0.2395 0.097 Uiso 1 1 calc R U . . .
H22E H 0.2293 0.7626 0.2349 0.097 Uiso 1 1 calc R U . . .
H22F H 0.2374 0.6628 0.2529 0.097 Uiso 1 1 calc R U . . .
C261 C 0.38291(16) 0.6970(3) 0.13506(8) 0.0515(8) Uani 1 1 d . . . . .
H261 H 0.3432 0.7149 0.1234 0.062 Uiso 1 1 calc R U . . .
C262 C 0.4111(2) 0.6084(3) 0.12068(10) 0.0660(11) Uani 1 1 d . . . . .
H26A H 0.4510 0.5910 0.1313 0.099 Uiso 1 1 calc R U . . .
H26B H 0.4180 0.6248 0.1007 0.099 Uiso 1 1 calc R U . . .
H26C H 0.3824 0.5526 0.1209 0.099 Uiso 1 1 calc R U . . .
C263 C 0.4272(2) 0.7849(3) 0.13497(11) 0.0715(12) Uani 1 1 d . . . . .
H26D H 0.4666 0.7689 0.1462 0.107 Uiso 1 1 calc R U . . .
H26E H 0.4080 0.8418 0.1435 0.107 Uiso 1 1 calc R U . . .
H26F H 0.4354 0.8002 0.1151 0.107 Uiso 1 1 calc R U . . .
N1 N 0.18224(12) 0.66784(17) 0.11746(5) 0.0350(5) Uani 1 1 d . . . . .
N2 N 0.25579(11) 0.68869(18) 0.15179(5) 0.0340(5) Uani 1 1 d . . . . .
N3 N 0.20227(11) 0.23632(17) 0.08925(5) 0.0330(5) Uani 1 1 d . . . . .
N4 N 0.26676(12) 0.25173(17) 0.12761(5) 0.0376(5) Uani 1 1 d . . . . .
P1 P 0.25555(4) 0.49428(6) 0.13713(2) 0.03764(17) Uani 1 1 d . . . . .
P2 P 0.20160(4) 0.42906(6) 0.10411(2) 0.04037(18) Uani 1 1 d . . . . .
Cl1 Cl 0.29418(13) 0.91338(11) 0.09627(3) 0.0569(4) Uani 0.912(5) 1 d D . P A 1
Cl2 Cl 0.39359(8) 0.86735(15) 0.04063(3) 0.0781(6) Uani 0.912(5) 1 d D . P A 1
Cl3 Cl 0.25772(9) 1.01753(13) 0.02755(4) 0.0483(3) Uani 0.912(5) 1 d D . P A 1
Cl4 Cl 0.38690(5) 1.10597(14) 0.07114(2) 0.0537(4) Uani 0.912(5) 1 d D . P A 1
Ga1 Ga 0.33409(4) 0.97455(11) 0.05877(2) 0.04040(19) Uani 0.912(5) 1 d D . P A
1
Cl1' Cl 0.2755(6) 0.9011(13) 0.0941(3) 0.043(4) Uiso 0.088(5) 1 d D . P A 2
Cl2' Cl 0.3763(7) 0.8174(13) 0.0436(3) 0.073(4) Uiso 0.088(5) 1 d D . P A 2
Cl3' Cl 0.2693(8) 1.0052(14) 0.0238(4) 0.052(6) Uiso 0.088(5) 1 d D . P A 2
Cl4' Cl 0.3941(6) 1.0590(13) 0.0760(3) 0.058(4) Uiso 0.088(5) 1 d D . P A 2
Ga1' Ga 0.3299(4) 0.9449(8) 0.05968(16) 0.039(2) Uiso 0.088(5) 1 d D . P A 2
Cl5 Cl 0.13830(9) 0.00313(8) 0.14193(2) 0.0730(6) Uani 0.857(3) 1 d D . P B 3
Cl6 Cl 0.08402(6) -0.17176(11) 0.19044(3) 0.0585(4) Uani 0.857(3) 1 d D . P B 3
Cl7 Cl 0.22149(5) -0.03526(8) 0.20910(3) 0.0575(4) Uani 0.857(3) 1 d D . P B 3
Cl8 Cl 0.07538(7) 0.08501(14) 0.20593(3) 0.0616(4) Uani 0.857(3) 1 d D . P B 3
Ga2 Ga 0.12752(4) -0.02991(6) 0.18702(2) 0.0417(2) Uani 0.857(3) 1 d D . P B 3
Cl5' Cl 0.0957(4) -0.0201(6) 0.13585(16) 0.069(2) Uiso 0.143(3) 1 d D . P B 4
Cl6' Cl 0.0858(9) -0.1604(14) 0.1967(4) 0.166(11) Uiso 0.143(3) 1 d D . P B 4
Cl7' Cl 0.2193(3) -0.0120(6) 0.1923(2) 0.067(2) Uiso 0.143(3) 1 d D . P B 4
Cl8' Cl 0.0816(7) 0.1133(10) 0.1988(3) 0.116(7) Uiso 0.143(3) 1 d D . P B 4
Ga2' Ga 0.1209(4) -0.0213(6) 0.18125(17) 0.076(3) Uiso 0.143(3) 1 d D . P B 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.352(4) . ?
C1 N2 1.355(4) . ?
C1 P1 1.822(3) . ?
C2 C3 1.359(4) . ?
C2 N1 1.373(4) . ?
C2 H2 0.9500 . ?
C3 N2 1.365(4) . ?
C3 H3 0.9500 . ?
C4 N4 1.357(3) . ?
C4 N3 1.358(4) . ?
C4 P2 1.816(3) . ?
C5 C6 1.356(4) . ?
C5 N3 1.379(4) . ?
C5 H5 0.9500 . ?
C6 N4 1.376(4) . ?
C6 H6 0.9500 . ?
C11 C16 1.396(5) . ?
C11 C12 1.396(5) . ?
C11 N1 1.451(4) . ?
C12 C13 1.399(5) . ?
C12 C121 1.512(5) . ?
C13 C14 1.375(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.353(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.410(5) . ?
C15 H15 0.9500 . ?
C16 C161 1.509(6) . ?
C21 C26 1.396(5) . ?
C21 C22 1.403(5) . ?
C21 N2 1.445(4) . ?
C22 C23 1.393(5) . ?
C22 C221 1.521(5) . ?
C23 C24 1.382(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(5) . ?
C25 H25 0.9500 . ?
C26 C261 1.513(5) . ?
C31 C32 1.386(4) . ?
C31 C36 1.396(4) . ?
C31 N3 1.451(3) . ?
C32 C33 1.395(4) . ?
C32 C37 1.508(4) . ?
C33 C34 1.392(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(5) . ?
C34 C38 1.512(4) . ?
C35 C36 1.390(4) . ?
C35 H35 0.9500 . ?
C36 C39 1.497(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C41 C46 1.385(5) . ?
C41 C42 1.401(5) . ?
C41 N4 1.451(4) . ?
C42 C43 1.407(5) . ?
C42 C47 1.493(6) . ?
C43 C44 1.386(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.394(6) . ?
C44 C48 1.520(5) . ?
C45 C46 1.397(5) . ?
C45 H45 0.9500 . ?
C46 C49 1.502(5) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C121 C122 1.525(6) . ?
C121 C123 1.539(5) . ?
C121 H121 1.0000 . ?
C122 H12A 0.9800 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C123 H12D 0.9800 . ?
C123 H12E 0.9800 . ?
C123 H12F 0.9800 . ?
C161 C162 1.525(7) . ?
C161 C163 1.529(5) . ?
C161 H161 1.0000 . ?
C162 H16A 0.9800 . ?
C162 H16B 0.9800 . ?
C162 H16C 0.9800 . ?
C163 H16D 0.9800 . ?
C163 H16E 0.9800 . ?
C163 H16F 0.9800 . ?
C221 C222 1.515(7) . ?
C221 C223 1.522(5) . ?
C221 H221 1.0000 . ?
C222 H22A 0.9800 . ?
C222 H22B 0.9800 . ?
C222 H22C 0.9800 . ?
C223 H22D 0.9800 . ?
C223 H22E 0.9800 . ?
C223 H22F 0.9800 . ?
C261 C263 1.531(5) . ?
C261 C262 1.532(5) . ?
C261 H261 1.0000 . ?
C262 H26A 0.9800 . ?
C262 H26B 0.9800 . ?
C262 H26C 0.9800 . ?
C263 H26D 0.9800 . ?
C263 H26E 0.9800 . ?
C263 H26F 0.9800 . ?
P1 P2 2.0450(11) . ?
Cl1 Ga1 2.1775(14) . ?
Cl2 Ga1 2.1623(12) . ?
Cl3 Ga1 2.1746(12) . ?
Cl4 Ga1 2.1710(14) . ?
Cl1' Ga1' 2.150(11) . ?
Cl2' Ga1' 2.169(11) . ?
Cl3' Ga1' 2.187(12) . ?
Cl4' Ga1' 2.173(10) . ?
Cl5 Ga2 2.1782(14) . ?
Cl6 Ga2 2.1597(14) . ?
Cl7 Ga2 2.1857(14) . ?
Cl8 Ga2 2.1588(12) . ?
Cl5' Ga2' 2.134(9) . ?
Cl6' Ga2' 2.187(12) . ?
Cl7' Ga2' 2.136(9) . ?
Cl8' Ga2' 2.207(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 106.2(2) . . ?
N1 C1 P1 135.5(2) . . ?
N2 C1 P1 118.1(2) . . ?
C3 C2 N1 107.6(3) . . ?
C3 C2 H2 126.2 . . ?
N1 C2 H2 126.2 . . ?
C2 C3 N2 106.7(3) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
N4 C4 N3 106.2(2) . . ?
N4 C4 P2 136.7(2) . . ?
N3 C4 P2 117.0(2) . . ?
C6 C5 N3 106.6(3) . . ?
C6 C5 H5 126.7 . . ?
N3 C5 H5 126.7 . . ?
C5 C6 N4 107.8(3) . . ?
C5 C6 H6 126.1 . . ?
N4 C6 H6 126.1 . . ?
C16 C11 C12 124.9(3) . . ?
C16 C11 N1 117.6(3) . . ?
C12 C11 N1 117.3(3) . . ?
C11 C12 C13 115.7(4) . . ?
C11 C12 C121 123.1(3) . . ?
C13 C12 C121 121.2(4) . . ?
C14 C13 C12 121.3(4) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C15 C14 C13 121.0(4) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 121.8(4) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C11 C16 C15 115.2(4) . . ?
C11 C16 C161 123.0(3) . . ?
C15 C16 C161 121.8(3) . . ?
C26 C21 C22 124.7(3) . . ?
C26 C21 N2 118.0(3) . . ?
C22 C21 N2 117.2(3) . . ?
C23 C22 C21 116.2(4) . . ?
C23 C22 C221 121.1(3) . . ?
C21 C22 C221 122.7(3) . . ?
C24 C23 C22 120.7(4) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 121.3(4) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
C24 C25 C26 120.7(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C21 116.2(3) . . ?
C25 C26 C261 120.3(3) . . ?
C21 C26 C261 123.5(3) . . ?
C32 C31 C36 123.9(3) . . ?
C32 C31 N3 118.2(3) . . ?
C36 C31 N3 118.0(3) . . ?
C31 C32 C33 116.8(3) . . ?
C31 C32 C37 122.0(3) . . ?
C33 C32 C37 121.1(3) . . ?
C34 C33 C32 121.7(3) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C35 C34 C33 118.8(3) . . ?
C35 C34 C38 121.2(3) . . ?
C33 C34 C38 120.1(3) . . ?
C34 C35 C36 122.3(3) . . ?
C34 C35 H35 118.9 . . ?
C36 C35 H35 118.9 . . ?
C35 C36 C31 116.5(3) . . ?
C35 C36 C39 121.9(3) . . ?
C31 C36 C39 121.5(3) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C46 C41 C42 124.3(3) . . ?
C46 C41 N4 118.2(3) . . ?
C42 C41 N4 117.4(3) . . ?
C41 C42 C43 115.7(4) . . ?
C41 C42 C47 121.8(3) . . ?
C43 C42 C47 122.4(4) . . ?
C44 C43 C42 122.4(4) . . ?
C44 C43 H43 118.8 . . ?
C42 C43 H43 118.8 . . ?
C43 C44 C45 118.8(4) . . ?
C43 C44 C48 120.3(4) . . ?
C45 C44 C48 120.7(5) . . ?
C44 C45 C46 121.7(4) . . ?
C44 C45 H45 119.2 . . ?
C46 C45 H45 119.2 . . ?
C41 C46 C45 117.0(4) . . ?
C41 C46 C49 121.7(3) . . ?
C45 C46 C49 121.3(4) . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C12 C121 C122 113.8(3) . . ?
C12 C121 C123 110.0(3) . . ?
C122 C121 C123 110.3(4) . . ?
C12 C121 H121 107.5 . . ?
C122 C121 H121 107.5 . . ?
C123 C121 H121 107.5 . . ?
C121 C122 H12A 109.5 . . ?
C121 C122 H12B 109.5 . . ?
H12A C122 H12B 109.5 . . ?
C121 C122 H12C 109.5 . . ?
H12A C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C121 C123 H12D 109.5 . . ?
C121 C123 H12E 109.5 . . ?
H12D C123 H12E 109.5 . . ?
C121 C123 H12F 109.5 . . ?
H12D C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
C16 C161 C162 113.0(3) . . ?
C16 C161 C163 112.3(4) . . ?
C162 C161 C163 109.7(4) . . ?
C16 C161 H161 107.2 . . ?
C162 C161 H161 107.2 . . ?
C163 C161 H161 107.2 . . ?
C161 C162 H16A 109.5 . . ?
C161 C162 H16B 109.5 . . ?
H16A C162 H16B 109.5 . . ?
C161 C162 H16C 109.5 . . ?
H16A C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C161 C163 H16D 109.5 . . ?
C161 C163 H16E 109.5 . . ?
H16D C163 H16E 109.5 . . ?
C161 C163 H16F 109.5 . . ?
H16D C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
C222 C221 C22 111.8(4) . . ?
C222 C221 C223 109.8(3) . . ?
C22 C221 C223 111.6(3) . . ?
C222 C221 H221 107.8 . . ?
C22 C221 H221 107.8 . . ?
C223 C221 H221 107.8 . . ?
C221 C222 H22A 109.5 . . ?
C221 C222 H22B 109.5 . . ?
H22A C222 H22B 109.5 . . ?
C221 C222 H22C 109.5 . . ?
H22A C222 H22C 109.5 . . ?
H22B C222 H22C 109.5 . . ?
C221 C223 H22D 109.5 . . ?
C221 C223 H22E 109.5 . . ?
H22D C223 H22E 109.5 . . ?
C221 C223 H22F 109.5 . . ?
H22D C223 H22F 109.5 . . ?
H22E C223 H22F 109.5 . . ?
C26 C261 C263 111.4(3) . . ?
C26 C261 C262 111.1(3) . . ?
C263 C261 C262 110.2(3) . . ?
C26 C261 H261 108.0 . . ?
C263 C261 H261 108.0 . . ?
C262 C261 H261 108.0 . . ?
C261 C262 H26A 109.5 . . ?
C261 C262 H26B 109.5 . . ?
H26A C262 H26B 109.5 . . ?
C261 C262 H26C 109.5 . . ?
H26A C262 H26C 109.5 . . ?
H26B C262 H26C 109.5 . . ?
C261 C263 H26D 109.5 . . ?
C261 C263 H26E 109.5 . . ?
H26D C263 H26E 109.5 . . ?
C261 C263 H26F 109.5 . . ?
H26D C263 H26F 109.5 . . ?
H26E C263 H26F 109.5 . . ?
C1 N1 C2 109.3(2) . . ?
C1 N1 C11 125.0(2) . . ?
C2 N1 C11 125.6(2) . . ?
C1 N2 C3 110.2(2) . . ?
C1 N2 C21 124.5(3) . . ?
C3 N2 C21 125.3(2) . . ?
C4 N3 C5 110.0(2) . . ?
C4 N3 C31 125.7(2) . . ?
C5 N3 C31 124.3(2) . . ?
C4 N4 C6 109.4(2) . . ?
C4 N4 C41 126.9(2) . . ?
C6 N4 C41 123.8(2) . . ?
C1 P1 P2 100.77(9) . . ?
C4 P2 P1 100.17(10) . . ?
Cl2 Ga1 Cl4 110.31(6) . . ?
Cl2 Ga1 Cl3 111.04(8) . . ?
Cl4 Ga1 Cl3 107.54(6) . . ?
Cl2 Ga1 Cl1 110.06(7) . . ?
Cl4 Ga1 Cl1 109.71(6) . . ?
Cl3 Ga1 Cl1 108.10(8) . . ?
Cl1' Ga1' Cl2' 109.4(6) . . ?
Cl1' Ga1' Cl4' 108.0(5) . . ?
Cl2' Ga1' Cl4' 113.4(6) . . ?
Cl1' Ga1' Cl3' 110.3(8) . . ?
Cl2' Ga1' Cl3' 107.4(6) . . ?
Cl4' Ga1' Cl3' 108.4(6) . . ?
Cl8 Ga2 Cl6 112.04(8) . . ?
Cl8 Ga2 Cl5 110.27(7) . . ?
Cl6 Ga2 Cl5 109.87(7) . . ?
Cl8 Ga2 Cl7 108.93(6) . . ?
Cl6 Ga2 Cl7 108.90(6) . . ?
Cl5 Ga2 Cl7 106.67(7) . . ?
Cl5' Ga2' Cl7' 113.4(5) . . ?
Cl5' Ga2' Cl6' 105.5(6) . . ?
Cl7' Ga2' Cl6' 109.6(6) . . ?
Cl5' Ga2' Cl8' 106.8(5) . . ?
Cl7' Ga2' Cl8' 105.4(5) . . ?
Cl6' Ga2' Cl8' 116.3(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 -0.2(3) . . . . ?
N3 C5 C6 N4 0.6(4) . . . . ?
C16 C11 C12 C13 1.4(5) . . . . ?
N1 C11 C12 C13 -174.6(3) . . . . ?
C16 C11 C12 C121 -177.1(3) . . . . ?
N1 C11 C12 C121 7.0(4) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C121 C12 C13 C14 178.4(3) . . . . ?
C12 C13 C14 C15 -0.4(6) . . . . ?
C13 C14 C15 C16 -0.3(6) . . . . ?
C12 C11 C16 C15 -2.0(5) . . . . ?
N1 C11 C16 C15 173.9(3) . . . . ?
C12 C11 C16 C161 177.5(3) . . . . ?
N1 C11 C16 C161 -6.6(5) . . . . ?
C14 C15 C16 C11 1.5(5) . . . . ?
C14 C15 C16 C161 -178.0(3) . . . . ?
C26 C21 C22 C23 0.2(6) . . . . ?
N2 C21 C22 C23 179.6(4) . . . . ?
C26 C21 C22 C221 -178.2(4) . . . . ?
N2 C21 C22 C221 1.1(5) . . . . ?
C21 C22 C23 C24 0.1(7) . . . . ?
C221 C22 C23 C24 178.5(5) . . . . ?
C22 C23 C24 C25 -0.2(9) . . . . ?
C23 C24 C25 C26 0.1(8) . . . . ?
C24 C25 C26 C21 0.2(7) . . . . ?
C24 C25 C26 C261 -179.8(4) . . . . ?
C22 C21 C26 C25 -0.4(6) . . . . ?
N2 C21 C26 C25 -179.7(3) . . . . ?
C22 C21 C26 C261 179.7(4) . . . . ?
N2 C21 C26 C261 0.3(5) . . . . ?
C36 C31 C32 C33 1.3(4) . . . . ?
N3 C31 C32 C33 -178.0(3) . . . . ?
C36 C31 C32 C37 -176.7(3) . . . . ?
N3 C31 C32 C37 4.0(4) . . . . ?
C31 C32 C33 C34 -0.9(5) . . . . ?
C37 C32 C33 C34 177.2(3) . . . . ?
C32 C33 C34 C35 0.2(5) . . . . ?
C32 C33 C34 C38 -178.2(3) . . . . ?
C33 C34 C35 C36 0.1(5) . . . . ?
C38 C34 C35 C36 178.6(3) . . . . ?
C34 C35 C36 C31 0.2(4) . . . . ?
C34 C35 C36 C39 -178.7(3) . . . . ?
C32 C31 C36 C35 -1.0(4) . . . . ?
N3 C31 C36 C35 178.3(2) . . . . ?
C32 C31 C36 C39 178.0(3) . . . . ?
N3 C31 C36 C39 -2.7(4) . . . . ?
C46 C41 C42 C43 -1.2(5) . . . . ?
N4 C41 C42 C43 178.0(3) . . . . ?
C46 C41 C42 C47 179.1(3) . . . . ?
N4 C41 C42 C47 -1.7(5) . . . . ?
C41 C42 C43 C44 -1.6(6) . . . . ?
C47 C42 C43 C44 178.1(4) . . . . ?
C42 C43 C44 C45 2.6(6) . . . . ?
C42 C43 C44 C48 -174.0(4) . . . . ?
C43 C44 C45 C46 -0.9(6) . . . . ?
C48 C44 C45 C46 175.7(4) . . . . ?
C42 C41 C46 C45 2.8(5) . . . . ?
N4 C41 C46 C45 -176.4(3) . . . . ?
C42 C41 C46 C49 -176.7(3) . . . . ?
N4 C41 C46 C49 4.1(5) . . . . ?
C44 C45 C46 C41 -1.7(5) . . . . ?
C44 C45 C46 C49 177.8(4) . . . . ?
C11 C12 C121 C122 -132.7(4) . . . . ?
C13 C12 C121 C122 49.0(5) . . . . ?
C11 C12 C121 C123 102.9(4) . . . . ?
C13 C12 C121 C123 -75.4(4) . . . . ?
C11 C16 C161 C162 106.4(4) . . . . ?
C15 C16 C161 C162 -74.1(5) . . . . ?
C11 C16 C161 C163 -128.8(4) . . . . ?
C15 C16 C161 C163 50.6(5) . . . . ?
C23 C22 C221 C222 -74.2(5) . . . . ?
C21 C22 C221 C222 104.1(4) . . . . ?
C23 C22 C221 C223 49.2(6) . . . . ?
C21 C22 C221 C223 -132.4(4) . . . . ?
C25 C26 C261 C263 -56.6(5) . . . . ?
C21 C26 C261 C263 123.4(4) . . . . ?
C25 C26 C261 C262 66.7(5) . . . . ?
C21 C26 C261 C262 -113.3(4) . . . . ?
N2 C1 N1 C2 0.0(3) . . . . ?
P1 C1 N1 C2 176.2(3) . . . . ?
N2 C1 N1 C11 -178.0(3) . . . . ?
P1 C1 N1 C11 -1.8(5) . . . . ?
C3 C2 N1 C1 0.2(4) . . . . ?
C3 C2 N1 C11 178.1(3) . . . . ?
C16 C11 N1 C1 -93.4(4) . . . . ?
C12 C11 N1 C1 82.8(4) . . . . ?
C16 C11 N1 C2 88.9(4) . . . . ?
C12 C11 N1 C2 -94.8(4) . . . . ?
N1 C1 N2 C3 -0.1(3) . . . . ?
P1 C1 N2 C3 -177.1(2) . . . . ?
N1 C1 N2 C21 178.3(3) . . . . ?
P1 C1 N2 C21 1.3(4) . . . . ?
C2 C3 N2 C1 0.2(3) . . . . ?
C2 C3 N2 C21 -178.1(3) . . . . ?
C26 C21 N2 C1 86.7(4) . . . . ?
C22 C21 N2 C1 -92.6(4) . . . . ?
C26 C21 N2 C3 -95.1(4) . . . . ?
C22 C21 N2 C3 85.5(4) . . . . ?
N4 C4 N3 C5 0.4(3) . . . . ?
P2 C4 N3 C5 -178.5(2) . . . . ?
N4 C4 N3 C31 -179.6(3) . . . . ?
P2 C4 N3 C31 1.5(4) . . . . ?
C6 C5 N3 C4 -0.6(4) . . . . ?
C6 C5 N3 C31 179.3(3) . . . . ?
C32 C31 N3 C4 -95.5(3) . . . . ?
C36 C31 N3 C4 85.2(3) . . . . ?
C32 C31 N3 C5 84.5(4) . . . . ?
C36 C31 N3 C5 -94.8(3) . . . . ?
N3 C4 N4 C6 0.0(3) . . . . ?
P2 C4 N4 C6 178.6(3) . . . . ?
N3 C4 N4 C41 179.7(3) . . . . ?
P2 C4 N4 C41 -1.8(5) . . . . ?
C5 C6 N4 C4 -0.4(4) . . . . ?
C5 C6 N4 C41 179.9(3) . . . . ?
C46 C41 N4 C4 -90.5(4) . . . . ?
C42 C41 N4 C4 90.3(4) . . . . ?
C46 C41 N4 C6 89.1(4) . . . . ?
C42 C41 N4 C6 -90.1(4) . . . . ?
N1 C1 P1 P2 6.6(3) . . . . ?
N2 C1 P1 P2 -177.5(2) . . . . ?
N4 C4 P2 P1 3.7(3) . . . . ?
N3 C4 P2 P1 -177.8(2) . . . . ?

_refine_diff_density_max         0.524
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.059


