# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2018

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

data_140313-zz2
_database_code_depnum_ccdc_archive 'CCDC 1838785'
_audit_update_record             
;
2018-04-22 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_audit_creation_date             2014-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.44(C27 H20 N3 O P)'
_chemical_formula_sum            'C11 H10 N0.11 O2 P'
_chemical_formula_weight         206.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   8.7349(3)
_cell_length_b                   18.3308(5)
_cell_length_c                   14.1743(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.763(3)
_cell_angle_gamma                90.00
_cell_volume                     2261.71(12)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    3007
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5618
_cell_measurement_theta_min      3.2211
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             970
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10325
_diffrn_reflns_theta_full        29.63
_diffrn_reflns_theta_max         29.63
_diffrn_reflns_theta_min         3.23
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0081944000
_diffrn_orient_matrix_UB_12      -0.0349947000
_diffrn_orient_matrix_UB_13      -0.0211751000
_diffrn_orient_matrix_UB_21      0.0085695000
_diffrn_orient_matrix_UB_22      0.0156625000
_diffrn_orient_matrix_UB_23      -0.0450197000
_diffrn_orient_matrix_UB_31      0.0806203000
_diffrn_orient_matrix_UB_32      -0.0051954000
_diffrn_orient_matrix_UB_33      0.0068163000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4203
_reflns_number_total             5637
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5637
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0522
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1737
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
P1 P 0.13694(5) 0.26388(2) 0.39258(3) 0.03770(16) Uani 1 1 d . . .
O1 O 0.19683(16) 0.25775(8) 0.29854(9) 0.0505(3) Uani 1 1 d . . .
N2 N 0.26502(15) 0.39858(8) 0.40593(10) 0.0382(3) Uani 1 1 d . . .
N3 N 0.21112(15) 0.48532(8) 0.52330(10) 0.0399(3) Uani 1 1 d . . .
N4 N 0.10344(15) 0.36688(8) 0.52677(10) 0.0403(3) Uani 1 1 d . . .
C5 C 0.12892(17) 0.43390(9) 0.56309(12) 0.0372(4) Uani 1 1 d . . .
C6 C 0.37253(18) 0.52020(9) 0.40066(12) 0.0377(4) Uani 1 1 d . . .
C7 C 0.17408(17) 0.35376(9) 0.44838(11) 0.0363(4) Uani 1 1 d . . .
C8 C 0.27813(17) 0.46542(9) 0.44603(11) 0.0360(4) Uani 1 1 d . . .
C9 C 0.21941(19) 0.19690(9) 0.47426(12) 0.0394(4) Uani 1 1 d . . .
C10 C 0.06215(19) 0.45161(10) 0.65248(12) 0.0415(4) Uani 1 1 d . . .
C11 C 0.3862(2) 0.59094(10) 0.43630(14) 0.0478(4) Uani 1 1 d . . .
H11 H 0.3367 0.6040 0.4894 0.057 Uiso 1 1 calc . . R
C12 C -0.0692(2) 0.25721(11) 0.38741(18) 0.0558(6) Uani 1 1 d . . .
C13 C 0.4498(2) 0.50149(11) 0.32239(13) 0.0478(4) Uani 1 1 d . . .
H13 H 0.4437 0.4541 0.2990 0.057 Uiso 1 1 calc . . R
C14 C -0.0277(2) 0.40145(12) 0.69602(14) 0.0519(5) Uani 1 1 d . . .
H14 H -0.0480 0.3563 0.6678 0.062 Uiso 1 1 calc . . R
C15 C 0.5485(2) 0.62314(12) 0.31416(14) 0.0537(5) Uani 1 1 d . . .
H15 H 0.6071 0.6576 0.2852 0.064 Uiso 1 1 calc . . R
C16 C -0.0873(3) 0.41765(14) 0.78078(17) 0.0663(6) Uani 1 1 d . . .
H16 H -0.1483 0.3837 0.8090 0.080 Uiso 1 1 calc . . R
C17 C 0.2345(2) 0.20329(11) 0.57290(13) 0.0483(4) Uani 1 1 d . . .
H17 H 0.1972 0.2445 0.6016 0.058 Uiso 1 1 calc . . R
C18 C 0.4738(2) 0.64169(11) 0.39240(15) 0.0551(5) Uani 1 1 d . . .
H18 H 0.4821 0.6890 0.4161 0.066 Uiso 1 1 calc . . R
C19 C 0.0901(3) 0.51919(12) 0.69485(17) 0.0651(6) Uani 1 1 d . . .
H19 H 0.1484 0.5539 0.6662 0.078 Uiso 1 1 calc . . R
C20 C 0.5358(2) 0.55312(12) 0.27909(13) 0.0544(5) Uani 1 1 d . . .
H20 H 0.5854 0.5405 0.2259 0.065 Uiso 1 1 calc . . R
C21 C -0.3103(4) 0.2274(2) 0.4468(3) 0.1216(16) Uani 1 1 d . . .
H21 H -0.3652 0.2082 0.4945 0.146 Uiso 1 1 calc . . R
C22 C 0.3043(3) 0.14870(13) 0.62764(14) 0.0616(6) Uani 1 1 d . . .
H22 H 0.3144 0.1530 0.6932 0.074 Uiso 1 1 calc . . R
C23 C 0.2736(3) 0.13450(13) 0.43224(14) 0.0646(6) Uani 1 1 d . . .
H23 H 0.2632 0.1294 0.3667 0.078 Uiso 1 1 calc . . R
C24 C 0.3590(3) 0.08801(15) 0.58518(16) 0.0799(8) Uani 1 1 d . . .
H24 H 0.4077 0.0516 0.6223 0.096 Uiso 1 1 calc . . R
C25 C -0.0567(3) 0.48356(15) 0.82315(18) 0.0771(7) Uani 1 1 d . . .
H25 H -0.0945 0.4941 0.8810 0.092 Uiso 1 1 calc . . R
C26 C 0.3427(4) 0.08025(15) 0.48792(18) 0.0912(9) Uani 1 1 d . . .
H26 H 0.3785 0.0383 0.4600 0.109 Uiso 1 1 calc . . R
C27 C -0.1496(3) 0.28042(15) 0.3043(3) 0.0898(10) Uani 1 1 d . . .
H27 H -0.0962 0.2973 0.2545 0.108 Uiso 1 1 calc . . R
C28 C -0.1486(3) 0.23060(17) 0.4592(2) 0.0857(9) Uani 1 1 d . . .
H28 H -0.0966 0.2148 0.5154 0.103 Uiso 1 1 calc . . R
C29 C -0.3862(4) 0.2522(2) 0.3657(4) 0.1307(19) Uani 1 1 d . . .
H29 H -0.4930 0.2509 0.3590 0.157 Uiso 1 1 calc . . R
C30 C 0.0302(4) 0.53430(16) 0.7802(2) 0.0859(8) Uani 1 1 d . . .
H30 H 0.0490 0.5794 0.8088 0.103 Uiso 1 1 calc . . R
C32 C -0.3086(4) 0.2786(2) 0.2947(4) 0.1214(16) Uani 1 1 d . . .
H32 H -0.3618 0.2956 0.2395 0.146 Uiso 1 1 calc . . R


_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
P1 O1 1.4760(14) . ?
P1 C7 1.8447(17) . ?
P1 C9 1.7968(18) . ?
P1 C12 1.800(2) . ?
N2 C7 1.322(2) . ?
N2 C8 1.351(2) . ?
N3 C5 1.338(2) . ?
N3 C8 1.335(2) . ?
N4 C5 1.343(2) . ?
N4 C7 1.337(2) . ?
C5 C10 1.474(2) . ?
C6 C8 1.480(2) . ?
C6 C11 1.393(2) . ?
C6 C13 1.389(2) . ?
C9 C17 1.398(2) . ?
C9 C23 1.391(3) . ?
C10 C14 1.386(3) . ?
C10 C19 1.389(3) . ?
C11 C18 1.384(3) . ?
C12 C27 1.388(4) . ?
C12 C28 1.368(4) . ?
C13 C20 1.383(3) . ?
C14 C16 1.381(3) . ?
C15 C18 1.376(3) . ?
C15 C20 1.378(3) . ?
C16 C25 1.366(4) . ?
C17 C22 1.377(3) . ?
C19 C30 1.385(3) . ?
C21 C28 1.410(4) . ?
C21 C29 1.357(7) . ?
C22 C24 1.370(3) . ?
C23 C26 1.378(3) . ?
C24 C26 1.381(3) . ?
C25 C30 1.374(4) . ?
C27 C32 1.385(4) . ?
C29 C32 1.349(6) . ?

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
O1 P1 C7 113.10(8) . . ?
O1 P1 C9 112.13(8) . . ?
O1 P1 C12 112.73(10) . . ?
C9 P1 C7 106.69(8) . . ?
C9 P1 C12 109.02(10) . . ?
C12 P1 C7 102.58(8) . . ?
C7 N2 C8 113.91(14) . . ?
C8 N3 C5 116.15(15) . . ?
C7 N4 C5 114.18(15) . . ?
N3 C5 N4 124.09(16) . . ?
N3 C5 C10 118.14(15) . . ?
N4 C5 C10 117.77(15) . . ?
C11 C6 C8 120.55(16) . . ?
C13 C6 C8 120.32(16) . . ?
C13 C6 C11 119.13(16) . . ?
N2 C7 P1 116.80(12) . . ?
N2 C7 N4 127.07(15) . . ?
N4 C7 P1 116.11(12) . . ?
N2 C8 C6 117.60(15) . . ?
N3 C8 N2 124.41(15) . . ?
N3 C8 C6 117.99(15) . . ?
C17 C9 P1 125.90(14) . . ?
C23 C9 P1 114.74(14) . . ?
C23 C9 C17 119.34(17) . . ?
C14 C10 C5 121.02(17) . . ?
C14 C10 C19 118.98(18) . . ?
C19 C10 C5 120.00(17) . . ?
C18 C11 C6 119.77(18) . . ?
C27 C12 P1 116.6(2) . . ?
C28 C12 P1 124.1(2) . . ?
C28 C12 C27 119.3(2) . . ?
C20 C13 C6 120.23(18) . . ?
C16 C14 C10 120.9(2) . . ?
C18 C15 C20 119.47(19) . . ?
C25 C16 C14 119.9(2) . . ?
C22 C17 C9 120.19(18) . . ?
C15 C18 C11 120.87(19) . . ?
C30 C19 C10 119.4(2) . . ?
C15 C20 C13 120.51(19) . . ?
C29 C21 C28 120.4(4) . . ?
C24 C22 C17 119.80(19) . . ?
C26 C23 C9 119.81(19) . . ?
C22 C24 C26 120.8(2) . . ?
C16 C25 C30 119.9(2) . . ?
C23 C26 C24 120.1(2) . . ?
C32 C27 C12 120.6(4) . . ?
C12 C28 C21 119.1(3) . . ?
C32 C29 C21 120.8(3) . . ?
C25 C30 C19 120.9(3) . . ?
C29 C32 C27 119.8(4) . . ?

####################################################################### 
# 
# 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_140303-jjl
_database_code_depnum_ccdc_archive 'CCDC 1838786'
_audit_update_record             
;
2018-04-22 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C160 H112 Cl8 N20 O4 P4'
_chemical_formula_weight         2786.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   18.7793(7)
_cell_length_b                   8.0735(2)
_cell_length_c                   26.4549(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 122.492(3)
_cell_angle_gamma                90.00
_cell_volume                     3383.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9486
_exptl_absorpt_correction_T_max  0.9538
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17348
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         29.62
_reflns_number_total             8468
_reflns_number_gt                5939
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 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     
'calc w=1/[σ²(Fo²)+(0.0534P)²+1.1289P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8468
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1299
_refine_ls_wR_factor_gt          0.1144
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.32642(3) 0.62888(5) 0.58875(2) 0.03618(12) Uani 1 1 d . . .
O26 O 0.29252(10) 0.79493(16) 0.58825(6) 0.0533(4) Uani 1 1 d . . .
N5 N 0.27758(9) 0.58181(18) 0.40426(6) 0.0357(3) Uani 1 1 d . . .
N7 N 0.16077(9) 0.41935(18) 0.37831(6) 0.0359(3) Uani 1 1 d . . .
N12 N 0.36971(10) 0.66482(19) 0.50611(6) 0.0389(3) Uani 1 1 d . . .
N19 N 0.24534(9) 0.50915(18) 0.47670(6) 0.0368(3) Uani 1 1 d . . .
N22 N 0.39531(9) 0.74240(18) 0.43260(7) 0.0383(3) Uani 1 1 d . . .
C11 C 0.23048(11) 0.5067(2) 0.42096(7) 0.0332(4) Uani 1 1 d . . .
C13 C 0.31478(11) 0.5903(2) 0.51593(7) 0.0340(4) Uani 1 1 d . . .
C15 C 0.43521(12) 0.6048(2) 0.64734(8) 0.0371(4) Uani 1 1 d . . .
C20 C 0.49317(13) 0.5085(3) 0.64377(9) 0.0518(5) Uani 1 1 d . . .
H20A H 0.4772 0.4530 0.6084 0.062 Uiso 1 1 calc R . .
C27 C 0.36658(13) 0.8119(2) 0.37531(9) 0.0412(4) Uani 1 1 d . . .
C29 C 0.14532(11) 0.3626(2) 0.32228(8) 0.0376(4) Uani 1 1 d . . .
C30 C 0.09331(11) 0.3619(2) 0.38397(8) 0.0374(4) Uani 1 1 d . . .
C32 C 0.26825(12) 0.4639(2) 0.59542(7) 0.0367(4) Uani 1 1 d . . .
C36 C 0.00497(14) 0.3154(3) 0.42111(11) 0.0563(5) Uani 1 1 d . . .
H36A H -0.0068 0.3290 0.4508 0.068 Uiso 1 1 calc R . .
C38 C 0.34575(11) 0.6588(2) 0.44821(8) 0.0347(4) Uani 1 1 d . . .
C44 C 0.50814(13) 0.8693(2) 0.43810(10) 0.0457(5) Uani 1 1 d . . .
C45 C 0.19291(13) 0.3794(3) 0.29655(8) 0.0460(4) Uani 1 1 d . . .
H45A H 0.2430 0.4395 0.3154 0.055 Uiso 1 1 calc R . .
C48 C 0.57518(15) 0.4945(3) 0.69285(11) 0.0642(6) Uani 1 1 d . . .
H48A H 0.6141 0.4298 0.6902 0.077 Uiso 1 1 calc R . .
C50 C 0.48232(12) 0.7818(2) 0.47132(9) 0.0408(4) Uani 1 1 d . . .
C51 C 0.42320(18) 0.9724(3) 0.32775(12) 0.0643(6) Uani 1 1 d . . .
H51A H 0.4682 1.0246 0.3289 0.077 Uiso 1 1 calc R . .
C52 C 0.14919(17) 0.3760(3) 0.59924(12) 0.0666(7) Uani 1 1 d . . .
H52A H 0.1016 0.4018 0.6001 0.080 Uiso 1 1 calc R . .
C53 C 0.07024(12) 0.2719(2) 0.29387(9) 0.0440(4) Uani 1 1 d . . .
C55 C 0.27659(17) 0.9008(3) 0.27462(11) 0.0654(6) Uani 1 1 d . . .
H55A H 0.2234 0.9059 0.2395 0.078 Uiso 1 1 calc R . .
C59 C 0.28993(13) 0.2989(2) 0.59651(8) 0.0440(4) Uani 1 1 d . . .
H59A H 0.3375 0.2722 0.5957 0.053 Uiso 1 1 calc R . .
C60 C 0.24135(15) 0.1742(3) 0.59881(9) 0.0532(5) Uani 1 1 d . . .
H60A H 0.2561 0.0638 0.5995 0.064 Uiso 1 1 calc R . .
C61 C 0.43547(14) 0.8898(2) 0.37811(10) 0.0467(5) Uani 1 1 d . . .
C63 C 0.08783(17) 0.2139(4) 0.21325(11) 0.0728(7) Uani 1 1 d . . .
H63A H 0.0691 0.1646 0.1764 0.087 Uiso 1 1 calc R . .
C64 C 0.03714(12) 0.2734(2) 0.33215(9) 0.0441(4) Uani 1 1 d . . .
C65 C -0.03565(14) 0.2047(3) 0.32538(11) 0.0593(6) Uani 1 1 d . . .
H65A H -0.0733 0.1453 0.2910 0.071 Uiso 1 1 calc R . .
C66 C 0.28614(14) 0.8180(3) 0.32387(9) 0.0504(5) Uani 1 1 d . . .
H66A H 0.2404 0.7686 0.3225 0.060 Uiso 1 1 calc R . .
C68 C 0.53855(13) 0.7421(3) 0.53125(10) 0.0514(5) Uani 1 1 d . . .
H68A H 0.5215 0.6826 0.5530 0.062 Uiso 1 1 calc R . .
C69 C 0.07774(13) 0.3851(3) 0.42921(9) 0.0484(5) Uani 1 1 d . . .
H69A H 0.1147 0.4451 0.4636 0.058 Uiso 1 1 calc R . .
C71 C 0.62125(14) 0.7951(3) 0.55707(12) 0.0613(6) Uani 1 1 d . . .
H71A H 0.6603 0.7717 0.5972 0.074 Uiso 1 1 calc R . .
C73 C 0.46040(14) 0.6858(3) 0.70078(9) 0.0525(5) Uani 1 1 d . . .
H73A H 0.4219 0.7505 0.7039 0.063 Uiso 1 1 calc R . .
C74 C 0.59181(15) 0.9201(3) 0.46550(13) 0.0589(6) Uani 1 1 d . . .
H74A H 0.6096 0.9789 0.4440 0.071 Uiso 1 1 calc R . .
C79 C 0.64721(15) 0.8824(3) 0.52444(14) 0.0666(7) Uani 1 1 d . . .
H79A H 0.7032 0.9156 0.5431 0.080 Uiso 1 1 calc R . .
C81 C 0.17110(16) 0.2140(3) 0.60013(10) 0.0612(6) Uani 1 1 d . . .
H81A H 0.1383 0.1302 0.6016 0.073 Uiso 1 1 calc R . .
C83 C 0.19743(14) 0.5012(3) 0.59710(10) 0.0523(5) Uani 1 1 d . . .
H83A H 0.1824 0.6111 0.5968 0.063 Uiso 1 1 calc R . .
C84 C 0.54220(16) 0.6708(3) 0.74919(10) 0.0648(6) Uani 1 1 d . . .
H84A H 0.5587 0.7257 0.7848 0.078 Uiso 1 1 calc R . .
C85 C 0.59918(15) 0.5756(3) 0.74516(10) 0.0636(6) Uani 1 1 d . . .
H85A H 0.6543 0.5658 0.7780 0.076 Uiso 1 1 calc R . .
C88 C -0.05077(14) 0.2262(3) 0.37025(12) 0.0634(6) Uani 1 1 d . . .
H88A H -0.0989 0.1804 0.3664 0.076 Uiso 1 1 calc R . .
C89 C 0.04153(15) 0.1978(3) 0.23882(10) 0.0644(6) Uani 1 1 d . . .
H89A H -0.0086 0.1380 0.2196 0.077 Uiso 1 1 calc R . .
C91 C 0.16266(15) 0.3031(3) 0.24181(10) 0.0605(6) Uani 1 1 d . . .
H91A H 0.1934 0.3119 0.2237 0.073 Uiso 1 1 calc R . .
C94 C 0.3443(2) 0.9759(3) 0.27651(12) 0.0746(7) Uani 1 1 d . . .
H94A H 0.3361 1.0293 0.2426 0.090 Uiso 1 1 calc R . .
Cl1 Cl 0.13588(5) 0.87693(10) 0.39886(4) 0.0886(2) Uani 1 1 d . . .
Cl3 Cl 0.06125(6) 0.84503(13) 0.47049(5) 0.1204(4) Uani 1 1 d . . .
C47 C 0.13745(16) 0.9403(3) 0.46243(12) 0.0692(7) Uani 1 1 d . . .
H47A H 0.1927 0.9168 0.4976 0.083 Uiso 1 1 calc R . .
H47B H 0.1290 1.0593 0.4605 0.083 Uiso 1 1 calc R . .


_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
P1 O26 1.4812(13) . ?
P1 C32 1.7908(19) . ?
P1 C15 1.7923(19) . ?
P1 C13 1.8447(17) . ?
N5 C11 1.329(2) . ?
N5 C38 1.334(2) . ?
N7 C11 1.377(2) . ?
N7 C29 1.425(2) . ?
N7 C30 1.430(2) . ?
N12 C13 1.335(2) . ?
N12 C38 1.346(2) . ?
N19 C13 1.324(2) . ?
N19 C11 1.346(2) . ?
N22 C38 1.380(2) . ?
N22 C50 1.422(2) . ?
N22 C27 1.423(2) . ?
C15 C20 1.382(3) . ?
C15 C73 1.390(2) . ?
C20 C48 1.386(3) . ?
C20 H20A 0.9300 . ?
C27 C66 1.388(3) . ?
C27 C61 1.404(3) . ?
C29 C45 1.391(3) . ?
C29 C53 1.397(3) . ?
C30 C69 1.389(3) . ?
C30 C64 1.396(3) . ?
C32 C83 1.387(3) . ?
C32 C59 1.388(2) . ?
C36 C88 1.383(3) . ?
C36 C69 1.384(3) . ?
C36 H36A 0.9300 . ?
C44 C74 1.393(3) . ?
C44 C50 1.401(3) . ?
C44 C61 1.443(3) . ?
C45 C91 1.384(3) . ?
C45 H45A 0.9300 . ?
C48 C85 1.370(3) . ?
C48 H48A 0.9300 . ?
C50 C68 1.390(3) . ?
C51 C94 1.369(4) . ?
C51 C61 1.394(3) . ?
C51 H51A 0.9300 . ?
C52 C81 1.367(3) . ?
C52 C83 1.379(3) . ?
C52 H52A 0.9300 . ?
C53 C89 1.388(3) . ?
C53 C64 1.445(3) . ?
C55 C94 1.386(4) . ?
C55 C66 1.387(3) . ?
C55 H55A 0.9300 . ?
C59 C60 1.382(3) . ?
C59 H59A 0.9300 . ?
C60 C81 1.376(3) . ?
C60 H60A 0.9300 . ?
C63 C89 1.365(4) . ?
C63 C91 1.387(3) . ?
C63 H63A 0.9300 . ?
C64 C65 1.395(3) . ?
C65 C88 1.372(3) . ?
C65 H65A 0.9300 . ?
C66 H66A 0.9300 . ?
C68 C71 1.386(3) . ?
C68 H68A 0.9300 . ?
C69 H69A 0.9300 . ?
C71 C79 1.390(4) . ?
C71 H71A 0.9300 . ?
C73 C84 1.379(3) . ?
C73 H73A 0.9300 . ?
C74 C79 1.365(4) . ?
C74 H74A 0.9300 . ?
C79 H79A 0.9300 . ?
C81 H81A 0.9300 . ?
C83 H83A 0.9300 . ?
C84 C85 1.367(4) . ?
C84 H84A 0.9300 . ?
C85 H85A 0.9300 . ?
C88 H88A 0.9300 . ?
C89 H89A 0.9300 . ?
C91 H91A 0.9300 . ?
C94 H94A 0.9300 . ?
Cl1 C47 1.743(3) . ?
Cl3 C47 1.736(3) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?

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
O26 P1 C32 113.09(9) . . ?
O26 P1 C15 113.00(8) . . ?
C32 P1 C15 107.84(8) . . ?
O26 P1 C13 109.54(8) . . ?
C32 P1 C13 103.93(8) . . ?
C15 P1 C13 108.99(8) . . ?
C11 N5 C38 114.95(14) . . ?
C11 N7 C29 126.13(15) . . ?
C11 N7 C30 125.86(15) . . ?
C29 N7 C30 107.93(14) . . ?
C13 N12 C38 112.63(15) . . ?
C13 N19 C11 113.81(15) . . ?
C38 N22 C50 126.33(15) . . ?
C38 N22 C27 125.50(15) . . ?
C50 N22 C27 108.09(15) . . ?
N5 C11 N19 125.06(16) . . ?
N5 C11 N7 118.10(15) . . ?
N19 C11 N7 116.85(15) . . ?
N19 C13 N12 127.52(16) . . ?
N19 C13 P1 114.62(13) . . ?
N12 C13 P1 117.17(13) . . ?
C20 C15 C73 118.97(18) . . ?
C20 C15 P1 125.15(14) . . ?
C73 C15 P1 115.83(15) . . ?
C15 C20 C48 120.09(19) . . ?
C15 C20 H20A 120.0 . . ?
C48 C20 H20A 120.0 . . ?
C66 C27 C61 121.48(18) . . ?
C66 C27 N22 130.42(17) . . ?
C61 C27 N22 108.00(17) . . ?
C45 C29 C53 121.09(17) . . ?
C45 C29 N7 130.75(17) . . ?
C53 C29 N7 108.11(16) . . ?
C69 C30 C64 121.16(18) . . ?
C69 C30 N7 130.90(17) . . ?
C64 C30 N7 107.92(16) . . ?
C83 C32 C59 118.89(18) . . ?
C83 C32 P1 119.18(14) . . ?
C59 C32 P1 121.88(14) . . ?
C88 C36 C69 122.1(2) . . ?
C88 C36 H36A 119.0 . . ?
C69 C36 H36A 119.0 . . ?
N5 C38 N12 125.91(16) . . ?
N5 C38 N22 116.94(15) . . ?
N12 C38 N22 117.15(15) . . ?
C74 C44 C50 119.7(2) . . ?
C74 C44 C61 132.4(2) . . ?
C50 C44 C61 107.83(17) . . ?
C91 C45 C29 117.3(2) . . ?
C91 C45 H45A 121.4 . . ?
C29 C45 H45A 121.4 . . ?
C85 C48 C20 120.3(2) . . ?
C85 C48 H48A 119.9 . . ?
C20 C48 H48A 119.9 . . ?
C68 C50 C44 121.65(18) . . ?
C68 C50 N22 130.15(18) . . ?
C44 C50 N22 108.16(17) . . ?
C94 C51 C61 119.4(2) . . ?
C94 C51 H51A 120.3 . . ?
C61 C51 H51A 120.3 . . ?
C81 C52 C83 120.2(2) . . ?
C81 C52 H52A 119.9 . . ?
C83 C52 H52A 119.9 . . ?
C89 C53 C29 120.1(2) . . ?
C89 C53 C64 131.9(2) . . ?
C29 C53 C64 107.98(16) . . ?
C94 C55 C66 121.6(2) . . ?
C94 C55 H55A 119.2 . . ?
C66 C55 H55A 119.2 . . ?
C60 C59 C32 120.45(19) . . ?
C60 C59 H59A 119.8 . . ?
C32 C59 H59A 119.8 . . ?
C81 C60 C59 119.7(2) . . ?
C81 C60 H60A 120.2 . . ?
C59 C60 H60A 120.2 . . ?
C51 C61 C27 119.3(2) . . ?
C51 C61 C44 132.8(2) . . ?
C27 C61 C44 107.86(17) . . ?
C89 C63 C91 120.5(2) . . ?
C89 C63 H63A 119.7 . . ?
C91 C63 H63A 119.7 . . ?
C65 C64 C30 120.1(2) . . ?
C65 C64 C53 131.9(2) . . ?
C30 C64 C53 108.04(17) . . ?
C88 C65 C64 118.9(2) . . ?
C88 C65 H65A 120.6 . . ?
C64 C65 H65A 120.6 . . ?
C55 C66 C27 117.5(2) . . ?
C55 C66 H66A 121.3 . . ?
C27 C66 H66A 121.3 . . ?
C71 C68 C50 117.0(2) . . ?
C71 C68 H68A 121.5 . . ?
C50 C68 H68A 121.5 . . ?
C36 C69 C30 117.3(2) . . ?
C36 C69 H69A 121.3 . . ?
C30 C69 H69A 121.3 . . ?
C68 C71 C79 121.6(2) . . ?
C68 C71 H71A 119.2 . . ?
C79 C71 H71A 119.2 . . ?
C84 C73 C15 120.3(2) . . ?
C84 C73 H73A 119.9 . . ?
C15 C73 H73A 119.9 . . ?
C79 C74 C44 118.9(2) . . ?
C79 C74 H74A 120.6 . . ?
C44 C74 H74A 120.6 . . ?
C74 C79 C71 121.1(2) . . ?
C74 C79 H79A 119.5 . . ?
C71 C79 H79A 119.5 . . ?
C52 C81 C60 120.4(2) . . ?
C52 C81 H81A 119.8 . . ?
C60 C81 H81A 119.8 . . ?
C52 C83 C32 120.3(2) . . ?
C52 C83 H83A 119.9 . . ?
C32 C83 H83A 119.9 . . ?
C85 C84 C73 120.3(2) . . ?
C85 C84 H84A 119.8 . . ?
C73 C84 H84A 119.8 . . ?
C84 C85 C48 120.1(2) . . ?
C84 C85 H85A 120.0 . . ?
C48 C85 H85A 120.0 . . ?
C65 C88 C36 120.5(2) . . ?
C65 C88 H88A 119.8 . . ?
C36 C88 H88A 119.8 . . ?
C63 C89 C53 119.2(2) . . ?
C63 C89 H89A 120.4 . . ?
C53 C89 H89A 120.4 . . ?
C45 C91 C63 121.8(2) . . ?
C45 C91 H91A 119.1 . . ?
C63 C91 H91A 119.1 . . ?
C51 C94 C55 120.7(2) . . ?
C51 C94 H94A 119.7 . . ?
C55 C94 H94A 119.7 . . ?
Cl3 C47 Cl1 113.61(15) . . ?
Cl3 C47 H47A 108.8 . . ?
Cl1 C47 H47A 108.8 . . ?
Cl3 C47 H47B 108.8 . . ?
Cl1 C47 H47B 108.8 . . ?
H47A C47 H47B 107.7 . . ?

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
C38 N5 C11 N19 2.5(2) . . . . ?
C38 N5 C11 N7 -177.62(15) . . . . ?
C13 N19 C11 N5 -2.3(2) . . . . ?
C13 N19 C11 N7 177.80(14) . . . . ?
C29 N7 C11 N5 18.2(2) . . . . ?
C30 N7 C11 N5 -165.48(15) . . . . ?
C29 N7 C11 N19 -161.98(16) . . . . ?
C30 N7 C11 N19 14.4(2) . . . . ?
C11 N19 C13 N12 -0.9(3) . . . . ?
C11 N19 C13 P1 169.26(12) . . . . ?
C38 N12 C13 N19 3.4(3) . . . . ?
C38 N12 C13 P1 -166.55(12) . . . . ?
O26 P1 C13 N19 -94.27(14) . . . . ?
C32 P1 C13 N19 26.85(15) . . . . ?
C15 P1 C13 N19 141.63(13) . . . . ?
O26 P1 C13 N12 76.96(15) . . . . ?
C32 P1 C13 N12 -161.92(13) . . . . ?
C15 P1 C13 N12 -47.13(15) . . . . ?
O26 P1 C15 C20 -147.46(17) . . . . ?
C32 P1 C15 C20 86.80(18) . . . . ?
C13 P1 C15 C20 -25.43(19) . . . . ?
O26 P1 C15 C73 35.15(18) . . . . ?
C32 P1 C15 C73 -90.59(16) . . . . ?
C13 P1 C15 C73 157.18(15) . . . . ?
C73 C15 C20 C48 -0.4(3) . . . . ?
P1 C15 C20 C48 -177.70(18) . . . . ?
C38 N22 C27 C66 2.0(3) . . . . ?
C50 N22 C27 C66 -175.0(2) . . . . ?
C38 N22 C27 C61 178.41(16) . . . . ?
C50 N22 C27 C61 1.4(2) . . . . ?
C11 N7 C29 C45 -0.5(3) . . . . ?
C30 N7 C29 C45 -177.38(19) . . . . ?
C11 N7 C29 C53 176.80(16) . . . . ?
C30 N7 C29 C53 -0.10(19) . . . . ?
C11 N7 C30 C69 4.2(3) . . . . ?
C29 N7 C30 C69 -178.88(19) . . . . ?
C11 N7 C30 C64 -177.57(16) . . . . ?
C29 N7 C30 C64 -0.66(19) . . . . ?
O26 P1 C32 C83 2.47(18) . . . . ?
C15 P1 C32 C83 128.15(16) . . . . ?
C13 P1 C32 C83 -116.25(16) . . . . ?
O26 P1 C32 C59 179.78(14) . . . . ?
C15 P1 C32 C59 -54.53(17) . . . . ?
C13 P1 C32 C59 61.07(17) . . . . ?
C11 N5 C38 N12 0.5(3) . . . . ?
C11 N5 C38 N22 -178.30(15) . . . . ?
C13 N12 C38 N5 -3.1(3) . . . . ?
C13 N12 C38 N22 175.63(15) . . . . ?
C50 N22 C38 N5 -156.27(16) . . . . ?
C27 N22 C38 N5 27.3(2) . . . . ?
C50 N22 C38 N12 24.8(2) . . . . ?
C27 N22 C38 N12 -151.57(17) . . . . ?
C53 C29 C45 C91 0.1(3) . . . . ?
N7 C29 C45 C91 177.12(19) . . . . ?
C15 C20 C48 C85 0.2(4) . . . . ?
C74 C44 C50 C68 -0.8(3) . . . . ?
C61 C44 C50 C68 179.86(17) . . . . ?
C74 C44 C50 N22 -178.77(16) . . . . ?
C61 C44 C50 N22 1.9(2) . . . . ?
C38 N22 C50 C68 3.3(3) . . . . ?
C27 N22 C50 C68 -179.80(19) . . . . ?
C38 N22 C50 C44 -179.03(16) . . . . ?
C27 N22 C50 C44 -2.09(19) . . . . ?
C45 C29 C53 C89 -0.5(3) . . . . ?
N7 C29 C53 C89 -178.11(19) . . . . ?
C45 C29 C53 C64 178.39(17) . . . . ?
N7 C29 C53 C64 0.8(2) . . . . ?
C83 C32 C59 C60 0.4(3) . . . . ?
P1 C32 C59 C60 -176.89(15) . . . . ?
C32 C59 C60 C81 -0.1(3) . . . . ?
C94 C51 C61 C27 0.0(3) . . . . ?
C94 C51 C61 C44 -177.2(2) . . . . ?
C66 C27 C61 C51 -1.3(3) . . . . ?
N22 C27 C61 C51 -178.12(18) . . . . ?
C66 C27 C61 C44 176.53(17) . . . . ?
N22 C27 C61 C44 -0.3(2) . . . . ?
C74 C44 C61 C51 -2.8(4) . . . . ?
C50 C44 C61 C51 176.4(2) . . . . ?
C74 C44 C61 C27 179.8(2) . . . . ?
C50 C44 C61 C27 -1.0(2) . . . . ?
C69 C30 C64 C65 -0.8(3) . . . . ?
N7 C30 C64 C65 -179.18(17) . . . . ?
C69 C30 C64 C53 179.58(17) . . . . ?
N7 C30 C64 C53 1.2(2) . . . . ?
C89 C53 C64 C65 -2.1(4) . . . . ?
C29 C53 C64 C65 179.2(2) . . . . ?
C89 C53 C64 C30 177.5(2) . . . . ?
C29 C53 C64 C30 -1.2(2) . . . . ?
C30 C64 C65 C88 0.2(3) . . . . ?
C53 C64 C65 C88 179.7(2) . . . . ?
C94 C55 C66 C27 -0.5(4) . . . . ?
C61 C27 C66 C55 1.6(3) . . . . ?
N22 C27 C66 C55 177.6(2) . . . . ?
C44 C50 C68 C71 1.0(3) . . . . ?
N22 C50 C68 C71 178.42(18) . . . . ?
C88 C36 C69 C30 -0.1(3) . . . . ?
C64 C30 C69 C36 0.7(3) . . . . ?
N7 C30 C69 C36 178.75(18) . . . . ?
C50 C68 C71 C79 -0.8(3) . . . . ?
C20 C15 C73 C84 0.4(3) . . . . ?
P1 C15 C73 C84 178.00(18) . . . . ?
C50 C44 C74 C79 0.4(3) . . . . ?
C61 C44 C74 C79 179.5(2) . . . . ?
C44 C74 C79 C71 -0.2(3) . . . . ?
C68 C71 C79 C74 0.4(3) . . . . ?
C83 C52 C81 C60 -0.1(4) . . . . ?
C59 C60 C81 C52 -0.1(3) . . . . ?
C81 C52 C83 C32 0.4(4) . . . . ?
C59 C32 C83 C52 -0.6(3) . . . . ?
P1 C32 C83 C52 176.80(18) . . . . ?
C15 C73 C84 C85 -0.3(4) . . . . ?
C73 C84 C85 C48 0.0(4) . . . . ?
C20 C48 C85 C84 0.0(4) . . . . ?
C64 C65 C88 C36 0.4(3) . . . . ?
C69 C36 C88 C65 -0.4(4) . . . . ?
C91 C63 C89 C53 0.0(4) . . . . ?
C29 C53 C89 C63 0.5(3) . . . . ?
C64 C53 C89 C63 -178.2(2) . . . . ?
C29 C45 C91 C63 0.3(3) . . . . ?
C89 C63 C91 C45 -0.4(4) . . . . ?
C61 C51 C94 C55 1.1(4) . . . . ?
C66 C55 C94 C51 -0.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.888
_diffrn_reflns_theta_full        29.62
_diffrn_measured_fraction_theta_full 0.888
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.048
