# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_204E
_database_code_depnum_ccdc_archive 'CCDC 1903889'
loop_
_audit_author_name
_audit_author_address
'Marek Daszkiewicz'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2019-03-18 deposited with the CCDC.	2019-07-23 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         'C9 H17 N2 O4 P'
_chemical_formula_sum            'C9 H17 N2 O4 P'
_chemical_formula_weight         248.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

_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'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.0382(2)
_cell_length_b                   9.9050(2)
_cell_length_c                   9.8427(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1173.64(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    7655
_cell_measurement_theta_min      2.6850
_cell_measurement_theta_max      28.2930

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_F_000             528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.453
_exptl_crystal_size_mid          0.303
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.236
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.958
_oxdiff_exptl_absorpt_empirical_full_max 1.054
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.4350
_diffrn_reflns_number            11526
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.673
_diffrn_reflns_theta_max         27.862
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2721
_reflns_number_gt                2614
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_max     0.963
_reflns_Friedel_fraction_full    0.999

_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       
'CrysAlis CCD 1.171.33.42 (Oxford Diffraction, 2009)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.34a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.34a (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+0.0747P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1064 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         2721
_refine_ls_number_parameters     164
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0649
_refine_ls_wR_factor_gt          0.0635
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001

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 0.05680(15) 0.3228(2) 0.26623(19) 0.0286(4) Uani 1 1 d . . . . .
H1 H 0.0781 0.4169 0.2498 0.034 Uiso 1 1 calc R U . . .
C2 C 0.16111(14) 0.24172(18) 0.29406(17) 0.0259(4) Uani 1 1 d . . . . .
H2 H 0.1413 0.1463 0.3041 0.031 Uiso 1 1 calc R U . . .
C3 C 0.24257(18) 0.2567(2) 0.1771(2) 0.0405(5) Uani 1 1 d . . . . .
H3A H 0.3093 0.2050 0.1955 0.049 Uiso 1 1 calc R U . . .
H3AB H 0.2632 0.3507 0.1663 0.049 Uiso 1 1 calc R U . . .
C4 C 0.1865(2) 0.2048(3) 0.0468(2) 0.0606(7) Uani 1 1 d . . . . .
H4A H 0.2365 0.2173 -0.0295 0.073 Uiso 1 1 calc R U . . .
H4AB H 0.1720 0.1089 0.0558 0.073 Uiso 1 1 calc R U . . .
C5 C 0.0777(2) 0.2785(4) 0.0187(2) 0.0593(7) Uani 1 1 d . . . . .
H5A H 0.0421 0.2390 -0.0603 0.071 Uiso 1 1 calc R U . . .
H5AB H 0.0931 0.3726 -0.0012 0.071 Uiso 1 1 calc R U . . .
C6 C -0.0006(2) 0.2695(3) 0.1404(2) 0.0474(6) Uani 1 1 d . . . . .
H6A H -0.0671 0.3219 0.1227 0.057 Uiso 1 1 calc R U . . .
H6AB H -0.0224 0.1763 0.1547 0.057 Uiso 1 1 calc R U . . .
C7 C 0.01160(14) 0.29936(16) 0.51276(18) 0.0245(3) Uani 1 1 d . . . . .
C8 C 0.13346(13) 0.27059(16) 0.54879(17) 0.0212(3) Uani 1 1 d . . . . .
C9 C 0.17119(17) 0.36726(19) 0.66099(19) 0.0315(4) Uani 1 1 d . . . . .
H9A H 0.2482 0.3516 0.6810 0.047 Uiso 1 1 calc R U . . .
H9B H 0.1276 0.3521 0.7412 0.047 Uiso 1 1 calc R U . . .
H9C H 0.1615 0.4588 0.6311 0.047 Uiso 1 1 calc R U . . .
N1 N -0.01662(13) 0.31871(16) 0.38353(16) 0.0302(3) Uani 1 1 d . . . . .
H1N H -0.082(2) 0.344(2) 0.370(2) 0.037(6) Uiso 1 1 d . . . . .
N2 N 0.20798(12) 0.29261(15) 0.42591(14) 0.0223(3) Uani 1 1 d . . . . .
H2N H 0.272(2) 0.254(2) 0.435(2) 0.040(6) Uiso 1 1 d . . . . .
H3N H 0.218(2) 0.384(3) 0.416(3) 0.055(7) Uiso 1 1 d . . . . .
O1 O -0.05772(11) 0.30164(13) 0.60456(15) 0.0345(3) Uani 1 1 d . . . . .
O2 O 0.10243(10) 0.00512(13) 0.49030(13) 0.0299(3) Uani 1 1 d . . . . .
H2O H 0.0000 0.0000 0.498(5) 0.114(19) Uiso 1 2 d S . P . .
O3 O 0.08270(12) 0.07754(14) 0.73654(13) 0.0305(3) Uani 1 1 d . . . . .
H3O H 0.035(4) 0.031(5) 0.738(5) 0.041(14) Uiso 0.5 1 d . . P . .
O4 O 0.27077(10) 0.06911(12) 0.62144(16) 0.0346(3) Uani 1 1 d . . . . .
P1 P 0.14874(3) 0.09264(4) 0.60599(4) 0.02262(12) 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 1.455(2) . ?
C1 C6 1.513(3) . ?
C1 C2 1.515(2) . ?
C1 H1 0.9800 . ?
C2 N2 1.502(2) . ?
C2 C3 1.519(2) . ?
C2 H2 0.9800 . ?
C3 C4 1.538(3) . ?
C3 H3A 0.9700 . ?
C3 H3AB 0.9700 . ?
C4 C5 1.525(4) . ?
C4 H4A 0.9700 . ?
C4 H4AB 0.9700 . ?
C5 C6 1.527(3) . ?
C5 H5A 0.9700 . ?
C5 H5AB 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6AB 0.9700 . ?
C7 O1 1.230(2) . ?
C7 N1 1.330(2) . ?
C7 C8 1.536(2) . ?
C8 N2 1.522(2) . ?
C8 C9 1.531(2) . ?
C8 P1 1.8595(17) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
N1 H1N 0.84(3) . ?
N2 H2N 0.87(3) . ?
N2 H3N 0.92(3) . ?
O2 P1 1.5359(13) . ?
O2 H2O 1.236(3) . ?
O3 P1 1.5184(13) . ?
O3 H3O 0.74(4) . ?
O4 P1 1.4951(12) . ?

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 C6 111.26(15) . . ?
N1 C1 C2 110.20(15) . . ?
C6 C1 C2 109.95(16) . . ?
N1 C1 H1 108.5 . . ?
C6 C1 H1 108.5 . . ?
C2 C1 H1 108.5 . . ?
N2 C2 C1 106.83(14) . . ?
N2 C2 C3 112.30(15) . . ?
C1 C2 C3 110.26(16) . . ?
N2 C2 H2 109.1 . . ?
C1 C2 H2 109.1 . . ?
C3 C2 H2 109.1 . . ?
C2 C3 C4 108.42(17) . . ?
C2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
C2 C3 H3AB 110.0 . . ?
C4 C3 H3AB 110.0 . . ?
H3A C3 H3AB 108.4 . . ?
C5 C4 C3 111.6(2) . . ?
C5 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C5 C4 H4AB 109.3 . . ?
C3 C4 H4AB 109.3 . . ?
H4A C4 H4AB 108.0 . . ?
C4 C5 C6 111.1(2) . . ?
C4 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
C4 C5 H5AB 109.4 . . ?
C6 C5 H5AB 109.4 . . ?
H5A C5 H5AB 108.0 . . ?
C1 C6 C5 109.88(18) . . ?
C1 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C1 C6 H6AB 109.7 . . ?
C5 C6 H6AB 109.7 . . ?
H6A C6 H6AB 108.2 . . ?
O1 C7 N1 121.77(16) . . ?
O1 C7 C8 118.79(15) . . ?
N1 C7 C8 119.43(15) . . ?
N2 C8 C9 108.00(13) . . ?
N2 C8 C7 110.67(13) . . ?
C9 C8 C7 109.51(14) . . ?
N2 C8 P1 108.56(11) . . ?
C9 C8 P1 110.19(12) . . ?
C7 C8 P1 109.89(11) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 N1 C1 127.43(15) . . ?
C7 N1 H1N 115.8(16) . . ?
C1 N1 H1N 116.0(16) . . ?
C2 N2 C8 114.66(12) . . ?
C2 N2 H2N 106.1(15) . . ?
C8 N2 H2N 112.4(15) . . ?
C2 N2 H3N 106.7(17) . . ?
C8 N2 H3N 107.9(17) . . ?
H2N N2 H3N 109(2) . . ?
P1 O2 H2O 110(2) . . ?
P1 O3 H3O 119(4) . . ?
O4 P1 O3 114.39(8) . . ?
O4 P1 O2 110.13(8) . . ?
O3 P1 O2 112.45(7) . . ?
O4 P1 C8 106.01(7) . . ?
O3 P1 C8 107.32(8) . . ?
O2 P1 C8 105.94(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -52.38(18) . . . . ?
C6 C1 C2 N2 -175.38(16) . . . . ?
N1 C1 C2 C3 -174.67(16) . . . . ?
C6 C1 C2 C3 62.3(2) . . . . ?
N2 C2 C3 C4 -178.89(18) . . . . ?
C1 C2 C3 C4 -59.9(2) . . . . ?
C2 C3 C4 C5 56.5(3) . . . . ?
C3 C4 C5 C6 -55.1(3) . . . . ?
N1 C1 C6 C5 178.6(2) . . . . ?
C2 C1 C6 C5 -59.1(3) . . . . ?
C4 C5 C6 C1 55.6(3) . . . . ?
O1 C7 C8 N2 -171.60(15) . . . . ?
N1 C7 C8 N2 9.6(2) . . . . ?
O1 C7 C8 C9 -52.7(2) . . . . ?
N1 C7 C8 C9 128.53(17) . . . . ?
O1 C7 C8 P1 68.52(18) . . . . ?
N1 C7 C8 P1 -110.30(16) . . . . ?
O1 C7 N1 C1 177.94(17) . . . . ?
C8 C7 N1 C1 -3.3(3) . . . . ?
C6 C1 N1 C7 148.10(19) . . . . ?
C2 C1 N1 C7 25.9(3) . . . . ?
C1 C2 N2 C8 63.38(18) . . . . ?
C3 C2 N2 C8 -175.62(15) . . . . ?
C9 C8 N2 C2 -160.71(14) . . . . ?
C7 C8 N2 C2 -40.85(19) . . . . ?
P1 C8 N2 C2 79.83(16) . . . . ?
N2 C8 P1 O4 51.78(13) . . . . ?
C9 C8 P1 O4 -66.30(14) . . . . ?
C7 C8 P1 O4 172.94(11) . . . . ?
N2 C8 P1 O3 174.43(10) . . . . ?
C9 C8 P1 O3 56.35(13) . . . . ?
C7 C8 P1 O3 -64.41(13) . . . . ?
N2 C8 P1 O2 -65.23(11) . . . . ?
C9 C8 P1 O2 176.68(12) . . . . ?
C7 C8 P1 O2 55.92(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3O O3 0.74(4) 1.78(4) 2.515(3) 178(6) 2
N1 H1N O4 0.84(3) 1.97(3) 2.7908(19) 166(2) 4_456
N2 H2N O1 0.87(3) 2.16(3) 2.986(2) 160(2) 4_556
N2 H3N O4 0.92(3) 1.88(3) 2.790(2) 174(2) 3_556

_refine_diff_density_max         0.223
_refine_diff_density_min         -0.131
_refine_diff_density_rms         0.037

####################################################################### 
# 
# 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_TOABr423F100K
_database_code_depnum_ccdc_archive 'CCDC 1903892'
loop_
_audit_author_name
_audit_author_address
'Marek Daszkiewicz'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2019-03-26 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C16 H23 N2 O4 P), C2 H6 O, 0.282(C2 H6 O), 0.144(O)'
_chemical_formula_sum            'C17.32 H26.62 N2 O4.71 P'
_chemical_formula_weight         369.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.1042(5)
_cell_length_b                   11.9889(7)
_cell_length_c                   28.0715(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3737.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    19800
_cell_measurement_theta_min      2.5830
_cell_measurement_theta_max      29.1150

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_F_000             1578
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.577
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.033
_exptl_absorpt_coefficient_mu    0.175
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_T_max  0.994
_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 0.781
_oxdiff_exptl_absorpt_empirical_full_max 1.194
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            71497
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.500
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8806
_reflns_number_gt                8326
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_max     0.977
_reflns_Friedel_fraction_full    1.000

_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-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0679P)²+8.9165P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3120 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         8806
_refine_ls_number_parameters     498
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0777
_refine_ls_wR_factor_ref         0.1914
_refine_ls_wR_factor_gt          0.1894
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001

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
P1 P 0.17969(10) 0.65115(10) 0.51862(5) 0.0151(3) Uani 1 1 d . . . . .
O1 O 0.0189(3) 0.4374(3) 0.52577(15) 0.0220(8) Uani 1 1 d . . . . .
O2 O 0.2372(3) 0.5916(3) 0.47629(15) 0.0195(8) Uani 1 1 d . . . . .
O3 O 0.2087(3) 0.5954(3) 0.56649(14) 0.0196(8) Uani 1 1 d . . . . .
H3 H 0.245080 0.536914 0.561735 0.029 Uiso 1 1 calc R U . . .
O4 O 0.2066(3) 0.7740(3) 0.52011(16) 0.0220(8) Uani 1 1 d . . . . .
N1 N -0.0547(4) 0.4858(4) 0.45443(18) 0.0228(10) Uani 1 1 d . . . . .
H1N1 H -0.069675 0.416717 0.448710 0.027 Uiso 1 1 calc R U . . .
N2 N -0.0349(3) 0.7122(3) 0.47373(15) 0.0130(8) Uani 1 1 d . . . . .
H1N2 H -0.113573 0.721658 0.478235 0.016 Uiso 1 1 calc R U . . .
H2N2 H 0.000545 0.778182 0.477522 0.016 Uiso 1 1 calc R U . . .
C1 C -0.0830(5) 0.5652(5) 0.4169(2) 0.0224(11) Uani 1 1 d . . . . .
H1 H -0.169279 0.581905 0.418470 0.027 Uiso 1 1 calc R U . . .
C2 C -0.0143(4) 0.6730(4) 0.42352(19) 0.0169(10) Uani 1 1 d . . . . .
H2 H 0.071814 0.658111 0.419209 0.020 Uiso 1 1 calc R U . . .
C3 C -0.0535(5) 0.7601(5) 0.3871(2) 0.0245(12) Uani 1 1 d . . . . .
H3A H -0.138067 0.777533 0.391697 0.029 Uiso 1 1 calc R U . . .
H3B H -0.007519 0.828029 0.391695 0.029 Uiso 1 1 calc R U . . .
C4 C -0.0338(6) 0.7163(7) 0.3368(2) 0.0352(15) Uani 1 1 d . . . . .
H4A H 0.051994 0.711235 0.330645 0.042 Uiso 1 1 calc R U . . .
H4B H -0.067790 0.768751 0.314168 0.042 Uiso 1 1 calc R U . . .
C5 C -0.0915(7) 0.6010(6) 0.3290(2) 0.0402(17) Uani 1 1 d . . . . .
H5A H -0.178429 0.608651 0.329031 0.048 Uiso 1 1 calc R U . . .
H5B H -0.067458 0.572482 0.298086 0.048 Uiso 1 1 calc R U . . .
C6 C -0.0548(7) 0.5192(6) 0.3670(2) 0.0362(16) Uani 1 1 d . . . . .
H6A H 0.030834 0.504192 0.364490 0.043 Uiso 1 1 calc R U . . .
H6B H -0.097482 0.449429 0.362354 0.043 Uiso 1 1 calc R U . . .
C7 C -0.0080(4) 0.5101(4) 0.4967(2) 0.0165(10) Uani 1 1 d . . . . .
C8 C 0.0126(4) 0.6325(4) 0.51134(18) 0.0151(10) Uani 1 1 d . . . . .
C9A C -0.0555(5) 0.6493(5) 0.55855(19) 0.0230(11) Uani 0.574(12) 1 d . . P A 1
H9A1 H -0.140632 0.638042 0.552574 0.028 Uiso 0.574(12) 1 calc R U P A 1
H9A2 H -0.029754 0.591746 0.580588 0.028 Uiso 0.574(12) 1 calc R U P A 1
C10A C -0.0402(5) 0.7601(5) 0.5825(2) 0.0171(13) Uani 0.574(12) 1 d . . P A 1
H10A H -0.079397 0.816890 0.563372 0.021 Uiso 0.574(12) 1 calc R U P A 1
H10B H 0.044956 0.777925 0.583845 0.021 Uiso 0.574(12) 1 calc R U P A 1
C11A C -0.0911(6) 0.7633(6) 0.6320(2) 0.0257(16) Uani 0.574(12) 1 d . . P A 1
C12A C -0.0379(10) 0.7023(9) 0.6672(4) 0.029(3) Uiso 0.574(12) 1 d . . P A 1
H12A H 0.025964 0.655494 0.659508 0.035 Uiso 0.574(12) 1 calc R U P A 1
C13A C -0.0756(11) 0.7082(11) 0.7135(4) 0.033(3) Uiso 0.574(12) 1 d . . P A 1
H13A H -0.041428 0.663671 0.736987 0.040 Uiso 0.574(12) 1 calc R U P A 1
C14A C -0.1712(11) 0.7865(12) 0.7244(4) 0.032(3) Uiso 0.574(12) 1 d . . P A 1
H14A H -0.199460 0.792400 0.755500 0.039 Uiso 0.574(12) 1 calc R U P A 1
C15A C -0.2214(10) 0.8532(11) 0.6888(4) 0.029(2) Uiso 0.574(12) 1 d . . P A 1
H15A H -0.281117 0.904904 0.695986 0.035 Uiso 0.574(12) 1 calc R U P A 1
C16A C -0.1809(9) 0.8410(9) 0.6429(3) 0.021(2) Uiso 0.574(12) 1 d . . P A 1
H16A H -0.213427 0.884948 0.618797 0.025 Uiso 0.574(12) 1 calc R U P A 1
C9B C -0.0555(5) 0.6493(5) 0.55855(19) 0.0230(11) Uani 0.272(13) 1 d . . P A 2
H9B1 H -0.140632 0.638042 0.552574 0.028 Uiso 0.272(13) 1 calc R U P A 2
H9B2 H -0.029754 0.591746 0.580588 0.028 Uiso 0.272(13) 1 calc R U P A 2
C10B C -0.0402(5) 0.7601(5) 0.5825(2) 0.0171(13) Uani 0.272(13) 1 d . . P A 2
H10C H -0.079397 0.816890 0.563372 0.021 Uiso 0.272(13) 1 calc R U P A 2
H10D H 0.044956 0.777925 0.583845 0.021 Uiso 0.272(13) 1 calc R U P A 2
C11B C -0.0911(6) 0.7633(6) 0.6320(2) 0.0257(16) Uani 0.272(13) 1 d D . P A 2
C12B C -0.042(3) 0.784(3) 0.6751(9) 0.070(11) Uiso 0.272(13) 1 d D . P A 2
H12B H 0.035374 0.814052 0.674875 0.084 Uiso 0.272(13) 1 calc R U P A 2
C13B C -0.090(4) 0.767(3) 0.7170(15) 0.072(11) Uiso 0.272(13) 1 d . . P A 2
H13B H -0.042273 0.782769 0.743524 0.087 Uiso 0.272(13) 1 calc R U P A 2
C14B C -0.191(3) 0.732(3) 0.7243(10) 0.036(6) Uiso 0.272(13) 1 d . . P A 2
H14B H -0.220683 0.728499 0.755199 0.044 Uiso 0.272(13) 1 calc R U P A 2
C15B C -0.265(3) 0.695(2) 0.6849(10) 0.040(7) Uiso 0.272(13) 1 d . . P A 2
H15B H -0.339647 0.661918 0.689410 0.048 Uiso 0.272(13) 1 calc R U P A 2
C16B C -0.218(3) 0.713(3) 0.6401(11) 0.044(7) Uiso 0.272(13) 1 d . . P A 2
H16B H -0.263778 0.694851 0.613635 0.053 Uiso 0.272(13) 1 calc R U P A 2
C9C C -0.0555(5) 0.6493(5) 0.55855(19) 0.0230(11) Uani 0.167(10) 1 d . . P A 3
H9C1 H -0.020001 0.593762 0.579382 0.028 Uiso 0.167(10) 1 calc R U P A 3
H9C2 H -0.025192 0.720329 0.570000 0.028 Uiso 0.167(10) 1 calc R U P A 3
C10C C -0.168(3) 0.651(3) 0.5714(12) 0.026(8) Uiso 0.167(10) 1 d . . P A 3
H10E H -0.202715 0.579400 0.562595 0.031 Uiso 0.167(10) 1 calc R U P A 3
H10F H -0.208260 0.707339 0.552704 0.031 Uiso 0.167(10) 1 calc R U P A 3
C11C C -0.199(3) 0.672(3) 0.6244(14) 0.028(8) Uiso 0.167(10) 1 d . . P A 3
C12C C -0.180(3) 0.777(5) 0.6420(16) 0.040(10) Uiso 0.167(10) 1 d . . P A 3
H12C H -0.153516 0.834341 0.621939 0.047 Uiso 0.167(10) 1 calc R U P A 3
C13C C -0.201(3) 0.800(4) 0.6939(14) 0.029(8) Uiso 0.167(10) 1 d . . P A 3
H13C H -0.188797 0.869539 0.707796 0.035 Uiso 0.167(10) 1 calc R U P A 3
C14C C -0.241(5) 0.710(5) 0.7187(19) 0.048(13) Uiso 0.167(10) 1 d . . P A 3
H14C H -0.264709 0.718106 0.750271 0.058 Uiso 0.167(10) 1 calc R U P A 3
C15C C -0.246(5) 0.613(6) 0.699(2) 0.063(16) Uiso 0.167(10) 1 d . . P A 3
H15C H -0.257182 0.553400 0.719196 0.076 Uiso 0.167(10) 1 calc R U P A 3
C16C C -0.239(5) 0.589(6) 0.655(2) 0.063(16) Uiso 0.167(10) 1 d . . P A 3
H16C H -0.258768 0.518068 0.643249 0.076 Uiso 0.167(10) 1 calc R U P A 3
P2 P 0.35811(10) 0.34815(10) 0.52593(5) 0.0139(3) Uani 1 1 d . . . . .
O5 O 0.5311(3) 0.5615(3) 0.53699(15) 0.0222(8) Uani 1 1 d . . . . .
O6 O 0.3016(3) 0.3962(3) 0.47994(15) 0.0194(8) Uani 1 1 d . . . . .
H6 H 0.279323 0.491248 0.484193 0.029 Uiso 1 1 d . U . . .
O7 O 0.3214(3) 0.4131(3) 0.57010(14) 0.0189(8) Uani 1 1 d . . . . .
O8 O 0.3365(3) 0.2245(3) 0.52863(15) 0.0186(8) Uani 1 1 d . . . . .
N3 N 0.6032(4) 0.5114(4) 0.46542(17) 0.0195(9) Uani 1 1 d . . . . .
H1N3 H 0.625530 0.579295 0.461059 0.023 Uiso 1 1 calc R U . . .
N4 N 0.5734(3) 0.2887(3) 0.48257(15) 0.0136(8) Uani 1 1 d . . . . .
H1N4 H 0.652529 0.281115 0.486361 0.016 Uiso 1 1 calc R U . . .
H2N4 H 0.539947 0.221796 0.486306 0.016 Uiso 1 1 calc R U . . .
C21 C 0.6232(5) 0.4336(4) 0.4260(2) 0.0183(10) Uani 1 1 d . . . . .
H21 H 0.708475 0.412402 0.425775 0.022 Uiso 1 1 calc R U . . .
C22 C 0.5484(4) 0.3296(4) 0.43294(18) 0.0156(10) Uani 1 1 d . . . . .
H22 H 0.462981 0.349026 0.430313 0.019 Uiso 1 1 calc R U . . .
C23 C 0.5790(5) 0.2431(5) 0.3952(2) 0.0191(11) Uani 1 1 d . . . . .
H23A H 0.530608 0.176625 0.399850 0.023 Uiso 1 1 calc R U . . .
H23B H 0.663237 0.222465 0.397492 0.023 Uiso 1 1 calc R U . . .
C24 C 0.5528(5) 0.2940(5) 0.3458(2) 0.0261(12) Uani 1 1 d . . . . .
H24A H 0.575907 0.241160 0.321328 0.031 Uiso 1 1 calc R U . . .
H24B H 0.467064 0.307601 0.342851 0.031 Uiso 1 1 calc R U . . .
C25 C 0.6204(6) 0.4027(6) 0.3381(2) 0.0315(14) Uani 1 1 d . . . . .
H25A H 0.597458 0.434585 0.307697 0.038 Uiso 1 1 calc R U . . .
H25B H 0.706317 0.388045 0.337345 0.038 Uiso 1 1 calc R U . . .
C26 C 0.5925(6) 0.4862(5) 0.3781(2) 0.0260(12) Uani 1 1 d . . . . .
H26A H 0.639466 0.553551 0.373557 0.031 Uiso 1 1 calc R U . . .
H26B H 0.507849 0.506031 0.377263 0.031 Uiso 1 1 calc R U . . .
C27 C 0.5538(4) 0.4873(4) 0.5072(2) 0.0154(10) Uani 1 1 d . . . . .
C28 C 0.5257(4) 0.3661(4) 0.52032(19) 0.0138(9) Uani 1 1 d . . . . .
C29A C 0.5800(5) 0.3372(5) 0.56930(19) 0.0198(11) Uani 0.54(2) 1 d . . P B 4
H29A H 0.538402 0.380483 0.593406 0.024 Uiso 0.54(2) 1 calc R U P B 4
H29B H 0.564437 0.259066 0.575821 0.024 Uiso 0.54(2) 1 calc R U P B 4
C30A C 0.7132(9) 0.3577(10) 0.5743(4) 0.007(2) Uiso 0.54(2) 1 d . . P B 4
H30A H 0.733141 0.433787 0.565605 0.008 Uiso 0.54(2) 1 calc R U P B 4
H30B H 0.758628 0.307095 0.554225 0.008 Uiso 0.54(2) 1 calc R U P B 4
C31A C 0.7414(9) 0.3359(12) 0.6284(4) 0.015(3) Uiso 0.54(2) 1 d . . P B 4
C32A C 0.7774(10) 0.4169(13) 0.6577(5) 0.027(3) Uiso 0.54(2) 1 d . . P B 4
H32A H 0.789789 0.488665 0.646066 0.033 Uiso 0.54(2) 1 calc R U P B 4
C33A C 0.7965(12) 0.3935(15) 0.7059(5) 0.036(4) Uiso 0.54(2) 1 d . . P B 4
H33A H 0.823332 0.450036 0.725946 0.044 Uiso 0.54(2) 1 calc R U P B 4
C34A C 0.7759(12) 0.2848(17) 0.7252(5) 0.030(3) Uiso 0.54(2) 1 d . . P B 4
H34A H 0.786704 0.271016 0.757476 0.035 Uiso 0.54(2) 1 calc R U P B 4
C35A C 0.7413(11) 0.2047(14) 0.6962(5) 0.028(3) Uiso 0.54(2) 1 d . . P B 4
H35A H 0.727526 0.133279 0.707909 0.034 Uiso 0.54(2) 1 calc R U P B 4
C36A C 0.7254(11) 0.2275(13) 0.6482(5) 0.024(3) Uiso 0.54(2) 1 d . . P B 4
H36A H 0.703250 0.169504 0.627990 0.028 Uiso 0.54(2) 1 calc R U P B 4
C29B C 0.5800(5) 0.3372(5) 0.56930(19) 0.0198(11) Uani 0.32(2) 1 d . . P B 5
H29C H 0.552366 0.262223 0.576296 0.024 Uiso 0.32(2) 1 calc R U P B 5
H29D H 0.539409 0.385654 0.591828 0.024 Uiso 0.32(2) 1 calc R U P B 5
C30B C 0.7147(18) 0.3391(19) 0.5841(8) 0.018(5) Uiso 0.32(2) 1 d . . P B 5
H30C H 0.759825 0.295463 0.561127 0.022 Uiso 0.32(2) 1 calc R U P B 5
H30D H 0.743226 0.415413 0.581932 0.022 Uiso 0.32(2) 1 calc R U P B 5
C31B C 0.7403(15) 0.300(2) 0.6280(6) 0.015(5) Uiso 0.32(2) 1 d . . P B 5
C32B C 0.7704(17) 0.382(2) 0.6664(9) 0.034(6) Uiso 0.32(2) 1 d . . P B 5
H32B H 0.781109 0.456943 0.659754 0.041 Uiso 0.32(2) 1 calc R U P B 5
C33B C 0.7825(17) 0.338(3) 0.7157(8) 0.028(5) Uiso 0.32(2) 1 d . . P B 5
H33B H 0.804309 0.383943 0.741011 0.034 Uiso 0.32(2) 1 calc R U P B 5
C34B C 0.761(2) 0.231(3) 0.7217(9) 0.034(6) Uiso 0.32(2) 1 d . . P B 5
H34B H 0.761335 0.203649 0.752621 0.041 Uiso 0.32(2) 1 calc R U P B 5
C35B C 0.7383(19) 0.159(2) 0.6858(8) 0.033(6) Uiso 0.32(2) 1 d . . P B 5
H35B H 0.731073 0.084004 0.693140 0.039 Uiso 0.32(2) 1 calc R U P B 5
C36B C 0.7249(19) 0.192(2) 0.6382(9) 0.027(5) Uiso 0.32(2) 1 d . . P B 5
H36B H 0.706143 0.140640 0.614519 0.033 Uiso 0.32(2) 1 calc R U P B 5
C29C C 0.5800(5) 0.3372(5) 0.56930(19) 0.0198(11) Uani 0.141(10) 1 d . . P B 6
H29E H 0.664199 0.358667 0.567989 0.024 Uiso 0.141(10) 1 calc R U P B 6
H29F H 0.541933 0.386460 0.592197 0.024 Uiso 0.141(10) 1 calc R U P B 6
C30C C 0.577(5) 0.230(5) 0.5891(19) 0.045(13) Uiso 0.141(10) 1 d . . P B 6
H30E H 0.603059 0.178092 0.564859 0.054 Uiso 0.141(10) 1 calc R U P B 6
H30F H 0.493468 0.212944 0.596343 0.054 Uiso 0.141(10) 1 calc R U P B 6
C31C C 0.649(3) 0.209(3) 0.6326(13) 0.020(8) Uiso 0.141(10) 1 d D . P B 6
C32C C 0.659(4) 0.275(4) 0.6714(17) 0.038(11) Uiso 0.141(10) 1 d . . P B 6
H32C H 0.623725 0.344952 0.668897 0.046 Uiso 0.141(10) 1 calc R U P B 6
C33C C 0.714(5) 0.254(5) 0.713(2) 0.042(14) Uiso 0.141(10) 1 d . . P B 6
H33C H 0.714877 0.307040 0.737032 0.051 Uiso 0.141(10) 1 calc R U P B 6
C34C C 0.763(3) 0.162(3) 0.7190(13) 0.018(8) Uiso 0.141(10) 1 d D . P B 6
H34C H 0.801435 0.145134 0.747583 0.021 Uiso 0.141(10) 1 calc R U P B 6
C35C C 0.759(6) 0.085(5) 0.6820(16) 0.062(18) Uiso 0.141(10) 1 d D . P B 6
H35C H 0.790645 0.013697 0.687057 0.074 Uiso 0.141(10) 1 calc R U P B 6
C36C C 0.710(5) 0.109(4) 0.6381(19) 0.052(15) Uiso 0.141(10) 1 d D . P B 6
H36C H 0.718269 0.059744 0.612725 0.062 Uiso 0.141(10) 1 calc R U P B 6
O1E O 0.3503(9) 0.3079(8) 0.6616(3) 0.095(3) Uiso 1 1 d . . . . .
H1E H 0.354645 0.338334 0.632607 0.142 Uiso 1 1 d . U . . .
C1E C 0.4297(10) 0.3569(10) 0.6929(4) 0.071(3) Uiso 1 1 d . . . . .
H1EA H 0.510913 0.353791 0.680231 0.085 Uiso 1 1 calc R U . . .
H1EB H 0.428402 0.318016 0.723207 0.085 Uiso 1 1 calc R U . . .
C2E C 0.391(2) 0.4762(18) 0.6994(8) 0.164(8) Uiso 1 1 d . . . . .
H2EA H 0.437197 0.523265 0.678621 0.246 Uiso 1 1 calc R U . . .
H2EB H 0.404372 0.498207 0.731871 0.246 Uiso 1 1 calc R U . . .
H2EC H 0.307091 0.483165 0.691913 0.246 Uiso 1 1 calc R U . . .
O2E O 0.1919(19) 0.6114(17) 0.6638(7) 0.049(6) Uiso 0.282(13) 1 d . . P . .
H2E H 0.209349 0.633707 0.636698 0.074 Uiso 0.2818 1 d . U P . .
C3E C 0.105(3) 0.517(3) 0.6741(13) 0.063(9) Uiso 0.282(13) 1 d . . P . .
H3E1 H 0.040928 0.517623 0.650771 0.075 Uiso 0.282(13) 1 calc R U P . .
H3E2 H 0.147378 0.446318 0.671434 0.075 Uiso 0.282(13) 1 calc R U P . .
C4E C 0.058(4) 0.527(4) 0.7184(14) 0.079(12) Uiso 0.282(13) 1 d . . P . .
H4E1 H 0.109702 0.490175 0.740939 0.119 Uiso 0.282(13) 1 calc R U P . .
H4E2 H -0.020214 0.492565 0.719106 0.119 Uiso 0.282(13) 1 calc R U P . .
H4E3 H 0.050902 0.604174 0.726541 0.119 Uiso 0.282(13) 1 calc R U P . .
O1W O 0.433(3) 0.140(3) 0.7189(10) 0.030(10) Uiso 0.147(18) 1 d . . P . .


_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 O4 1.503(4) . ?
P1 O2 1.527(4) . ?
P1 O3 1.535(4) . ?
P1 C8 1.880(5) . ?
O1 C7 1.232(6) . ?
O2 H6 1.3093 . ?
O3 H3 0.8200 . ?
N1 C7 1.327(7) . ?
N1 C1 1.453(7) . ?
N1 H1N1 0.8600 . ?
N2 C2 1.503(7) . ?
N2 C8 1.518(6) . ?
N2 H1N2 0.8900 . ?
N2 H2N2 0.8900 . ?
C1 C2 1.512(7) . ?
C1 C6 1.537(8) . ?
C1 H1 0.9800 . ?
C2 C3 1.524(8) . ?
C2 H2 0.9800 . ?
C3 C4 1.524(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.538(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.507(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.541(7) . ?
C8 C9C 1.539(7) . ?
C8 C9B 1.539(7) . ?
C8 C9A 1.539(7) . ?
C9Aa C10A 1.497(8) . ?
C9Aa H9A1 0.9700 . ?
C9Aa H9A2 0.9700 . ?
C10Aa C11A 1.502(9) . ?
C10Aa H10A 0.9700 . ?
C10Aa H10B 0.9700 . ?
C11Aa C12A 1.364(13) . ?
C11Aa C16A 1.399(12) . ?
C12Aa C13A 1.366(16) . ?
C12Aa H12A 0.9300 . ?
C13Aa C14A 1.450(19) . ?
C13Aa H13A 0.9300 . ?
C14Aa C15A 1.397(17) . ?
C14Aa H14A 0.9300 . ?
C15Aa C16A 1.372(14) . ?
C15Aa H15A 0.9300 . ?
C16Aa H16A 0.9300 . ?
C9Bb C10B 1.497(8) . ?
C9Bb H9B1 0.9700 . ?
C9Bb H9B2 0.9700 . ?
C10Bb C11B 1.502(9) . ?
C10Bb H10C 0.9700 . ?
C10Bb H10D 0.9700 . ?
C11Bb C12B 1.35(2) . ?
C11Bb C16B 1.54(3) . ?
C12Bb C13B 1.31(5) . ?
C12Bb H12B 0.9300 . ?
C13Bb C14B 1.22(6) . ?
C13Bb H13B 0.9300 . ?
C14Bb C15B 1.45(4) . ?
C14Bb H14B 0.9300 . ?
C15Bb C16B 1.38(4) . ?
C15Bb H15B 0.9300 . ?
C16Bb H16B 0.9300 . ?
C9Cc C10C 1.30(3) . ?
C9Cc H9C1 0.9700 . ?
C9Cc H9C2 0.9700 . ?
C10Cc C11C 1.55(5) . ?
C10Cc H10E 0.9700 . ?
C10Cc H10F 0.9700 . ?
C11Cc C12C 1.37(7) . ?
C11Cc C16C 1.38(7) . ?
C12Cc C13C 1.50(6) . ?
C12Cc H12C 0.9300 . ?
C13Cc C14C 1.36(7) . ?
C13Cc H13C 0.9300 . ?
C14Cc C15C 1.29(8) . ?
C14Cc H14C 0.9300 . ?
C15Cc C16C 1.28(8) . ?
C15Cc H15C 0.9300 . ?
C16Cc H16C 0.9300 . ?
P2 O8 1.504(3) . ?
P2 O7 1.520(4) . ?
P2 O6 1.547(4) . ?
P2 C28 1.880(5) . ?
O5 C27 1.247(6) . ?
O6 H6 1.1717 . ?
N3 C27 1.326(7) . ?
N3 C21 1.464(7) . ?
N3 H1N3 0.8600 . ?
N4 C22 1.503(6) . ?
N4 C28 1.505(6) . ?
N4 H1N4 0.8900 . ?
N4 H2N4 0.8900 . ?
C21 C22 1.511(7) . ?
C21 C26 1.525(8) . ?
C21 H21 0.9800 . ?
C22 C23 1.521(7) . ?
C22 H22 0.9800 . ?
C23 C24 1.541(8) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.519(9) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.534(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.531(6) . ?
C28 C29C 1.541(7) . ?
C28 C29B 1.541(7) . ?
C28 C29A 1.541(7) . ?
C29Ad C30A 1.505(11) . ?
C29Ad H29A 0.9700 . ?
C29Ad H29B 0.9700 . ?
C30Ad C31A 1.572(15) . ?
C30Ad H30A 0.9700 . ?
C30Ad H30B 0.9700 . ?
C31Ad C32A 1.333(18) . ?
C31Ad C36A 1.424(17) . ?
C32Ad C33A 1.40(2) . ?
C32Ad H32A 0.9300 . ?
C33Ad C34A 1.43(2) . ?
C33Ad H33A 0.9300 . ?
C34Ad C35A 1.31(2) . ?
C34Ad H34A 0.9300 . ?
C35Ad C36A 1.388(18) . ?
C35Ad H35A 0.9300 . ?
C36Ad H36A 0.9300 . ?
C29Be C30B 1.55(2) . ?
C29Be H29C 0.9700 . ?
C29Be H29D 0.9700 . ?
C30Be C31B 1.35(3) . ?
C30Be H30C 0.9700 . ?
C30Be H30D 0.9700 . ?
C31Be C36B 1.34(3) . ?
C31Be C32B 1.49(3) . ?
C32Be C33B 1.49(4) . ?
C32Be H32B 0.9300 . ?
C33Be C34B 1.31(3) . ?
C33Be H33B 0.9300 . ?
C34Be C35B 1.35(4) . ?
C34Be H34B 0.9300 . ?
C35Be C36B 1.40(3) . ?
C35Be H35B 0.9300 . ?
C36Be H36B 0.9300 . ?
C29Cf C30C 1.40(6) . ?
C29Cf H29E 0.9700 . ?
C29Cf H29F 0.9700 . ?
C30Cf C31C 1.48(6) . ?
C30Cf H30E 0.9700 . ?
C30Cf H30F 0.9700 . ?
C31Cf C32C 1.35(6) . ?
C31Cf C36C 1.39(3) . ?
C32Cf C33C 1.34(8) . ?
C32Cf H32C 0.9300 . ?
C33Cf C34C 1.24(8) . ?
C33Cf H33C 0.9300 . ?
C34Cf C35C 1.40(3) . ?
C34Cf H34C 0.9300 . ?
C35Cf C36C 1.38(3) . ?
C35Cf H35C 0.9300 . ?
C36Cf H36C 0.9300 . ?
O1E C1E 1.376(13) . ?
O1E H1E 0.8934 . ?
C1E C2E 1.50(2) . ?
C1E H1EA 0.9700 . ?
C1E H1EB 0.9700 . ?
C2E H2EA 0.9600 . ?
C2E H2EB 0.9600 . ?
C2E H2EC 0.9600 . ?
O2E C3E 1.51(4) . ?
O2E H2E 0.8286 . ?
C3E C4E 1.36(5) . ?
C3E H3E1 0.9700 . ?
C3E H3E2 0.9700 . ?
C4E H4E1 0.9600 . ?
C4E H4E2 0.9600 . ?
C4E H4E3 0.9600 . ?

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
O4 P1 O2 113.4(2) . . ?
O4 P1 O3 111.1(2) . . ?
O2 P1 O3 112.9(2) . . ?
O4 P1 C8 108.4(2) . . ?
O2 P1 C8 105.8(2) . . ?
O3 P1 C8 104.5(2) . . ?
P1 O2 H6 116.6 . . ?
P1 O3 H3 109.5 . . ?
C7 N1 C1 126.0(4) . . ?
C7 N1 H1N1 117.0 . . ?
C1 N1 H1N1 117.0 . . ?
C2 N2 C8 113.7(4) . . ?
C2 N2 H1N2 108.8 . . ?
C8 N2 H1N2 108.8 . . ?
C2 N2 H2N2 108.8 . . ?
C8 N2 H2N2 108.8 . . ?
H1N2 N2 H2N2 107.7 . . ?
N1 C1 C2 111.2(4) . . ?
N1 C1 C6 112.4(5) . . ?
C2 C1 C6 108.4(5) . . ?
N1 C1 H1 108.2 . . ?
C2 C1 H1 108.2 . . ?
C6 C1 H1 108.2 . . ?
N2 C2 C1 107.8(4) . . ?
N2 C2 C3 111.8(4) . . ?
C1 C2 C3 111.1(4) . . ?
N2 C2 H2 108.7 . . ?
C1 C2 H2 108.7 . . ?
C3 C2 H2 108.7 . . ?
C4 C3 C2 110.1(5) . . ?
C4 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C3 C4 C5 112.4(5) . . ?
C3 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C4 111.8(6) . . ?
C6 C5 H5A 109.2 . . ?
C4 C5 H5A 109.2 . . ?
C6 C5 H5B 109.2 . . ?
C4 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C5 C6 C1 110.9(5) . . ?
C5 C6 H6A 109.5 . . ?
C1 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 108.0 . . ?
O1 C7 N1 122.1(5) . . ?
O1 C7 C8 117.5(5) . . ?
N1 C7 C8 120.4(4) . . ?
N2 C8 C9C 110.2(4) . . ?
N2 C8 C9B 110.2(4) . . ?
N2 C8 C9A 110.2(4) . . ?
N2 C8 C7 111.2(4) . . ?
C9Cc C8 C7 106.4(4) . . ?
C9Bb C8 C7 106.4(4) . . ?
C9Aa C8 C7 106.4(4) . . ?
N2 C8 P1 110.1(3) . . ?
C9Cc C8 P1 112.1(4) . . ?
C9Bb C8 P1 112.1(4) . . ?
C9Aa C8 P1 112.1(4) . . ?
C7 C8 P1 106.8(3) . . ?
C10Aa C9Aa C8 116.5(5) . . ?
C10Aa C9Aa H9A1 108.2 . . ?
C8 C9Aa H9A1 108.2 . . ?
C10Aa C9Aa H9A2 108.2 . . ?
C8 C9Aa H9A2 108.2 . . ?
H9A1a C9Aa H9A2 107.3 . . ?
C9Aa C10Aa C11A 113.3(5) . . ?
C9Aa C10Aa H10A 108.9 . . ?
C11Aa C10Aa H10A 108.9 . . ?
C9Aa C10Aa H10B 108.9 . . ?
C11Aa C10Aa H10B 108.9 . . ?
H10Aa C10Aa H10B 107.7 . . ?
C12Aa C11Aa C16A 120.5(8) . . ?
C12Aa C11Aa C10A 119.6(7) . . ?
C16Aa C11Aa C10A 119.2(7) . . ?
C11Aa C12Aa C13A 121.9(11) . . ?
C11Aa C12Aa H12A 119.0 . . ?
C13Aa C12Aa H12A 119.0 . . ?
C12Aa C13Aa C14A 117.3(12) . . ?
C12Aa C13Aa H13A 121.3 . . ?
C14Aa C13Aa H13A 121.3 . . ?
C15Aa C14Aa C13A 120.7(11) . . ?
C15Aa C14Aa H14A 119.6 . . ?
C13Aa C14Aa H14A 119.6 . . ?
C16Aa C15Aa C14A 118.7(12) . . ?
C16Aa C15Aa H15A 120.6 . . ?
C14Aa C15Aa H15A 120.6 . . ?
C15Aa C16Aa C11A 120.6(10) . . ?
C15Aa C16Aa H16A 119.7 . . ?
C11Aa C16Aa H16A 119.7 . . ?
C10Bb C9Bb C8 116.5(5) . . ?
C10Bb C9Bb H9B1 108.2 . . ?
C8 C9Bb H9B1 108.2 . . ?
C10Bb C9Bb H9B2 108.2 . . ?
C8 C9Bb H9B2 108.2 . . ?
H9B1b C9Bb H9B2 107.3 . . ?
C9Bb C10Bb C11B 113.3(5) . . ?
C9Bb C10Bb H10C 108.9 . . ?
C11Bb C10Bb H10C 108.9 . . ?
C9Bb C10Bb H10D 108.9 . . ?
C11Bb C10Bb H10D 108.9 . . ?
H10Cb C10Bb H10D 107.7 . . ?
C12Bb C11Bb C10B 132.9(18) . . ?
C12Bb C11Bb C16B 108(2) . . ?
C10Bb C11Bb C16B 118.0(13) . . ?
C13Bb C12Bb C11B 128(4) . . ?
C13Bb C12Bb H12B 116.1 . . ?
C11Bb C12Bb H12B 116.1 . . ?
C14Bb C13Bb C12B 125(4) . . ?
C14Bb C13Bb H13B 117.3 . . ?
C12Bb C13Bb H13B 117.3 . . ?
C13Bb C14Bb C15B 120(3) . . ?
C13Bb C14Bb H14B 119.9 . . ?
C15Bb C14Bb H14B 119.9 . . ?
C16Bb C15Bb C14B 116(3) . . ?
C16Bb C15Bb H15B 122.2 . . ?
C14Bb C15Bb H15B 122.2 . . ?
C15Bb C16Bb C11B 123(3) . . ?
C15Bb C16Bb H16B 118.6 . . ?
C11Bb C16Bb H16B 118.6 . . ?
C10Cc C9Cc C8 135.5(15) . . ?
C10Cc C9Cc H9C1 103.3 . . ?
C8 C9Cc H9C1 103.3 . . ?
C10Cc C9Cc H9C2 103.3 . . ?
C8 C9Cc H9C2 103.3 . . ?
H9C1c C9Cc H9C2 105.2 . . ?
C9Cc C10Cc C11C 119(3) . . ?
C9Cc C10Cc H10E 107.6 . . ?
C11Cc C10Cc H10E 107.6 . . ?
C9Cc C10Cc H10F 107.6 . . ?
C11Cc C10Cc H10F 107.6 . . ?
H10Ec C10Cc H10F 107.0 . . ?
C12Cc C11Cc C16C 120(5) . . ?
C12Cc C11Cc C10C 118(4) . . ?
C16Cc C11Cc C10C 123(4) . . ?
C11Cc C12Cc C13C 119(4) . . ?
C11Cc C12Cc H12C 120.3 . . ?
C13Cc C12Cc H12C 120.3 . . ?
C14Cc C13Cc C12C 114(4) . . ?
C14Cc C13Cc H13C 123.0 . . ?
C12Cc C13Cc H13C 123.0 . . ?
C15Cc C14Cc C13C 120(5) . . ?
C15Cc C14Cc H14C 119.8 . . ?
C13Cc C14Cc H14C 119.8 . . ?
C16Cc C15Cc C14C 129(7) . . ?
C16Cc C15Cc H15C 115.5 . . ?
C14Cc C15Cc H15C 115.5 . . ?
C15Cc C16Cc C11C 117(6) . . ?
C15Cc C16Cc H16C 121.7 . . ?
C11Cc C16Cc H16C 121.7 . . ?
O8 P2 O7 114.9(2) . . ?
O8 P2 O6 110.2(2) . . ?
O7 P2 O6 112.4(2) . . ?
O8 P2 C28 106.0(2) . . ?
O7 P2 C28 106.0(2) . . ?
O6 P2 C28 106.8(2) . . ?
P2 O6 H6 111.3 . . ?
C27 N3 C21 126.3(4) . . ?
C27 N3 H1N3 116.8 . . ?
C21 N3 H1N3 116.8 . . ?
C22 N4 C28 112.8(4) . . ?
C22 N4 H1N4 109.0 . . ?
C28 N4 H1N4 109.0 . . ?
C22 N4 H2N4 109.0 . . ?
C28 N4 H2N4 109.0 . . ?
H1N4 N4 H2N4 107.8 . . ?
N3 C21 C22 110.2(4) . . ?
N3 C21 C26 111.7(4) . . ?
C22 C21 C26 109.4(4) . . ?
N3 C21 H21 108.5 . . ?
C22 C21 H21 108.5 . . ?
C26 C21 H21 108.5 . . ?
N4 C22 C21 106.7(4) . . ?
N4 C22 C23 112.5(4) . . ?
C21 C22 C23 110.5(4) . . ?
N4 C22 H22 109.0 . . ?
C21 C22 H22 109.0 . . ?
C23 C22 H22 109.0 . . ?
C22 C23 C24 108.3(4) . . ?
C22 C23 H23A 110.0 . . ?
C24 C23 H23A 110.0 . . ?
C22 C23 H23B 110.0 . . ?
C24 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
C25 C24 C23 112.0(5) . . ?
C25 C24 H24A 109.2 . . ?
C23 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C24 C25 C26 110.8(5) . . ?
C24 C25 H25A 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C21 C26 C25 109.3(5) . . ?
C21 C26 H26A 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C21 C26 H26B 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
O5 C27 N3 121.4(5) . . ?
O5 C27 C28 118.3(5) . . ?
N3 C27 C28 120.3(4) . . ?
N4 C28 C27 110.1(4) . . ?
N4 C28 C29C 110.6(4) . . ?
C27 C28 C29C 110.4(4) . . ?
N4 C28 C29B 110.6(4) . . ?
C27 C28 C29B 110.4(4) . . ?
N4 C28 C29A 110.6(4) . . ?
C27 C28 C29A 110.4(4) . . ?
N4 C28 P2 109.7(3) . . ?
C27 C28 P2 109.3(3) . . ?
C29Cf C28 P2 106.7(3) . . ?
C29Be C28 P2 106.7(3) . . ?
C29Ad C28 P2 106.7(3) . . ?
C30Ad C29Ad C28 115.5(6) . . ?
C30Ad C29Ad H29A 108.4 . . ?
C28 C29Ad H29A 108.4 . . ?
C30Ad C29Ad H29B 108.4 . . ?
C28 C29Ad H29B 108.4 . . ?
H29Ad C29Ad H29B 107.5 . . ?
C29Ad C30Ad C31A 105.0(8) . . ?
C29Ad C30Ad H30A 110.7 . . ?
C31Ad C30Ad H30A 110.7 . . ?
C29Ad C30Ad H30B 110.7 . . ?
C31Ad C30Ad H30B 110.7 . . ?
H30Ad C30Ad H30B 108.8 . . ?
C32Ad C31Ad C36A 117.5(11) . . ?
C32Ad C31Ad C30A 122.3(12) . . ?
C36Ad C31Ad C30A 120.2(11) . . ?
C31Ad C32Ad C33A 119.7(14) . . ?
C31Ad C32Ad H32A 120.2 . . ?
C33Ad C32Ad H32A 120.2 . . ?
C32Ad C33Ad C34A 121.7(13) . . ?
C32Ad C33Ad H33A 119.2 . . ?
C34Ad C33Ad H33A 119.2 . . ?
C35Ad C34Ad C33A 118.6(13) . . ?
C35Ad C34Ad H34A 120.7 . . ?
C33Ad C34Ad H34A 120.7 . . ?
C34Ad C35Ad C36A 119.6(14) . . ?
C34Ad C35Ad H35A 120.2 . . ?
C36Ad C35Ad H35A 120.2 . . ?
C35Ad C36Ad C31A 122.8(13) . . ?
C35Ad C36Ad H36A 118.6 . . ?
C31Ad C36Ad H36A 118.6 . . ?
C28 C29Be C30B 127.8(10) . . ?
C28 C29Be H29C 105.4 . . ?
C30Be C29Be H29C 105.4 . . ?
C28 C29Be H29D 105.4 . . ?
C30Be C29Be H29D 105.4 . . ?
H29Ce C29Be H29D 106.0 . . ?
C31Be C30Be C29B 116.3(17) . . ?
C31Be C30Be H30C 108.2 . . ?
C29Be C30Be H30C 108.2 . . ?
C31Be C30Be H30D 108.2 . . ?
C29Be C30Be H30D 108.2 . . ?
H30Ce C30Be H30D 107.4 . . ?
C36Be C31Be C30B 120(2) . . ?
C36Be C31Be C32B 120(2) . . ?
C30Be C31Be C32B 119(2) . . ?
C33Be C32Be C31B 118(2) . . ?
C33Be C32Be H32B 121.1 . . ?
C31Be C32Be H32B 121.1 . . ?
C34Be C33Be C32B 116(2) . . ?
C34Be C33Be H33B 121.8 . . ?
C32Be C33Be H33B 121.8 . . ?
C33Be C34Be C35B 124(2) . . ?
C33Be C34Be H34B 117.9 . . ?
C35Be C34Be H34B 117.9 . . ?
C34Be C35Be C36B 123(3) . . ?
C34Be C35Be H35B 118.3 . . ?
C36Be C35Be H35B 118.3 . . ?
C31Be C36Be C35B 117(2) . . ?
C31Be C36Be H36B 121.3 . . ?
C35Be C36Be H36B 121.3 . . ?
C30Cf C29Cf C28 123(2) . . ?
C30Cf C29Cf H29E 106.5 . . ?
C28 C29Cf H29E 106.5 . . ?
C30Cf C29Cf H29F 106.5 . . ?
C28 C29Cf H29F 106.5 . . ?
H29Ef C29Cf H29F 106.5 . . ?
C29Cf C30Cf C31C 118(4) . . ?
C29Cf C30Cf H30E 107.8 . . ?
C31Cf C30Cf H30E 107.8 . . ?
C29Cf C30Cf H30F 107.8 . . ?
C31Cf C30Cf H30F 107.8 . . ?
H30Ef C30Cf H30F 107.1 . . ?
C32Cf C31Cf C36C 112(4) . . ?
C32Cf C31Cf C30C 128(4) . . ?
C36Cf C31Cf C30C 120(4) . . ?
C33Cf C32Cf C31C 129(5) . . ?
C33Cf C32Cf H32C 115.4 . . ?
C31Cf C32Cf H32C 115.4 . . ?
C34Cf C33Cf C32C 119(6) . . ?
C34Cf C33Cf H33C 120.4 . . ?
C32Cf C33Cf H33C 120.4 . . ?
C33Cf C34Cf C35C 118(5) . . ?
C33Cf C34Cf H34C 120.8 . . ?
C35Cf C34Cf H34C 120.8 . . ?
C36Cf C35Cf C34C 123(5) . . ?
C36Cf C35Cf H35C 118.7 . . ?
C34Cf C35Cf H35C 118.7 . . ?
C35Cf C36Cf C31C 118(5) . . ?
C35Cf C36Cf H36C 120.8 . . ?
C31Cf C36Cf H36C 120.8 . . ?
C1E O1E H1E 111.9 . . ?
O1E C1E C2E 107.5(12) . . ?
O1E C1E H1EA 110.2 . . ?
C2E C1E H1EA 110.2 . . ?
O1E C1E H1EB 110.2 . . ?
C2E C1E H1EB 110.2 . . ?
H1EA C1E H1EB 108.5 . . ?
C1E C2E H2EA 109.5 . . ?
C1E C2E H2EB 109.5 . . ?
H2EA C2E H2EB 109.5 . . ?
C1E C2E H2EC 109.5 . . ?
H2EA C2E H2EC 109.5 . . ?
H2EB C2E H2EC 109.5 . . ?
C3E O2E H2E 124.4 . . ?
C4E C3E O2E 111(3) . . ?
C4E C3E H3E1 109.4 . . ?
O2E C3E H3E1 109.4 . . ?
C4E C3E H3E2 109.4 . . ?
O2E C3E H3E2 109.4 . . ?
H3E1 C3E H3E2 108.0 . . ?
C3E C4E H4E1 109.5 . . ?
C3E C4E H4E2 109.5 . . ?
H4E1 C4E H4E2 109.5 . . ?
C3E C4E H4E3 109.5 . . ?
H4E1 C4E H4E3 109.5 . . ?
H4E2 C4E H4E3 109.5 . . ?

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
C7 N1 C1 C2 20.3(8) . . . . ?
C7 N1 C1 C6 142.0(6) . . . . ?
C8 N2 C2 C1 62.7(5) . . . . ?
C8 N2 C2 C3 -175.1(4) . . . . ?
N1 C1 C2 N2 -51.5(6) . . . . ?
C6 C1 C2 N2 -175.6(4) . . . . ?
N1 C1 C2 C3 -174.2(5) . . . . ?
C6 C1 C2 C3 61.7(6) . . . . ?
N2 C2 C3 C4 -178.8(4) . . . . ?
C1 C2 C3 C4 -58.4(6) . . . . ?
C2 C3 C4 C5 52.2(7) . . . . ?
C3 C4 C5 C6 -51.4(8) . . . . ?
C4 C5 C6 C1 54.8(8) . . . . ?
N1 C1 C6 C5 176.9(6) . . . . ?
C2 C1 C6 C5 -59.8(7) . . . . ?
C1 N1 C7 O1 -176.4(5) . . . . ?
C1 N1 C7 C8 4.6(8) . . . . ?
C2 N2 C8 C9Cc -155.9(4) . . . . ?
C2 N2 C8 C9Bb -155.9(4) . . . . ?
C2 N2 C8 C9Aa -155.9(4) . . . . ?
C2 N2 C8 C7 -38.2(5) . . . . ?
C2 N2 C8 P1 80.0(4) . . . . ?
O1 C7 C8 N2 -175.0(4) . . . . ?
N1 C7 C8 N2 4.1(6) . . . . ?
O1 C7 C8 C9Cc -54.9(6) . . . . ?
N1 C7 C8 C9Cc 124.1(5) . . . . ?
O1 C7 C8 C9Bb -54.9(6) . . . . ?
N1 C7 C8 C9Bb 124.1(5) . . . . ?
O1 C7 C8 C9Aa -54.9(6) . . . . ?
N1 C7 C8 C9Aa 124.1(5) . . . . ?
O1 C7 C8 P1 64.9(5) . . . . ?
N1 C7 C8 P1 -116.1(5) . . . . ?
O4 P1 C8 N2 44.4(4) . . . . ?
O2 P1 C8 N2 -77.5(4) . . . . ?
O3 P1 C8 N2 163.0(3) . . . . ?
O4 P1 C8 C9Cc -78.7(4) . . . . ?
O2 P1 C8 C9Cc 159.4(3) . . . . ?
O3 P1 C8 C9Cc 39.9(4) . . . . ?
O4 P1 C8 C9Bb -78.7(4) . . . . ?
O2 P1 C8 C9Bb 159.4(3) . . . . ?
O3 P1 C8 C9Bb 39.9(4) . . . . ?
O4 P1 C8 C9Aa -78.7(4) . . . . ?
O2 P1 C8 C9Aa 159.4(3) . . . . ?
O3 P1 C8 C9Aa 39.9(4) . . . . ?
O4 P1 C8 C7 165.3(3) . . . . ?
O2 P1 C8 C7 43.3(4) . . . . ?
O3 P1 C8 C7 -76.1(4) . . . . ?
N2 C8 C9Aa C10Aa -64.5(6) . . . . ?
C7 C8 C9Aa C10Aa 174.8(4) . . . . ?
P1 C8 C9Aa C10Aa 58.5(5) . . . . ?
C8 C9Aa C10Aa C11Aa -170.0(5) . . . . ?
C9Aa C10Aa C11Aa C12Aa 68.3(8) . . . . ?
C9Aa C10Aa C11Aa C16Aa -121.2(8) . . . . ?
C16Aa C11Aa C12Aa C13Aa 5.1(13) . . . . ?
C10Aa C11Aa C12Aa C13Aa 175.5(9) . . . . ?
C11Aa C12Aa C13Aa C14Aa -3.2(15) . . . . ?
C12Aa C13Aa C14Aa C15Aa -0.3(18) . . . . ?
C13Aa C14Aa C15Aa C16Aa 1.8(19) . . . . ?
C14Aa C15Aa C16Aa C11Aa 0.1(16) . . . . ?
C12Aa C11Aa C16Aa C15Aa -3.5(14) . . . . ?
C10Aa C11Aa C16Aa C15Aa -173.9(9) . . . . ?
N2 C8 C9Bb C10Bb -64.5(6) . . . . ?
C7 C8 C9Bb C10Bb 174.8(4) . . . . ?
P1 C8 C9Bb C10Bb 58.5(5) . . . . ?
C8 C9Bb C10Bb C11Bb -170.0(5) . . . . ?
C9Bb C10Bb C11Bb C12Bb 120.5(18) . . . . ?
C9Bb C10Bb C11Bb C16Bb -45.8(15) . . . . ?
C10Bb C11Bb C12Bb C13Bb -167.6(16) . . . . ?
C16Bb C11Bb C12Bb C13Bb 0(2) . . . . ?
C11Bb C12Bb C13Bb C14Bb -3(3) . . . . ?
C12Bb C13Bb C14Bb C15Bb 6(5) . . . . ?
C13Bb C14Bb C15Bb C16Bb -6(5) . . . . ?
C14Bb C15Bb C16Bb C11Bb 3(4) . . . . ?
C12Bb C11Bb C16Bb C15Bb 0(3) . . . . ?
C10Bb C11Bb C16Bb C15Bb 169(2) . . . . ?
N2 C8 C9Cc C10Cc 53(3) . . . . ?
C7 C8 C9Cc C10Cc -67(3) . . . . ?
P1 C8 C9Cc C10Cc 176(3) . . . . ?
C8 C9Cc C10Cc C11Cc -179.6(19) . . . . ?
C9Cc C10Cc C11Cc C12Cc 70(4) . . . . ?
C9Cc C10Cc C11Cc C16Cc -107(4) . . . . ?
C16Cc C11Cc C12Cc C13Cc 1(3) . . . . ?
C10Cc C11Cc C12Cc C13Cc -176(3) . . . . ?
C11Cc C12Cc C13Cc C14Cc -1(3) . . . . ?
C12Cc C13Cc C14Cc C15Cc 6(6) . . . . ?
C13Cc C14Cc C15Cc C16Cc -13(9) . . . . ?
C14Cc C15Cc C16Cc C11Cc 13(8) . . . . ?
C12Cc C11Cc C16Cc C15Cc -6(6) . . . . ?
C10Cc C11Cc C16Cc C15Cc 171(4) . . . . ?
C27 N3 C21 C22 16.5(7) . . . . ?
C27 N3 C21 C26 138.3(5) . . . . ?
C28 N4 C22 C21 67.6(5) . . . . ?
C28 N4 C22 C23 -171.0(4) . . . . ?
N3 C21 C22 N4 -51.2(5) . . . . ?
C26 C21 C22 N4 -174.3(4) . . . . ?
N3 C21 C22 C23 -173.8(4) . . . . ?
C26 C21 C22 C23 63.1(5) . . . . ?
N4 C22 C23 C24 -178.8(4) . . . . ?
C21 C22 C23 C24 -59.6(5) . . . . ?
C22 C23 C24 C25 55.9(6) . . . . ?
C23 C24 C25 C26 -55.3(7) . . . . ?
N3 C21 C26 C25 177.6(5) . . . . ?
C22 C21 C26 C25 -60.2(6) . . . . ?
C24 C25 C26 C21 56.5(7) . . . . ?
C21 N3 C27 O5 -173.8(5) . . . . ?
C21 N3 C27 C28 7.6(8) . . . . ?
C22 N4 C28 C27 -43.5(5) . . . . ?
C22 N4 C28 C29Cf -165.8(4) . . . . ?
C22 N4 C28 C29Be -165.8(4) . . . . ?
C22 N4 C28 C29Ad -165.8(4) . . . . ?
C22 N4 C28 P2 76.8(4) . . . . ?
O5 C27 C28 N4 -172.9(4) . . . . ?
N3 C27 C28 N4 5.7(6) . . . . ?
O5 C27 C28 C29Cf -50.5(6) . . . . ?
N3 C27 C28 C29Cf 128.2(5) . . . . ?
O5 C27 C28 C29Be -50.5(6) . . . . ?
N3 C27 C28 C29Be 128.2(5) . . . . ?
O5 C27 C28 C29Ad -50.5(6) . . . . ?
N3 C27 C28 C29Ad 128.2(5) . . . . ?
O5 C27 C28 P2 66.5(5) . . . . ?
N3 C27 C28 P2 -114.8(4) . . . . ?
O8 P2 C28 N4 47.7(4) . . . . ?
O7 P2 C28 N4 170.3(3) . . . . ?
O6 P2 C28 N4 -69.7(3) . . . . ?
O8 P2 C28 C27 168.5(4) . . . . ?
O7 P2 C28 C27 -69.0(4) . . . . ?
O6 P2 C28 C27 51.1(4) . . . . ?
O8 P2 C28 C29Cf -72.1(4) . . . . ?
O7 P2 C28 C29Cf 50.4(4) . . . . ?
O6 P2 C28 C29Cf 170.5(3) . . . . ?
O8 P2 C28 C29Be -72.1(4) . . . . ?
O7 P2 C28 C29Be 50.4(4) . . . . ?
O6 P2 C28 C29Be 170.5(3) . . . . ?
O8 P2 C28 C29Ad -72.1(4) . . . . ?
O7 P2 C28 C29Ad 50.4(4) . . . . ?
O6 P2 C28 C29Ad 170.5(3) . . . . ?
N4 C28 C29Ad C30Ad 67.0(7) . . . . ?
C27 C28 C29Ad C30Ad -55.2(7) . . . . ?
P2 C28 C29Ad C30Ad -173.8(5) . . . . ?
C28 C29Ad C30Ad C31Ad 173.3(7) . . . . ?
C29Ad C30Ad C31Ad C32Ad -114.1(10) . . . . ?
C29Ad C30Ad C31Ad C36Ad 64.0(11) . . . . ?
C36Ad C31Ad C32Ad C33Ad -0.7(14) . . . . ?
C30Ad C31Ad C32Ad C33Ad 177.4(10) . . . . ?
C31Ad C32Ad C33Ad C34Ad -1.4(15) . . . . ?
C32Ad C33Ad C34Ad C35Ad 1.9(18) . . . . ?
C33Ad C34Ad C35Ad C36Ad -0.2(19) . . . . ?
C34Ad C35Ad C36Ad C31Ad -2.0(19) . . . . ?
C32Ad C31Ad C36Ad C35Ad 2.4(16) . . . . ?
C30Ad C31Ad C36Ad C35Ad -175.7(10) . . . . ?
N4 C28 C29Be C30Be 61.2(12) . . . . ?
C27 C28 C29Be C30Be -61.0(12) . . . . ?
P2 C28 C29Be C30Be -179.6(11) . . . . ?
C28 C29Be C30Be C31Be -174.2(14) . . . . ?
C29Be C30Be C31Be C36Be 67(2) . . . . ?
C29Be C30Be C31Be C32Be -105.1(18) . . . . ?
C36Be C31Be C32Be C33Be 0.1(18) . . . . ?
C30Be C31Be C32Be C33Be 172.2(17) . . . . ?
C31Be C32Be C33Be C34Be -2.6(19) . . . . ?
C32Be C33Be C34Be C35Be 5(3) . . . . ?
C33Be C34Be C35Be C36Be -6(4) . . . . ?
C30Be C31Be C36Be C35Be -172.0(19) . . . . ?
C32Be C31Be C36Be C35Be 0(3) . . . . ?
C34Be C35Be C36Be C31Be 3(3) . . . . ?
N4 C28 C29Cf C30Cf -53(3) . . . . ?
C27 C28 C29Cf C30Cf -175(3) . . . . ?
P2 C28 C29Cf C30Cf 66(3) . . . . ?
C28 C29Cf C30Cf C31Cf 170(3) . . . . ?
C29Cf C30Cf C31Cf C32Cf 44(6) . . . . ?
C29Cf C30Cf C31Cf C36Cf -140(4) . . . . ?
C36Cf C31Cf C32Cf C33Cf -3(3) . . . . ?
C30Cf C31Cf C32Cf C33Cf 173(4) . . . . ?
C31Cf C32Cf C33Cf C34Cf 0(4) . . . . ?
C32Cf C33Cf C34Cf C35Cf 0(6) . . . . ?
C33Cf C34Cf C35Cf C36Cf 5(8) . . . . ?
C34Cf C35Cf C36Cf C31Cf -9(8) . . . . ?
C32Cf C31Cf C36Cf C35Cf 7(6) . . . . ?
C30Cf C31Cf C36Cf C35Cf -169(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O7 0.82 1.73 2.520(5) 162.8 .
N1 H1N1 O8_$1 0.86 2.09 2.836(6) 145.2 4_456
N2 H1N2 O4_$2 0.89 2.00 2.881(5) 171.0 4_466
N2 H2N2 O4 0.89 2.58 3.071(5) 115.4 .
N2 H2N2 O5_$2 0.89 1.99 2.827(5) 155.2 4_466
O6 H6 O2 1.17 1.31 2.451(5) 162.0 .
N3 H1N3 O4_$3 0.86 2.05 2.847(6) 154.8 4_566
N4 H2N4 O1_$4 0.89 1.95 2.787(5) 155.6 4_556
N4 H2N4 O8 0.89 2.55 3.031(5) 114.4 .
N4 H1N4 O8_$4 0.89 2.09 2.942(5) 161.1 4_556
O1E H1E O7 0.89 2.00 2.880(10) 166.0 .
O2E H2E O3 0.83 2.02 2.74(2) 145.0 .

_refine_diff_density_max         0.986
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.097

####################################################################### 
# 
# 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_ew-ki351e_sq
_database_code_depnum_ccdc_archive 'CCDC 1915269'
loop_
_audit_author_name
_audit_author_address
'Marek Daszkiewicz'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C15 H29 N2 O4 P) [+ solvent]'
_chemical_formula_sum            'C60 H116 N8 O16 P4 [+ solvent]'
_chemical_formula_weight         332.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_H-M_alt        'P 61'
_space_group_name_Hall           'P 61'

_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'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'

_cell_length_a                   26.6639(8)
_cell_length_b                   26.6639(8)
_cell_length_c                   18.0496(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11113.4(7)
_cell_formula_units_Z            24
_cell_measurement_temperature    100.0(3)
_cell_measurement_reflns_used    9858
_cell_measurement_theta_min      2.8600
_cell_measurement_theta_max      21.9710

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_F_000             4320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.076
_exptl_absorpt_coefficient_mu    0.166
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.834
_oxdiff_exptl_absorpt_empirical_full_max 1.239
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(3)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            93137
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.423
_diffrn_reflns_theta_max         25.136
_diffrn_reflns_theta_full        25.136
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_point_group_measured_fraction_full 0.911
_reflns_number_total             12061
_reflns_number_gt                9097
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_max     0.865
_reflns_Friedel_fraction_full    0.865

_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    'SHELXS-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          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)+(0.0518P)²+7.3068P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3382 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         12061
_refine_ls_number_parameters     852
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0646
_refine_ls_wR_factor_ref         0.1310
_refine_ls_wR_factor_gt          0.1200
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         <0.001

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
P1 P 0.36019(7) 0.35893(7) 0.12063(9) 0.0315(4) Uani 1 1 d . . . . .
O1 O 0.2809(2) 0.3161(3) 0.2660(2) 0.0668(17) Uani 1 1 d . . . . .
O2 O 0.39140(18) 0.42165(18) 0.1546(2) 0.0378(11) Uani 1 1 d . . . . .
O3 O 0.37789(18) 0.3247(2) 0.1752(2) 0.0409(11) Uani 1 1 d . . . . .
O4 O 0.37519(19) 0.3573(2) 0.0427(2) 0.0418(12) Uani 1 1 d . . . . .
N1 N 0.2525(2) 0.3779(3) 0.2260(3) 0.0404(15) Uani 1 1 d . . . . .
H1N H 0.241(3) 0.377(3) 0.270(4) 0.049 Uiso 1 1 d . U . . .
N2 N 0.2707(2) 0.3624(2) 0.0798(3) 0.0327(13) Uani 1 1 d . . . . .
H2N H 0.263(3) 0.344(3) 0.042(4) 0.039 Uiso 1 1 d . U . . .
C1 C 0.2415(3) 0.4101(3) 0.1686(3) 0.0355(16) Uani 1 1 d . . . . .
H1A H 0.277242 0.446836 0.159422 0.043 Uiso 1 1 calc R U . . .
C2 C 0.2243(3) 0.3744(3) 0.0986(3) 0.0317(15) Uani 1 1 d . . . . .
H2 H 0.188478 0.337728 0.107381 0.038 Uiso 1 1 calc R U . . .
C3 C 0.2147(3) 0.4067(3) 0.0366(3) 0.0384(16) Uani 1 1 d . . . . .
H3A H 0.203411 0.383394 -0.008053 0.046 Uiso 1 1 calc R U . . .
H3B H 0.250472 0.442448 0.026511 0.046 Uiso 1 1 calc R U . . .
C4 C 0.1677(3) 0.4205(3) 0.0579(4) 0.0494(19) Uani 1 1 d . . . . .
H4A H 0.131063 0.384661 0.063090 0.059 Uiso 1 1 calc R U . . .
H4B H 0.163411 0.443064 0.018850 0.059 Uiso 1 1 calc R U . . .
C5 C 0.1823(3) 0.4545(3) 0.1310(4) 0.0474(18) Uani 1 1 d . . . . .
H5A H 0.216117 0.492402 0.123961 0.057 Uiso 1 1 calc R U . . .
H5B H 0.150203 0.459819 0.145262 0.057 Uiso 1 1 calc R U . . .
C6 C 0.1941(3) 0.4226(3) 0.1922(4) 0.0393(17) Uani 1 1 d . . . . .
H6A H 0.158967 0.386559 0.203194 0.047 Uiso 1 1 calc R U . . .
H6B H 0.205924 0.446081 0.236812 0.047 Uiso 1 1 calc R U . . .
C7 C 0.2721(3) 0.3414(3) 0.2146(3) 0.0396(17) Uani 1 1 d . . . . .
C8 C 0.2826(3) 0.3290(3) 0.1358(3) 0.0344(16) Uani 1 1 d . . . . .
C9A C 0.2439(8) 0.2647(7) 0.1327(10) 0.047(6) Uiso 0.541(11) 1 d . . P A 1
H9A1 H 0.203911 0.255887 0.131547 0.057 Uiso 0.541(11) 1 calc R U P A 1
H9A2 H 0.249213 0.247773 0.177474 0.057 Uiso 0.541(11) 1 calc R U P A 1
C10A C 0.2550(7) 0.2367(6) 0.0657(10) 0.067(5) Uani 0.541(11) 1 d . . P A 1
H10A H 0.291900 0.238258 0.071659 0.081 Uiso 0.541(11) 1 calc R U P A 1
H10B H 0.257060 0.258193 0.021369 0.081 Uiso 0.541(11) 1 calc R U P A 1
C11A C 0.2056(9) 0.1717(9) 0.0564(12) 0.094(6) Uiso 0.541(11) 1 d . . P A 1
H11A H 0.196011 0.155166 0.106334 0.112 Uiso 0.541(11) 1 calc R U P A 1
C12A C 0.2168(14) 0.1425(14) 0.0225(18) 0.169(12) Uiso 0.541(11) 1 d . . P A 1
H12A H 0.181901 0.107355 0.010211 0.254 Uiso 0.541(11) 1 calc R U P A 1
H12B H 0.241653 0.133439 0.051058 0.254 Uiso 0.541(11) 1 calc R U P A 1
H12C H 0.236308 0.162073 -0.022139 0.254 Uiso 0.541(11) 1 calc R U P A 1
C13A C 0.1546(8) 0.1665(8) 0.0268(11) 0.080(6) Uiso 0.541(11) 1 d . . P A 1
H13A H 0.126660 0.126248 0.019932 0.119 Uiso 0.541(11) 1 calc R U P A 1
H13B H 0.162921 0.186040 -0.020113 0.119 Uiso 0.541(11) 1 calc R U P A 1
H13C H 0.139342 0.183520 0.060174 0.119 Uiso 0.541(11) 1 calc R U P A 1
C9B C 0.2545(7) 0.2612(8) 0.1143(11) 0.027(5) Uiso 0.459(11) 1 d . . P A 2
H9B1 H 0.269813 0.258167 0.066890 0.033 Uiso 0.459(11) 1 calc R U P A 2
H9B2 H 0.265964 0.242358 0.151098 0.033 Uiso 0.459(11) 1 calc R U P A 2
C10B C 0.1886(7) 0.2294(6) 0.1098(8) 0.041(4) Uani 0.459(11) 1 d . . P A 2
H10C H 0.173659 0.231446 0.158101 0.049 Uiso 0.459(11) 1 calc R U P A 2
H10D H 0.177518 0.250059 0.075245 0.049 Uiso 0.459(11) 1 calc R U P A 2
C11B C 0.1589(8) 0.1662(8) 0.0863(10) 0.059(5) Uiso 0.459(11) 1 d . . P A 2
H11B H 0.177399 0.166283 0.039298 0.071 Uiso 0.459(11) 1 calc R U P A 2
C12B C 0.1739(12) 0.1332(11) 0.1369(14) 0.111(9) Uiso 0.459(11) 1 d . . P A 2
H12D H 0.140800 0.095373 0.144048 0.167 Uiso 0.459(11) 1 calc R U P A 2
H12E H 0.185588 0.152893 0.183645 0.167 Uiso 0.459(11) 1 calc R U P A 2
H12F H 0.205115 0.129516 0.116394 0.167 Uiso 0.459(11) 1 calc R U P A 2
C13B C 0.1008(17) 0.1410(17) 0.070(2) 0.179(15) Uiso 0.459(11) 1 d . . P A 2
H13D H 0.095506 0.136595 0.017108 0.268 Uiso 0.459(11) 1 calc R U P A 2
H13E H 0.086256 0.165211 0.087763 0.268 Uiso 0.459(11) 1 calc R U P A 2
H13F H 0.080087 0.103686 0.093059 0.268 Uiso 0.459(11) 1 calc R U P A 2
C14 C 0.4063(3) 0.4717(3) 0.1084(4) 0.059(2) Uani 1 1 d . . . . .
H14A H 0.389564 0.459075 0.060144 0.088 Uiso 1 1 calc R U . . .
H14B H 0.447693 0.494626 0.103977 0.088 Uiso 1 1 calc R U . . .
H14C H 0.391668 0.494543 0.130511 0.088 Uiso 1 1 calc R U . . .
C15 C 0.4365(3) 0.3338(4) 0.1732(4) 0.054(2) Uani 1 1 d . . . . .
H15A H 0.449223 0.337689 0.122686 0.080 Uiso 1 1 calc R U . . .
H15B H 0.436859 0.301320 0.195519 0.080 Uiso 1 1 calc R U . . .
H15C H 0.462046 0.368425 0.200037 0.080 Uiso 1 1 calc R U . . .
P2 P 0.22081(7) 0.38216(7) 0.45019(9) 0.0288(4) Uani 1 1 d . . . . .
O5 O 0.2797(2) 0.35919(19) 0.5955(2) 0.0451(12) Uani 1 1 d . . . . .
O6 O 0.15830(17) 0.34519(18) 0.4834(2) 0.0340(10) Uani 1 1 d . . . . .
O7 O 0.2494(2) 0.43592(19) 0.5037(3) 0.0494(13) Uani 1 1 d . . . . .
O8 O 0.22165(18) 0.39808(19) 0.3721(2) 0.0383(11) Uani 1 1 d . . . . .
N3 N 0.2212(2) 0.2663(2) 0.5621(3) 0.0319(13) Uani 1 1 d . . . . .
H3N H 0.214(3) 0.253(3) 0.611(4) 0.038 Uiso 1 1 d . U . . .
N4 N 0.2273(2) 0.2941(2) 0.4142(3) 0.0293(12) Uani 1 1 d . . . . .
H4N H 0.245(3) 0.310(3) 0.374(4) 0.035 Uiso 1 1 d . U . . .
C21 C 0.1887(3) 0.2203(3) 0.5077(3) 0.0351(16) Uani 1 1 d . . . . .
H21 H 0.150153 0.215778 0.501338 0.042 Uiso 1 1 calc R U . . .
C22 C 0.2204(3) 0.2383(3) 0.4349(3) 0.0313(15) Uani 1 1 d . . . . .
H22 H 0.258570 0.241734 0.440316 0.038 Uiso 1 1 calc R U . . .
C23 C 0.1854(3) 0.1926(3) 0.3770(3) 0.0434(18) Uani 1 1 d . . . . .
H23A H 0.205411 0.203694 0.329792 0.052 Uiso 1 1 calc R U . . .
H23B H 0.147920 0.189673 0.370942 0.052 Uiso 1 1 calc R U . . .
C24 C 0.1772(3) 0.1340(3) 0.4009(4) 0.055(2) Uani 1 1 d . . . . .
H24A H 0.153176 0.104784 0.364879 0.065 Uiso 1 1 calc R U . . .
H24B H 0.214596 0.136043 0.402087 0.065 Uiso 1 1 calc R U . . .
C25 C 0.1491(4) 0.1164(3) 0.4772(4) 0.067(2) Uani 1 1 d . . . . .
H25A H 0.109533 0.108840 0.474216 0.080 Uiso 1 1 calc R U . . .
H25B H 0.147844 0.081020 0.492727 0.080 Uiso 1 1 calc R U . . .
C26 C 0.1820(4) 0.1633(3) 0.5339(4) 0.052(2) Uani 1 1 d . . . . .
H26A H 0.219956 0.167564 0.541612 0.062 Uiso 1 1 calc R U . . .
H26B H 0.161433 0.152501 0.580698 0.062 Uiso 1 1 calc R U . . .
C27 C 0.2531(3) 0.3222(3) 0.5473(3) 0.0311(15) Uani 1 1 d . . . . .
C28 C 0.2591(3) 0.3421(3) 0.4659(3) 0.0289(14) Uani 1 1 d . . . . .
C29 C 0.3241(3) 0.3813(3) 0.4472(4) 0.0401(17) Uani 1 1 d . . . . .
H29A H 0.327495 0.397750 0.398226 0.048 Uiso 1 1 calc R U . . .
H29B H 0.341107 0.413052 0.482329 0.048 Uiso 1 1 calc R U . . .
C30 C 0.3584(3) 0.3493(3) 0.4489(5) 0.057(2) Uani 1 1 d . . . . .
H30A H 0.354363 0.332408 0.497650 0.068 Uiso 1 1 calc R U . . .
H30B H 0.341498 0.317869 0.413354 0.068 Uiso 1 1 calc R U . . .
C31 C 0.4229(3) 0.3872(4) 0.4316(4) 0.062(2) Uani 1 1 d . . . . .
H31 H 0.437549 0.360055 0.429014 0.074 Uiso 1 1 calc R U . . .
C32 C 0.4538(4) 0.4248(5) 0.4910(6) 0.127(5) Uani 1 1 d . . . . .
H32A H 0.494469 0.445085 0.479877 0.191 Uiso 1 1 calc R U . . .
H32B H 0.447101 0.402514 0.535489 0.191 Uiso 1 1 calc R U . . .
H32C H 0.440816 0.452128 0.498006 0.191 Uiso 1 1 calc R U . . .
C33 C 0.4332(3) 0.4130(4) 0.3574(5) 0.068(3) Uani 1 1 d . . . . .
H33A H 0.422975 0.442814 0.356855 0.102 Uiso 1 1 calc R U . . .
H33B H 0.409970 0.383680 0.321903 0.102 Uiso 1 1 calc R U . . .
H33C H 0.473392 0.429498 0.344835 0.102 Uiso 1 1 calc R U . . .
C34 C 0.1094(3) 0.3092(3) 0.4356(4) 0.0470(19) Uani 1 1 d . . . . .
H34A H 0.119274 0.321923 0.385180 0.071 Uiso 1 1 calc R U . . .
H34B H 0.076524 0.312319 0.450371 0.071 Uiso 1 1 calc R U . . .
H34C H 0.100256 0.269595 0.439496 0.071 Uiso 1 1 calc R U . . .
C35 C 0.2314(4) 0.4792(4) 0.4946(6) 0.084(3) Uani 1 1 d . . . . .
H35A H 0.247685 0.500565 0.449722 0.125 Uiso 1 1 calc R U . . .
H35B H 0.244680 0.505210 0.536013 0.125 Uiso 1 1 calc R U . . .
H35C H 0.189883 0.460078 0.491938 0.125 Uiso 1 1 calc R U . . .
P3 P 0.20363(7) 0.22918(7) 0.78586(9) 0.0344(4) Uani 1 1 d . . . . .
O9 O 0.2308(2) 0.3070(3) 0.9316(3) 0.0676(17) Uani 1 1 d . . . . .
O10 O 0.2360(2) 0.2011(2) 0.8246(2) 0.0462(12) Uani 1 1 d . . . . .
O11 O 0.1487(2) 0.2098(2) 0.8368(2) 0.0490(12) Uani 1 1 d . . . . .
O12 O 0.19011(19) 0.2132(2) 0.7077(2) 0.0407(11) Uani 1 1 d . . . . .
N5 N 0.3232(2) 0.3394(2) 0.8969(3) 0.0407(14) Uani 1 1 d . . . . .
H5N H 0.333(3) 0.346(3) 0.946(4) 0.049 Uiso 1 1 d . U . . .
N6 N 0.2946(2) 0.3238(2) 0.7481(3) 0.0309(12) Uani 1 1 d . . . . .
H6N H 0.281(3) 0.332(3) 0.700(4) 0.037 Uiso 1 1 d . U . . .
C41 C 0.3688(3) 0.3556(3) 0.8416(3) 0.0300(15) Uani 1 1 d . . . . .
H41 H 0.372591 0.321588 0.830955 0.036 Uiso 1 1 calc R U . . .
C42 C 0.3502(3) 0.3725(3) 0.7716(3) 0.0291(14) Uani 1 1 d . . . . .
H42 H 0.345490 0.406086 0.781720 0.035 Uiso 1 1 calc R U . . .
C43 C 0.3958(3) 0.3883(3) 0.7121(3) 0.0339(15) Uani 1 1 d . . . . .
H43A H 0.398518 0.354339 0.699480 0.041 Uiso 1 1 calc R U . . .
H43B H 0.384392 0.400731 0.667877 0.041 Uiso 1 1 calc R U . . .
C44 C 0.4543(3) 0.4360(3) 0.7377(4) 0.0414(17) Uani 1 1 d . . . . .
H44A H 0.452846 0.471432 0.744017 0.050 Uiso 1 1 calc R U . . .
H44B H 0.483025 0.442961 0.700142 0.050 Uiso 1 1 calc R U . . .
C45 C 0.4722(3) 0.4207(3) 0.8107(4) 0.0463(18) Uani 1 1 d . . . . .
H45A H 0.479642 0.389012 0.802434 0.056 Uiso 1 1 calc R U . . .
H45B H 0.507924 0.453781 0.827889 0.056 Uiso 1 1 calc R U . . .
C46 C 0.4261(3) 0.4032(3) 0.8701(3) 0.0366(16) Uani 1 1 d . . . . .
H46A H 0.437191 0.389983 0.913855 0.044 Uiso 1 1 calc R U . . .
H46B H 0.422461 0.436467 0.883940 0.044 Uiso 1 1 calc R U . . .
C47 C 0.2670(3) 0.3181(3) 0.8824(3) 0.0439(18) Uani 1 1 d . . . . .
C48 C 0.2468(3) 0.3074(3) 0.8011(3) 0.0337(15) Uani 1 1 d . . . . .
C49A C 0.2189(8) 0.3464(9) 0.7987(11) 0.052(5) Uiso 0.493(12) 1 d . . P B 3
H49A H 0.180138 0.320322 0.780680 0.062 Uiso 0.493(12) 1 calc R U P B 3
H49B H 0.214140 0.352165 0.850726 0.062 Uiso 0.493(12) 1 calc R U P B 3
C50A C 0.2303(6) 0.3925(5) 0.7710(9) 0.042(4) Uani 0.493(12) 1 d . . P B 3
H50A H 0.254837 0.396733 0.728992 0.050 Uiso 0.493(12) 1 calc R U P B 3
H50B H 0.255370 0.421347 0.806754 0.050 Uiso 0.493(12) 1 calc R U P B 3
C51A C 0.1904(7) 0.4141(8) 0.7430(8) 0.051(4) Uiso 0.493(12) 1 d D . P B 3
H51A H 0.212112 0.456454 0.745964 0.062 Uiso 0.493(12) 1 calc R U P B 3
C52A C 0.1706(11) 0.3990(11) 0.6673(11) 0.105(8) Uiso 0.493(12) 1 d D . P B 3
H52A H 0.203277 0.410751 0.635221 0.157 Uiso 0.493(12) 1 calc R U P B 3
H52B H 0.149877 0.418314 0.652955 0.157 Uiso 0.493(12) 1 calc R U P B 3
H52C H 0.145385 0.357847 0.663604 0.157 Uiso 0.493(12) 1 calc R U P B 3
C53A C 0.1361(9) 0.3932(9) 0.7914(11) 0.057(5) Uiso 0.493(12) 1 d . . P B 3
H53A H 0.114606 0.411134 0.775068 0.086 Uiso 0.493(12) 1 calc R U P B 3
H53B H 0.147503 0.403436 0.842149 0.086 Uiso 0.493(12) 1 calc R U P B 3
H53C H 0.112428 0.351872 0.787345 0.086 Uiso 0.493(12) 1 calc R U P B 3
C49B C 0.2037(7) 0.3282(7) 0.7762(10) 0.031(4) Uiso 0.502(12) 1 d . . P B 4
H49C H 0.169658 0.303034 0.805243 0.038 Uiso 0.502(12) 1 calc R U P B 4
H49D H 0.220183 0.365567 0.800566 0.038 Uiso 0.502(12) 1 calc R U P B 4
C50B C 0.1845(6) 0.3353(7) 0.7274(7) 0.042(4) Uani 0.502(12) 1 d . . P B 4
H50C H 0.151097 0.297964 0.716114 0.051 Uiso 0.502(12) 1 calc R U P B 4
H50D H 0.212089 0.343247 0.687842 0.051 Uiso 0.502(12) 1 calc R U P B 4
C51B C 0.1634(7) 0.3805(7) 0.7166(10) 0.055(5) Uiso 0.502(12) 1 d D . P B 4
H51B H 0.141438 0.368119 0.670209 0.066 Uiso 0.502(12) 1 calc R U P B 4
C52B C 0.2096(8) 0.4442(8) 0.7014(12) 0.086(6) Uiso 0.502(12) 1 d D . P B 4
H52D H 0.231829 0.461030 0.745500 0.129 Uiso 0.502(12) 1 calc R U P B 4
H52E H 0.190851 0.465376 0.686771 0.129 Uiso 0.502(12) 1 calc R U P B 4
H52F H 0.234804 0.445701 0.662362 0.129 Uiso 0.502(12) 1 calc R U P B 4
C53B C 0.1183(10) 0.3720(10) 0.7735(12) 0.078(7) Uiso 0.502(12) 1 d . . P B 4
H53D H 0.090449 0.331503 0.777842 0.116 Uiso 0.502(12) 1 calc R U P B 4
H53E H 0.099024 0.392584 0.758236 0.116 Uiso 0.502(12) 1 calc R U P B 4
H53F H 0.136631 0.386553 0.820549 0.116 Uiso 0.502(12) 1 calc R U P B 4
C54 C 0.2711(3) 0.1840(3) 0.7832(4) 0.0538(19) Uani 1 1 d . . . . .
H54A H 0.252992 0.168140 0.736409 0.081 Uiso 1 1 calc R U . . .
H54B H 0.275006 0.155246 0.810596 0.081 Uiso 1 1 calc R U . . .
H54C H 0.308676 0.217114 0.775063 0.081 Uiso 1 1 calc R U . . .
C55 C 0.1034(3) 0.1503(4) 0.8384(5) 0.071(3) Uani 1 1 d . . . . .
H55A H 0.070907 0.147005 0.865456 0.106 Uiso 1 1 calc R U . . .
H55B H 0.117341 0.127388 0.862200 0.106 Uiso 1 1 calc R U . . .
H55C H 0.091741 0.136685 0.788680 0.106 Uiso 1 1 calc R U . . .
P4 P 0.58510(7) 0.23040(7) 0.06282(8) 0.0282(4) Uani 1 1 d . . . . .
O13 O 0.62329(17) 0.29400(18) 0.2240(2) 0.0345(10) Uani 1 1 d . . . . .
O14 O 0.61827(19) 0.19630(17) 0.0753(2) 0.0371(11) Uani 1 1 d . . . . .
O15 O 0.53438(18) 0.20313(17) 0.1195(2) 0.0425(11) Uani 1 1 d . . . . .
O16 O 0.56471(18) 0.22820(18) -0.0134(2) 0.0360(11) Uani 1 1 d . . . . .
N7 N 0.7116(2) 0.3194(2) 0.1793(3) 0.0284(12) Uani 1 1 d . . . . .
H7N H 0.726(3) 0.321(3) 0.221(3) 0.034 Uiso 1 1 d . U . . .
N8 N 0.6790(2) 0.3244(2) 0.0346(3) 0.0270(12) Uani 1 1 d . . . . .
H8N H 0.668(3) 0.340(3) -0.006(3) 0.032 Uiso 1 1 d . U . . .
C61 C 0.7533(2) 0.3334(3) 0.1186(3) 0.0296(14) Uani 1 1 d . . . . .
H61 H 0.748911 0.297140 0.098995 0.036 Uiso 1 1 calc R U . . .
C62 C 0.7388(2) 0.3630(2) 0.0578(3) 0.0264(14) Uani 1 1 d . . . . .
H62 H 0.742454 0.399002 0.077035 0.032 Uiso 1 1 calc R U . . .
C63 C 0.7796(3) 0.3768(3) -0.0076(3) 0.0353(16) Uani 1 1 d . . . . .
H63A H 0.771270 0.398029 -0.044604 0.042 Uiso 1 1 calc R U . . .
H63B H 0.773327 0.341059 -0.029891 0.042 Uiso 1 1 calc R U . . .
C64 C 0.8427(3) 0.4129(3) 0.0168(3) 0.0406(17) Uani 1 1 d . . . . .
H64A H 0.850282 0.450801 0.032777 0.049 Uiso 1 1 calc R U . . .
H64B H 0.867835 0.418227 -0.024892 0.049 Uiso 1 1 calc R U . . .
C65 C 0.8563(3) 0.3835(3) 0.0802(3) 0.0431(17) Uani 1 1 d . . . . .
H65A H 0.853152 0.347680 0.062595 0.052 Uiso 1 1 calc R U . . .
H65B H 0.895807 0.408557 0.096840 0.052 Uiso 1 1 calc R U . . .
C66 C 0.8149(3) 0.3706(3) 0.1450(3) 0.0369(16) Uani 1 1 d . . . . .
H66A H 0.823233 0.350591 0.183737 0.044 Uiso 1 1 calc R U . . .
H66B H 0.820072 0.406562 0.165327 0.044 Uiso 1 1 calc R U . . .
C67 C 0.6563(3) 0.3055(2) 0.1713(3) 0.0271(14) Uani 1 1 d . . . . .
C68 C 0.6338(2) 0.3052(2) 0.0924(3) 0.0255(14) Uani 1 1 d . . . . .
C69 C 0.5992(3) 0.3374(2) 0.0927(3) 0.0290(14) Uani 1 1 d . . . . .
H69A H 0.580414 0.331865 0.044908 0.035 Uiso 1 1 calc R U . . .
H69B H 0.569013 0.320003 0.129911 0.035 Uiso 1 1 calc R U . . .
C70 C 0.6353(3) 0.4020(3) 0.1079(4) 0.0371(16) Uani 1 1 d . . . . .
H70A H 0.662846 0.420098 0.067913 0.045 Uiso 1 1 calc R U . . .
H70B H 0.657088 0.407727 0.153229 0.045 Uiso 1 1 calc R U . . .
C71 C 0.5995(3) 0.4321(3) 0.1156(5) 0.059(2) Uani 1 1 d . . . . .
H71 H 0.568604 0.409951 0.151488 0.071 Uiso 1 1 calc R U . . .
C72 C 0.5717(4) 0.4330(4) 0.0447(6) 0.085(3) Uani 1 1 d . . . . .
H72A H 0.600875 0.452018 0.007351 0.127 Uiso 1 1 calc R U . . .
H72B H 0.550999 0.453537 0.051447 0.127 Uiso 1 1 calc R U . . .
H72C H 0.545203 0.394004 0.029336 0.127 Uiso 1 1 calc R U . . .
C73 C 0.6351(4) 0.4928(3) 0.1451(5) 0.080(3) Uani 1 1 d . . . . .
H73A H 0.667015 0.514992 0.112350 0.120 Uiso 1 1 calc R U . . .
H73B H 0.649530 0.491584 0.193429 0.120 Uiso 1 1 calc R U . . .
H73C H 0.611373 0.510393 0.148397 0.120 Uiso 1 1 calc R U . . .
C74 C 0.6486(3) 0.1866(3) 0.0149(4) 0.0475(19) Uani 1 1 d . . . . .
H74A H 0.620901 0.159863 -0.019931 0.071 Uiso 1 1 calc R U . . .
H74B H 0.671328 0.170825 0.034277 0.071 Uiso 1 1 calc R U . . .
H74C H 0.673507 0.222655 -0.009512 0.071 Uiso 1 1 calc R U . . .
C75A C 0.5259(6) 0.1690(6) 0.1799(7) 0.042(4) Uiso 0.59(2) 1 d . . P C 5
H75A H 0.509208 0.129339 0.164473 0.063 Uiso 0.59(2) 1 calc R U P C 5
H75B H 0.500207 0.172523 0.213958 0.063 Uiso 0.59(2) 1 calc R U P C 5
H75C H 0.562371 0.181002 0.203778 0.063 Uiso 0.59(2) 1 calc R U P C 5
C75B C 0.5020(8) 0.1441(8) 0.1374(10) 0.043(6) Uiso 0.41(2) 1 d . . P C 6
H75D H 0.487567 0.121815 0.092765 0.064 Uiso 0.41(2) 1 calc R U P C 6
H75E H 0.470033 0.137519 0.168485 0.064 Uiso 0.41(2) 1 calc R U P C 6
H75F H 0.526148 0.132684 0.163139 0.064 Uiso 0.41(2) 1 calc R U P C 6


_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 O4 1.470(4) . ?
P1 O3 1.567(4) . ?
P1 O2 1.573(5) . ?
P1 C8 1.827(7) . ?
O1 C7 1.238(7) . ?
O2 C14 1.450(8) . ?
O3 C15 1.458(8) . ?
N1 C7 1.331(8) . ?
N1 C1 1.465(8) . ?
N2 C2 1.462(8) . ?
N2 C8 1.483(8) . ?
C1 C2 1.510(8) . ?
C1 C6 1.523(9) . ?
C2 C3 1.511(8) . ?
C3 C4 1.522(10) . ?
C4 C5 1.536(9) . ?
C5 C6 1.519(9) . ?
C7 C8 1.518(8) . ?
C8 C9A 1.496(18) . ?
C8 C9B 1.62(2) . ?
C9A C10A 1.53(2) . ?
C10A C11A 1.57(2) . ?
C11A C12A 1.14(3) . ?
C11A C13A 1.40(3) . ?
C9B C10B 1.52(2) . ?
C10B C11B 1.52(2) . ?
C11B C13B 1.38(4) . ?
C11B C12B 1.46(3) . ?
P2 O8 1.469(4) . ?
P2 O6 1.571(4) . ?
P2 O7 1.574(5) . ?
P2 C28 1.832(6) . ?
O5 C27 1.238(7) . ?
O6 C34 1.454(7) . ?
O7 C35 1.464(9) . ?
N3 C27 1.323(8) . ?
N3 C21 1.469(8) . ?
N4 C22 1.453(8) . ?
N4 C28 1.464(8) . ?
C21 C22 1.505(8) . ?
C21 C26 1.513(9) . ?
C22 C23 1.520(9) . ?
C23 C24 1.527(10) . ?
C24 C25 1.526(10) . ?
C25 C26 1.511(10) . ?
C27 C28 1.543(8) . ?
C28 C29 1.548(9) . ?
C29 C30 1.531(9) . ?
C30 C31 1.530(10) . ?
C31 C32 1.416(12) . ?
C31 C33 1.468(11) . ?
P3 O12 1.465(4) . ?
P3 O10 1.564(5) . ?
P3 O11 1.581(5) . ?
P3 C48 1.830(7) . ?
O9 C47 1.234(8) . ?
O10 C54 1.437(8) . ?
O11 C55 1.435(9) . ?
N5 C47 1.336(9) . ?
N5 C41 1.461(8) . ?
N6 C42 1.463(8) . ?
N6 C48 1.474(8) . ?
C41 C42 1.506(8) . ?
C41 C46 1.508(9) . ?
C42 C43 1.517(8) . ?
C43 C44 1.510(9) . ?
C44 C45 1.526(9) . ?
C45 C46 1.520(9) . ?
C47 C48 1.541(9) . ?
C48 C49A 1.553(19) . ?
C48 C49B 1.570(17) . ?
C49A C50A 1.22(2) . ?
C50A C51A 1.53(2) . ?
C51A C52A 1.45(2) . ?
C51A C53A 1.54(2) . ?
C49B C50B 1.082(18) . ?
C50B C51B 1.57(2) . ?
C51B C53B 1.51(3) . ?
C51B C52B 1.54(2) . ?
P4 O16 1.470(4) . ?
P4 O15 1.556(4) . ?
P4 O14 1.570(4) . ?
P4 C68 1.833(6) . ?
O13 C67 1.227(7) . ?
O14 C74 1.456(7) . ?
O15 C75A 1.366(12) . ?
O15 C75B 1.402(17) . ?
N7 C67 1.337(8) . ?
N7 C61 1.468(7) . ?
N8 C62 1.462(7) . ?
N8 C68 1.479(7) . ?
C61 C66 1.510(8) . ?
C61 C62 1.510(8) . ?
C62 C63 1.519(8) . ?
C63 C64 1.527(9) . ?
C64 C65 1.530(9) . ?
C65 C66 1.524(8) . ?
C67 C68 1.543(8) . ?
C68 C69 1.542(8) . ?
C69 C70 1.520(8) . ?
C70 C71 1.529(10) . ?
C71 C72 1.487(12) . ?
C71 C73 1.505(12) . ?

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
O4 P1 O3 114.8(3) . . ?
O4 P1 O2 113.4(3) . . ?
O3 P1 O2 102.7(2) . . ?
O4 P1 C8 113.3(3) . . ?
O3 P1 C8 104.8(3) . . ?
O2 P1 C8 106.8(3) . . ?
C14 O2 P1 120.7(4) . . ?
C15 O3 P1 119.9(4) . . ?
C7 N1 C1 125.9(6) . . ?
C2 N2 C8 115.6(5) . . ?
N1 C1 C2 108.0(5) . . ?
N1 C1 C6 111.2(5) . . ?
C2 C1 C6 110.5(5) . . ?
N2 C2 C1 107.9(5) . . ?
N2 C2 C3 110.9(5) . . ?
C1 C2 C3 110.1(5) . . ?
C2 C3 C4 110.3(5) . . ?
C3 C4 C5 111.2(5) . . ?
C6 C5 C4 111.0(5) . . ?
C5 C6 C1 110.2(6) . . ?
O1 C7 N1 122.3(6) . . ?
O1 C7 C8 118.5(6) . . ?
N1 C7 C8 119.2(5) . . ?
N2 C8 C9A 115.5(8) . . ?
N2 C8 C7 112.8(5) . . ?
C9A C8 C7 100.8(8) . . ?
N2 C8 C9B 112.9(8) . . ?
C7 C8 C9B 115.7(9) . . ?
N2 C8 P1 99.9(4) . . ?
C9A C8 P1 118.6(8) . . ?
C7 C8 P1 109.7(4) . . ?
C9B C8 P1 104.2(7) . . ?
C8 C9A C10A 113.5(13) . . ?
C9A C10A C11A 111.3(15) . . ?
C12A C11A C13A 107(2) . . ?
C12A C11A C10A 117(3) . . ?
C13A C11A C10A 112.7(17) . . ?
C10B C9B C8 113.3(13) . . ?
C11B C10B C9B 116.5(14) . . ?
C13B C11B C12B 115(2) . . ?
C13B C11B C10B 116(2) . . ?
C12B C11B C10B 110.3(17) . . ?
O8 P2 O6 114.0(2) . . ?
O8 P2 O7 113.3(3) . . ?
O6 P2 O7 102.5(3) . . ?
O8 P2 C28 112.6(3) . . ?
O6 P2 C28 107.5(3) . . ?
O7 P2 C28 106.2(3) . . ?
C34 O6 P2 120.4(4) . . ?
C35 O7 P2 116.6(4) . . ?
C27 N3 C21 125.8(5) . . ?
C22 N4 C28 116.9(5) . . ?
N3 C21 C22 108.3(5) . . ?
N3 C21 C26 110.7(5) . . ?
C22 C21 C26 111.0(5) . . ?
N4 C22 C21 108.4(5) . . ?
N4 C22 C23 110.9(5) . . ?
C21 C22 C23 108.8(5) . . ?
C22 C23 C24 110.1(5) . . ?
C25 C24 C23 111.4(6) . . ?
C26 C25 C24 111.3(6) . . ?
C25 C26 C21 110.3(6) . . ?
O5 C27 N3 123.0(6) . . ?
O5 C27 C28 118.4(5) . . ?
N3 C27 C28 118.6(5) . . ?
N4 C28 C27 113.0(5) . . ?
N4 C28 C29 114.5(5) . . ?
C27 C28 C29 109.2(5) . . ?
N4 C28 P2 99.4(4) . . ?
C27 C28 P2 110.8(4) . . ?
C29 C28 P2 109.5(4) . . ?
C30 C29 C28 113.4(5) . . ?
C31 C30 C29 114.6(6) . . ?
C32 C31 C33 117.0(9) . . ?
C32 C31 C30 112.1(7) . . ?
C33 C31 C30 112.3(6) . . ?
O12 P3 O10 114.0(3) . . ?
O12 P3 O11 114.3(3) . . ?
O10 P3 O11 103.1(3) . . ?
O12 P3 C48 113.5(3) . . ?
O10 P3 C48 107.2(3) . . ?
O11 P3 C48 103.8(3) . . ?
C54 O10 P3 121.5(4) . . ?
C55 O11 P3 120.2(5) . . ?
C47 N5 C41 125.6(5) . . ?
C42 N6 C48 114.6(5) . . ?
N5 C41 C42 108.1(5) . . ?
N5 C41 C46 110.9(5) . . ?
C42 C41 C46 112.3(5) . . ?
N6 C42 C41 108.4(5) . . ?
N6 C42 C43 110.8(5) . . ?
C41 C42 C43 109.8(5) . . ?
C44 C43 C42 111.3(5) . . ?
C43 C44 C45 111.6(6) . . ?
C46 C45 C44 112.1(5) . . ?
C41 C46 C45 109.9(5) . . ?
O9 C47 N5 122.6(6) . . ?
O9 C47 C48 118.9(6) . . ?
N5 C47 C48 118.6(6) . . ?
N6 C48 C47 113.2(5) . . ?
N6 C48 C49A 114.6(8) . . ?
C47 C48 C49A 98.2(9) . . ?
N6 C48 C49B 112.7(7) . . ?
C47 C48 C49B 117.1(8) . . ?
N6 C48 P3 101.5(4) . . ?
C47 C48 P3 108.5(4) . . ?
C49A C48 P3 121.4(9) . . ?
C49B C48 P3 101.8(7) . . ?
C50A C49A C48 136.6(15) . . ?
C49A C50A C51A 130.4(15) . . ?
C52A C51A C50A 115.7(16) . . ?
C52A C51A C53A 106.8(17) . . ?
C50A C51A C53A 112.5(14) . . ?
C50B C49B C48 142.1(14) . . ?
C49B C50B C51B 128.1(15) . . ?
C53B C51B C52B 115.0(16) . . ?
C53B C51B C50B 111.3(14) . . ?
C52B C51B C50B 118.0(13) . . ?
O16 P4 O15 112.3(3) . . ?
O16 P4 O14 114.6(2) . . ?
O15 P4 O14 104.2(2) . . ?
O16 P4 C68 111.3(3) . . ?
O15 P4 C68 107.1(2) . . ?
O14 P4 C68 106.9(3) . . ?
C74 O14 P4 121.3(4) . . ?
C75A O15 P4 130.7(6) . . ?
C75B O15 P4 125.4(8) . . ?
C67 N7 C61 125.4(5) . . ?
C62 N8 C68 117.1(4) . . ?
N7 C61 C66 111.6(5) . . ?
N7 C61 C62 108.4(5) . . ?
C66 C61 C62 111.4(5) . . ?
N8 C62 C61 108.4(5) . . ?
N8 C62 C63 110.2(5) . . ?
C61 C62 C63 110.7(5) . . ?
C62 C63 C64 111.0(5) . . ?
C63 C64 C65 111.2(5) . . ?
C66 C65 C64 111.0(5) . . ?
C61 C66 C65 109.5(5) . . ?
O13 C67 N7 122.7(5) . . ?
O13 C67 C68 119.0(5) . . ?
N7 C67 C68 118.3(5) . . ?
N8 C68 C69 114.8(5) . . ?
N8 C68 C67 113.6(5) . . ?
C69 C68 C67 109.5(5) . . ?
N8 C68 P4 100.5(4) . . ?
C69 C68 P4 108.2(4) . . ?
C67 C68 P4 109.7(4) . . ?
C70 C69 C68 114.5(5) . . ?
C69 C70 C71 113.8(6) . . ?
C72 C71 C73 109.8(7) . . ?
C72 C71 C70 112.2(7) . . ?
C73 C71 C70 112.0(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
O4 P1 O2 C14 30.5(6) . . . . ?
O3 P1 O2 C14 155.0(5) . . . . ?
C8 P1 O2 C14 -95.0(5) . . . . ?
O4 P1 O3 C15 49.3(6) . . . . ?
O2 P1 O3 C15 -74.2(5) . . . . ?
C8 P1 O3 C15 174.3(5) . . . . ?
C7 N1 C1 C2 30.3(9) . . . . ?
C7 N1 C1 C6 151.7(6) . . . . ?
C8 N2 C2 C1 61.3(7) . . . . ?
C8 N2 C2 C3 -178.0(5) . . . . ?
N1 C1 C2 N2 -56.6(6) . . . . ?
C6 C1 C2 N2 -178.5(5) . . . . ?
N1 C1 C2 C3 -177.9(5) . . . . ?
C6 C1 C2 C3 60.3(7) . . . . ?
N2 C2 C3 C4 -178.3(5) . . . . ?
C1 C2 C3 C4 -58.8(7) . . . . ?
C2 C3 C4 C5 56.0(7) . . . . ?
C3 C4 C5 C6 -54.4(8) . . . . ?
C4 C5 C6 C1 55.2(8) . . . . ?
N1 C1 C6 C5 -178.3(5) . . . . ?
C2 C1 C6 C5 -58.4(7) . . . . ?
C1 N1 C7 O1 179.3(7) . . . . ?
C1 N1 C7 C8 -2.4(10) . . . . ?
C2 N2 C8 C9A 82.7(10) . . . . ?
C2 N2 C8 C7 -32.6(8) . . . . ?
C2 N2 C8 C9B 101.0(9) . . . . ?
C2 N2 C8 P1 -148.9(4) . . . . ?
O1 C7 C8 N2 -179.7(6) . . . . ?
N1 C7 C8 N2 1.9(9) . . . . ?
O1 C7 C8 C9A 56.5(10) . . . . ?
N1 C7 C8 C9A -121.9(9) . . . . ?
O1 C7 C8 C9B 48.1(11) . . . . ?
N1 C7 C8 C9B -130.3(9) . . . . ?
O1 C7 C8 P1 -69.4(7) . . . . ?
N1 C7 C8 P1 112.3(6) . . . . ?
O4 P1 C8 N2 -51.9(5) . . . . ?
O3 P1 C8 N2 -177.8(4) . . . . ?
O2 P1 C8 N2 73.7(4) . . . . ?
O4 P1 C8 C9A 74.5(9) . . . . ?
O3 P1 C8 C9A -51.4(9) . . . . ?
O2 P1 C8 C9A -160.0(8) . . . . ?
O4 P1 C8 C7 -170.5(4) . . . . ?
O3 P1 C8 C7 63.5(5) . . . . ?
O2 P1 C8 C7 -45.0(5) . . . . ?
O4 P1 C8 C9B 65.0(8) . . . . ?
O3 P1 C8 C9B -61.0(8) . . . . ?
O2 P1 C8 C9B -169.5(7) . . . . ?
N2 C8 C9A C10A 71.4(15) . . . . ?
C7 C8 C9A C10A -166.7(11) . . . . ?
P1 C8 C9A C10A -47.0(14) . . . . ?
C8 C9A C10A C11A -168.7(13) . . . . ?
C9A C10A C11A C12A -159(3) . . . . ?
C9A C10A C11A C13A 76(2) . . . . ?
N2 C8 C9B C10B -62.5(15) . . . . ?
C7 C8 C9B C10B 69.6(14) . . . . ?
P1 C8 C9B C10B -169.9(11) . . . . ?
C8 C9B C10B C11B 177.1(13) . . . . ?
C9B C10B C11B C13B -169(2) . . . . ?
C9B C10B C11B C12B 58(2) . . . . ?
O8 P2 O6 C34 26.4(5) . . . . ?
O7 P2 O6 C34 149.1(5) . . . . ?
C28 P2 O6 C34 -99.2(5) . . . . ?
O8 P2 O7 C35 48.0(7) . . . . ?
O6 P2 O7 C35 -75.2(6) . . . . ?
C28 P2 O7 C35 172.1(6) . . . . ?
C27 N3 C21 C22 30.6(8) . . . . ?
C27 N3 C21 C26 152.5(6) . . . . ?
C28 N4 C22 C21 59.3(7) . . . . ?
C28 N4 C22 C23 178.7(5) . . . . ?
N3 C21 C22 N4 -56.1(6) . . . . ?
C26 C21 C22 N4 -177.9(6) . . . . ?
N3 C21 C22 C23 -176.8(5) . . . . ?
C26 C21 C22 C23 61.4(7) . . . . ?
N4 C22 C23 C24 -178.5(5) . . . . ?
C21 C22 C23 C24 -59.3(7) . . . . ?
C22 C23 C24 C25 56.0(8) . . . . ?
C23 C24 C25 C26 -53.6(9) . . . . ?
C24 C25 C26 C21 54.4(9) . . . . ?
N3 C21 C26 C25 -179.5(6) . . . . ?
C22 C21 C26 C25 -59.1(8) . . . . ?
C21 N3 C27 O5 -179.9(6) . . . . ?
C21 N3 C27 C28 -1.9(9) . . . . ?
C22 N4 C28 C27 -29.8(7) . . . . ?
C22 N4 C28 C29 96.1(6) . . . . ?
C22 N4 C28 P2 -147.3(4) . . . . ?
O5 C27 C28 N4 177.9(5) . . . . ?
N3 C27 C28 N4 -0.2(8) . . . . ?
O5 C27 C28 C29 49.2(7) . . . . ?
N3 C27 C28 C29 -128.9(6) . . . . ?
O5 C27 C28 P2 -71.5(7) . . . . ?
N3 C27 C28 P2 110.4(5) . . . . ?
O8 P2 C28 N4 -56.5(4) . . . . ?
O6 P2 C28 N4 69.9(4) . . . . ?
O7 P2 C28 N4 179.0(4) . . . . ?
O8 P2 C28 C27 -175.6(4) . . . . ?
O6 P2 C28 C27 -49.2(5) . . . . ?
O7 P2 C28 C27 59.9(5) . . . . ?
O8 P2 C28 C29 63.9(5) . . . . ?
O6 P2 C28 C29 -169.8(4) . . . . ?
O7 P2 C28 C29 -60.6(5) . . . . ?
N4 C28 C29 C30 -61.9(7) . . . . ?
C27 C28 C29 C30 66.0(7) . . . . ?
P2 C28 C29 C30 -172.6(5) . . . . ?
C28 C29 C30 C31 -179.3(6) . . . . ?
C29 C30 C31 C32 73.7(11) . . . . ?
C29 C30 C31 C33 -60.4(10) . . . . ?
O12 P3 O10 C54 26.1(6) . . . . ?
O11 P3 O10 C54 150.5(5) . . . . ?
C48 P3 O10 C54 -100.3(5) . . . . ?
O12 P3 O11 C55 54.5(6) . . . . ?
O10 P3 O11 C55 -69.7(6) . . . . ?
C48 P3 O11 C55 178.6(5) . . . . ?
C47 N5 C41 C42 27.6(9) . . . . ?
C47 N5 C41 C46 151.2(7) . . . . ?
C48 N6 C42 C41 62.4(6) . . . . ?
C48 N6 C42 C43 -177.0(5) . . . . ?
N5 C41 C42 N6 -57.5(6) . . . . ?
C46 C41 C42 N6 179.8(5) . . . . ?
N5 C41 C42 C43 -178.6(5) . . . . ?
C46 C41 C42 C43 58.6(6) . . . . ?
N6 C42 C43 C44 -176.4(5) . . . . ?
C41 C42 C43 C44 -56.7(7) . . . . ?
C42 C43 C44 C45 54.5(7) . . . . ?
C43 C44 C45 C46 -53.1(8) . . . . ?
N5 C41 C46 C45 -178.1(5) . . . . ?
C42 C41 C46 C45 -56.9(7) . . . . ?
C44 C45 C46 C41 53.4(8) . . . . ?
C41 N5 C47 O9 -177.6(7) . . . . ?
C41 N5 C47 C48 1.9(10) . . . . ?
C42 N6 C48 C47 -31.8(7) . . . . ?
C42 N6 C48 C49A 79.6(11) . . . . ?
C42 N6 C48 C49B 104.0(9) . . . . ?
C42 N6 C48 P3 -147.8(4) . . . . ?
O9 C47 C48 N6 178.6(6) . . . . ?
N5 C47 C48 N6 -1.0(9) . . . . ?
O9 C47 C48 C49A 57.4(11) . . . . ?
N5 C47 C48 C49A -122.2(9) . . . . ?
O9 C47 C48 C49B 44.9(11) . . . . ?
N5 C47 C48 C49B -134.7(9) . . . . ?
O9 C47 C48 P3 -69.6(8) . . . . ?
N5 C47 C48 P3 110.8(6) . . . . ?
O12 P3 C48 N6 -50.9(5) . . . . ?
O10 P3 C48 N6 75.8(4) . . . . ?
O11 P3 C48 N6 -175.5(4) . . . . ?
O12 P3 C48 C47 -170.3(4) . . . . ?
O10 P3 C48 C47 -43.6(5) . . . . ?
O11 P3 C48 C47 65.1(5) . . . . ?
O12 P3 C48 C49A 77.5(9) . . . . ?
O10 P3 C48 C49A -155.8(9) . . . . ?
O11 P3 C48 C49A -47.2(9) . . . . ?
O12 P3 C48 C49B 65.6(7) . . . . ?
O10 P3 C48 C49B -167.7(7) . . . . ?
O11 P3 C48 C49B -59.1(7) . . . . ?
N6 C48 C49A C50A -12(3) . . . . ?
C47 C48 C49A C50A 108(3) . . . . ?
P3 C48 C49A C50A -134(2) . . . . ?
C48 C49A C50A C51A 149.0(19) . . . . ?
C49A C50A C51A C52A -86(3) . . . . ?
C49A C50A C51A C53A 37(3) . . . . ?
N6 C48 C49B C50B 34(3) . . . . ?
C47 C48 C49B C50B 168(2) . . . . ?
P3 C48 C49B C50B -74(3) . . . . ?
C48 C49B C50B C51B -150.9(18) . . . . ?
C49B C50B C51B C53B -58(2) . . . . ?
C49B C50B C51B C52B 78(2) . . . . ?
O16 P4 O14 C74 26.3(5) . . . . ?
O15 P4 O14 C74 149.3(5) . . . . ?
C68 P4 O14 C74 -97.5(5) . . . . ?
O16 P4 O15 C75A 140.3(9) . . . . ?
O14 P4 O15 C75A 15.7(9) . . . . ?
C68 P4 O15 C75A -97.3(9) . . . . ?
O16 P4 O15 C75B 85.7(11) . . . . ?
O14 P4 O15 C75B -38.8(11) . . . . ?
C68 P4 O15 C75B -151.9(10) . . . . ?
C67 N7 C61 C66 155.5(6) . . . . ?
C67 N7 C61 C62 32.5(8) . . . . ?
C68 N8 C62 C61 57.0(6) . . . . ?
C68 N8 C62 C63 178.2(5) . . . . ?
N7 C61 C62 N8 -57.3(6) . . . . ?
C66 C61 C62 N8 179.5(5) . . . . ?
N7 C61 C62 C63 -178.3(5) . . . . ?
C66 C61 C62 C63 58.5(6) . . . . ?
N8 C62 C63 C64 -175.3(5) . . . . ?
C61 C62 C63 C64 -55.4(7) . . . . ?
C62 C63 C64 C65 54.0(7) . . . . ?
C63 C64 C65 C66 -55.2(7) . . . . ?
N7 C61 C66 C65 179.6(5) . . . . ?
C62 C61 C66 C65 -59.0(7) . . . . ?
C64 C65 C66 C61 57.1(7) . . . . ?
C61 N7 C67 O13 179.7(5) . . . . ?
C61 N7 C67 C68 -1.4(9) . . . . ?
C62 N8 C68 C69 101.7(6) . . . . ?
C62 N8 C68 C67 -25.5(7) . . . . ?
C62 N8 C68 P4 -142.6(4) . . . . ?
O13 C67 C68 N8 175.3(5) . . . . ?
N7 C67 C68 N8 -3.6(7) . . . . ?
O13 C67 C68 C69 45.4(7) . . . . ?
N7 C67 C68 C69 -133.5(5) . . . . ?
O13 C67 C68 P4 -73.2(6) . . . . ?
N7 C67 C68 P4 107.9(5) . . . . ?
O16 P4 C68 N8 -57.6(4) . . . . ?
O15 P4 C68 N8 179.4(3) . . . . ?
O14 P4 C68 N8 68.2(4) . . . . ?
O16 P4 C68 C69 63.1(4) . . . . ?
O15 P4 C68 C69 -59.9(4) . . . . ?
O14 P4 C68 C69 -171.1(3) . . . . ?
O16 P4 C68 C67 -177.5(4) . . . . ?
O15 P4 C68 C67 59.5(4) . . . . ?
O14 P4 C68 C67 -51.7(4) . . . . ?
N8 C68 C69 C70 -62.4(6) . . . . ?
C67 C68 C69 C70 66.9(6) . . . . ?
P4 C68 C69 C70 -173.6(4) . . . . ?
C68 C69 C70 C71 -174.2(6) . . . . ?
C69 C70 C71 C72 -67.2(8) . . . . ?
C69 C70 C71 C73 168.9(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1N O8 0.84(7) 2.07(7) 2.892(7) 165(7) . yes
N2 H2N O9 0.81(7) 2.20(7) 2.983(7) 163(6) 1_554 yes
N3 H3N O12 0.93(7) 1.98(7) 2.902(6) 171(6) . yes
N4 H4N O1 0.86(6) 2.14(7) 2.950(6) 157(6) . yes
N5 H5N O4 0.92(7) 2.01(7) 2.900(7) 161(6) 1_556 yes
N6 H6N O5 1.01(6) 2.03(7) 3.002(6) 163(5) . yes
N7 H7N O16 0.83(6) 2.09(6) 2.915(6) 172(6) 2_655 yes
N8 H8N O13 0.96(6) 2.10(7) 3.008(7) 159(5) 3_664 yes

_refine_diff_density_max         0.440
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.050



