# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelxl_hqp
_database_code_depnum_ccdc_archive 'CCDC 1413010'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-04-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H18 N3 O4 P'
_chemical_formula_weight         479.41

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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   13.3936(15)
_cell_length_b                   13.3936(15)
_cell_length_c                   13.3936(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2402.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2833
_cell_measurement_theta_min      5.49
_cell_measurement_theta_max      27.41

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2833
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         5.49
_diffrn_reflns_theta_max         27.41
_reflns_number_total             1636
_reflns_number_gt                1299
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  'Microsoft word 2007'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1057P)²+0.0461P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_number_reflns         1636
_refine_ls_number_parameters     106
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1424
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_restrained_S_all      0.854
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.010

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O -0.03163(14) 0.46837(14) 1.03163(14) 0.0473(8) Uani 1 3 d S . .
C1 C 0.1723(2) 0.3959(2) 0.9566(2) 0.0402(6) Uani 1 1 d . . .
C2 C 0.1348(3) 0.3262(3) 0.8945(3) 0.0571(8) Uani 1 1 d . . .
H2 H 0.0861 0.3432 0.8481 0.069 Uiso 1 1 calc R . .
C3 C 0.1703(3) 0.2270(3) 0.9007(3) 0.0705(11) Uani 1 1 d . . .
H3 H 0.1431 0.1779 0.8598 0.085 Uiso 1 1 calc R . .
C4 C 0.2439(3) 0.2031(2) 0.9661(3) 0.0657(10) Uani 1 1 d . . .
H4 H 0.2673 0.1378 0.9687 0.079 Uiso 1 1 calc R . .
C5 C 0.2851(2) 0.2751(2) 1.0297(3) 0.0508(7) Uani 1 1 d . . .
C6 C 0.3629(3) 0.2556(3) 1.0983(3) 0.0660(10) Uani 1 1 d . . .
H6 H 0.3900 0.1919 1.1026 0.079 Uiso 1 1 calc R . .
C7 C 0.3977(3) 0.3287(3) 1.1571(3) 0.0676(10) Uani 1 1 d . . .
H7 H 0.4483 0.3159 1.2029 0.081 Uiso 1 1 calc R . .
C8 C 0.3566(3) 0.4250(3) 1.1487(3) 0.0604(9) Uani 1 1 d . . .
H8 H 0.3820 0.4750 1.1897 0.073 Uiso 1 1 calc R . .
C9 C 0.2489(2) 0.3744(2) 1.0264(2) 0.0403(6) Uani 1 1 d . . .
N1 N 0.28416(19) 0.44867(18) 1.0864(2) 0.0479(6) Uani 1 1 d . . .
O1 O 0.14169(14) 0.49646(14) 0.95332(17) 0.0485(6) Uani 1 1 d . . .
P1 P 0.03091(5) 0.53091(5) 0.96909(5) 0.0333(3) Uani 1 3 d S . .


_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
O2 P1 1.451(3) . ?
C1 C2 1.347(4) . ?
C1 O1 1.409(3) . ?
C1 C9 1.418(4) . ?
C2 C3 1.414(5) . ?
C3 C4 1.356(5) . ?
C4 C5 1.401(5) . ?
C5 C6 1.413(5) . ?
C5 C9 1.416(4) . ?
C6 C7 1.340(6) . ?
C7 C8 1.408(6) . ?
C8 N1 1.318(4) . ?
C9 N1 1.363(4) . ?
O1 P1 1.5681(19) . ?
P1 O1 1.5680(19) 8_656 ?
P1 O1 1.5680(19) 11_466 ?

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
C2 C1 O1 122.3(3) . . ?
C2 C1 C9 122.5(3) . . ?
O1 C1 C9 115.2(2) . . ?
C1 C2 C3 119.3(3) . . ?
C4 C3 C2 120.3(3) . . ?
C3 C4 C5 121.1(3) . . ?
C6 C5 C9 116.5(3) . . ?
C6 C5 C4 124.0(3) . . ?
C9 C5 C4 119.5(3) . . ?
C7 C6 C5 120.2(3) . . ?
C6 C7 C8 119.1(3) . . ?
N1 C8 C7 123.9(3) . . ?
N1 C9 C5 123.3(3) . . ?
N1 C9 C1 119.4(2) . . ?
C5 C9 C1 117.3(3) . . ?
C8 N1 C9 116.9(3) . . ?
C1 O1 P1 123.57(17) . . ?
O2 P1 O1 117.01(8) . 8_656 ?
O2 P1 O1 117.00(8) . 11_466 ?
O1 P1 O1 101.00(10) 8_656 11_466 ?
O2 P1 O1 117.01(8) . . ?
O1 P1 O1 100.99(10) 8_656 . ?
O1 P1 O1 100.99(10) 11_466 . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.41
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.033
####################################################################### 
# 
# 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_shelxl_pb4hq6clo4
_database_code_depnum_ccdc_archive 'CCDC 1413011'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-04-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H36 Cl2 N6 O14 P0 Pb4'
_chemical_formula_weight         1892.55

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.247
_cell_length_b                   11.756
_cell_length_c                   12.669
_cell_angle_alpha                65.39
_cell_angle_beta                 75.83
_cell_angle_gamma                82.73
_cell_volume                     1344.8
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17213
_cell_measurement_theta_min      1.81
_cell_measurement_theta_max      27.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             876
_exptl_absorpt_coefficient_mu    12.654
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17213
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5615
_reflns_number_gt                3795
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  'Microsoft word 2007'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0378P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5615
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0790
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6872(10) 0.6691(10) 0.4456(8) 0.052(3) Uani 1 1 d . . .
H1 H 0.6197 0.6107 0.4851 0.063 Uiso 1 1 calc R . .
C2 C 0.8173(11) 0.6261(10) 0.4158(9) 0.059(3) Uani 1 1 d . . .
H2 H 0.8357 0.5410 0.4354 0.070 Uiso 1 1 calc R . .
C3 C 0.9166(10) 0.7082(10) 0.3586(9) 0.057(3) Uani 1 1 d . . .
H3 H 1.0044 0.6799 0.3388 0.069 Uiso 1 1 calc R . .
C4 C 0.8890(8) 0.8369(9) 0.3282(7) 0.041(2) Uani 1 1 d . . .
C5 C 0.9851(9) 0.9323(10) 0.2695(8) 0.051(3) Uani 1 1 d . . .
H5 H 1.0750 0.9110 0.2469 0.061 Uiso 1 1 calc R . .
C6 C 0.9495(9) 1.0511(9) 0.2463(7) 0.046(2) Uani 1 1 d . . .
H6 H 1.0143 1.1119 0.2051 0.055 Uiso 1 1 calc R . .
C7 C 0.8131(8) 1.0882(9) 0.2831(7) 0.039(2) Uani 1 1 d . . .
H7 H 0.7896 1.1717 0.2682 0.047 Uiso 1 1 calc R . .
C8 C 0.7183(8) 0.9975(8) 0.3409(7) 0.0337(19) Uani 1 1 d . . .
C9 C 0.7545(8) 0.8722(8) 0.3646(6) 0.0305(18) Uani 1 1 d . . .
C11 C 0.3004(12) 1.4500(12) 0.0683(11) 0.069(3) Uani 1 1 d . . .
H11 H 0.3751 1.4780 0.0064 0.083 Uiso 1 1 calc R . .
C12 C 0.1835(17) 1.5250(12) 0.0631(13) 0.088(4) Uani 1 1 d . . .
H12 H 0.1805 1.6010 -0.0014 0.105 Uiso 1 1 calc R . .
C13 C 0.0714(15) 1.4849(12) 0.1556(13) 0.082(4) Uani 1 1 d . . .
H13 H -0.0070 1.5345 0.1544 0.098 Uiso 1 1 calc R . .
C14 C 0.0776(11) 1.3712(11) 0.2486(10) 0.057(3) Uani 1 1 d . . .
C17 C 0.1013(9) 1.1371(10) 0.4304(8) 0.046(2) Uani 1 1 d . . .
H17 H 0.1063 1.0581 0.4907 0.055 Uiso 1 1 calc R . .
C18 C 0.2140(8) 1.1829(9) 0.3387(8) 0.038(2) Uani 1 1 d . . .
C19 C 0.2006(9) 1.2982(9) 0.2484(8) 0.041(2) Uani 1 1 d . . .
C21 C 0.3144(10) 1.2070(10) -0.0262(8) 0.050(2) Uani 1 1 d . . .
H21 H 0.3278 1.2915 -0.0492 0.060 Uiso 1 1 calc R . .
C22 C 0.2406(11) 1.1738(11) -0.0879(8) 0.060(3) Uani 1 1 d . . .
H22 H 0.2078 1.2351 -0.1512 0.072 Uiso 1 1 calc R . .
C23 C 0.2175(10) 1.0534(11) -0.0553(8) 0.059(3) Uani 1 1 d . . .
H23 H 0.1660 1.0303 -0.0939 0.070 Uiso 1 1 calc R . .
C24 C 0.2717(9) 0.9617(10) 0.0378(7) 0.044(2) Uani 1 1 d . . .
C25 C 0.2523(9) 0.8298(10) 0.0784(8) 0.050(2) Uani 1 1 d . . .
H25 H 0.2021 0.8013 0.0428 0.060 Uiso 1 1 calc R . .
C26 C 0.3077(10) 0.7482(9) 0.1684(9) 0.052(3) Uani 1 1 d . . .
H26 H 0.2956 0.6629 0.1944 0.063 Uiso 1 1 calc R . .
C27 C 0.3848(9) 0.7899(9) 0.2247(8) 0.047(2) Uani 1 1 d . . .
H27 H 0.4218 0.7307 0.2864 0.057 Uiso 1 1 calc R . .
C28 C 0.4062(8) 0.9136(8) 0.1913(7) 0.036(2) Uani 1 1 d . . .
C29 C 0.3449(8) 1.0029(8) 0.0964(7) 0.034(2) Uani 1 1 d . . .
C15 C 0.0186(10) 0.7922(11) 0.5667(9) 0.057(3) Uani 1 1 d . . .
H15 H 0.0916 0.8235 0.5037 0.068 Uiso 1 1 calc R . .
N1 N 0.6536(6) 0.7877(6) 0.4211(6) 0.0335(16) Uani 1 1 d . . .
N2 N 0.3100(8) 1.3403(7) 0.1577(7) 0.0455(19) Uani 1 1 d . . .
N3 N 0.3649(7) 1.1267(7) 0.0611(6) 0.0403(18) Uani 1 1 d . . .
O4 O 0.5045(11) 0.4859(11) 0.7440(14) 0.189(6) Uani 1 1 d . . .
O1 O 0.5878(5) 1.0314(5) 0.3825(4) 0.0331(13) Uani 1 1 d . . .
O2 O 0.3269(6) 1.1161(6) 0.3370(5) 0.0413(14) Uani 1 1 d . . .
O3 O 0.4797(6) 0.9568(5) 0.2385(5) 0.0402(14) Uani 1 1 d . . .
O5 O 0.2836(11) 0.5107(16) 0.7911(9) 0.230(9) Uani 1 1 d . . .
O6 O 0.4167(15) 0.6758(9) 0.7081(11) 0.171(6) Uani 1 1 d . . .
O7 O 0.3765(10) 0.5895(11) 0.5955(8) 0.126(4) Uani 1 1 d . . .
C16 C 0.0293(11) 0.6803(12) 0.6535(12) 0.068(3) Uani 1 1 d . . .
H16 H 0.1100 0.6346 0.6493 0.082 Uiso 1 1 calc R . .
Cl1 Cl 0.3970(3) 0.5616(3) 0.7124(3) 0.0668(7) Uani 1 1 d . . .
Pb1 Pb 0.42548(3) 0.88618(3) 0.45098(3) 0.03415(11) Uani 1 1 d . . .
Pb2 Pb 0.49746(3) 1.17754(3) 0.17641(3) 0.03971(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 1.315(11) . ?
C1 C2 1.385(13) . ?
C2 C3 1.341(13) . ?
C3 C4 1.406(13) . ?
C4 C9 1.410(11) . ?
C4 C5 1.417(12) . ?
C5 C6 1.323(13) . ?
C6 C7 1.434(12) . ?
C7 C8 1.371(11) . ?
C8 O1 1.385(9) . ?
C8 C9 1.395(11) . ?
C9 N1 1.369(10) . ?
C11 N2 1.327(13) . ?
C11 C12 1.393(16) . ?
C12 C13 1.390(17) . ?
C13 C14 1.372(15) . ?
C14 C16 1.408(15) 2_576 ?
C14 C19 1.432(13) . ?
C17 C15 1.396(13) 2_576 ?
C17 C18 1.397(12) . ?
C18 O2 1.315(10) . ?
C18 C19 1.379(12) . ?
C19 N2 1.362(11) . ?
C21 N3 1.291(11) . ?
C21 C22 1.398(12) . ?
C22 C23 1.334(13) . ?
C23 C24 1.404(13) . ?
C24 C29 1.418(10) . ?
C24 C25 1.440(13) . ?
C25 C26 1.346(13) . ?
C26 C27 1.428(12) . ?
C27 C28 1.366(11) . ?
C28 O3 1.323(9) . ?
C28 C29 1.447(11) . ?
C29 N3 1.360(10) . ?
C15 C16 1.330(14) . ?
C15 C17 1.396(13) 2_576 ?
N1 Pb1 2.489(6) . ?
N2 Pb2 2.515(8) . ?
N3 Pb2 2.498(7) . ?
O4 Cl1 1.356(10) . ?
O1 Pb1 2.283(5) . ?
O1 Pb1 2.634(5) 2_676 ?
O2 Pb2 2.252(5) . ?
O2 Pb1 2.680(6) . ?
O3 Pb2 2.395(6) . ?
O3 Pb1 2.402(5) . ?
O5 Cl1 1.348(10) . ?
O6 Cl1 1.359(9) . ?
O7 Cl1 1.440(9) . ?
C16 C14 1.408(15) 2_576 ?
Pb1 O1 2.634(5) 2_676 ?

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 C2 123.8(10) . . ?
C3 C2 C1 119.4(10) . . ?
C2 C3 C4 120.4(9) . . ?
C3 C4 C9 116.5(8) . . ?
C3 C4 C5 125.7(9) . . ?
C9 C4 C5 117.7(8) . . ?
C6 C5 C4 121.3(9) . . ?
C5 C6 C7 121.5(9) . . ?
C8 C7 C6 118.3(9) . . ?
C7 C8 O1 118.8(7) . . ?
C7 C8 C9 120.6(8) . . ?
O1 C8 C9 120.5(7) . . ?
N1 C9 C8 117.0(7) . . ?
N1 C9 C4 122.4(8) . . ?
C8 C9 C4 120.5(8) . . ?
N2 C11 C12 122.9(12) . . ?
C13 C12 C11 119.2(12) . . ?
C14 C13 C12 119.2(12) . . ?
C13 C14 C16 124.6(11) . 2_576 ?
C13 C14 C19 118.9(12) . . ?
C16 C14 C19 116.6(10) 2_576 . ?
C15 C17 C18 121.2(10) 2_576 . ?
O2 C18 C19 121.5(8) . . ?
O2 C18 C17 120.9(9) . . ?
C19 C18 C17 117.6(8) . . ?
N2 C19 C18 117.1(8) . . ?
N2 C19 C14 120.9(9) . . ?
C18 C19 C14 122.0(9) . . ?
N3 C21 C22 123.5(9) . . ?
C23 C22 C21 119.5(9) . . ?
C22 C23 C24 119.4(8) . . ?
C23 C24 C29 117.7(9) . . ?
C23 C24 C25 123.1(8) . . ?
C29 C24 C25 119.1(9) . . ?
C26 C25 C24 119.3(8) . . ?
C25 C26 C27 121.3(9) . . ?
C28 C27 C26 122.4(9) . . ?
O3 C28 C27 124.7(8) . . ?
O3 C28 C29 118.2(7) . . ?
C27 C28 C29 117.0(7) . . ?
N3 C29 C24 120.9(8) . . ?
N3 C29 C28 118.3(7) . . ?
C24 C29 C28 120.7(8) . . ?
C16 C15 C17 120.5(10) . 2_576 ?
C1 N1 C9 117.4(7) . . ?
C1 N1 Pb1 128.9(6) . . ?
C9 N1 Pb1 113.6(5) . . ?
C11 N2 C19 118.9(9) . . ?
C11 N2 Pb2 128.9(7) . . ?
C19 N2 Pb2 111.8(6) . . ?
C21 N3 C29 118.8(7) . . ?
C21 N3 Pb2 125.7(6) . . ?
C29 N3 Pb2 115.4(5) . . ?
C8 O1 Pb1 117.8(5) . . ?
C8 O1 Pb1 111.9(4) . 2_676 ?
Pb1 O1 Pb1 107.50(18) . 2_676 ?
C18 O2 Pb2 120.5(5) . . ?
C18 O2 Pb1 140.5(5) . . ?
Pb2 O2 Pb1 97.5(2) . . ?
C28 O3 Pb2 120.4(5) . . ?
C28 O3 Pb1 116.8(5) . . ?
Pb2 O3 Pb1 101.69(18) . . ?
C15 C16 C14 122.1(10) . 2_576 ?
O5 Cl1 O4 109.7(8) . . ?
O5 Cl1 O6 111.4(11) . . ?
O4 Cl1 O6 108.4(8) . . ?
O5 Cl1 O7 107.6(7) . . ?
O4 Cl1 O7 116.3(9) . . ?
O6 Cl1 O7 103.4(6) . . ?
O1 Pb1 O3 73.65(17) . . ?
O1 Pb1 N1 69.4(2) . . ?
O3 Pb1 N1 79.4(2) . . ?
O1 Pb1 O1 72.50(18) . 2_676 ?
O3 Pb1 O1 140.46(17) . 2_676 ?
N1 Pb1 O1 106.68(18) . 2_676 ?
O1 Pb1 O2 69.31(18) . . ?
O3 Pb1 O2 66.24(18) . . ?
N1 Pb1 O2 131.9(2) . . ?
O1 Pb1 O2 83.01(16) 2_676 . ?
O2 Pb2 O3 73.61(19) . . ?
O2 Pb2 N3 90.3(2) . . ?
O3 Pb2 N3 67.4(2) . . ?
O2 Pb2 N2 68.4(2) . . ?
O3 Pb2 N2 127.8(2) . . ?
N3 Pb2 N2 78.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         1.345
_refine_diff_density_min         -1.989
_refine_diff_density_rms         0.208
####################################################################### 
# 
# 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_shelxl_np
_database_code_depnum_ccdc_archive 'CCDC 1413012'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-04-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H21 O4 P'
_chemical_formula_weight         476.44

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   13.7844(15)
_cell_length_b                   9.8719(11)
_cell_length_c                   21.2839(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.688(5)
_cell_angle_gamma                90.00
_cell_volume                     2352.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    30574
_cell_measurement_theta_min      1.82
_cell_measurement_theta_max      27.64

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30574
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         27.64
_reflns_number_total             5372
_reflns_number_gt                3275
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  'Microsoft word 2007'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0514P)²+0.6439P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5372
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1292
_refine_ls_wR_factor_gt          0.1083
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.26759(5) -0.69936(5) 0.03863(3) 0.04840(16) Uani 1 1 d . . .
O1 O 0.18014(12) -0.69596(13) -0.05237(7) 0.0529(4) Uani 1 1 d . . .
O2 O 0.36891(12) -0.79527(14) 0.05231(8) 0.0534(4) Uani 1 1 d . . .
O3 O 0.20708(12) -0.78975(14) 0.06751(8) 0.0540(4) Uani 1 1 d . . .
O21 O 0.29967(14) -0.56832(15) 0.07550(9) 0.0656(4) Uani 1 1 d . . .
C1 C 0.09590(17) -0.5918(2) -0.09327(11) 0.0485(5) Uani 1 1 d . . .
C2 C 0.0096(2) -0.5665(2) -0.08293(13) 0.0631(6) Uani 1 1 d . . .
H2 H 0.0069 -0.6161 -0.0468 0.076 Uiso 1 1 calc R . .
C3 C -0.0752(2) -0.4660(3) -0.12642(17) 0.0807(8) Uani 1 1 d . . .
H3 H -0.1343 -0.4482 -0.1192 0.097 Uiso 1 1 calc R . .
C4 C -0.0713(2) -0.3946(3) -0.17917(17) 0.0875(9) Uani 1 1 d . . .
H4 H -0.1280 -0.3275 -0.2077 0.105 Uiso 1 1 calc R . .
C5 C 0.0171(2) -0.4197(2) -0.19181(13) 0.0676(6) Uani 1 1 d . . .
C6 C 0.0231(3) -0.3497(3) -0.24715(18) 0.1070(11) Uani 1 1 d . . .
H6 H -0.0330 -0.2827 -0.2769 0.128 Uiso 1 1 calc R . .
C7 C 0.1077(4) -0.3773(4) -0.25794(19) 0.1221(14) Uani 1 1 d . . .
H7 H 0.1099 -0.3292 -0.2947 0.146 Uiso 1 1 calc R . .
C8 C 0.1922(3) -0.4774(4) -0.21438(18) 0.1002(10) Uani 1 1 d . . .
H8 H 0.2506 -0.4955 -0.2223 0.120 Uiso 1 1 calc R . .
C9 C 0.1908(2) -0.5494(3) -0.16031(13) 0.0677(6) Uani 1 1 d . . .
H9 H 0.2473 -0.6168 -0.1321 0.081 Uiso 1 1 calc R . .
C10 C 0.10395(18) -0.5216(2) -0.14723(11) 0.0516(5) Uani 1 1 d . . .
C11 C 0.42470(19) -0.7751(2) 0.01450(12) 0.0538(5) Uani 1 1 d . . .
C12 C 0.5081(2) -0.6768(3) 0.03945(16) 0.0738(7) Uani 1 1 d . . .
H12 H 0.5291 -0.6225 0.0813 0.089 Uiso 1 1 calc R . .
C13 C 0.5622(3) -0.6582(3) 0.0015(2) 0.0956(10) Uani 1 1 d . . .
H13 H 0.6193 -0.5906 0.0181 0.115 Uiso 1 1 calc R . .
C14 C 0.5328(3) -0.7365(4) -0.0586(2) 0.0954(10) Uani 1 1 d . . .
H14 H 0.5687 -0.7211 -0.0838 0.114 Uiso 1 1 calc R . .
C15 C 0.4481(2) -0.8424(3) -0.08457(15) 0.0748(7) Uani 1 1 d . . .
C16 C 0.4163(3) -0.9299(4) -0.14631(19) 0.1044(11) Uani 1 1 d . . .
H16 H 0.4513 -0.9182 -0.1723 0.125 Uiso 1 1 calc R . .
C17 C 0.3363(3) -1.0298(4) -0.16817(19) 0.1141(13) Uani 1 1 d . . .
H17 H 0.3166 -1.0857 -0.2092 0.137 Uiso 1 1 calc R . .
C18 C 0.2824(3) -1.0510(3) -0.13035(18) 0.0982(10) Uani 1 1 d . . .
H18 H 0.2273 -1.1206 -0.1462 0.118 Uiso 1 1 calc R . .
C19 C 0.3105(2) -0.9699(3) -0.07023(15) 0.0710(7) Uani 1 1 d . . .
H19 H 0.2751 -0.9851 -0.0447 0.085 Uiso 1 1 calc R . .
C20 C 0.39262(19) -0.8634(2) -0.04647(13) 0.0563(5) Uani 1 1 d . . .
C21 C 0.18906(18) -0.9308(2) 0.05292(12) 0.0529(5) Uani 1 1 d . . .
C22 C 0.1033(2) -0.9786(3) -0.01795(14) 0.0684(6) Uani 1 1 d . . .
H22 H 0.0537 -0.9194 -0.0585 0.082 Uiso 1 1 calc R . .
C23 C 0.0900(2) -1.1201(3) -0.02974(18) 0.0829(8) Uani 1 1 d . . .
H23 H 0.0317 -1.1541 -0.0786 0.099 Uiso 1 1 calc R . .
C24 C 0.1608(3) -1.2069(3) 0.0290(2) 0.0803(8) Uani 1 1 d . . .
H24 H 0.1515 -1.2997 0.0198 0.096 Uiso 1 1 calc R . .
C25 C 0.2487(2) -1.1584(2) 0.10432(16) 0.0641(6) Uani 1 1 d . . .
C26 C 0.3231(3) -1.2458(3) 0.1674(2) 0.0840(9) Uani 1 1 d . . .
H26 H 0.3139 -1.3391 0.1602 0.101 Uiso 1 1 calc R . .
C27 C 0.4080(3) -1.1951(3) 0.2385(2) 0.0868(9) Uani 1 1 d . . .
H27 H 0.4558 -1.2539 0.2796 0.104 Uiso 1 1 calc R . .
C28 C 0.4240(2) -1.0563(3) 0.25041(15) 0.0768(7) Uani 1 1 d . . .
H28 H 0.4836 -1.0231 0.2992 0.092 Uiso 1 1 calc R . .
C29 C 0.3533(2) -0.9681(2) 0.19128(13) 0.0614(6) Uani 1 1 d . . .
H29 H 0.3643 -0.8753 0.2003 0.074 Uiso 1 1 calc R . .
C30 C 0.26328(19) -1.0168(2) 0.11624(13) 0.0519(5) 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
P1 O21 1.4422(15) . ?
P1 O2 1.5677(14) . ?
P1 O3 1.5709(14) . ?
P1 O1 1.5752(14) . ?
O1 C1 1.409(2) . ?
O2 C11 1.415(2) . ?
O3 C21 1.417(3) . ?
C1 C2 1.353(3) . ?
C1 C10 1.400(3) . ?
C2 C3 1.394(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.353(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.415(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.409(4) . ?
C5 C10 1.421(3) . ?
C6 C7 1.343(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.390(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.362(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.405(3) . ?
C9 H9 0.9300 . ?
C11 C12 1.354(3) . ?
C11 C20 1.403(3) . ?
C12 C13 1.394(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.340(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.417(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.412(4) . ?
C15 C20 1.417(3) . ?
C16 C17 1.345(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.393(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.360(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.406(3) . ?
C19 H19 0.9300 . ?
C21 C22 1.347(3) . ?
C21 C30 1.406(3) . ?
C22 C23 1.412(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.351(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.415(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.411(4) . ?
C25 C30 1.414(3) . ?
C26 C27 1.359(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.387(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.364(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.418(3) . ?
C29 H29 0.9300 . ?

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
O21 P1 O2 118.91(9) . . ?
O21 P1 O3 111.15(9) . . ?
O2 P1 O3 101.72(7) . . ?
O21 P1 O1 114.95(8) . . ?
O2 P1 O1 101.60(7) . . ?
O3 P1 O1 107.04(8) . . ?
C1 O1 P1 122.61(12) . . ?
C11 O2 P1 122.04(12) . . ?
C21 O3 P1 122.53(12) . . ?
C2 C1 C10 122.7(2) . . ?
C2 C1 O1 121.33(19) . . ?
C10 C1 O1 115.91(17) . . ?
C1 C2 C3 119.9(2) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 121.4(2) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 123.3(3) . . ?
C6 C5 C10 118.0(3) . . ?
C4 C5 C10 118.7(2) . . ?
C7 C6 C5 121.6(3) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C6 C7 C8 120.2(3) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 119.9(3) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C1 C10 C9 123.4(2) . . ?
C1 C10 C5 117.3(2) . . ?
C9 C10 C5 119.3(2) . . ?
C12 C11 C20 123.0(2) . . ?
C12 C11 O2 119.8(2) . . ?
C20 C11 O2 117.14(19) . . ?
C11 C12 C13 119.1(3) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 120.7(3) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 121.3(3) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C16 C15 C14 123.5(3) . . ?
C16 C15 C20 117.7(3) . . ?
C14 C15 C20 118.8(3) . . ?
C17 C16 C15 121.2(3) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 121.1(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 120.0(3) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C11 C20 C19 123.4(2) . . ?
C11 C20 C15 117.0(2) . . ?
C19 C20 C15 119.6(2) . . ?
C22 C21 C30 122.3(2) . . ?
C22 C21 O3 121.1(2) . . ?
C30 C21 O3 116.57(19) . . ?
C21 C22 C23 118.9(3) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C24 C23 C22 120.9(3) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 120.8(2) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 122.5(3) . . ?
C26 C25 C30 119.0(3) . . ?
C24 C25 C30 118.4(2) . . ?
C27 C26 C25 120.7(3) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 120.6(3) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C29 C28 C27 120.7(3) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 120.5(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C21 C30 C25 118.5(2) . . ?
C21 C30 C29 123.0(2) . . ?
C25 C30 C29 118.5(2) . . ?

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
O21 P1 O1 C1 -29.40(17) . . . . ?
O2 P1 O1 C1 -159.18(14) . . . . ?
O3 P1 O1 C1 94.57(15) . . . . ?
O21 P1 O2 C11 -76.83(18) . . . . ?
O3 P1 O2 C11 160.79(15) . . . . ?
O1 P1 O2 C11 50.42(16) . . . . ?
O21 P1 O3 C21 -166.87(15) . . . . ?
O2 P1 O3 C21 -39.30(17) . . . . ?
O1 P1 O3 C21 66.86(16) . . . . ?
P1 O1 C1 C2 -59.8(2) . . . . ?
P1 O1 C1 C10 123.09(16) . . . . ?
C10 C1 C2 C3 -0.7(3) . . . . ?
O1 C1 C2 C3 -177.57(19) . . . . ?
C1 C2 C3 C4 0.3(4) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C3 C4 C5 C6 178.7(3) . . . . ?
C3 C4 C5 C10 -0.6(4) . . . . ?
C4 C5 C6 C7 -179.4(3) . . . . ?
C10 C5 C6 C7 -0.1(4) . . . . ?
C5 C6 C7 C8 0.3(5) . . . . ?
C6 C7 C8 C9 0.1(5) . . . . ?
C7 C8 C9 C10 -0.8(4) . . . . ?
C2 C1 C10 C9 -178.0(2) . . . . ?
O1 C1 C10 C9 -1.0(3) . . . . ?
C2 C1 C10 C5 0.4(3) . . . . ?
O1 C1 C10 C5 177.39(17) . . . . ?
C8 C9 C10 C1 179.4(2) . . . . ?
C8 C9 C10 C5 1.1(3) . . . . ?
C6 C5 C10 C1 -179.1(2) . . . . ?
C4 C5 C10 C1 0.3(3) . . . . ?
C6 C5 C10 C9 -0.6(3) . . . . ?
C4 C5 C10 C9 178.8(2) . . . . ?
P1 O2 C11 C12 77.2(2) . . . . ?
P1 O2 C11 C20 -105.00(19) . . . . ?
C20 C11 C12 C13 2.4(4) . . . . ?
O2 C11 C12 C13 -179.9(2) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
C12 C13 C14 C15 -1.4(5) . . . . ?
C13 C14 C15 C16 -178.4(3) . . . . ?
C13 C14 C15 C20 1.0(4) . . . . ?
C14 C15 C16 C17 179.3(3) . . . . ?
C20 C15 C16 C17 -0.1(4) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
C16 C17 C18 C19 0.0(5) . . . . ?
C17 C18 C19 C20 0.8(4) . . . . ?
C12 C11 C20 C19 176.7(2) . . . . ?
O2 C11 C20 C19 -1.0(3) . . . . ?
C12 C11 C20 C15 -2.7(3) . . . . ?
O2 C11 C20 C15 179.62(17) . . . . ?
C18 C19 C20 C11 179.3(2) . . . . ?
C18 C19 C20 C15 -1.3(3) . . . . ?
C16 C15 C20 C11 -179.7(2) . . . . ?
C14 C15 C20 C11 0.9(3) . . . . ?
C16 C15 C20 C19 0.9(3) . . . . ?
C14 C15 C20 C19 -178.5(2) . . . . ?
P1 O3 C21 C22 -74.1(2) . . . . ?
P1 O3 C21 C30 107.15(17) . . . . ?
C30 C21 C22 C23 -2.2(3) . . . . ?
O3 C21 C22 C23 179.18(19) . . . . ?
C21 C22 C23 C24 0.8(4) . . . . ?
C22 C23 C24 C25 1.2(4) . . . . ?
C23 C24 C25 C26 179.1(2) . . . . ?
C23 C24 C25 C30 -1.9(3) . . . . ?
C24 C25 C26 C27 178.8(2) . . . . ?
C30 C25 C26 C27 -0.3(3) . . . . ?
C25 C26 C27 C28 -0.7(4) . . . . ?
C26 C27 C28 C29 1.3(4) . . . . ?
C27 C28 C29 C30 -1.0(3) . . . . ?
C22 C21 C30 C25 1.4(3) . . . . ?
O3 C21 C30 C25 -179.83(16) . . . . ?
C22 C21 C30 C29 -179.54(19) . . . . ?
O3 C21 C30 C29 -0.8(3) . . . . ?
C26 C25 C30 C21 179.66(18) . . . . ?
C24 C25 C30 C21 0.6(3) . . . . ?
C26 C25 C30 C29 0.6(3) . . . . ?
C24 C25 C30 C29 -178.47(19) . . . . ?
C28 C29 C30 C21 -179.0(2) . . . . ?
C28 C29 C30 C25 0.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.64
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.039
