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

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

data_a
_audit_block_doi                 10.5517/cc145m0y
_database_code_depnum_ccdc_archive 'CCDC 1048079'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H29 Cl N O P Pd'
_chemical_formula_weight         532.31

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   16.151(3)
_cell_length_b                   9.5824(19)
_cell_length_c                   16.403(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.38(3)
_cell_angle_gamma                90.00
_cell_volume                     2363.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7382
_exptl_absorpt_correction_T_max  0.8971

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9443
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4108
_reflns_number_gt                3940
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


_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)+(0.0450P)²+2.0633P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4108
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0818
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.003
_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
Pd1 Pd 0.265347(12) 1.004124(18) 0.063309(12) 0.01769(9) Uani 1 1 d . . .
P1 P 0.31611(4) 0.81660(7) 0.01469(4) 0.01849(15) Uani 1 1 d . . .
Cl1 Cl 0.14531(5) 1.03948(8) -0.07704(4) 0.02909(16) Uani 1 1 d . . .
N1 N 0.22961(14) 1.1646(2) 0.13222(14) 0.0231(5) Uani 1 1 d . . .
O1 O 0.14509(13) 1.2191(2) 0.12148(14) 0.0359(5) Uani 1 1 d . . .
C14 C 0.24101(17) 0.6682(3) -0.00075(16) 0.0218(5) Uani 1 1 d . . .
C8 C 0.32576(16) 0.8446(3) -0.09141(16) 0.0208(5) Uani 1 1 d . . .
C3 C 0.37569(19) 1.0233(3) 0.17334(18) 0.0232(6) Uani 1 1 d . . .
H3A H 0.3692 0.9683 0.2218 0.028 Uiso 1 1 calc R . .
H3B H 0.4288 0.9895 0.1627 0.028 Uiso 1 1 calc R . .
C20 C 0.42236(17) 0.7389(3) 0.08236(16) 0.0203(5) Uani 1 1 d . . .
C21 C 0.43509(18) 0.7007(3) 0.16831(18) 0.0260(6) Uani 1 1 d . . .
H21 H 0.3898 0.7194 0.1909 0.031 Uiso 1 1 calc R . .
C2 C 0.38481(17) 1.1797(3) 0.19634(17) 0.0258(6) Uani 1 1 d . . .
C23 C 0.57938(19) 0.6095(3) 0.18867(19) 0.0323(7) Uani 1 1 d . . .
H23 H 0.6328 0.5652 0.2247 0.039 Uiso 1 1 calc R . .
C12 C 0.31274(19) 0.7729(3) -0.23648(18) 0.0327(7) Uani 1 1 d . . .
H12 H 0.2979 0.7038 -0.2811 0.039 Uiso 1 1 calc R . .
C4 C 0.42463(19) 1.2579(3) 0.1376(2) 0.0326(7) Uani 1 1 d . . .
H4B H 0.4851 1.2239 0.1491 0.049 Uiso 1 1 calc R . .
H4C H 0.4265 1.3581 0.1502 0.049 Uiso 1 1 calc R . .
H4A H 0.3878 1.2417 0.0761 0.049 Uiso 1 1 calc R . .
C25 C 0.49035(19) 0.7123(3) 0.05110(18) 0.0281(6) Uani 1 1 d . . .
H25 H 0.4835 0.7386 -0.0068 0.034 Uiso 1 1 calc R . .
C7 C 0.07797(18) 1.1157(4) 0.0912(2) 0.0379(7) Uani 1 1 d . . .
H7B H 0.0726 1.0854 0.0325 0.057 Uiso 1 1 calc R . .
H7C H 0.0211 1.1547 0.0892 0.057 Uiso 1 1 calc R . .
H7A H 0.0938 1.0357 0.1312 0.057 Uiso 1 1 calc R . .
C15 C 0.2713(2) 0.5319(3) 0.00076(18) 0.0263(6) Uani 1 1 d . . .
H15 H 0.3325 0.5153 0.0120 0.032 Uiso 1 1 calc R . .
C9 C 0.3560(2) 0.9740(3) -0.1069(2) 0.0300(6) Uani 1 1 d . . .
H9 H 0.3706 1.0438 -0.0628 0.036 Uiso 1 1 calc R . .
C22 C 0.51261(19) 0.6361(3) 0.22082(18) 0.0299(6) Uani 1 1 d . . .
H22 H 0.5202 0.6100 0.2790 0.036 Uiso 1 1 calc R . .
C13 C 0.30431(18) 0.7437(3) -0.15644(17) 0.0278(6) Uani 1 1 d . . .
H13 H 0.2839 0.6547 -0.1465 0.033 Uiso 1 1 calc R . .
C24 C 0.56800(19) 0.6474(3) 0.1045(2) 0.0351(7) Uani 1 1 d . . .
H24 H 0.6138 0.6290 0.0826 0.042 Uiso 1 1 calc R . .
C1 C 0.29396(18) 1.2381(3) 0.18214(17) 0.0280(6) Uani 1 1 d . . .
C17 C 0.1251(2) 0.4420(3) -0.02888(18) 0.0328(7) Uani 1 1 d . . .
H17 H 0.0856 0.3651 -0.0383 0.039 Uiso 1 1 calc R . .
C5 C 0.4468(2) 1.1981(4) 0.2927(2) 0.0436(8) Uani 1 1 d . . .
H5A H 0.4182 1.1593 0.3311 0.065 Uiso 1 1 calc R . .
H5C H 0.4587 1.2976 0.3055 0.065 Uiso 1 1 calc R . .
H5B H 0.5029 1.1490 0.3028 0.065 Uiso 1 1 calc R . .
C19 C 0.15148(19) 0.6894(3) -0.0163(2) 0.0340(7) Uani 1 1 d . . .
H19 H 0.1294 0.7816 -0.0175 0.041 Uiso 1 1 calc R . .
C16 C 0.2134(2) 0.4205(3) -0.01389(17) 0.0303(6) Uani 1 1 d . . .
H16 H 0.2349 0.3281 -0.0136 0.036 Uiso 1 1 calc R . .
C18 C 0.0942(2) 0.5766(3) -0.0301(2) 0.0401(8) Uani 1 1 d . . .
H18 H 0.0331 0.5921 -0.0404 0.048 Uiso 1 1 calc R . .
C11 C 0.34259(18) 0.9016(3) -0.25070(18) 0.0321(7) Uani 1 1 d . . .
H11 H 0.3476 0.9213 -0.3055 0.039 Uiso 1 1 calc R . .
C10 C 0.3652(2) 1.0023(3) -0.1864(2) 0.0342(8) Uani 1 1 d . . .
H10 H 0.3870 1.0903 -0.1962 0.041 Uiso 1 1 calc R . .
C6 C 0.2817(2) 1.3738(4) 0.2220(2) 0.0479(9) Uani 1 1 d . . .
H6B H 0.2275 1.4199 0.1830 0.072 Uiso 1 1 calc R . .
H6C H 0.3330 1.4343 0.2303 0.072 Uiso 1 1 calc R . .
H6A H 0.2764 1.3560 0.2787 0.072 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C3 2.030(3) . ?
Pd1 N1 2.110(2) . ?
Pd1 P1 2.2392(7) . ?
Pd1 Cl1 2.4330(12) . ?
P1 C8 1.823(2) . ?
P1 C14 1.826(3) . ?
P1 C20 1.828(3) . ?
N1 C1 1.276(4) . ?
N1 O1 1.411(3) . ?
O1 C7 1.418(4) . ?
C14 C19 1.389(4) . ?
C14 C15 1.392(4) . ?
C8 C13 1.387(4) . ?
C8 C9 1.389(4) . ?
C3 C2 1.539(4) . ?
C20 C25 1.394(4) . ?
C20 C21 1.397(4) . ?
C21 C22 1.381(4) . ?
C2 C1 1.507(4) . ?
C2 C4 1.534(4) . ?
C2 C5 1.543(4) . ?
C23 C24 1.373(4) . ?
C23 C22 1.386(4) . ?
C12 C11 1.375(4) . ?
C12 C13 1.397(4) . ?
C25 C24 1.388(4) . ?
C15 C16 1.382(4) . ?
C9 C10 1.393(4) . ?
C1 C6 1.501(4) . ?
C17 C16 1.372(4) . ?
C17 C18 1.380(5) . ?
C19 C18 1.387(4) . ?
C11 C10 1.376(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Pd1 N1 77.33(10) . . ?
C3 Pd1 P1 94.15(8) . . ?
N1 Pd1 P1 169.40(6) . . ?
C3 Pd1 Cl1 165.25(8) . . ?
N1 Pd1 Cl1 97.25(6) . . ?
P1 Pd1 Cl1 92.50(3) . . ?
C8 P1 C14 105.42(12) . . ?
C8 P1 C20 104.58(12) . . ?
C14 P1 C20 101.32(12) . . ?
C8 P1 Pd1 113.05(9) . . ?
C14 P1 Pd1 111.32(9) . . ?
C20 P1 Pd1 119.67(8) . . ?
C1 N1 O1 113.6(2) . . ?
C1 N1 Pd1 115.38(17) . . ?
O1 N1 Pd1 130.08(16) . . ?
N1 O1 C7 111.5(2) . . ?
C19 C14 C15 118.5(3) . . ?
C19 C14 P1 120.4(2) . . ?
C15 C14 P1 121.1(2) . . ?
C13 C8 C9 119.2(2) . . ?
C13 C8 P1 123.2(2) . . ?
C9 C8 P1 117.6(2) . . ?
C2 C3 Pd1 106.29(17) . . ?
C25 C20 C21 118.5(2) . . ?
C25 C20 P1 122.8(2) . . ?
C21 C20 P1 118.7(2) . . ?
C22 C21 C20 120.9(2) . . ?
C1 C2 C4 109.2(2) . . ?
C1 C2 C3 108.9(2) . . ?
C4 C2 C3 110.3(2) . . ?
C1 C2 C5 110.3(2) . . ?
C4 C2 C5 108.9(2) . . ?
C3 C2 C5 109.3(2) . . ?
C24 C23 C22 119.7(3) . . ?
C11 C12 C13 120.0(3) . . ?
C24 C25 C20 120.1(3) . . ?
C16 C15 C14 120.7(3) . . ?
C8 C9 C10 120.6(3) . . ?
C21 C22 C23 120.0(3) . . ?
C8 C13 C12 120.1(3) . . ?
C23 C24 C25 120.8(3) . . ?
N1 C1 C6 123.5(3) . . ?
N1 C1 C2 114.4(2) . . ?
C6 C1 C2 122.1(3) . . ?
C16 C17 C18 119.4(3) . . ?
C18 C19 C14 120.3(3) . . ?
C17 C16 C15 120.6(3) . . ?
C17 C18 C19 120.6(3) . . ?
C12 C11 C10 120.7(3) . . ?
C11 C10 C9 119.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.061
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1057827'
_audit_update_record             
;
2015-04-03 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_absolute_configuration rm
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H65 N O5'
_chemical_formula_weight         724.00

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2

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

_cell_length_a                   35.188(7)
_cell_length_b                   7.4837(15)
_cell_length_c                   16.526(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.87(3)
_cell_angle_gamma                90.00
_cell_volume                     4299.8(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1576
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9804
_exptl_absorpt_correction_T_max  0.9965

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30058
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.17
_diffrn_reflns_theta_max         27.48
_reflns_number_total             9845
_reflns_number_gt                7661
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


_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)+(0.0822P)²+9.0740P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_number_reflns         9845
_refine_ls_number_parameters     487
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0992
_refine_ls_wR_factor_ref         0.2303
_refine_ls_wR_factor_gt          0.2153
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
C16 C 0.29312(11) 0.5125(5) 0.3187(2) 0.0321(8) Uani 1 1 d . . .
C13 C 0.27764(11) 0.4890(5) 0.2294(2) 0.0339(9) Uani 1 1 d . . .
O5 O 0.40725(9) 1.0178(4) 0.6315(2) 0.0484(8) Uani 1 1 d . . .
C4 C 0.30586(11) 0.7030(5) 0.4463(2) 0.0294(8) Uani 1 1 d . . .
C19 C 0.33942(11) 0.5695(5) 0.4742(2) 0.0311(8) Uani 1 1 d . . .
H19 H 0.3587 0.5931 0.4368 0.037 Uiso 1 1 calc R . .
C27 C 0.37715(13) 0.3712(6) 0.7546(2) 0.0394(10) Uani 1 1 d . . .
H27 H 0.3774 0.2624 0.7251 0.047 Uiso 1 1 calc R . .
C3 C 0.32138(12) 0.8954(5) 0.4662(2) 0.0337(9) Uani 1 1 d . . .
H3A H 0.3417 0.9221 0.4327 0.040 Uiso 1 1 calc R . .
H3B H 0.3002 0.9823 0.4511 0.040 Uiso 1 1 calc R . .
C17 C 0.31136(14) 0.3553(5) 0.3632(3) 0.0418(10) Uani 1 1 d . . .
H17A H 0.3335 0.3184 0.3366 0.050 Uiso 1 1 calc R . .
H17B H 0.2926 0.2558 0.3564 0.050 Uiso 1 1 calc R . .
C1 C 0.37012(12) 0.7891(6) 0.5804(2) 0.0348(9) Uani 1 1 d . . .
C10 C 0.23079(12) 0.5604(5) 0.1114(2) 0.0345(9) Uani 1 1 d . . .
H10 H 0.2508 0.5987 0.0782 0.041 Uiso 1 1 calc R . .
C39 C 0.19125(12) 0.6265(6) 0.0663(3) 0.0385(9) Uani 1 1 d . . .
H39 H 0.1707 0.5870 0.0979 0.046 Uiso 1 1 calc R . .
C34 C 0.46622(11) 0.4810(7) 0.3697(3) 0.0416(10) Uani 1 1 d . . .
C18 C 0.32559(12) 0.3793(5) 0.4546(2) 0.0334(9) Uani 1 1 d . . .
H18A H 0.3045 0.3509 0.4857 0.040 Uiso 1 1 calc R . .
H18B H 0.3470 0.2949 0.4720 0.040 Uiso 1 1 calc R . .
C9 C 0.24431(11) 0.6218(5) 0.2011(2) 0.0290(8) Uani 1 1 d . . .
C2 C 0.33767(12) 0.9180(5) 0.5563(2) 0.0358(9) Uani 1 1 d . . .
H2A H 0.3471 1.0418 0.5665 0.043 Uiso 1 1 calc R . .
H2B H 0.3172 0.8963 0.5900 0.043 Uiso 1 1 calc R . .
O1 O 0.48999(12) 0.3421(6) 0.2583(2) 0.0692(11) Uani 1 1 d . . .
O2 O 0.50521(10) 0.6254(6) 0.2881(2) 0.0620(10) Uani 1 1 d . . .
N1 N 0.40406(10) 0.8319(4) 0.6151(2) 0.0371(8) Uani 1 1 d . . .
C20 C 0.36250(11) 0.5898(5) 0.5629(2) 0.0301(8) Uani 1 1 d . . .
C30 C 0.40054(12) 0.4787(5) 0.5700(2) 0.0345(9) Uani 1 1 d . . .
H30A H 0.4176 0.5192 0.6199 0.041 Uiso 1 1 calc R . .
H30B H 0.3940 0.3523 0.5790 0.041 Uiso 1 1 calc R . .
C6 C 0.29328(11) 0.6767(5) 0.3530(2) 0.0316(8) Uani 1 1 d . . .
C7 C 0.27704(13) 0.8375(6) 0.3058(2) 0.0379(9) Uani 1 1 d . . .
H7A H 0.2977 0.9282 0.3086 0.045 Uiso 1 1 calc R . .
H7B H 0.2566 0.8881 0.3340 0.045 Uiso 1 1 calc R . .
C8 C 0.26010(12) 0.8099(5) 0.2153(2) 0.0351(9) Uani 1 1 d . . .
H8A H 0.2392 0.8976 0.1992 0.042 Uiso 1 1 calc R . .
H8B H 0.2803 0.8306 0.1808 0.042 Uiso 1 1 calc R . .
C5 C 0.26897(12) 0.6726(6) 0.4845(3) 0.0375(9) Uani 1 1 d . . .
H5A H 0.2622 0.5456 0.4812 0.056 Uiso 1 1 calc R . .
H5B H 0.2479 0.7429 0.4545 0.056 Uiso 1 1 calc R . .
H5C H 0.2735 0.7102 0.5420 0.056 Uiso 1 1 calc R . .
C31 C 0.42337(11) 0.4838(6) 0.5003(2) 0.0349(9) Uani 1 1 d . . .
C23 C 0.35949(15) 0.6781(6) 0.7615(3) 0.0490(12) Uani 1 1 d . . .
H23 H 0.3478 0.7820 0.7355 0.059 Uiso 1 1 calc R . .
C21 C 0.33880(12) 0.5157(6) 0.6285(2) 0.0385(9) Uani 1 1 d . . .
H21A H 0.3147 0.5857 0.6252 0.046 Uiso 1 1 calc R . .
H21B H 0.3315 0.3905 0.6144 0.046 Uiso 1 1 calc R . .
O4 O 0.42814(16) 0.4050(7) 0.9954(2) 0.0998(18) Uani 1 1 d . . .
C12 C 0.25845(13) 0.3094(6) 0.2012(3) 0.0415(10) Uani 1 1 d . . .
H12A H 0.2781 0.2185 0.1938 0.050 Uiso 1 1 calc R . .
H12B H 0.2427 0.2645 0.2417 0.050 Uiso 1 1 calc R . .
C22 C 0.35937(12) 0.5209(5) 0.7162(2) 0.0348(9) Uani 1 1 d . . .
C37 C 0.48790(13) 0.4721(7) 0.2997(3) 0.0449(11) Uani 1 1 d . . .
C32 C 0.44177(14) 0.6346(7) 0.4778(3) 0.0507(12) Uani 1 1 d . . .
H32 H 0.4399 0.7424 0.5073 0.061 Uiso 1 1 calc R . .
C11 C 0.23297(13) 0.3516(6) 0.1191(3) 0.0389(10) Uani 1 1 d . . .
H11A H 0.2069 0.3008 0.1182 0.047 Uiso 1 1 calc R . .
H11B H 0.2443 0.2999 0.0731 0.047 Uiso 1 1 calc R . .
C15 C 0.21142(12) 0.5961(6) 0.2507(2) 0.0370(9) Uani 1 1 d . . .
H15A H 0.1990 0.4805 0.2369 0.056 Uiso 1 1 calc R . .
H15B H 0.1925 0.6921 0.2376 0.056 Uiso 1 1 calc R . .
H15C H 0.2216 0.5993 0.3093 0.056 Uiso 1 1 calc R . .
C26 C 0.39441(14) 0.3792(7) 0.8348(3) 0.0506(12) Uani 1 1 d . . .
H26 H 0.4069 0.2767 0.8604 0.061 Uiso 1 1 calc R . .
C36 C 0.42753(15) 0.3297(7) 0.4558(3) 0.0505(12) Uani 1 1 d . . .
H36 H 0.4158 0.2224 0.4700 0.061 Uiso 1 1 calc R . .
C25 C 0.39358(15) 0.5394(8) 0.8792(3) 0.0536(13) Uani 1 1 d . . .
C40 C 0.19023(14) 0.8308(7) 0.0599(3) 0.0468(11) Uani 1 1 d . . .
H40A H 0.1918 0.8826 0.1148 0.070 Uiso 1 1 calc R . .
H40B H 0.1662 0.8683 0.0262 0.070 Uiso 1 1 calc R . .
H40C H 0.2121 0.8723 0.0346 0.070 Uiso 1 1 calc R . .
C24 C 0.37586(17) 0.6880(7) 0.8418(3) 0.0590(14) Uani 1 1 d . . .
H24 H 0.3750 0.7963 0.8715 0.071 Uiso 1 1 calc R . .
C43 C 0.13874(14) 0.4836(8) -0.1509(3) 0.0517(12) Uani 1 1 d . . .
H43A H 0.1608 0.5152 -0.1789 0.062 Uiso 1 1 calc R . .
H43B H 0.1404 0.3536 -0.1397 0.062 Uiso 1 1 calc R . .
C41 C 0.18354(12) 0.5425(7) -0.0190(2) 0.0421(10) Uani 1 1 d . . .
H41A H 0.1866 0.4115 -0.0129 0.051 Uiso 1 1 calc R . .
H41B H 0.2035 0.5854 -0.0506 0.051 Uiso 1 1 calc R . .
C33 C 0.46295(14) 0.6340(7) 0.4135(3) 0.0548(13) Uani 1 1 d . . .
H33 H 0.4753 0.7404 0.3999 0.066 Uiso 1 1 calc R . .
C42 C 0.14404(13) 0.5805(7) -0.0689(3) 0.0456(11) Uani 1 1 d . . .
H42A H 0.1238 0.5418 -0.0373 0.055 Uiso 1 1 calc R . .
H42B H 0.1412 0.7107 -0.0785 0.055 Uiso 1 1 calc R . .
C44 C 0.10228(14) 0.5171(8) -0.2103(3) 0.0538(12) Uani 1 1 d . . .
H44 H 0.0988 0.6494 -0.2157 0.065 Uiso 1 1 calc R . .
C35 C 0.44846(15) 0.3277(7) 0.3907(3) 0.0537(12) Uani 1 1 d . . .
H35 H 0.4505 0.2204 0.3609 0.064 Uiso 1 1 calc R . .
C14 C 0.31217(12) 0.5112(6) 0.1820(3) 0.0437(10) Uani 1 1 d . . .
H14A H 0.3225 0.6325 0.1901 0.066 Uiso 1 1 calc R . .
H14B H 0.3035 0.4906 0.1234 0.066 Uiso 1 1 calc R . .
H14C H 0.3322 0.4244 0.2024 0.066 Uiso 1 1 calc R . .
C38 C 0.52790(17) 0.6317(10) 0.2216(3) 0.0730(18) Uani 1 1 d . . .
H38A H 0.5137 0.6973 0.1752 0.110 Uiso 1 1 calc R . .
H38B H 0.5329 0.5098 0.2044 0.110 Uiso 1 1 calc R . .
H38C H 0.5524 0.6924 0.2403 0.110 Uiso 1 1 calc R . .
C28 C 0.4103(2) 0.5546(11) 0.9664(4) 0.089(2) Uani 1 1 d . . .
O3 O 0.4084(3) 0.6876(9) 1.0075(3) 0.160(3) Uani 1 1 d . . .
C50 C 0.44648(16) 1.0570(8) 0.6622(4) 0.0700(17) Uani 1 1 d . . .
H50A H 0.4628 1.0171 0.6227 0.105 Uiso 1 1 calc R . .
H50B H 0.4541 0.9947 0.7144 0.105 Uiso 1 1 calc R . .
H50C H 0.4496 1.1861 0.6708 0.105 Uiso 1 1 calc R . .
C46 C 0.10685(19) 0.4439(10) -0.2944(3) 0.082(2) Uani 1 1 d . . .
H46A H 0.1270 0.5111 -0.3161 0.122 Uiso 1 1 calc R . .
H46B H 0.0825 0.4563 -0.3317 0.122 Uiso 1 1 calc R . .
H46C H 0.1141 0.3175 -0.2895 0.122 Uiso 1 1 calc R . .
C45 C 0.06713(18) 0.4423(11) -0.1794(4) 0.089(2) Uani 1 1 d . . .
H45A H 0.0683 0.3114 -0.1791 0.133 Uiso 1 1 calc R . .
H45B H 0.0439 0.4814 -0.2154 0.133 Uiso 1 1 calc R . .
H45C H 0.0665 0.4856 -0.1237 0.133 Uiso 1 1 calc R . .
C29 C 0.4451(3) 0.4153(15) 1.0823(4) 0.143(4) Uani 1 1 d . . .
H29A H 0.4656 0.5054 1.0894 0.215 Uiso 1 1 calc R . .
H29B H 0.4559 0.2987 1.1005 0.215 Uiso 1 1 calc R . .
H29C H 0.4252 0.4487 1.1149 0.215 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C16 C6 1.353(5) . ?
C16 C17 1.481(6) . ?
C16 C13 1.501(5) . ?
C13 C12 1.544(6) . ?
C13 C14 1.553(6) . ?
C13 C9 1.554(5) . ?
O5 N1 1.419(5) . ?
O5 C50 1.426(6) . ?
C4 C5 1.546(5) . ?
C4 C6 1.549(5) . ?
C4 C3 1.557(5) . ?
C4 C19 1.561(5) . ?
C19 C18 1.523(5) . ?
C19 C20 1.570(5) . ?
C27 C26 1.372(6) . ?
C27 C22 1.388(6) . ?
C3 C2 1.521(6) . ?
C17 C18 1.527(6) . ?
C1 N1 1.283(5) . ?
C1 C2 1.501(6) . ?
C1 C20 1.535(5) . ?
C10 C39 1.555(6) . ?
C10 C9 1.555(5) . ?
C10 C11 1.569(6) . ?
C39 C41 1.528(6) . ?
C39 C40 1.533(7) . ?
C34 C33 1.369(7) . ?
C34 C35 1.376(7) . ?
C34 C37 1.482(6) . ?
C9 C8 1.518(5) . ?
C9 C15 1.529(5) . ?
O1 C37 1.199(6) . ?
O2 C37 1.327(6) . ?
O2 C38 1.455(6) . ?
C20 C30 1.565(5) . ?
C20 C21 1.567(5) . ?
C30 C31 1.503(5) . ?
C6 C7 1.498(5) . ?
C7 C8 1.536(6) . ?
C31 C32 1.380(6) . ?
C31 C36 1.388(6) . ?
C23 C24 1.365(7) . ?
C23 C22 1.395(6) . ?
C21 C22 1.517(6) . ?
O4 C28 1.336(9) . ?
O4 C29 1.470(8) . ?
C12 C11 1.539(6) . ?
C32 C33 1.389(6) . ?
C26 C25 1.408(7) . ?
C36 C35 1.393(6) . ?
C25 C24 1.374(8) . ?
C25 C28 1.475(7) . ?
C43 C44 1.511(7) . ?
C43 C42 1.523(6) . ?
C41 C42 1.530(6) . ?
C44 C45 1.516(8) . ?
C44 C46 1.526(7) . ?
C28 O3 1.213(9) . ?

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
C6 C16 C17 122.7(4) . . ?
C6 C16 C13 119.7(4) . . ?
C17 C16 C13 117.3(3) . . ?
C16 C13 C12 118.3(3) . . ?
C16 C13 C14 106.9(3) . . ?
C12 C13 C14 106.2(3) . . ?
C16 C13 C9 111.3(3) . . ?
C12 C13 C9 101.0(3) . . ?
C14 C13 C9 113.1(3) . . ?
N1 O5 C50 108.3(4) . . ?
C5 C4 C6 105.0(3) . . ?
C5 C4 C3 109.8(3) . . ?
C6 C4 C3 111.4(3) . . ?
C5 C4 C19 115.5(3) . . ?
C6 C4 C19 107.4(3) . . ?
C3 C4 C19 107.7(3) . . ?
C18 C19 C4 109.4(3) . . ?
C18 C19 C20 113.0(3) . . ?
C4 C19 C20 118.2(3) . . ?
C26 C27 C22 120.6(4) . . ?
C2 C3 C4 112.1(3) . . ?
C16 C17 C18 116.7(3) . . ?
N1 C1 C2 125.2(4) . . ?
N1 C1 C20 116.7(4) . . ?
C2 C1 C20 118.1(4) . . ?
C39 C10 C9 118.9(3) . . ?
C39 C10 C11 112.6(3) . . ?
C9 C10 C11 102.3(3) . . ?
C41 C39 C40 110.3(4) . . ?
C41 C39 C10 109.3(3) . . ?
C40 C39 C10 111.1(4) . . ?
C33 C34 C35 119.0(4) . . ?
C33 C34 C37 123.1(5) . . ?
C35 C34 C37 117.9(4) . . ?
C19 C18 C17 111.5(3) . . ?
C8 C9 C15 108.8(3) . . ?
C8 C9 C13 107.8(3) . . ?
C15 C9 C13 110.9(3) . . ?
C8 C9 C10 118.2(3) . . ?
C15 C9 C10 109.1(3) . . ?
C13 C9 C10 101.8(3) . . ?
C1 C2 C3 110.2(3) . . ?
C37 O2 C38 117.1(4) . . ?
C1 N1 O5 111.8(3) . . ?
C1 C20 C30 112.3(3) . . ?
C1 C20 C21 108.1(3) . . ?
C30 C20 C21 107.5(3) . . ?
C1 C20 C19 108.7(3) . . ?
C30 C20 C19 109.4(3) . . ?
C21 C20 C19 111.0(3) . . ?
C31 C30 C20 118.7(3) . . ?
C16 C6 C7 122.3(4) . . ?
C16 C6 C4 121.0(3) . . ?
C7 C6 C4 116.3(3) . . ?
C6 C7 C8 117.3(3) . . ?
C9 C8 C7 110.7(3) . . ?
C32 C31 C36 116.3(4) . . ?
C32 C31 C30 123.8(4) . . ?
C36 C31 C30 119.9(4) . . ?
C24 C23 C22 122.2(5) . . ?
C22 C21 C20 115.2(3) . . ?
C28 O4 C29 113.9(7) . . ?
C11 C12 C13 104.8(3) . . ?
C27 C22 C23 118.1(4) . . ?
C27 C22 C21 122.1(4) . . ?
C23 C22 C21 119.7(4) . . ?
O1 C37 O2 123.3(4) . . ?
O1 C37 C34 124.5(5) . . ?
O2 C37 C34 112.2(4) . . ?
C31 C32 C33 122.2(4) . . ?
C12 C11 C10 106.9(3) . . ?
C27 C26 C25 119.9(5) . . ?
C31 C36 C35 122.0(5) . . ?
C24 C25 C26 120.0(4) . . ?
C24 C25 C28 117.5(5) . . ?
C26 C25 C28 122.5(6) . . ?
C23 C24 C25 119.2(5) . . ?
C44 C43 C42 118.3(4) . . ?
C39 C41 C42 116.0(4) . . ?
C34 C33 C32 120.4(5) . . ?
C43 C42 C41 111.6(4) . . ?
C43 C44 C45 112.0(4) . . ?
C43 C44 C46 109.5(4) . . ?
C45 C44 C46 112.4(5) . . ?
C34 C35 C36 120.0(4) . . ?
O3 C28 O4 123.4(6) . . ?
O3 C28 C25 124.2(8) . . ?
O4 C28 C25 112.4(6) . . ?

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
C6 C16 C13 C12 -149.1(4) . . . . ?
C17 C16 C13 C12 37.2(5) . . . . ?
C6 C16 C13 C14 91.2(4) . . . . ?
C17 C16 C13 C14 -82.6(4) . . . . ?
C6 C16 C13 C9 -32.7(5) . . . . ?
C17 C16 C13 C9 153.5(4) . . . . ?
C5 C4 C19 C18 57.7(4) . . . . ?
C6 C4 C19 C18 -59.0(4) . . . . ?
C3 C4 C19 C18 -179.1(3) . . . . ?
C5 C4 C19 C20 -73.6(4) . . . . ?
C6 C4 C19 C20 169.6(3) . . . . ?
C3 C4 C19 C20 49.5(4) . . . . ?
C5 C4 C3 C2 70.0(4) . . . . ?
C6 C4 C3 C2 -174.1(3) . . . . ?
C19 C4 C3 C2 -56.5(4) . . . . ?
C6 C16 C17 C18 8.6(6) . . . . ?
C13 C16 C17 C18 -177.8(4) . . . . ?
C9 C10 C39 C41 -177.5(4) . . . . ?
C11 C10 C39 C41 -58.0(5) . . . . ?
C9 C10 C39 C40 60.5(5) . . . . ?
C11 C10 C39 C40 -180.0(4) . . . . ?
C4 C19 C18 C17 58.7(4) . . . . ?
C20 C19 C18 C17 -167.3(3) . . . . ?
C16 C17 C18 C19 -32.5(5) . . . . ?
C16 C13 C9 C8 60.3(4) . . . . ?
C12 C13 C9 C8 -173.2(3) . . . . ?
C14 C13 C9 C8 -60.1(4) . . . . ?
C16 C13 C9 C15 -58.8(4) . . . . ?
C12 C13 C9 C15 67.7(4) . . . . ?
C14 C13 C9 C15 -179.1(3) . . . . ?
C16 C13 C9 C10 -174.8(3) . . . . ?
C12 C13 C9 C10 -48.2(4) . . . . ?
C14 C13 C9 C10 64.9(4) . . . . ?
C39 C10 C9 C8 -77.3(5) . . . . ?
C11 C10 C9 C8 158.0(3) . . . . ?
C39 C10 C9 C15 47.7(5) . . . . ?
C11 C10 C9 C15 -77.0(4) . . . . ?
C39 C10 C9 C13 165.0(3) . . . . ?
C11 C10 C9 C13 40.2(4) . . . . ?
N1 C1 C2 C3 126.0(4) . . . . ?
C20 C1 C2 C3 -54.3(5) . . . . ?
C4 C3 C2 C1 59.6(5) . . . . ?
C2 C1 N1 O5 2.4(5) . . . . ?
C20 C1 N1 O5 -177.3(3) . . . . ?
C50 O5 N1 C1 -174.2(4) . . . . ?
N1 C1 C20 C30 -14.9(5) . . . . ?
C2 C1 C20 C30 165.4(3) . . . . ?
N1 C1 C20 C21 103.5(4) . . . . ?
C2 C1 C20 C21 -76.3(4) . . . . ?
N1 C1 C20 C19 -136.1(4) . . . . ?
C2 C1 C20 C19 44.2(4) . . . . ?
C18 C19 C20 C1 -172.2(3) . . . . ?
C4 C19 C20 C1 -42.6(4) . . . . ?
C18 C19 C20 C30 64.8(4) . . . . ?
C4 C19 C20 C30 -165.5(3) . . . . ?
C18 C19 C20 C21 -53.6(4) . . . . ?
C4 C19 C20 C21 76.1(4) . . . . ?
C1 C20 C30 C31 -78.5(4) . . . . ?
C21 C20 C30 C31 162.8(4) . . . . ?
C19 C20 C30 C31 42.2(5) . . . . ?
C17 C16 C6 C7 175.9(4) . . . . ?
C13 C16 C6 C7 2.4(6) . . . . ?
C17 C16 C6 C4 -11.7(6) . . . . ?
C13 C16 C6 C4 174.8(3) . . . . ?
C5 C4 C6 C16 -86.9(4) . . . . ?
C3 C4 C6 C16 154.3(4) . . . . ?
C19 C4 C6 C16 36.5(5) . . . . ?
C5 C4 C6 C7 86.0(4) . . . . ?
C3 C4 C6 C7 -32.9(5) . . . . ?
C19 C4 C6 C7 -150.6(3) . . . . ?
C16 C6 C7 C8 -0.4(6) . . . . ?
C4 C6 C7 C8 -173.1(3) . . . . ?
C15 C9 C8 C7 62.7(4) . . . . ?
C13 C9 C8 C7 -57.6(4) . . . . ?
C10 C9 C8 C7 -172.1(3) . . . . ?
C6 C7 C8 C9 29.4(5) . . . . ?
C20 C30 C31 C32 66.5(5) . . . . ?
C20 C30 C31 C36 -115.0(4) . . . . ?
C1 C20 C21 C22 -63.8(4) . . . . ?
C30 C20 C21 C22 57.6(4) . . . . ?
C19 C20 C21 C22 177.1(3) . . . . ?
C16 C13 C12 C11 158.9(4) . . . . ?
C14 C13 C12 C11 -81.1(4) . . . . ?
C9 C13 C12 C11 37.2(4) . . . . ?
C26 C27 C22 C23 -0.2(6) . . . . ?
C26 C27 C22 C21 -177.9(4) . . . . ?
C24 C23 C22 C27 -1.0(7) . . . . ?
C24 C23 C22 C21 176.7(4) . . . . ?
C20 C21 C22 C27 -99.4(5) . . . . ?
C20 C21 C22 C23 83.0(5) . . . . ?
C38 O2 C37 O1 -0.5(7) . . . . ?
C38 O2 C37 C34 179.1(4) . . . . ?
C33 C34 C37 O1 -176.9(5) . . . . ?
C35 C34 C37 O1 2.7(7) . . . . ?
C33 C34 C37 O2 3.5(6) . . . . ?
C35 C34 C37 O2 -176.9(4) . . . . ?
C36 C31 C32 C33 0.8(7) . . . . ?
C30 C31 C32 C33 179.3(4) . . . . ?
C13 C12 C11 C10 -12.4(5) . . . . ?
C39 C10 C11 C12 -146.1(3) . . . . ?
C9 C10 C11 C12 -17.3(4) . . . . ?
C22 C27 C26 C25 1.1(7) . . . . ?
C32 C31 C36 C35 -1.3(7) . . . . ?
C30 C31 C36 C35 -179.9(4) . . . . ?
C27 C26 C25 C24 -0.7(7) . . . . ?
C27 C26 C25 C28 177.6(5) . . . . ?
C22 C23 C24 C25 1.4(8) . . . . ?
C26 C25 C24 C23 -0.5(8) . . . . ?
C28 C25 C24 C23 -178.9(5) . . . . ?
C40 C39 C41 C42 -62.9(5) . . . . ?
C10 C39 C41 C42 174.7(4) . . . . ?
C35 C34 C33 C32 -0.5(8) . . . . ?
C37 C34 C33 C32 179.1(5) . . . . ?
C31 C32 C33 C34 0.1(8) . . . . ?
C44 C43 C42 C41 -175.8(4) . . . . ?
C39 C41 C42 C43 -177.3(4) . . . . ?
C42 C43 C44 C45 -67.9(7) . . . . ?
C42 C43 C44 C46 166.8(5) . . . . ?
C33 C34 C35 C36 0.0(8) . . . . ?
C37 C34 C35 C36 -179.6(4) . . . . ?
C31 C36 C35 C34 0.9(8) . . . . ?
C29 O4 C28 O3 0.3(12) . . . . ?
C29 O4 C28 C25 -179.9(6) . . . . ?
C24 C25 C28 O3 2.3(11) . . . . ?
C26 C25 C28 O3 -176.0(8) . . . . ?
C24 C25 C28 O4 -177.4(6) . . . . ?
C26 C25 C28 O4 4.2(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.066
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.100 0.000 0.762 8.9 1.3
2 0.500 0.002 1.000 125.4 30.0
3 0.500 0.020 0.500 16.2 0.7
4 0.900 0.000 0.238 8.9 1.3
5 0.000 0.502 0.000 125.4 30.0
6 0.000 0.520 0.500 16.2 0.7
7 0.400 0.500 0.238 8.9 1.3
8 0.600 0.500 0.762 8.9 1.3
_platon_squeeze_details          
; ?
;
