# 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_becker2
_database_code_depnum_ccdc_archive 'CCDC 986846'
_audit_update_record             
;
2015-02-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        'sodium 1,4,2-diazaphospholidine-3,5-dionide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H50 N2 Na1 O4 P1'
_chemical_formula_sum            'C34 H50 N2 Na1 O4 P1'
_chemical_formula_weight         604.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0360 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   10.6728(3)
_cell_length_b                   15.0865(4)
_cell_length_c                   21.8147(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.643(3)
_cell_angle_gamma                90
_cell_volume                     3505.42(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5460
_cell_measurement_theta_min      2.939
_cell_measurement_theta_max      25.691

_exptl_crystal_description       block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.128
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.99172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
Empirical absorption correction using spherical harmonics
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34338
_diffrn_reflns_av_unetI/netI     0.0990
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.858
_diffrn_reflns_theta_max         30.694
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9890
_reflns_number_gt                5941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

One THF Molecules shows positional disorder and was described by two positions with an occupancy ratio of 1:2.
;

_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'Olex 2'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_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)+(0.0396P)²+1.5461P] 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_number_reflns         9890
_refine_ls_number_parameters     419
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.0747
_refine_ls_wR_factor_ref         0.1523
_refine_ls_wR_factor_gt          0.1273
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8341(2) 0.32482(14) 0.16646(10) 0.0195(5) Uani 1 1 d . . . . .
C2 C 0.7834(2) 0.46420(14) 0.20883(10) 0.0221(5) Uani 1 1 d . . . . .
C3 C 0.8536(2) 0.34384(14) 0.05796(9) 0.0223(5) Uani 1 1 d . . . . .
C4 C 0.7466(2) 0.31529(16) 0.02328(10) 0.0288(5) Uani 1 1 d . . . . .
C5 C 0.7639(3) 0.27990(17) -0.03470(11) 0.0355(6) Uani 1 1 d . . . . .
H5 H 0.6943 0.2607 -0.0590 0.042 Uiso 1 1 d . U . . .
C6 C 0.8814(3) 0.27241(18) -0.05661(11) 0.0386(7) Uani 1 1 d . . . . .
H6 H 0.8907 0.2483 -0.0953 0.046 Uiso 1 1 d . U . . .
C7 C 0.9854(3) 0.30051(18) -0.02124(11) 0.0353(6) Uani 1 1 d . . . . .
H7 H 1.0645 0.2954 -0.0364 0.043 Uiso 1 1 d . U . . .
C8 C 0.9742(2) 0.33674(15) 0.03696(10) 0.0268(5) Uani 1 1 d . . . . .
C9 C 1.0893(2) 0.36543(17) 0.07598(12) 0.0348(6) Uani 1 1 d . . . . .
H9 H 1.0610 0.3969 0.1118 0.042 Uiso 1 1 d . U . . .
C10 C 1.1632(3) 0.2843(2) 0.09933(17) 0.0674(10) Uani 1 1 d . . . . .
H10A H 1.1105 0.2472 0.1222 0.101 Uiso 1 1 d . U . . .
H10B H 1.2343 0.3033 0.1253 0.101 Uiso 1 1 d . U . . .
H10C H 1.1922 0.2520 0.0650 0.101 Uiso 1 1 d . U . . .
C11 C 1.1712(3) 0.4288(2) 0.04150(16) 0.0646(10) Uani 1 1 d . . . . .
H11A H 1.1918 0.4021 0.0034 0.097 Uiso 1 1 d . U . . .
H11B H 1.2473 0.4408 0.0660 0.097 Uiso 1 1 d . U . . .
H11C H 1.1267 0.4831 0.0333 0.097 Uiso 1 1 d . U . . .
C12 C 0.6167(2) 0.32086(19) 0.04699(12) 0.0400(7) Uani 1 1 d . . . . .
H12 H 0.6245 0.3510 0.0867 0.048 Uiso 1 1 d . U . . .
C13 C 0.5616(3) 0.2293(2) 0.05730(14) 0.0501(8) Uani 1 1 d . . . . .
H13A H 0.5525 0.1980 0.0190 0.075 Uiso 1 1 d . U . . .
H13B H 0.4808 0.2353 0.0740 0.075 Uiso 1 1 d . U . . .
H13C H 0.6166 0.1967 0.0857 0.075 Uiso 1 1 d . U . . .
C14 C 0.5308(3) 0.3767(2) 0.00422(17) 0.0655(10) Uani 1 1 d . . . . .
H14A H 0.5660 0.4348 0.0005 0.099 Uiso 1 1 d . U . . .
H14B H 0.4496 0.3811 0.0205 0.099 Uiso 1 1 d . U . . .
H14C H 0.5225 0.3492 -0.0356 0.099 Uiso 1 1 d . U . . .
C15 C 0.7994(2) 0.32871(13) 0.27611(9) 0.0195(5) Uani 1 1 d . . . . .
C16 C 0.6957(2) 0.27438(14) 0.28640(10) 0.0221(5) Uani 1 1 d . . . . .
C17 C 0.6967(2) 0.22960(15) 0.34241(11) 0.0281(5) Uani 1 1 d . . . . .
H17 H 0.6304 0.1921 0.3501 0.033 Uiso 1 1 d . U . . .
C18 C 0.7942(2) 0.24038(16) 0.38625(11) 0.0295(6) Uani 1 1 d . . . . .
H18 H 0.7932 0.2098 0.4232 0.035 Uiso 1 1 d . U . . .
C19 C 0.8934(2) 0.29566(16) 0.37572(10) 0.0278(5) Uani 1 1 d . . . . .
H19 H 0.9577 0.3031 0.4062 0.033 Uiso 1 1 d . U . . .
C20 C 0.8990(2) 0.34083(14) 0.32014(10) 0.0235(5) Uani 1 1 d . . . . .
C21 C 1.0118(2) 0.39800(16) 0.30814(11) 0.0284(5) Uani 1 1 d . . . . .
H21 H 0.9927 0.4303 0.2697 0.034 Uiso 1 1 d . U . . .
C22 C 1.0388(3) 0.4661(2) 0.35863(13) 0.0505(8) Uani 1 1 d . . . . .
H22A H 0.9662 0.5028 0.3624 0.076 Uiso 1 1 d . U . . .
H22B H 1.1086 0.5026 0.3485 0.076 Uiso 1 1 d . U . . .
H22C H 1.0592 0.4364 0.3969 0.076 Uiso 1 1 d . U . . .
C23 C 1.1260(3) 0.3398(2) 0.29932(17) 0.0587(9) Uani 1 1 d . . . . .
H23A H 1.1430 0.3040 0.3353 0.089 Uiso 1 1 d . U . . .
H23B H 1.1973 0.3764 0.2928 0.089 Uiso 1 1 d . U . . .
H23C H 1.1090 0.3020 0.2643 0.089 Uiso 1 1 d . U . . .
C24 C 0.5847(2) 0.26836(15) 0.23941(11) 0.0275(5) Uani 1 1 d . . . . .
H24 H 0.6173 0.2730 0.1986 0.033 Uiso 1 1 d . U . . .
C25 C 0.5127(3) 0.18154(17) 0.24193(13) 0.0415(7) Uani 1 1 d . . . . .
H25A H 0.5697 0.1328 0.2392 0.062 Uiso 1 1 d . U . . .
H25B H 0.4505 0.1791 0.2081 0.062 Uiso 1 1 d . U . . .
H25C H 0.4721 0.1781 0.2799 0.062 Uiso 1 1 d . U . . .
C26 C 0.4960(3) 0.34620(19) 0.24720(15) 0.0494(8) Uani 1 1 d . . . . .
H26A H 0.4628 0.3434 0.2870 0.073 Uiso 1 1 d . U . . .
H26B H 0.4283 0.3434 0.2161 0.073 Uiso 1 1 d . U . . .
H26C H 0.5410 0.4008 0.2433 0.073 Uiso 1 1 d . U . . .
C27 C 0.3360(5) 0.5572(4) 0.2737(2) 0.0350(11) Uani 0.662(7) 1 d . U P A 1
H27A H 0.2980 0.6036 0.2987 0.042 Uiso 0.662(7) 1 calc R U P A 1
H27B H 0.3569 0.5052 0.3000 0.042 Uiso 0.662(7) 1 calc R U P A 1
C27A C 0.3240(13) 0.5759(12) 0.2542(6) 0.058(3) Uani 0.338(7) 1 d . U P A 2
H27C H 0.2919 0.6329 0.2694 0.069 Uiso 0.338(7) 1 calc R U P A 2
H27D H 0.3029 0.5287 0.2834 0.069 Uiso 0.338(7) 1 calc R U P A 2
C28 C 0.2476(4) 0.5314(3) 0.2190(2) 0.0391(12) Uani 0.662(7) 1 d . U P A 1
H28A H 0.2582 0.4685 0.2076 0.047 Uiso 0.662(7) 1 calc R U P A 1
H28B H 0.1588 0.5422 0.2273 0.047 Uiso 0.662(7) 1 calc R U P A 1
C28A C 0.2635(11) 0.5561(10) 0.1920(6) 0.070(4) Uani 0.338(7) 1 d . U P A 2
H28C H 0.2086 0.5035 0.1938 0.084 Uiso 0.338(7) 1 calc R U P A 2
H28D H 0.2119 0.6071 0.1769 0.084 Uiso 0.338(7) 1 calc R U P A 2
C29 C 0.2904(5) 0.5928(3) 0.1698(2) 0.0442(13) Uani 0.662(7) 1 d . U P A 1
H29A H 0.2654 0.5704 0.1282 0.053 Uiso 0.662(7) 1 calc R U P A 1
H29B H 0.2565 0.6534 0.1745 0.053 Uiso 0.662(7) 1 calc R U P A 1
C29A C 0.3636(11) 0.5397(9) 0.1517(5) 0.065(3) Uani 0.338(7) 1 d . U P A 2
H29C H 0.3408 0.5615 0.1097 0.079 Uiso 0.338(7) 1 calc R U P A 2
H29D H 0.3830 0.4756 0.1498 0.079 Uiso 0.338(7) 1 calc R U P A 2
C30 C 0.4306(5) 0.5909(5) 0.1822(3) 0.0393(13) Uani 0.662(7) 1 d . U P A 1
H30A H 0.4669 0.5369 0.1647 0.047 Uiso 0.662(7) 1 calc R U P A 1
H30B H 0.4700 0.6436 0.1644 0.047 Uiso 0.662(7) 1 calc R U P A 1
C30A C 0.4747(12) 0.5916(12) 0.1813(7) 0.056(3) Uani 0.338(7) 1 d . U P A 2
H30C H 0.4713 0.6547 0.1689 0.067 Uiso 0.338(7) 1 calc R U P A 2
H30D H 0.5557 0.5659 0.1704 0.067 Uiso 0.338(7) 1 calc R U P A 2
C31 C 0.6455(3) 0.45098(17) 0.40916(13) 0.0436(7) Uani 1 1 d . . . . .
H31A H 0.6883 0.4217 0.3770 0.053 Uiso 1 1 d . U . . .
H31B H 0.5676 0.4199 0.4151 0.053 Uiso 1 1 d . U . . .
C32 C 0.7271(3) 0.4534(2) 0.46814(15) 0.0590(9) Uani 1 1 d . . . . .
H32A H 0.8152 0.4487 0.4598 0.070 Uiso 1 1 d . U . . .
H32B H 0.7060 0.4053 0.4950 0.070 Uiso 1 1 d . U . . .
C33 C 0.6989(3) 0.5437(2) 0.49681(14) 0.0502(8) Uani 1 1 d . . . . .
H33A H 0.6620 0.5362 0.5359 0.060 Uiso 1 1 d . U . . .
H33B H 0.7749 0.5787 0.5029 0.060 Uiso 1 1 d . U . . .
C34 C 0.6069(3) 0.58735(17) 0.45016(12) 0.0390(7) Uani 1 1 d . . . . .
H34A H 0.5215 0.5813 0.4626 0.047 Uiso 1 1 d . U . . .
H34B H 0.6258 0.6497 0.4460 0.047 Uiso 1 1 d . U . . .
N1 N 0.80466(17) 0.37177(11) 0.21773(8) 0.0184(4) Uani 1 1 d . . . . .
N2 N 0.83818(18) 0.37957(11) 0.11793(8) 0.0218(4) Uani 1 1 d . . . . .
Na2 Na 0.64092(9) 0.60688(6) 0.29977(4) 0.0279(2) Uani 1 1 d . . . . .
O1 O 0.85258(15) 0.24313(9) 0.16574(7) 0.0243(4) Uani 1 1 d . . . . .
O2 O 0.75612(15) 0.51114(10) 0.25349(7) 0.0269(4) Uani 1 1 d . . . . .
O3 O 0.4485(17) 0.5911(14) 0.2455(7) 0.0380(16) Uani 0.662(7) 1 d . U P A 1
O3A O 0.456(3) 0.581(3) 0.2509(14) 0.0380(16) Uani 0.338(7) 1 d . U P A 2
O4 O 0.62114(19) 0.54160(11) 0.39355(8) 0.0419(5) Uani 1 1 d . . . . .
P1 P 0.80471(7) 0.49289(4) 0.13209(3) 0.02806(16) 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 O1 1.248(2) . ?
C1 N2 1.346(3) . ?
C1 N1 1.377(3) . ?
C2 O2 1.254(3) . ?
C2 N1 1.424(3) . ?
C2 P1 1.758(2) . ?
C3 C4 1.397(3) . ?
C3 C8 1.397(3) . ?
C3 N2 1.434(3) . ?
C4 C5 1.396(3) . ?
C4 C12 1.512(4) . ?
C5 C6 1.376(4) . ?
C5 H5 0.931(3) . ?
C6 C7 1.378(4) . ?
C6 H6 0.930(2) . ?
C7 C8 1.395(3) . ?
C7 H7 0.929(3) . ?
C8 C9 1.513(3) . ?
C9 C11 1.525(4) . ?
C9 C10 1.526(4) . ?
C9 H9 0.979(2) . ?
C10 H10A 0.957(4) . ?
C10 H10B 0.961(3) . ?
C10 H10C 0.961(4) . ?
C11 H11A 0.961(3) . ?
C11 H11B 0.961(3) . ?
C11 H11C 0.958(4) . ?
C12 C14 1.521(4) . ?
C12 C13 1.524(4) . ?
C12 H12 0.977(3) . ?
C13 H13A 0.959(3) . ?
C13 H13B 0.961(3) . ?
C13 H13C 0.961(3) . ?
C14 H14A 0.960(4) . ?
C14 H14B 0.959(3) . ?
C14 H14C 0.961(4) . ?
C15 C20 1.399(3) . ?
C15 C16 1.407(3) . ?
C15 N1 1.434(3) . ?
C16 C17 1.396(3) . ?
C16 C24 1.519(3) . ?
C17 C18 1.377(3) . ?
C17 H17 0.930(2) . ?
C18 C19 1.379(3) . ?
C18 H18 0.929(2) . ?
C19 C20 1.395(3) . ?
C19 H19 0.932(2) . ?
C20 C21 1.518(3) . ?
C21 C22 1.520(4) . ?
C21 C23 1.524(4) . ?
C21 H21 0.980(2) . ?
C22 H22A 0.961(3) . ?
C22 H22B 0.963(3) . ?
C22 H22C 0.960(3) . ?
C23 H23A 0.960(3) . ?
C23 H23B 0.959(3) . ?
C23 H23C 0.961(4) . ?
C24 C25 1.521(3) . ?
C24 C26 1.525(4) . ?
C24 H24 0.979(2) . ?
C25 H25A 0.959(3) . ?
C25 H25B 0.962(3) . ?
C25 H25C 0.960(3) . ?
C26 H26A 0.959(3) . ?
C26 H26B 0.960(3) . ?
C26 H26C 0.960(3) . ?
C27 O3 1.47(2) . ?
C27 C28 1.524(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27A O3A 1.42(4) . ?
C27A C28A 1.495(17) . ?
C27A H27C 0.9900 . ?
C27A H27D 0.9900 . ?
C28 C29 1.510(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28A C29A 1.447(16) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C29 C30 1.504(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29A C30A 1.530(16) . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
C30 O3 1.381(16) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30A O3A 1.55(3) . ?
C30A H30C 0.9900 . ?
C30A H30D 0.9900 . ?
C31 O4 1.429(3) . ?
C31 C32 1.507(4) . ?
C31 H31A 0.968(3) . ?
C31 H31B 0.970(3) . ?
C32 C33 1.537(4) . ?
C32 H32A 0.972(3) . ?
C32 H32B 0.968(3) . ?
C33 C34 1.519(4) . ?
C33 H33A 0.969(3) . ?
C33 H33B 0.970(3) . ?
C34 O4 1.431(3) . ?
C34 H34A 0.972(3) . ?
C34 H34B 0.967(3) . ?
N2 P1 1.7776(18) . ?
Na2 O2 2.1851(17) . ?
Na2 O1 2.1886(16) 2_655 ?
Na2 O3A 2.22(3) . ?
Na2 O4 2.292(2) . ?
Na2 O3 2.317(16) . ?
O1 Na2 2.1886(16) 2_645 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N2 125.67(19) . . ?
O1 C1 N1 124.22(19) . . ?
N2 C1 N1 110.10(18) . . ?
O2 C2 N1 119.35(19) . . ?
O2 C2 P1 130.65(17) . . ?
N1 C2 P1 109.99(15) . . ?
C4 C3 C8 122.5(2) . . ?
C4 C3 N2 118.2(2) . . ?
C8 C3 N2 119.3(2) . . ?
C5 C4 C3 117.3(2) . . ?
C5 C4 C12 120.5(2) . . ?
C3 C4 C12 122.2(2) . . ?
C6 C5 C4 121.5(2) . . ?
C6 C5 H5 119.3(3) . . ?
C4 C5 H5 119.3(3) . . ?
C5 C6 C7 120.0(2) . . ?
C5 C6 H6 119.9(3) . . ?
C7 C6 H6 120.0(3) . . ?
C6 C7 C8 121.2(2) . . ?
C6 C7 H7 119.5(3) . . ?
C8 C7 H7 119.3(3) . . ?
C7 C8 C3 117.6(2) . . ?
C7 C8 C9 120.7(2) . . ?
C3 C8 C9 121.7(2) . . ?
C8 C9 C11 111.9(2) . . ?
C8 C9 C10 110.1(2) . . ?
C11 C9 C10 111.5(3) . . ?
C8 C9 H9 107.9(2) . . ?
C11 C9 H9 107.8(2) . . ?
C10 C9 H9 107.6(3) . . ?
C9 C10 H10A 109.6(3) . . ?
C9 C10 H10B 109.3(3) . . ?
H10A C10 H10B 109.6(4) . . ?
C9 C10 H10C 109.4(3) . . ?
H10A C10 H10C 109.7(3) . . ?
H10B C10 H10C 109.3(3) . . ?
C9 C11 H11A 109.5(3) . . ?
C9 C11 H11B 109.5(3) . . ?
H11A C11 H11B 109.2(3) . . ?
C9 C11 H11C 109.6(3) . . ?
H11A C11 H11C 109.6(4) . . ?
H11B C11 H11C 109.5(3) . . ?
C4 C12 C14 110.6(2) . . ?
C4 C12 C13 111.8(2) . . ?
C14 C12 C13 111.7(2) . . ?
C4 C12 H12 107.5(2) . . ?
C14 C12 H12 107.5(3) . . ?
C13 C12 H12 107.6(3) . . ?
C12 C13 H13A 109.6(3) . . ?
C12 C13 H13B 109.5(3) . . ?
H13A C13 H13B 109.5(3) . . ?
C12 C13 H13C 109.4(3) . . ?
H13A C13 H13C 109.5(3) . . ?
H13B C13 H13C 109.3(3) . . ?
C12 C14 H14A 109.5(3) . . ?
C12 C14 H14B 109.6(3) . . ?
H14A C14 H14B 109.6(3) . . ?
C12 C14 H14C 109.4(3) . . ?
H14A C14 H14C 109.4(4) . . ?
H14B C14 H14C 109.4(3) . . ?
C20 C15 C16 122.5(2) . . ?
C20 C15 N1 118.66(19) . . ?
C16 C15 N1 118.78(19) . . ?
C17 C16 C15 117.3(2) . . ?
C17 C16 C24 121.6(2) . . ?
C15 C16 C24 120.99(19) . . ?
C18 C17 C16 121.0(2) . . ?
C18 C17 H17 119.8(2) . . ?
C16 C17 H17 119.3(2) . . ?
C17 C18 C19 120.7(2) . . ?
C17 C18 H18 119.6(2) . . ?
C19 C18 H18 119.7(3) . . ?
C18 C19 C20 121.1(2) . . ?
C18 C19 H19 119.5(2) . . ?
C20 C19 H19 119.4(2) . . ?
C19 C20 C15 117.4(2) . . ?
C19 C20 C21 120.4(2) . . ?
C15 C20 C21 122.2(2) . . ?
C20 C21 C22 112.0(2) . . ?
C20 C21 C23 110.1(2) . . ?
C22 C21 C23 111.4(2) . . ?
C20 C21 H21 107.8(2) . . ?
C22 C21 H21 107.7(2) . . ?
C23 C21 H21 107.7(2) . . ?
C21 C22 H22A 109.6(2) . . ?
C21 C22 H22B 109.5(3) . . ?
H22A C22 H22B 109.2(3) . . ?
C21 C22 H22C 109.7(3) . . ?
H22A C22 H22C 109.5(3) . . ?
H22B C22 H22C 109.3(3) . . ?
C21 C23 H23A 109.4(3) . . ?
C21 C23 H23B 109.6(3) . . ?
H23A C23 H23B 109.5(3) . . ?
C21 C23 H23C 109.3(3) . . ?
H23A C23 H23C 109.4(3) . . ?
H23B C23 H23C 109.6(3) . . ?
C16 C24 C25 113.6(2) . . ?
C16 C24 C26 109.99(19) . . ?
C25 C24 C26 109.9(2) . . ?
C16 C24 H24 107.6(2) . . ?
C25 C24 H24 107.7(2) . . ?
C26 C24 H24 107.8(2) . . ?
C24 C25 H25A 109.5(2) . . ?
C24 C25 H25B 109.3(2) . . ?
H25A C25 H25B 109.4(3) . . ?
C24 C25 H25C 109.5(2) . . ?
H25A C25 H25C 109.6(3) . . ?
H25B C25 H25C 109.4(3) . . ?
C24 C26 H26A 109.5(3) . . ?
C24 C26 H26B 109.4(3) . . ?
H26A C26 H26B 109.5(3) . . ?
C24 C26 H26C 109.5(3) . . ?
H26A C26 H26C 109.5(3) . . ?
H26B C26 H26C 109.5(3) . . ?
O3 C27 C28 104.0(7) . . ?
O3 C27 H27A 111.0 . . ?
C28 C27 H27A 111.0 . . ?
O3 C27 H27B 111.0 . . ?
C28 C27 H27B 111.0 . . ?
H27A C27 H27B 109.0 . . ?
O3A C27A C28A 109.7(18) . . ?
O3A C27A H27C 109.7 . . ?
C28A C27A H27C 109.7 . . ?
O3A C27A H27D 109.7 . . ?
C28A C27A H27D 109.7 . . ?
H27C C27A H27D 108.2 . . ?
C29 C28 C27 101.5(4) . . ?
C29 C28 H28A 111.5 . . ?
C27 C28 H28A 111.5 . . ?
C29 C28 H28B 111.5 . . ?
C27 C28 H28B 111.5 . . ?
H28A C28 H28B 109.3 . . ?
C29A C28A C27A 107.1(10) . . ?
C29A C28A H28C 110.3 . . ?
C27A C28A H28C 110.3 . . ?
C29A C28A H28D 110.3 . . ?
C27A C28A H28D 110.3 . . ?
H28C C28A H28D 108.6 . . ?
C30 C29 C28 101.7(4) . . ?
C30 C29 H29A 111.4 . . ?
C28 C29 H29A 111.4 . . ?
C30 C29 H29B 111.4 . . ?
C28 C29 H29B 111.4 . . ?
H29A C29 H29B 109.3 . . ?
C28A C29A C30A 103.7(11) . . ?
C28A C29A H29C 111.0 . . ?
C30A C29A H29C 111.0 . . ?
C28A C29A H29D 111.0 . . ?
C30A C29A H29D 111.0 . . ?
H29C C29A H29D 109.0 . . ?
O3 C30 C29 104.6(9) . . ?
O3 C30 H30A 110.8 . . ?
C29 C30 H30A 110.8 . . ?
O3 C30 H30B 110.8 . . ?
C29 C30 H30B 110.8 . . ?
H30A C30 H30B 108.9 . . ?
C29A C30A O3A 102.4(17) . . ?
C29A C30A H30C 111.3 . . ?
O3A C30A H30C 111.3 . . ?
C29A C30A H30D 111.3 . . ?
O3A C30A H30D 111.3 . . ?
H30C C30A H30D 109.2 . . ?
O4 C31 C32 105.5(2) . . ?
O4 C31 H31A 110.5(2) . . ?
C32 C31 H31A 110.8(3) . . ?
O4 C31 H31B 110.5(3) . . ?
C32 C31 H31B 110.6(3) . . ?
H31A C31 H31B 108.9(3) . . ?
C31 C32 C33 104.5(2) . . ?
C31 C32 H32A 110.6(3) . . ?
C33 C32 H32A 110.9(3) . . ?
C31 C32 H32B 110.8(3) . . ?
C33 C32 H32B 111.0(3) . . ?
H32A C32 H32B 108.9(3) . . ?
C34 C33 C32 104.3(2) . . ?
C34 C33 H33A 111.0(3) . . ?
C32 C33 H33A 110.8(3) . . ?
C34 C33 H33B 110.8(3) . . ?
C32 C33 H33B 110.8(3) . . ?
H33A C33 H33B 109.1(3) . . ?
O4 C34 C33 105.6(2) . . ?
O4 C34 H34A 110.4(2) . . ?
C33 C34 H34A 110.5(2) . . ?
O4 C34 H34B 110.7(2) . . ?
C33 C34 H34B 110.8(3) . . ?
H34A C34 H34B 108.8(3) . . ?
C1 N1 C2 115.82(17) . . ?
C1 N1 C15 120.82(17) . . ?
C2 N1 C15 123.34(17) . . ?
C1 N2 C3 119.89(17) . . ?
C1 N2 P1 115.90(14) . . ?
C3 N2 P1 123.78(14) . . ?
O2 Na2 O1 140.64(7) . 2_655 ?
O2 Na2 O3A 99.8(12) . . ?
O1 Na2 O3A 109.9(12) 2_655 . ?
O2 Na2 O4 102.41(7) . . ?
O1 Na2 O4 95.71(7) 2_655 . ?
O3A Na2 O4 102.9(8) . . ?
O2 Na2 O3 101.7(6) . . ?
O1 Na2 O3 106.3(6) 2_655 . ?
O4 Na2 O3 106.4(4) . . ?
C1 O1 Na2 157.60(15) . 2_645 ?
C2 O2 Na2 153.89(16) . . ?
C30 O3 C27 110.6(12) . . ?
C30 O3 Na2 124.9(11) . . ?
C27 O3 Na2 122.8(7) . . ?
C27A O3A C30A 104.2(18) . . ?
C27A O3A Na2 147(2) . . ?
C30A O3A Na2 106.6(19) . . ?
C31 O4 C34 106.47(19) . . ?
C31 O4 Na2 126.74(15) . . ?
C34 O4 Na2 125.71(14) . . ?
C2 P1 N2 88.18(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 C3 C4 C5 -1.0(3) . . . . ?
N2 C3 C4 C5 -179.4(2) . . . . ?
C8 C3 C4 C12 178.3(2) . . . . ?
N2 C3 C4 C12 -0.1(3) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C12 C4 C5 C6 -178.5(2) . . . . ?
C4 C5 C6 C7 -0.3(4) . . . . ?
C5 C6 C7 C8 0.1(4) . . . . ?
C6 C7 C8 C3 -0.3(4) . . . . ?
C6 C7 C8 C9 178.6(2) . . . . ?
C4 C3 C8 C7 0.8(3) . . . . ?
N2 C3 C8 C7 179.1(2) . . . . ?
C4 C3 C8 C9 -178.1(2) . . . . ?
N2 C3 C8 C9 0.3(3) . . . . ?
C7 C8 C9 C11 53.2(3) . . . . ?
C3 C8 C9 C11 -128.0(3) . . . . ?
C7 C8 C9 C10 -71.4(3) . . . . ?
C3 C8 C9 C10 107.4(3) . . . . ?
C5 C4 C12 C14 -59.2(3) . . . . ?
C3 C4 C12 C14 121.6(3) . . . . ?
C5 C4 C12 C13 65.9(3) . . . . ?
C3 C4 C12 C13 -113.4(3) . . . . ?
C20 C15 C16 C17 -2.0(3) . . . . ?
N1 C15 C16 C17 176.56(19) . . . . ?
C20 C15 C16 C24 175.3(2) . . . . ?
N1 C15 C16 C24 -6.2(3) . . . . ?
C15 C16 C17 C18 1.7(3) . . . . ?
C24 C16 C17 C18 -175.6(2) . . . . ?
C16 C17 C18 C19 -0.1(4) . . . . ?
C17 C18 C19 C20 -1.2(4) . . . . ?
C18 C19 C20 C15 0.9(3) . . . . ?
C18 C19 C20 C21 -177.1(2) . . . . ?
C16 C15 C20 C19 0.7(3) . . . . ?
N1 C15 C20 C19 -177.80(19) . . . . ?
C16 C15 C20 C21 178.6(2) . . . . ?
N1 C15 C20 C21 0.1(3) . . . . ?
C19 C20 C21 C22 -53.8(3) . . . . ?
C15 C20 C21 C22 128.4(2) . . . . ?
C19 C20 C21 C23 70.8(3) . . . . ?
C15 C20 C21 C23 -107.1(3) . . . . ?
C17 C16 C24 C25 -28.9(3) . . . . ?
C15 C16 C24 C25 153.9(2) . . . . ?
C17 C16 C24 C26 94.8(3) . . . . ?
C15 C16 C24 C26 -82.4(3) . . . . ?
O3 C27 C28 C29 -26.9(10) . . . . ?
O3A C27A C28A C29A 6(3) . . . . ?
C27 C28 C29 C30 40.0(5) . . . . ?
C27A C28A C29A C30A -26.2(16) . . . . ?
C28 C29 C30 O3 -39.5(11) . . . . ?
C28A C29A C30A O3A 35(2) . . . . ?
O4 C31 C32 C33 23.5(3) . . . . ?
C31 C32 C33 C34 -2.3(3) . . . . ?
C32 C33 C34 O4 -19.6(3) . . . . ?
O1 C1 N1 C2 -178.2(2) . . . . ?
N2 C1 N1 C2 1.0(3) . . . . ?
O1 C1 N1 C15 3.2(3) . . . . ?
N2 C1 N1 C15 -177.59(18) . . . . ?
O2 C2 N1 C1 180.0(2) . . . . ?
P1 C2 N1 C1 -1.1(2) . . . . ?
O2 C2 N1 C15 -1.5(3) . . . . ?
P1 C2 N1 C15 177.45(16) . . . . ?
C20 C15 N1 C1 103.5(2) . . . . ?
C16 C15 N1 C1 -75.1(3) . . . . ?
C20 C15 N1 C2 -74.9(3) . . . . ?
C16 C15 N1 C2 106.5(2) . . . . ?
O1 C1 N2 C3 6.0(3) . . . . ?
N1 C1 N2 C3 -173.17(18) . . . . ?
O1 C1 N2 P1 178.72(18) . . . . ?
N1 C1 N2 P1 -0.4(2) . . . . ?
C4 C3 N2 C1 85.1(3) . . . . ?
C8 C3 N2 C1 -93.3(3) . . . . ?
C4 C3 N2 P1 -87.0(2) . . . . ?
C8 C3 N2 P1 94.6(2) . . . . ?
N2 C1 O1 Na2 -171.3(3) . . . 2_645 ?
N1 C1 O1 Na2 7.8(6) . . . 2_645 ?
N1 C2 O2 Na2 -127.5(3) . . . . ?
P1 C2 O2 Na2 53.8(5) . . . . ?
C29 C30 O3 C27 22.9(16) . . . . ?
C29 C30 O3 Na2 -171.7(11) . . . . ?
C28 C27 O3 C30 2.8(16) . . . . ?
C28 C27 O3 Na2 -163.0(11) . . . . ?
C28A C27A O3A C30A 17(3) . . . . ?
C28A C27A O3A Na2 177(4) . . . . ?
C29A C30A O3A C27A -32(3) . . . . ?
C29A C30A O3A Na2 159.2(17) . . . . ?
C32 C31 O4 C34 -37.2(3) . . . . ?
C32 C31 O4 Na2 131.4(2) . . . . ?
C33 C34 O4 C31 35.6(3) . . . . ?
C33 C34 O4 Na2 -133.14(19) . . . . ?
O2 C2 P1 N2 179.5(2) . . . . ?
N1 C2 P1 N2 0.64(16) . . . . ?
C1 N2 P1 C2 -0.13(18) . . . . ?
C3 N2 P1 C2 172.28(19) . . . . ?

_refine_diff_density_max         0.388
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.056

_shelxl_version_number           2014/6






_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_spiro-bi-pentacyclo-(p(co)(nbu)(co)(nbu))-_na(dme)
_database_code_depnum_ccdc_archive 'CCDC 986854'
_audit_update_record             
;
2014-02-14 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H88 N8 Na2 O10 P2'
_chemical_formula_sum            'C48 H88 N8 Na2 O10 P2'
_chemical_formula_weight         1045.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Na Na 0.0362 0.0249 '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                   19.3693(13)
_cell_length_b                   14.6742(10)
_cell_length_c                   21.9183(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.339(2)
_cell_angle_gamma                90.00
_cell_volume                     5802.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8325
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      23.25

_exptl_crystal_description       'prismatic blocks'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2256
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9773
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_process_details   'SADABS-2008/1 Bruker'


_exptl_special_details           
; 
One solvent molecule (THF) is disordered over two positions
with an occupancy of ~ 50/50. This atoms were not refined
anisotropically.
;

_diffrn_ambient_temperature      100(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  'CMOS 100-Bruker Area Detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            81997
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         23.25
_reflns_number_total             8325
_reflns_number_gt                6162
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0506P)²+5.9821P] 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         8325
_refine_ls_number_parameters     782
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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 -0.14005(4) 0.20359(5) 0.18477(4) 0.0283(2) Uani 1 1 d . . .
P2 P 0.37327(4) 0.20478(5) 0.19807(4) 0.0286(2) Uani 1 1 d . . .
Na1 Na 0.15046(6) 0.40146(7) 0.26380(5) 0.0279(3) Uani 1 1 d . A .
Na2 Na -0.34033(6) 0.01004(7) 0.28352(5) 0.0303(3) Uani 1 1 d . . .
N1 N -0.01110(12) 0.20839(16) 0.28956(11) 0.0282(6) Uani 1 1 d . . .
N2 N -0.06755(13) 0.29787(16) 0.20198(12) 0.0298(6) Uani 1 1 d . . .
N3 N -0.25997(12) 0.23628(15) 0.21728(11) 0.0258(6) Uani 1 1 d . . .
N4 N -0.20989(12) 0.11462(15) 0.18679(12) 0.0278(6) Uani 1 1 d . . .
N5 N 0.30092(12) 0.29426(15) 0.19176(12) 0.0281(6) Uani 1 1 d . . .
N6 N 0.24572(12) 0.17464(15) 0.21855(11) 0.0265(6) Uani 1 1 d . . .
N7 N 0.44668(12) 0.11148(16) 0.22334(11) 0.0283(6) Uani 1 1 d . . .
N8 N 0.49796(13) 0.20846(16) 0.30698(11) 0.0290(6) Uani 1 1 d . . .
O1 O -0.08684(11) 0.09293(14) 0.29509(10) 0.0375(5) Uani 1 1 d . . .
O2 O 0.05492(10) 0.32454(14) 0.26677(9) 0.0319(5) Uani 1 1 d . . .
O3 O -0.30476(10) -0.13511(13) 0.28395(10) 0.0336(5) Uani 1 1 d . . .
O4 O -0.31615(10) 0.09639(13) 0.20970(10) 0.0315(5) Uani 1 1 d . . .
O5 O 0.18579(11) 0.31337(13) 0.19824(9) 0.0304(5) Uani 1 1 d . . .
O6 O 0.18423(11) 0.54711(13) 0.26838(10) 0.0335(5) Uani 1 1 d . . .
O7 O -0.43205(10) 0.08959(13) 0.29304(10) 0.0316(5) Uani 1 1 d . . .
O8 O 0.41740(11) 0.32190(14) 0.30508(10) 0.0366(5) Uani 1 1 d . . .
O9 O -0.24128(11) 0.05998(14) 0.37455(10) 0.0399(5) Uani 1 1 d . . .
C1 C -0.07538(16) 0.1587(2) 0.26625(14) 0.0298(7) Uani 1 1 d . . .
C2 C -0.00488(16) 0.28339(19) 0.25164(14) 0.0263(7) Uani 1 1 d . . .
C3 C -0.20229(15) 0.2822(2) 0.20937(14) 0.0294(7) Uani 1 1 d . . .
C4 C -0.26467(16) 0.14133(19) 0.20426(13) 0.0264(7) Uani 1 1 d . . .
C5 C 0.24131(16) 0.26802(19) 0.20190(13) 0.0253(7) Uani 1 1 d . . .
C6 C 0.30748(16) 0.12917(19) 0.21956(14) 0.0275(7) Uani 1 1 d . . .
C7 C -0.49262(16) 0.12974(19) 0.27365(14) 0.0274(7) Uani 1 1 d . . .
C8 C 0.43211(17) 0.2547(2) 0.27919(15) 0.0307(7) Uani 1 1 d . . .
C11 C 0.05171(18) 0.1800(2) 0.34782(15) 0.0339(8) Uani 1 1 d . . .
C12 C 0.06283(18) 0.2395(2) 0.40645(15) 0.0345(8) Uani 1 1 d . . .
C13 C 0.13010(18) 0.2123(2) 0.46549(16) 0.0467(9) Uani 1 1 d . . .
H13A H 0.1219 0.1508 0.4800 0.056 Uiso 1 1 calc R . .
H13B H 0.1738 0.2091 0.4524 0.056 Uiso 1 1 calc R . .
C14 C 0.1463(2) 0.2769(3) 0.52152(17) 0.0616(11) Uani 1 1 d . . .
H14A H 0.1533 0.3383 0.5072 0.092 Uiso 1 1 calc R . .
H14B H 0.1915 0.2576 0.5572 0.092 Uiso 1 1 calc R . .
H14C H 0.1047 0.2771 0.5369 0.092 Uiso 1 1 calc R . .
C21 C -0.06716(18) 0.3632(2) 0.15187(15) 0.0317(7) Uani 1 1 d . . .
C22 C -0.0253(2) 0.3291(3) 0.10965(18) 0.0426(9) Uani 1 1 d . . .
C23 C -0.0106(2) 0.4047(3) 0.06770(18) 0.0513(10) Uani 1 1 d . . .
C24 C 0.05086(19) 0.4688(2) 0.10525(18) 0.0519(10) Uani 1 1 d . . .
H24A H 0.0395 0.4964 0.1412 0.078 Uiso 1 1 calc R . .
H24B H 0.0556 0.5167 0.0759 0.078 Uiso 1 1 calc R . .
H24C H 0.0976 0.4349 0.1231 0.078 Uiso 1 1 calc R . .
C31 C -0.31957(15) 0.2822(2) 0.23155(14) 0.0305(7) Uani 1 1 d . . .
H31A H -0.3002 0.3397 0.2551 0.037 Uiso 1 1 calc R . .
H31B H -0.3354 0.2430 0.2608 0.037 Uiso 1 1 calc R . .
C32 C -0.38602(17) 0.3033(2) 0.17072(16) 0.0305(7) Uani 1 1 d . . .
C33 C -0.44575(18) 0.3562(3) 0.18481(18) 0.0413(9) Uani 1 1 d . . .
C34 C -0.51101(18) 0.3800(3) 0.12310(19) 0.0571(11) Uani 1 1 d . . .
H34A H -0.4938 0.4171 0.0943 0.086 Uiso 1 1 calc R . .
H34B H -0.5477 0.4144 0.1348 0.086 Uiso 1 1 calc R . .
H34C H -0.5337 0.3239 0.1004 0.086 Uiso 1 1 calc R . .
C41 C -0.20586(17) 0.0195(2) 0.16966(16) 0.0304(7) Uani 1 1 d . . .
C42 C -0.25173(18) -0.0013(2) 0.09863(15) 0.0308(7) Uani 1 1 d . . .
C43 C -0.25344(19) -0.1018(2) 0.08222(16) 0.0341(8) Uani 1 1 d . . .
C44 C -0.29794(19) -0.1216(2) 0.01068(15) 0.0462(9) Uani 1 1 d . . .
H44A H -0.3495 -0.1027 0.0003 0.069 Uiso 1 1 calc R . .
H44B H -0.2963 -0.1871 0.0025 0.069 Uiso 1 1 calc R . .
H44C H -0.2768 -0.0879 -0.0169 0.069 Uiso 1 1 calc R . .
C51 C 0.30769(18) 0.3887(2) 0.17423(16) 0.0303(7) Uani 1 1 d . . .
C52 C 0.26632(18) 0.4089(2) 0.10252(15) 0.0306(7) Uani 1 1 d . . .
C53 C 0.26752(18) 0.5089(2) 0.08510(16) 0.0416(8) Uani 1 1 d . . .
H53A H 0.2474 0.5454 0.1128 0.050 Uiso 1 1 calc R . .
H53B H 0.3196 0.5279 0.0953 0.050 Uiso 1 1 calc R . .
C54 C 0.22369(18) 0.5294(2) 0.01439(16) 0.0485(9) Uani 1 1 d . . .
H54A H 0.2466 0.4990 -0.0133 0.073 Uiso 1 1 calc R . .
H54B H 0.2230 0.5954 0.0072 0.073 Uiso 1 1 calc R . .
H54C H 0.1728 0.5073 0.0031 0.073 Uiso 1 1 calc R . .
C61 C 0.18501(17) 0.1304(2) 0.23230(15) 0.0284(7) Uani 1 1 d . . .
C62 C 0.12357(17) 0.0971(2) 0.17189(16) 0.0328(8) Uani 1 1 d . . .
C63 C 0.05778(17) 0.0606(3) 0.18571(17) 0.0352(8) Uani 1 1 d . . .
C64 C -0.00471(18) 0.0292(3) 0.12513(17) 0.0508(9) Uani 1 1 d . . .
H64A H -0.0221 0.0803 0.0946 0.076 Uiso 1 1 calc R . .
H64B H -0.0456 0.0067 0.1373 0.076 Uiso 1 1 calc R . .
H64C H 0.0129 -0.0199 0.1041 0.076 Uiso 1 1 calc R . .
C71 C 0.45022(16) 0.04322(19) 0.17594(14) 0.0309(7) Uani 1 1 d . . .
H71A H 0.3992 0.0250 0.1481 0.037 Uiso 1 1 calc R . .
H71B H 0.4762 -0.0116 0.1997 0.037 Uiso 1 1 calc R . .
C72 C 0.49033(19) 0.0783(2) 0.13247(16) 0.0326(7) Uani 1 1 d . . .
C73 C 0.5003(2) 0.0057(2) 0.08658(17) 0.0410(9) Uani 1 1 d . . .
C74 C 0.55919(18) -0.0649(2) 0.12043(17) 0.0464(9) Uani 1 1 d . . .
H74A H 0.6070 -0.0345 0.1419 0.070 Uiso 1 1 calc R . .
H74B H 0.5633 -0.1083 0.0879 0.070 Uiso 1 1 calc R . .
H74C H 0.5453 -0.0976 0.1532 0.070 Uiso 1 1 calc R . .
C81 C 0.55682(18) 0.2434(2) 0.36553(15) 0.0320(7) Uani 1 1 d . . .
C82 C 0.55306(19) 0.2072(3) 0.42817(16) 0.0405(8) Uani 1 1 d . . .
C83 C 0.61320(18) 0.2461(2) 0.48917(15) 0.0452(9) Uani 1 1 d . . .
H83A H 0.6118 0.2132 0.5281 0.054 Uiso 1 1 calc R . .
H83B H 0.6622 0.2344 0.4861 0.054 Uiso 1 1 calc R . .
C84 C 0.6063(2) 0.3470(3) 0.49937(17) 0.0573(10) Uani 1 1 d . . .
H84A H 0.6101 0.3807 0.4621 0.086 Uiso 1 1 calc R . .
H84B H 0.6461 0.3663 0.5397 0.086 Uiso 1 1 calc R . .
H84C H 0.5581 0.3596 0.5029 0.086 Uiso 1 1 calc R . .
C91 C -0.2261(2) 0.1509(2) 0.39906(18) 0.0521(10) Uani 1 1 d . . .
H91A H -0.2419 0.1593 0.4368 0.063 Uiso 1 1 calc R . .
H91B H -0.2532 0.1952 0.3646 0.063 Uiso 1 1 calc R . .
C92 C -0.1459(2) 0.1652(3) 0.4193(2) 0.0685(9) Uani 1 1 d . . .
H92A H -0.1277 0.2074 0.4570 0.082 Uiso 1 1 calc R . .
H92B H -0.1331 0.1901 0.3828 0.082 Uiso 1 1 calc R . .
C93 C -0.1141(2) 0.0713(3) 0.4380(2) 0.0685(9) Uani 1 1 d . . .
H93A H -0.1070 0.0570 0.4840 0.082 Uiso 1 1 calc R . .
H93B H -0.0661 0.0649 0.4319 0.082 Uiso 1 1 calc R . .
C94 C -0.17268(17) 0.0112(2) 0.39100(16) 0.0432(9) Uani 1 1 d . . .
H94A H -0.1612 -0.0007 0.3512 0.052 Uiso 1 1 calc R . .
H94B H -0.1755 -0.0478 0.4119 0.052 Uiso 1 1 calc R . .
H11A H 0.0410(16) 0.115(2) 0.3568(14) 0.040(9) Uiso 1 1 d . . .
H11B H 0.0943(17) 0.183(2) 0.3368(14) 0.037(9) Uiso 1 1 d . . .
H12A H 0.0198(16) 0.2375(18) 0.4172(13) 0.024(7) Uiso 1 1 d . . .
H12B H 0.0646(16) 0.305(2) 0.3952(14) 0.037(9) Uiso 1 1 d . . .
H21A H -0.1211(16) 0.3784(18) 0.1236(13) 0.029(8) Uiso 1 1 d . . .
H21B H -0.0452(15) 0.419(2) 0.1719(13) 0.027(8) Uiso 1 1 d . . .
H22A H -0.0536(18) 0.281(2) 0.0826(16) 0.049(10) Uiso 1 1 d . . .
H22B H 0.0203(18) 0.303(2) 0.1371(15) 0.039(9) Uiso 1 1 d . . .
H23A H -0.0549(18) 0.439(2) 0.0478(15) 0.046(10) Uiso 1 1 d . . .
H23B H 0.0016(19) 0.379(2) 0.0325(18) 0.060(11) Uiso 1 1 d . . .
H32A H -0.4067(16) 0.248(2) 0.1486(14) 0.034(8) Uiso 1 1 d . . .
H32B H -0.3692(17) 0.336(2) 0.1406(15) 0.044(9) Uiso 1 1 d . . .
H33A H -0.4622(17) 0.325(2) 0.2150(16) 0.045(10) Uiso 1 1 d . . .
H33B H -0.4235(17) 0.412(2) 0.2099(16) 0.047(10) Uiso 1 1 d . . .
H41A H -0.2211(15) -0.019(2) 0.1985(14) 0.031(8) Uiso 1 1 d . . .
H41B H -0.1523(16) 0.0047(18) 0.1812(13) 0.027(7) Uiso 1 1 d . . .
H42A H -0.3014(17) 0.019(2) 0.0916(14) 0.037(9) Uiso 1 1 d . . .
H42B H -0.2311(16) 0.035(2) 0.0710(14) 0.037(8) Uiso 1 1 d . . .
H43A H -0.2746(15) -0.134(2) 0.1109(14) 0.034(8) Uiso 1 1 d . . .
H43B H -0.2006(17) -0.125(2) 0.0947(14) 0.037(8) Uiso 1 1 d . . .
H51A H 0.2899(16) 0.427(2) 0.2015(14) 0.036(9) Uiso 1 1 d . . .
H51B H 0.3617(16) 0.4005(18) 0.1847(13) 0.026(7) Uiso 1 1 d . . .
H52A H 0.2170(16) 0.3925(19) 0.0915(13) 0.028(8) Uiso 1 1 d . . .
H52B H 0.2873(16) 0.372(2) 0.0772(14) 0.035(9) Uiso 1 1 d . . .
H61A H 0.1690(16) 0.177(2) 0.2555(14) 0.036(9) Uiso 1 1 d . . .
H61B H 0.2055(14) 0.083(2) 0.2618(14) 0.026(8) Uiso 1 1 d . . .
H62A H 0.1093(16) 0.145(2) 0.1445(15) 0.037(9) Uiso 1 1 d . . .
H62B H 0.1431(17) 0.049(2) 0.1499(15) 0.045(9) Uiso 1 1 d . . .
H63A H 0.0431(17) 0.109(2) 0.2066(16) 0.048(10) Uiso 1 1 d . . .
H63B H 0.0741(17) 0.011(2) 0.2166(15) 0.043(9) Uiso 1 1 d . . .
H72A H 0.4632(16) 0.130(2) 0.1081(14) 0.031(8) Uiso 1 1 d . . .
H72B H 0.5376(16) 0.1021(19) 0.1607(14) 0.027(8) Uiso 1 1 d . . .
H73A H 0.4528(17) -0.027(2) 0.0625(15) 0.041(9) Uiso 1 1 d . . .
H73B H 0.5140(17) 0.039(2) 0.0563(16) 0.044(10) Uiso 1 1 d . . .
H81A H 0.6036(17) 0.2254(19) 0.3643(13) 0.031(8) Uiso 1 1 d . . .
H81B H 0.5506(15) 0.312(2) 0.3628(14) 0.035(8) Uiso 1 1 d . . .
H82A H 0.5563(18) 0.136(3) 0.4240(16) 0.060(11) Uiso 1 1 d . . .
H82B H 0.5045(18) 0.223(2) 0.4282(15) 0.041(9) Uiso 1 1 d . . .
O10 O 0.23768(11) 0.35958(15) 0.36485(10) 0.0419(6) Uani 1 1 d . . .
C101 C 0.2680(6) 0.4271(7) 0.4156(5) 0.060(3) Uiso 0.515(13) 1 d P A 1
H10A H 0.2376 0.4319 0.4433 0.072 Uiso 0.515(13) 1 calc PR A 1
H10B H 0.2702 0.4876 0.3964 0.072 Uiso 0.515(13) 1 calc PR A 1
C102 C 0.3443(5) 0.3928(7) 0.4546(5) 0.068(3) Uiso 0.515(13) 1 d P A 1
H10C H 0.3583 0.4083 0.5016 0.082 Uiso 0.515(13) 1 calc PR A 1
H10D H 0.3814 0.4190 0.4383 0.082 Uiso 0.515(13) 1 calc PR A 1
C103 C 0.3381(4) 0.2889(6) 0.4442(4) 0.048(3) Uiso 0.515(13) 1 d P A 1
H10E H 0.3857 0.2630 0.4453 0.058 Uiso 0.515(13) 1 calc PR A 1
H10F H 0.3239 0.2590 0.4784 0.058 Uiso 0.515(13) 1 calc PR A 1
C104 C 0.2792(6) 0.2767(6) 0.3783(4) 0.047(3) Uiso 0.515(13) 1 d P A 1
H10G H 0.3015 0.2656 0.3449 0.056 Uiso 0.515(13) 1 calc PR A 1
H10H H 0.2470 0.2244 0.3785 0.056 Uiso 0.515(13) 1 calc PR A 1
C201 C 0.2982(5) 0.2949(7) 0.3764(5) 0.045(3) Uiso 0.485(13) 1 d P A 2
H20A H 0.3137 0.2923 0.3381 0.054 Uiso 0.485(13) 1 calc PR A 2
H20B H 0.2827 0.2331 0.3844 0.054 Uiso 0.485(13) 1 calc PR A 2
C202 C 0.3607(5) 0.3292(7) 0.4359(4) 0.046(3) Uiso 0.485(13) 1 d P A 2
H20C H 0.3933 0.2788 0.4598 0.056 Uiso 0.485(13) 1 calc PR A 2
H20D H 0.3907 0.3755 0.4240 0.056 Uiso 0.485(13) 1 calc PR A 2
C203 C 0.3195(5) 0.3698(6) 0.4751(4) 0.052(3) Uiso 0.485(13) 1 d P A 2
H20E H 0.3493 0.4172 0.5054 0.063 Uiso 0.485(13) 1 calc PR A 2
H20F H 0.3049 0.3227 0.5004 0.063 Uiso 0.485(13) 1 calc PR A 2
C204 C 0.2529(5) 0.4103(6) 0.4225(4) 0.037(2) Uiso 0.485(13) 1 d P A 2
H20G H 0.2097 0.4088 0.4364 0.045 Uiso 0.485(13) 1 calc PR A 2
H20H H 0.2629 0.4746 0.4147 0.045 Uiso 0.485(13) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C3 1.884(3) . ?
P1 C1 1.888(3) . ?
P1 N4 1.892(2) . ?
P1 N2 1.909(2) . ?
P2 C6 1.874(3) . ?
P2 C8 1.877(3) . ?
P2 N5 1.888(2) . ?
P2 N7 1.905(2) . ?
Na1 O2 2.189(2) . ?
Na1 O5 2.218(2) . ?
Na1 O6 2.227(2) . ?
Na1 O10 2.327(2) . ?
Na2 O7 2.198(2) . ?
Na2 O4 2.235(2) . ?
Na2 O3 2.238(2) . ?
Na2 O9 2.327(2) . ?
N1 C1 1.371(4) . ?
N1 C2 1.410(4) . ?
N1 C11 1.467(4) . ?
N2 C2 1.320(4) . ?
N2 C21 1.460(4) . ?
N3 C3 1.369(4) . ?
N3 C4 1.418(4) . ?
N3 C31 1.465(3) . ?
N4 C4 1.312(4) . ?
N4 C41 1.455(4) . ?
N5 C5 1.311(4) . ?
N5 C51 1.457(4) . ?
N6 C6 1.363(4) . ?
N6 C5 1.413(4) . ?
N6 C61 1.467(4) . ?
N7 C7 1.314(4) 1_655 ?
N7 C71 1.463(4) . ?
N8 C8 1.376(4) . ?
N8 C7 1.414(4) 1_655 ?
N8 C81 1.465(4) . ?
O1 C1 1.218(3) . ?
O2 C2 1.240(3) . ?
O3 C3 1.224(3) 2_445 ?
O4 C4 1.237(3) . ?
O5 C5 1.242(3) . ?
O6 C6 1.231(3) 2 ?
O7 C7 1.242(3) . ?
O8 C8 1.221(3) . ?
O9 C91 1.429(4) . ?
O9 C94 1.435(4) . ?
C3 O3 1.224(3) 2_455 ?
C6 O6 1.231(3) 2_545 ?
C7 N7 1.314(4) 1_455 ?
C7 N8 1.414(4) 1_455 ?
C11 C12 1.502(4) . ?
C11 H11A 1.01(3) . ?
C11 H11B 0.94(3) . ?
C12 C13 1.518(4) . ?
C12 H12A 0.95(3) . ?
C12 H12B 0.99(3) . ?
C13 C14 1.491(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 C22 1.520(5) . ?
C21 H21A 1.03(3) . ?
C21 H21B 0.95(3) . ?
C22 C23 1.531(5) . ?
C22 H22A 0.96(3) . ?
C22 H22B 0.95(3) . ?
C23 C24 1.506(5) . ?
C23 H23A 0.95(3) . ?
C23 H23B 0.96(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C32 1.510(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.516(5) . ?
C32 H32A 0.95(3) . ?
C32 H32B 0.97(3) . ?
C33 C34 1.518(5) . ?
C33 H33A 0.95(3) . ?
C33 H33B 0.99(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C41 C42 1.516(4) . ?
C41 H41A 0.97(3) . ?
C41 H41B 1.00(3) . ?
C42 C43 1.515(4) . ?
C42 H42A 0.96(3) . ?
C42 H42B 0.99(3) . ?
C43 C44 1.518(4) . ?
C43 H43A 0.99(3) . ?
C43 H43B 1.02(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C51 C52 1.511(4) . ?
C51 H51A 0.97(3) . ?
C51 H51B 1.00(3) . ?
C52 C53 1.519(4) . ?
C52 H52A 0.93(3) . ?
C52 H52B 0.96(3) . ?
C53 C54 1.502(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C61 C62 1.504(4) . ?
C61 H61A 0.96(3) . ?
C61 H61B 0.94(3) . ?
C62 C63 1.511(4) . ?
C62 H62A 0.90(3) . ?
C62 H62B 1.00(3) . ?
C63 C64 1.507(4) . ?
C63 H63A 0.94(3) . ?
C63 H63B 0.97(3) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C71 C72 1.522(4) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.525(4) . ?
C72 H72A 0.97(3) . ?
C72 H72B 0.96(3) . ?
C73 C74 1.520(5) . ?
C73 H73A 1.00(3) . ?
C73 H73B 0.94(3) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C81 C82 1.499(5) . ?
C81 H81A 0.95(3) . ?
C81 H81B 1.01(3) . ?
C82 C83 1.529(5) . ?
C82 H82A 1.05(4) . ?
C82 H82B 0.97(3) . ?
C83 C84 1.511(5) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C91 C92 1.466(5) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 C93 1.504(6) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 C94 1.509(5) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
O10 C204 1.402(9) . ?
O10 C104 1.429(8) . ?
O10 C101 1.444(10) . ?
O10 C201 1.457(9) . ?
C101 C102 1.499(12) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C102 C103 1.540(15) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C103 C104 1.490(11) . ?
C103 H10E 0.9900 . ?
C103 H10F 0.9900 . ?
C104 H10G 0.9900 . ?
C104 H10H 0.9900 . ?
C201 C202 1.507(11) . ?
C201 H20A 0.9900 . ?
C201 H20B 0.9900 . ?
C202 C203 1.492(14) . ?
C202 H20C 0.9900 . ?
C202 H20D 0.9900 . ?
C203 C204 1.505(11) . ?
C203 H20E 0.9900 . ?
C203 H20F 0.9900 . ?
C204 H20G 0.9900 . ?
C204 H20H 0.9900 . ?

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 P1 C1 102.49(13) . . ?
C3 P1 N4 83.02(12) . . ?
C1 P1 N4 88.34(12) . . ?
C3 P1 N2 90.06(12) . . ?
C1 P1 N2 83.03(12) . . ?
N4 P1 N2 167.54(11) . . ?
C6 P2 C8 103.13(13) . . ?
C6 P2 N5 82.86(11) . . ?
C8 P2 N5 88.65(12) . . ?
C6 P2 N7 90.30(12) . . ?
C8 P2 N7 82.75(12) . . ?
N5 P2 N7 167.53(11) . . ?
O2 Na1 O5 100.50(8) . . ?
O2 Na1 O6 137.00(9) . . ?
O5 Na1 O6 115.70(8) . . ?
O2 Na1 O10 99.46(9) . . ?
O5 Na1 O10 100.05(8) . . ?
O6 Na1 O10 96.38(8) . . ?
O7 Na2 O4 99.04(8) . . ?
O7 Na2 O3 139.76(9) . . ?
O4 Na2 O3 113.41(9) . . ?
O7 Na2 O9 101.19(8) . . ?
O4 Na2 O9 96.76(8) . . ?
O3 Na2 O9 98.02(8) . . ?
C1 N1 C2 117.1(2) . . ?
C1 N1 C11 121.8(3) . . ?
C2 N1 C11 120.8(2) . . ?
C2 N2 C21 118.1(2) . . ?
C2 N2 P1 115.85(19) . . ?
C21 N2 P1 122.1(2) . . ?
C3 N3 C4 117.0(2) . . ?
C3 N3 C31 122.9(2) . . ?
C4 N3 C31 119.8(2) . . ?
C4 N4 C41 119.1(2) . . ?
C4 N4 P1 117.49(19) . . ?
C41 N4 P1 123.4(2) . . ?
C5 N5 C51 119.6(2) . . ?
C5 N5 P2 117.35(19) . . ?
C51 N5 P2 123.0(2) . . ?
C6 N6 C5 116.7(2) . . ?
C6 N6 C61 123.0(2) . . ?
C5 N6 C61 120.3(2) . . ?
C7 N7 C71 118.5(2) 1_655 . ?
C7 N7 P2 116.26(19) 1_655 . ?
C71 N7 P2 120.57(18) . . ?
C8 N8 C7 116.6(2) . 1_655 ?
C8 N8 C81 121.0(2) . . ?
C7 N8 C81 122.2(2) 1_655 . ?
C2 O2 Na1 163.97(19) . . ?
C3 O3 Na2 164.8(2) 2_445 . ?
C4 O4 Na2 139.53(19) . . ?
C5 O5 Na1 137.24(18) . . ?
C6 O6 Na1 164.2(2) 2 . ?
C7 O7 Na2 156.24(19) . . ?
C91 O9 C94 109.0(2) . . ?
C91 O9 Na2 127.56(18) . . ?
C94 O9 Na2 117.22(17) . . ?
O1 C1 N1 122.7(3) . . ?
O1 C1 P1 125.7(2) . . ?
N1 C1 P1 111.5(2) . . ?
O2 C2 N2 129.2(3) . . ?
O2 C2 N1 119.6(3) . . ?
N2 C2 N1 111.2(2) . . ?
O3 C3 N3 122.3(3) 2_455 . ?
O3 C3 P1 125.9(2) 2_455 . ?
N3 C3 P1 111.8(2) . . ?
O4 C4 N4 129.4(3) . . ?
O4 C4 N3 120.0(3) . . ?
N4 C4 N3 110.6(2) . . ?
O5 C5 N5 128.8(3) . . ?
O5 C5 N6 120.4(3) . . ?
N5 C5 N6 110.8(2) . . ?
O6 C6 N6 121.9(3) 2_545 . ?
O6 C6 P2 125.8(2) 2_545 . ?
N6 C6 P2 112.3(2) . . ?
O7 C7 N7 129.5(3) . 1_455 ?
O7 C7 N8 119.6(3) . 1_455 ?
N7 C7 N8 110.9(2) 1_455 1_455 ?
O8 C8 N8 121.9(3) . . ?
O8 C8 P2 126.3(2) . . ?
N8 C8 P2 111.8(2) . . ?
N1 C11 C12 113.3(3) . . ?
N1 C11 H11A 105.8(17) . . ?
C12 C11 H11A 110.8(17) . . ?
N1 C11 H11B 106.9(18) . . ?
C12 C11 H11B 109.2(18) . . ?
H11A C11 H11B 111(3) . . ?
C11 C12 C13 112.9(3) . . ?
C11 C12 H12A 109.3(16) . . ?
C13 C12 H12A 110.0(16) . . ?
C11 C12 H12B 110.8(17) . . ?
C13 C12 H12B 111.6(17) . . ?
H12A C12 H12B 102(2) . . ?
C14 C13 C12 113.2(3) . . ?
C14 C13 H13A 108.9 . . ?
C12 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C12 C13 H13B 108.9 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C21 C22 113.1(3) . . ?
N2 C21 H21A 108.3(15) . . ?
C22 C21 H21A 110.8(15) . . ?
N2 C21 H21B 109.8(17) . . ?
C22 C21 H21B 108.4(17) . . ?
H21A C21 H21B 106(2) . . ?
C21 C22 C23 112.6(3) . . ?
C21 C22 H22A 108(2) . . ?
C23 C22 H22A 111(2) . . ?
C21 C22 H22B 109.0(19) . . ?
C23 C22 H22B 109.9(19) . . ?
H22A C22 H22B 106(3) . . ?
C24 C23 C22 114.0(3) . . ?
C24 C23 H23A 109(2) . . ?
C22 C23 H23A 108.7(19) . . ?
C24 C23 H23B 108(2) . . ?
C22 C23 H23B 111(2) . . ?
H23A C23 H23B 106(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C31 C32 113.0(2) . . ?
N3 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
N3 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C31 C32 C33 113.2(3) . . ?
C31 C32 H32A 109.9(17) . . ?
C33 C32 H32A 109.2(17) . . ?
C31 C32 H32B 108.4(18) . . ?
C33 C32 H32B 110.6(18) . . ?
H32A C32 H32B 105(3) . . ?
C32 C33 C34 112.7(3) . . ?
C32 C33 H33A 111.4(19) . . ?
C34 C33 H33A 110.5(19) . . ?
C32 C33 H33B 108.9(19) . . ?
C34 C33 H33B 111.1(19) . . ?
H33A C33 H33B 102(3) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N4 C41 C42 113.0(2) . . ?
N4 C41 H41A 109.3(17) . . ?
C42 C41 H41A 110.5(17) . . ?
N4 C41 H41B 107.0(16) . . ?
C42 C41 H41B 112.5(15) . . ?
H41A C41 H41B 104(2) . . ?
C43 C42 C41 113.2(3) . . ?
C43 C42 H42A 108.9(18) . . ?
C41 C42 H42A 106.3(18) . . ?
C43 C42 H42B 110.8(17) . . ?
C41 C42 H42B 107.7(17) . . ?
H42A C42 H42B 110(2) . . ?
C42 C43 C44 112.8(3) . . ?
C42 C43 H43A 107.2(17) . . ?
C44 C43 H43A 110.8(17) . . ?
C42 C43 H43B 109.2(16) . . ?
C44 C43 H43B 110.5(16) . . ?
H43A C43 H43B 106(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N5 C51 C52 113.3(2) . . ?
N5 C51 H51A 107.7(17) . . ?
C52 C51 H51A 110.7(17) . . ?
N5 C51 H51B 106.9(15) . . ?
C52 C51 H51B 108.6(15) . . ?
H51A C51 H51B 109(2) . . ?
C51 C52 C53 113.6(3) . . ?
C51 C52 H52A 109.0(17) . . ?
C53 C52 H52A 107.1(17) . . ?
C51 C52 H52B 108.4(17) . . ?
C53 C52 H52B 110.1(17) . . ?
H52A C52 H52B 108(2) . . ?
C54 C53 C52 113.5(3) . . ?
C54 C53 H53A 108.9 . . ?
C52 C53 H53A 108.9 . . ?
C54 C53 H53B 108.9 . . ?
C52 C53 H53B 108.9 . . ?
H53A C53 H53B 107.7 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N6 C61 C62 113.5(3) . . ?
N6 C61 H61A 103.5(17) . . ?
C62 C61 H61A 112.9(17) . . ?
N6 C61 H61B 107.6(16) . . ?
C62 C61 H61B 111.3(17) . . ?
H61A C61 H61B 107(2) . . ?
C61 C62 C63 113.2(3) . . ?
C61 C62 H62A 107(2) . . ?
C63 C62 H62A 109.4(19) . . ?
C61 C62 H62B 109.7(17) . . ?
C63 C62 H62B 109.8(18) . . ?
H62A C62 H62B 108(3) . . ?
C64 C63 C62 113.4(3) . . ?
C64 C63 H63A 112(2) . . ?
C62 C63 H63A 105(2) . . ?
C64 C63 H63B 109.8(19) . . ?
C62 C63 H63B 108.9(18) . . ?
H63A C63 H63B 108(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N7 C71 C72 112.3(2) . . ?
N7 C71 H71A 109.1 . . ?
C72 C71 H71A 109.1 . . ?
N7 C71 H71B 109.1 . . ?
C72 C71 H71B 109.1 . . ?
H71A C71 H71B 107.9 . . ?
C71 C72 C73 113.1(3) . . ?
C71 C72 H72A 108.2(17) . . ?
C73 C72 H72A 111.0(17) . . ?
C71 C72 H72B 107.6(16) . . ?
C73 C72 H72B 111.0(16) . . ?
H72A C72 H72B 106(2) . . ?
C74 C73 C72 114.0(3) . . ?
C74 C73 H73A 108.3(18) . . ?
C72 C73 H73A 111.6(17) . . ?
C74 C73 H73B 110.4(19) . . ?
C72 C73 H73B 103.6(19) . . ?
H73A C73 H73B 109(3) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N8 C81 C82 113.3(3) . . ?
N8 C81 H81A 108.8(17) . . ?
C82 C81 H81A 107.0(17) . . ?
N8 C81 H81B 105.0(16) . . ?
C82 C81 H81B 111.3(16) . . ?
H81A C81 H81B 112(2) . . ?
C81 C82 C83 113.1(3) . . ?
C81 C82 H82A 104.4(19) . . ?
C83 C82 H82A 113.4(19) . . ?
C81 C82 H82B 106.8(18) . . ?
C83 C82 H82B 110.0(19) . . ?
H82A C82 H82B 109(3) . . ?
C84 C83 C82 114.6(3) . . ?
C84 C83 H83A 108.6 . . ?
C82 C83 H83A 108.6 . . ?
C84 C83 H83B 108.6 . . ?
C82 C83 H83B 108.6 . . ?
H83A C83 H83B 107.6 . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
O9 C91 C92 107.3(3) . . ?
O9 C91 H91A 110.3 . . ?
C92 C91 H91A 110.3 . . ?
O9 C91 H91B 110.3 . . ?
C92 C91 H91B 110.3 . . ?
H91A C91 H91B 108.5 . . ?
C91 C92 C93 103.6(3) . . ?
C91 C92 H92A 111.0 . . ?
C93 C92 H92A 111.0 . . ?
C91 C92 H92B 111.0 . . ?
C93 C92 H92B 111.0 . . ?
H92A C92 H92B 109.0 . . ?
C92 C93 C94 102.6(3) . . ?
C92 C93 H93A 111.3 . . ?
C94 C93 H93A 111.3 . . ?
C92 C93 H93B 111.3 . . ?
C94 C93 H93B 111.3 . . ?
H93A C93 H93B 109.2 . . ?
O9 C94 C93 106.1(3) . . ?
O9 C94 H94A 110.5 . . ?
C93 C94 H94A 110.5 . . ?
O9 C94 H94B 110.5 . . ?
C93 C94 H94B 110.5 . . ?
H94A C94 H94B 108.7 . . ?
C204 O10 C104 110.4(5) . . ?
C204 O10 C101 18.0(6) . . ?
C104 O10 C101 112.6(6) . . ?
C204 O10 C201 107.3(5) . . ?
C104 O10 C201 18.6(5) . . ?
C101 O10 C201 103.7(5) . . ?
C204 O10 Na1 124.0(4) . . ?
C104 O10 Na1 125.5(4) . . ?
C101 O10 Na1 120.2(4) . . ?
C201 O10 Na1 126.6(4) . . ?
O10 C101 C102 104.5(7) . . ?
O10 C101 H10A 110.9 . . ?
C102 C101 H10A 110.9 . . ?
O10 C101 H10B 110.9 . . ?
C102 C101 H10B 110.9 . . ?
H10A C101 H10B 108.9 . . ?
C101 C102 C103 103.9(7) . . ?
C101 C102 H10C 111.0 . . ?
C103 C102 H10C 111.0 . . ?
C101 C102 H10D 111.0 . . ?
C103 C102 H10D 111.0 . . ?
H10C C102 H10D 109.0 . . ?
C104 C103 C102 104.7(7) . . ?
C104 C103 H10E 110.8 . . ?
C102 C103 H10E 110.8 . . ?
C104 C103 H10F 110.8 . . ?
C102 C103 H10F 110.8 . . ?
H10E C103 H10F 108.9 . . ?
O10 C104 C103 105.8(6) . . ?
O10 C104 H10G 110.6 . . ?
C103 C104 H10G 110.6 . . ?
O10 C104 H10H 110.6 . . ?
C103 C104 H10H 110.6 . . ?
H10G C104 H10H 108.7 . . ?
O10 C201 C202 105.9(6) . . ?
O10 C201 H20A 110.5 . . ?
C202 C201 H20A 110.5 . . ?
O10 C201 H20B 110.5 . . ?
C202 C201 H20B 110.5 . . ?
H20A C201 H20B 108.7 . . ?
C203 C202 C201 101.7(7) . . ?
C203 C202 H20C 111.4 . . ?
C201 C202 H20C 111.4 . . ?
C203 C202 H20D 111.4 . . ?
C201 C202 H20D 111.4 . . ?
H20C C202 H20D 109.3 . . ?
C202 C203 C204 101.9(7) . . ?
C202 C203 H20E 111.4 . . ?
C204 C203 H20E 111.4 . . ?
C202 C203 H20F 111.4 . . ?
C204 C203 H20F 111.4 . . ?
H20E C203 H20F 109.3 . . ?
O10 C204 C203 108.7(6) . . ?
O10 C204 H20G 110.0 . . ?
C203 C204 H20G 110.0 . . ?
O10 C204 H20H 110.0 . . ?
C203 C204 H20H 110.0 . . ?
H20G C204 H20H 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        23.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_spiro-bi-pentacyclo-(p(co)(ncy)(co)(ncy))-_na(dme)
_database_code_depnum_ccdc_archive 'CCDC 986881'
_audit_update_record             
;
2014-02-14 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H54 N4 Na O6 P'
_chemical_formula_sum            'C32 H54 N4 Na O6 P'
_chemical_formula_weight         644.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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'

_cell_length_a                   10.4709(3)
_cell_length_b                   17.4983(5)
_cell_length_c                   18.6976(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3425.83(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1889
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      38.80

_exptl_crystal_description       blocks
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9130
_exptl_absorpt_correction_T_max  0.9643
_exptl_absorpt_process_details   'SADABS-2008/1 Bruker'

_exptl_special_details           
; 
The crystals inspected where extremely small.
The crystal measured (0.076 x 0.046 x 0.03 mm^3) with Cu-
radiation (t = 90s) diffrcted only to ~ 1.23 A.
The main alert type A is due to this fact. 

Due to the low resolution and small number of reflections, 
it is impossible to perform an anisotropic refinement.
The other alert type A refers to this situation.

There is an intrinsic low C-C bond precision due to the low
resolution.


;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Micro-Source HB-INCOATEC'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CMOS 100-Bruker Area Detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9948
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         38.80
_reflns_number_total             1889
_reflns_number_gt                1788
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0294P)²+6.5075P] 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   0.08(6)
_refine_ls_number_reflns         1889
_refine_ls_number_parameters     189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1001
_refine_ls_wR_factor_gt          0.0926
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_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 0.83051(18) 0.47504(11) 0.14759(10) 0.0324(6) Uani 1 1 d . . .
O1 O 0.8272(4) 0.6229(3) 0.1958(2) 0.0359(13) Uiso 1 1 d . . .
O2 O 0.6711(4) 0.4293(2) 0.3345(2) 0.0292(12) Uiso 1 1 d . . .
O3 O 1.0525(4) 0.4179(2) 0.2060(2) 0.0360(13) Uiso 1 1 d . . .
O4 O 1.0633(4) 0.5569(2) -0.0005(2) 0.0333(13) Uiso 1 1 d . . .
N1 N 0.7472(5) 0.5341(3) 0.2726(3) 0.0252(15) Uiso 1 1 d . . .
N2 N 0.7910(5) 0.4149(3) 0.2319(3) 0.0246(15) Uiso 1 1 d . . .
N3 N 1.0773(5) 0.4912(3) 0.1070(3) 0.0274(15) Uiso 1 1 d . . .
N4 N 0.8883(5) 0.5432(3) 0.0741(3) 0.0270(16) Uiso 1 1 d . . .
Na Na 0.4890(2) 0.39951(15) 0.39054(13) 0.0352(8) Uani 1 1 d . . .
C1 C 0.8034(6) 0.5568(4) 0.2093(3) 0.029(2) Uiso 1 1 d . . .
C2 C 0.7340(6) 0.4538(4) 0.2822(4) 0.026(2) Uiso 1 1 d . . .
C3 C 0.7190(6) 0.5919(4) 0.3283(3) 0.0259(19) Uiso 1 1 d . . .
H3 H 0.7403 0.6426 0.3067 0.031 Uiso 1 1 calc R . .
C4 C 0.8052(6) 0.5829(4) 0.3924(3) 0.033(2) Uiso 1 1 d . . .
H4A H 0.8955 0.5832 0.3767 0.040 Uiso 1 1 calc R . .
H4B H 0.7880 0.5333 0.4159 0.040 Uiso 1 1 calc R . .
C5 C 0.7830(7) 0.6482(4) 0.4460(4) 0.042(2) Uiso 1 1 d . . .
H5A H 0.8348 0.6389 0.4894 0.051 Uiso 1 1 calc R . .
H5B H 0.8119 0.6969 0.4245 0.051 Uiso 1 1 calc R . .
O5 O 0.2864(4) 0.4355(2) 0.3489(2) 0.0353(13) Uiso 1 1 d . . .
C6 C 0.6445(6) 0.6554(4) 0.4669(4) 0.040(2) Uiso 1 1 d . . .
H6A H 0.6336 0.7009 0.4978 0.048 Uiso 1 1 calc R . .
H6B H 0.6191 0.6099 0.4950 0.048 Uiso 1 1 calc R . .
O6 O 0.3951(4) 0.2918(2) 0.3415(2) 0.0320(13) Uiso 1 1 d . . .
C7 C 0.5576(6) 0.6626(4) 0.4020(3) 0.036(2) Uiso 1 1 d . . .
H7A H 0.5751 0.7115 0.3773 0.043 Uiso 1 1 calc R . .
H7B H 0.4673 0.6630 0.4178 0.043 Uiso 1 1 calc R . .
C8 C 0.5787(6) 0.5961(4) 0.3498(3) 0.034(2) Uiso 1 1 d . . .
H8A H 0.5530 0.5475 0.3728 0.041 Uiso 1 1 calc R . .
H8B H 0.5252 0.6035 0.3067 0.041 Uiso 1 1 calc R . .
C9 C 0.7824(6) 0.3313(3) 0.2346(3) 0.0238(19) Uiso 1 1 d . . .
H9 H 0.6952 0.3177 0.2524 0.029 Uiso 1 1 calc R . .
C10 C 0.8789(6) 0.2994(4) 0.2873(3) 0.031(2) Uiso 1 1 d . . .
H10A H 0.8634 0.3222 0.3350 0.037 Uiso 1 1 calc R . .
H10B H 0.9659 0.3143 0.2719 0.037 Uiso 1 1 calc R . .
C11 C 0.8718(7) 0.2124(4) 0.2932(3) 0.036(2) Uiso 1 1 d . . .
H11A H 0.9396 0.1940 0.3258 0.044 Uiso 1 1 calc R . .
H11B H 0.7882 0.1975 0.3136 0.044 Uiso 1 1 calc R . .
C12 C 0.8881(6) 0.1758(4) 0.2205(3) 0.035(2) Uiso 1 1 d . . .
H12A H 0.8770 0.1198 0.2248 0.042 Uiso 1 1 calc R . .
H12B H 0.9757 0.1856 0.2027 0.042 Uiso 1 1 calc R . .
C13 C 0.7920(7) 0.2070(4) 0.1672(4) 0.039(2) Uiso 1 1 d . . .
H13A H 0.7048 0.1918 0.1819 0.047 Uiso 1 1 calc R . .
H13B H 0.8088 0.1846 0.1195 0.047 Uiso 1 1 calc R . .
C14 C 0.7995(7) 0.2944(4) 0.1623(3) 0.034(2) Uiso 1 1 d . . .
H14A H 0.8834 0.3094 0.1423 0.041 Uiso 1 1 calc R . .
H14B H 0.7324 0.3132 0.1294 0.041 Uiso 1 1 calc R . .
C15 C 1.0054(6) 0.4569(4) 0.1587(4) 0.028(2) Uiso 1 1 d . . .
C16 C 1.0085(7) 0.5342(4) 0.0551(4) 0.027(2) Uiso 1 1 d . . .
C17 C 1.2160(6) 0.4800(4) 0.0993(3) 0.030(2) Uiso 1 1 d . . .
H17 H 1.2459 0.5147 0.0603 0.036 Uiso 1 1 calc R . .
C18 C 1.2493(6) 0.3994(4) 0.0777(4) 0.038(2) Uiso 1 1 d . . .
H18A H 1.2048 0.3865 0.0325 0.046 Uiso 1 1 calc R . .
H18B H 1.2200 0.3634 0.1150 0.046 Uiso 1 1 calc R . .
C19 C 1.3946(6) 0.3908(4) 0.0672(4) 0.043(2) Uiso 1 1 d . . .
H19A H 1.4151 0.3369 0.0559 0.052 Uiso 1 1 calc R . .
H19B H 1.4225 0.4227 0.0263 0.052 Uiso 1 1 calc R . .
C20 C 1.4658(7) 0.4148(4) 0.1340(4) 0.047(2) Uiso 1 1 d . . .
H20A H 1.4464 0.3784 0.1730 0.057 Uiso 1 1 calc R . .
H20B H 1.5588 0.4126 0.1246 0.057 Uiso 1 1 calc R . .
C21 C 1.4310(6) 0.4941(4) 0.1577(4) 0.043(2) Uiso 1 1 d . . .
H21A H 1.4611 0.5313 0.1216 0.052 Uiso 1 1 calc R . .
H21B H 1.4749 0.5055 0.2033 0.052 Uiso 1 1 calc R . .
C22 C 1.2858(6) 0.5036(4) 0.1680(3) 0.036(2) Uiso 1 1 d . . .
H22A H 1.2566 0.4714 0.2084 0.043 Uiso 1 1 calc R . .
H22B H 1.2659 0.5576 0.1794 0.043 Uiso 1 1 calc R . .
C23 C 0.8060(6) 0.5854(4) 0.0235(3) 0.0250(19) Uiso 1 1 d . . .
H23 H 0.8264 0.5672 -0.0258 0.030 Uiso 1 1 calc R . .
C24 C 0.6654(6) 0.5703(4) 0.0371(3) 0.0275(19) Uiso 1 1 d . . .
H24A H 0.6431 0.5867 0.0863 0.033 Uiso 1 1 calc R . .
H24B H 0.6483 0.5148 0.0332 0.033 Uiso 1 1 calc R . .
C25 C 0.5825(7) 0.6136(4) -0.0168(3) 0.034(2) Uiso 1 1 d . . .
H25A H 0.5975 0.5927 -0.0653 0.041 Uiso 1 1 calc R . .
H25B H 0.4913 0.6057 -0.0049 0.041 Uiso 1 1 calc R . .
C26 C 0.6117(6) 0.6984(4) -0.0168(4) 0.041(2) Uiso 1 1 d . . .
H26A H 0.5623 0.7236 -0.0553 0.049 Uiso 1 1 calc R . .
H26B H 0.5845 0.7208 0.0294 0.049 Uiso 1 1 calc R . .
C27 C 0.7519(6) 0.7135(4) -0.0278(4) 0.041(2) Uiso 1 1 d . . .
H27A H 0.7684 0.7690 -0.0233 0.049 Uiso 1 1 calc R . .
H27B H 0.7765 0.6977 -0.0768 0.049 Uiso 1 1 calc R . .
C28 C 0.8332(7) 0.6704(4) 0.0264(4) 0.036(2) Uiso 1 1 d . . .
H28A H 0.9248 0.6795 0.0163 0.043 Uiso 1 1 calc R . .
H28B H 0.8149 0.6898 0.0751 0.043 Uiso 1 1 calc R . .
C29 C 0.2233(7) 0.4999(4) 0.3803(4) 0.051(2) Uiso 1 1 d . . .
H29A H 0.2080 0.4899 0.4312 0.077 Uiso 1 1 calc R . .
H29B H 0.1416 0.5084 0.3560 0.077 Uiso 1 1 calc R . .
H29C H 0.2772 0.5453 0.3752 0.077 Uiso 1 1 calc R . .
C30 C 0.2097(7) 0.3687(4) 0.3514(4) 0.035(2) Uiso 1 1 d . . .
H30A H 0.1243 0.3797 0.3312 0.042 Uiso 1 1 calc R . .
H30B H 0.1985 0.3521 0.4016 0.042 Uiso 1 1 calc R . .
C31 C 0.2719(6) 0.3071(4) 0.3098(4) 0.034(2) Uiso 1 1 d . . .
H31A H 0.2185 0.2604 0.3108 0.041 Uiso 1 1 calc R . .
H31B H 0.2825 0.3232 0.2594 0.041 Uiso 1 1 calc R . .
C32 C 0.4583(7) 0.2290(4) 0.3082(4) 0.040(2) Uiso 1 1 d . . .
H32A H 0.4763 0.2416 0.2581 0.060 Uiso 1 1 calc R . .
H32B H 0.4034 0.1837 0.3103 0.060 Uiso 1 1 calc R . .
H32C H 0.5386 0.2186 0.3332 0.060 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.860(7) . ?
P1 C15 1.870(7) . ?
P1 N4 1.917(6) . ?
P1 N2 1.941(5) . ?
O1 C1 1.209(7) . ?
O2 C2 1.255(6) . ?
O2 Na 2.237(5) . ?
O3 C15 1.221(7) . ?
O4 C16 1.252(7) . ?
O4 Na 2.244(5) 2_664 ?
N1 C1 1.380(7) . ?
N1 C2 1.424(7) . ?
N1 C3 1.480(7) . ?
N2 C2 1.305(7) . ?
N2 C9 1.466(7) . ?
N3 C15 1.365(7) . ?
N3 C16 1.423(8) . ?
N3 C17 1.473(8) . ?
N4 C16 1.318(7) . ?
N4 C23 1.478(7) . ?
Na O4 2.244(5) 2_665 ?
Na O6 2.315(5) . ?
Na O5 2.346(5) . ?
C3 C4 1.510(8) . ?
C3 C8 1.524(8) . ?
C3 H3 1.0000 . ?
C4 C5 1.538(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.507(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
O5 C30 1.420(7) . ?
O5 C29 1.431(7) . ?
C6 C7 1.523(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O6 C32 1.426(7) . ?
O6 C31 1.445(7) . ?
C7 C8 1.535(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.509(8) . ?
C9 C10 1.517(8) . ?
C9 H9 1.0000 . ?
C10 C11 1.528(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.514(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.518(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.535(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C17 C18 1.508(9) . ?
C17 C22 1.534(8) . ?
C17 H17 1.0000 . ?
C18 C19 1.541(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.514(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.501(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.541(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C28 1.514(9) . ?
C23 C24 1.518(8) . ?
C23 H23 1.0000 . ?
C24 C25 1.532(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.515(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.507(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.525(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.479(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

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
C1 P1 C15 102.2(3) . . ?
C1 P1 N4 90.8(3) . . ?
C15 P1 N4 82.9(3) . . ?
C1 P1 N2 83.1(3) . . ?
C15 P1 N2 91.5(3) . . ?
N4 P1 N2 170.8(2) . . ?
C2 O2 Na 153.1(4) . . ?
C16 O4 Na 138.6(4) . 2_664 ?
C1 N1 C2 115.7(5) . . ?
C1 N1 C3 119.4(5) . . ?
C2 N1 C3 124.5(5) . . ?
C2 N2 C9 117.9(5) . . ?
C2 N2 P1 113.5(4) . . ?
C9 N2 P1 125.6(4) . . ?
C15 N3 C16 115.9(5) . . ?
C15 N3 C17 123.7(5) . . ?
C16 N3 C17 120.2(5) . . ?
C16 N4 C23 116.4(5) . . ?
C16 N4 P1 114.9(5) . . ?
C23 N4 P1 125.9(4) . . ?
O2 Na O4 123.70(19) . 2_665 ?
O2 Na O6 111.47(18) . . ?
O4 Na O6 122.16(18) 2_665 . ?
O2 Na O5 123.57(17) . . ?
O4 Na O5 89.37(17) 2_665 . ?
O6 Na O5 72.73(17) . . ?
O1 C1 N1 122.9(6) . . ?
O1 C1 P1 125.0(5) . . ?
N1 C1 P1 112.1(5) . . ?
O2 C2 N2 128.5(6) . . ?
O2 C2 N1 119.1(6) . . ?
N2 C2 N1 112.4(6) . . ?
N1 C3 C4 111.6(5) . . ?
N1 C3 C8 114.3(5) . . ?
C4 C3 C8 111.8(5) . . ?
N1 C3 H3 106.2 . . ?
C4 C3 H3 106.2 . . ?
C8 C3 H3 106.2 . . ?
C3 C4 C5 110.5(5) . . ?
C3 C4 H4A 109.6 . . ?
C5 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 C4 112.1(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 . . ?
C30 O5 C29 111.9(5) . . ?
C30 O5 Na 106.2(4) . . ?
C29 O5 Na 119.5(4) . . ?
C5 C6 C7 112.0(6) . . ?
C5 C6 H6A 109.2 . . ?
C7 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C7 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C32 O6 C31 112.2(5) . . ?
C32 O6 Na 127.1(4) . . ?
C31 O6 Na 113.0(4) . . ?
C6 C7 C8 111.0(6) . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C3 C8 C7 110.1(5) . . ?
C3 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
C3 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.2 . . ?
N2 C9 C14 112.9(5) . . ?
N2 C9 C10 110.4(5) . . ?
C14 C9 C10 110.2(5) . . ?
N2 C9 H9 107.7 . . ?
C14 C9 H9 107.7 . . ?
C10 C9 H9 107.7 . . ?
C9 C10 C11 112.4(6) . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C12 C11 C10 110.5(6) . . ?
C12 C11 H11A 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 111.3(5) . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C12 C13 C14 111.3(6) . . ?
C12 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C9 C14 C13 111.5(5) . . ?
C9 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C9 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
O3 C15 N3 122.4(6) . . ?
O3 C15 P1 124.8(5) . . ?
N3 C15 P1 112.8(5) . . ?
O4 C16 N4 128.6(6) . . ?
O4 C16 N3 120.1(6) . . ?
N4 C16 N3 111.2(6) . . ?
N3 C17 C18 112.3(5) . . ?
N3 C17 C22 110.6(5) . . ?
C18 C17 C22 111.5(5) . . ?
N3 C17 H17 107.4 . . ?
C18 C17 H17 107.4 . . ?
C22 C17 H17 107.4 . . ?
C17 C18 C19 110.7(6) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 110.7(6) . . ?
C20 C19 H19A 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C21 C20 C19 112.4(6) . . ?
C21 C20 H20A 109.1 . . ?
C19 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
C20 C21 C22 112.2(6) . . ?
C20 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C17 C22 C21 109.6(6) . . ?
C17 C22 H22A 109.7 . . ?
C21 C22 H22A 109.7 . . ?
C17 C22 H22B 109.7 . . ?
C21 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
N4 C23 C28 111.0(5) . . ?
N4 C23 C24 111.8(5) . . ?
C28 C23 C24 110.4(6) . . ?
N4 C23 H23 107.8 . . ?
C28 C23 H23 107.8 . . ?
C24 C23 H23 107.8 . . ?
C23 C24 C25 110.7(5) . . ?
C23 C24 H24A 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C26 C25 C24 111.7(6) . . ?
C26 C25 H25A 109.3 . . ?
C24 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
C24 C25 H25B 109.3 . . ?
H25A C25 H25B 107.9 . . ?
C27 C26 C25 111.6(6) . . ?
C27 C26 H26A 109.3 . . ?
C25 C26 H26A 109.3 . . ?
C27 C26 H26B 109.3 . . ?
C25 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C26 C27 C28 111.5(6) . . ?
C26 C27 H27A 109.3 . . ?
C28 C27 H27A 109.3 . . ?
C26 C27 H27B 109.3 . . ?
C28 C27 H27B 109.3 . . ?
H27A C27 H27B 108.0 . . ?
C23 C28 C27 110.9(5) . . ?
C23 C28 H28A 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.0 . . ?
O5 C29 H29A 109.5 . . ?
O5 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O5 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O5 C30 C31 109.5(5) . . ?
O5 C30 H30A 109.8 . . ?
C31 C30 H30A 109.8 . . ?
O5 C30 H30B 109.8 . . ?
C31 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
O6 C31 C30 108.2(5) . . ?
O6 C31 H31A 110.1 . . ?
C30 C31 H31A 110.1 . . ?
O6 C31 H31B 110.1 . . ?
C30 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        38.80
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.048


####################################################################### 
# 
# 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_p21n
_database_code_depnum_ccdc_archive 'CCDC 1049373'
_audit_update_record             
;
2015-02-13 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 [K(18-crown-6)][PC2O2(NDipp)2]
;
_contact_author_fax              '+44 1865 272690'
_chemical_name_common            .
_chemical_melting_point          .
_chemical_formula_moiety         'C12 H24 K O6, C26 H34 N2 O2 P'
_chemical_formula_sum            'C38 H58 K N2 O8 P'
_chemical_formula_weight         740.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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 2(1)/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   10.7457(2)
_cell_length_b                   17.6496(3)
_cell_length_c                   21.5074(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.8700(10)
_cell_angle_gamma                90.00
_cell_volume                     4018.66(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    41601
_cell_measurement_theta_min      3.2561
_cell_measurement_theta_max      76.6924

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1592
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6746
_exptl_absorpt_correction_T_max  0.8295
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            87300
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         76.89
_reflns_number_total             8414
_reflns_number_gt                7696
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'

_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 > 2σ(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)+(0.0992P)²+3.8426P] 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         8414
_refine_ls_number_parameters     479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1859
_refine_ls_wR_factor_gt          0.1822
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 1.08327(6) 0.55162(4) 0.20769(3) 0.04164(17) Uani 1 1 d . . .
C1 C 1.07837(19) 0.61043(12) 0.27437(9) 0.0263(4) Uani 1 1 d . . .
O1 O 1.09237(19) 0.59963(12) 0.32945(9) 0.0495(4) Uani 1 1 d . . .
C2 C 1.01936(18) 0.69561(12) 0.18341(10) 0.0295(4) Uani 1 1 d . . .
O2 O 0.98576(15) 0.75529(9) 0.15514(7) 0.0365(4) Uani 1 1 d . B .
N1 N 1.03947(17) 0.68745(11) 0.24847(8) 0.0310(4) Uani 1 1 d . . .
C3 C 1.0476(2) 0.75203(13) 0.28932(10) 0.0339(5) Uani 1 1 d . . .
C4 C 1.1561(2) 0.79703(14) 0.29590(11) 0.0372(5) Uani 1 1 d . . .
C5 C 1.1621(2) 0.86006(15) 0.33561(13) 0.0447(6) Uani 1 1 d . . .
H5 H 1.2334 0.8927 0.3400 0.054 Uiso 1 1 calc R . .
C6 C 1.0647(3) 0.87537(16) 0.36880(13) 0.0491(6) Uani 1 1 d . . .
H6 H 1.0704 0.9180 0.3961 0.059 Uiso 1 1 calc R . .
C7 C 0.9599(3) 0.82906(17) 0.36235(13) 0.0474(6) Uani 1 1 d . . .
H7 H 0.8944 0.8401 0.3855 0.057 Uiso 1 1 calc R . .
C8 C 0.9484(2) 0.76648(15) 0.32248(11) 0.0397(5) Uani 1 1 d . . .
C9 C 1.2641(2) 0.77909(16) 0.26096(12) 0.0420(5) Uani 1 1 d . . .
H9 H 1.2428 0.7304 0.2378 0.050 Uiso 1 1 calc R . .
C10 C 1.3879(3) 0.7667(3) 0.30642(17) 0.0771(12) Uani 1 1 d . . .
H10A H 1.3755 0.7284 0.3378 0.116 Uiso 0.50 1 calc PR . .
H10B H 1.4150 0.8144 0.3278 0.116 Uiso 0.50 1 calc PR . .
H10C H 1.4529 0.7492 0.2828 0.116 Uiso 0.50 1 calc PR . .
H10D H 1.4534 0.7996 0.2945 0.116 Uiso 0.50 1 calc PR . .
H10E H 1.4139 0.7136 0.3045 0.116 Uiso 0.50 1 calc PR . .
H10F H 1.3760 0.7788 0.3495 0.116 Uiso 0.50 1 calc PR . .
C11 C 1.2786(4) 0.8386(2) 0.21247(18) 0.0704(9) Uani 1 1 d . . .
H11A H 1.3492 0.8251 0.1912 0.106 Uiso 0.50 1 calc PR . .
H11B H 1.2954 0.8878 0.2333 0.106 Uiso 0.50 1 calc PR . .
H11C H 1.2007 0.8417 0.1813 0.106 Uiso 0.50 1 calc PR . .
H11D H 1.2143 0.8780 0.2127 0.106 Uiso 0.50 1 calc PR . .
H11E H 1.2681 0.8152 0.1706 0.106 Uiso 0.50 1 calc PR . .
H11F H 1.3628 0.8614 0.2226 0.106 Uiso 0.50 1 calc PR . .
C12 C 0.8324(2) 0.71594(18) 0.31303(14) 0.0483(6) Uani 1 1 d . . .
H12 H 0.8609 0.6633 0.3057 0.058 Uiso 1 1 calc R . .
C13 C 0.7643(3) 0.7134(3) 0.36963(17) 0.0711(10) Uani 1 1 d . . .
H13A H 0.6910 0.6797 0.3603 0.107 Uiso 0.50 1 calc PR . .
H13B H 0.7362 0.7644 0.3785 0.107 Uiso 0.50 1 calc PR . .
H13C H 0.8221 0.6942 0.4065 0.107 Uiso 0.50 1 calc PR . .
H13D H 0.8085 0.7459 0.4032 0.107 Uiso 0.50 1 calc PR . .
H13E H 0.7633 0.6611 0.3851 0.107 Uiso 0.50 1 calc PR . .
H13F H 0.6774 0.7314 0.3570 0.107 Uiso 0.50 1 calc PR . .
C14 C 0.7409(3) 0.7401(2) 0.25414(16) 0.0679(9) Uani 1 1 d . . .
H14A H 0.6665 0.7072 0.2485 0.102 Uiso 0.50 1 calc PR . .
H14B H 0.7827 0.7361 0.2172 0.102 Uiso 0.50 1 calc PR . .
H14C H 0.7149 0.7927 0.2589 0.102 Uiso 0.50 1 calc PR . .
H14D H 0.7762 0.7835 0.2346 0.102 Uiso 0.50 1 calc PR . .
H14E H 0.6600 0.7546 0.2659 0.102 Uiso 0.50 1 calc PR . .
H14F H 0.7278 0.6979 0.2241 0.102 Uiso 0.50 1 calc PR . .
N2 N 1.04129(17) 0.62912(10) 0.15637(8) 0.0309(4) Uani 1 1 d . . .
C15 C 1.0175(2) 0.61959(12) 0.08927(10) 0.0311(4) Uani 1 1 d . . .
C16 C 1.1180(2) 0.62871(13) 0.05565(11) 0.0353(5) Uani 1 1 d . . .
C17 C 1.0936(3) 0.61577(15) -0.00911(12) 0.0428(6) Uani 1 1 d . . .
H17 H 1.1598 0.6216 -0.0329 0.051 Uiso 1 1 calc R . .
C18 C 0.9748(3) 0.59466(16) -0.03945(12) 0.0445(6) Uani 1 1 d . . .
H18 H 0.9606 0.5849 -0.0835 0.053 Uiso 1 1 calc R . .
C19 C 0.8765(2) 0.58761(15) -0.00595(11) 0.0419(5) Uani 1 1 d . . .
H19 H 0.7950 0.5739 -0.0275 0.050 Uiso 1 1 calc R . .
C20 C 0.8953(2) 0.60031(14) 0.05925(11) 0.0348(5) Uani 1 1 d . . .
C21 C 1.2495(2) 0.64999(16) 0.08919(13) 0.0450(6) Uani 1 1 d . . .
H21 H 1.2410 0.6777 0.1288 0.054 Uiso 1 1 calc R . .
C22 C 1.3286(3) 0.5792(2) 0.10745(16) 0.0590(8) Uani 1 1 d . . .
H22A H 1.4129 0.5939 0.1291 0.089 Uiso 0.50 1 calc PR . .
H22B H 1.3363 0.5503 0.0693 0.089 Uiso 0.50 1 calc PR . .
H22C H 1.2876 0.5477 0.1356 0.089 Uiso 0.50 1 calc PR . .
H22D H 1.2783 0.5340 0.0936 0.089 Uiso 0.50 1 calc PR . .
H22E H 1.3549 0.5777 0.1534 0.089 Uiso 0.50 1 calc PR . .
H22F H 1.4036 0.5802 0.0871 0.089 Uiso 0.50 1 calc PR . .
C23 C 1.3212(3) 0.7014(2) 0.0495(2) 0.0693(10) Uani 1 1 d . . .
H23A H 1.4048 0.7133 0.0736 0.104 Uiso 0.50 1 calc PR . .
H23B H 1.2736 0.7485 0.0392 0.104 Uiso 0.50 1 calc PR . .
H23C H 1.3307 0.6752 0.0104 0.104 Uiso 0.50 1 calc PR . .
H23D H 1.2679 0.7114 0.0085 0.104 Uiso 0.50 1 calc PR . .
H23E H 1.3991 0.6762 0.0429 0.104 Uiso 0.50 1 calc PR . .
H23F H 1.3421 0.7494 0.0717 0.104 Uiso 0.50 1 calc PR . .
C24 C 0.7856(2) 0.59436(15) 0.09499(12) 0.0395(5) Uani 1 1 d . . .
H24 H 0.8206 0.6026 0.1406 0.047 Uiso 1 1 calc R . .
C25 C 0.7251(3) 0.51649(19) 0.08937(17) 0.0618(8) Uani 1 1 d . . .
H25A H 0.6553 0.5153 0.1133 0.093 Uiso 0.50 1 calc PR . .
H25B H 0.7882 0.4783 0.1063 0.093 Uiso 0.50 1 calc PR . .
H25C H 0.6928 0.5055 0.0449 0.093 Uiso 0.50 1 calc PR . .
H25D H 0.7689 0.4841 0.0630 0.093 Uiso 0.50 1 calc PR . .
H25E H 0.6360 0.5211 0.0700 0.093 Uiso 0.50 1 calc PR . .
H25F H 0.7314 0.4940 0.1314 0.093 Uiso 0.50 1 calc PR . .
C26 C 0.6893(3) 0.6567(2) 0.07509(17) 0.0605(8) Uani 1 1 d . . .
H26A H 0.7317 0.7060 0.0792 0.091 Uiso 0.50 1 calc PR . .
H26B H 0.6247 0.6554 0.1022 0.091 Uiso 0.50 1 calc PR . .
H26C H 0.6494 0.6488 0.0311 0.091 Uiso 0.50 1 calc PR . .
H26D H 0.6054 0.6341 0.0624 0.091 Uiso 0.50 1 calc PR . .
H26E H 0.7125 0.6848 0.0395 0.091 Uiso 0.50 1 calc PR . .
H26F H 0.6878 0.6913 0.1106 0.091 Uiso 0.50 1 calc PR . .
K1 K 0.86406(5) 0.88139(3) 0.11731(3) 0.04314(16) Uani 1 1 d . . .
O101 O 1.0817(2) 0.95973(14) 0.11147(11) 0.0617(6) Uani 1 1 d . B .
C101 C 1.1061(3) 1.0307(2) 0.14369(17) 0.0668(9) Uani 1 1 d . . .
H10G H 1.0634 1.0722 0.1173 0.080 Uiso 1 1 calc R B .
H10H H 1.1980 1.0411 0.1518 0.080 Uiso 1 1 calc R . .
C102 C 1.0587(3) 1.0270(2) 0.20351(17) 0.0660(9) Uani 1 1 d . B .
H10I H 1.0996 0.9845 0.2293 0.079 Uiso 1 1 calc R . .
H10J H 1.0791 1.0746 0.2274 0.079 Uiso 1 1 calc R . .
O102 O 0.9254(2) 1.01612(12) 0.19108(10) 0.0562(5) Uani 1 1 d . B .
C103 C 0.8736(4) 1.0113(2) 0.24653(17) 0.0685(9) Uani 1 1 d . . .
H10K H 0.8937 1.0578 0.2721 0.082 Uiso 1 1 calc R B .
H10L H 0.9099 0.9674 0.2720 0.082 Uiso 1 1 calc R . .
C104 C 0.7343(4) 1.0025(2) 0.2291(2) 0.0735(10) Uani 1 1 d . B .
H10M H 0.6946 1.0071 0.2672 0.088 Uiso 1 1 calc R . .
H10N H 0.6995 1.0427 0.1990 0.088 Uiso 1 1 calc R . .
O103 O 0.7072(2) 0.93084(14) 0.20122(12) 0.0630(6) Uani 1 1 d . B .
C105 C 0.5764(3) 0.9205(3) 0.1814(3) 0.1005(18) Uani 1 1 d . . .
H10O H 0.5570 0.8681 0.1933 0.121 Uiso 1 1 calc R A 1
H10P H 0.5335 0.9547 0.2074 0.121 Uiso 1 1 calc R A 1
C106 C 0.5226(7) 0.9296(5) 0.1248(4) 0.0625(19) Uani 0.534(8) 1 d P B 1
H10Q H 0.5314 0.9831 0.1122 0.075 Uiso 0.534(8) 1 calc PR B 1
H10R H 0.4315 0.9181 0.1209 0.075 Uiso 0.534(8) 1 calc PR B 1
O104 O 0.5780(4) 0.8811(2) 0.08421(19) 0.0520(15) Uani 0.534(8) 1 d P B 1
C107 C 0.5426(11) 0.8975(6) 0.0191(5) 0.059(2) Uani 0.534(8) 1 d P B 1
H10S H 0.5707 0.9492 0.0103 0.071 Uiso 0.534(8) 1 calc PR B 1
H10T H 0.4495 0.8954 0.0071 0.071 Uiso 0.534(8) 1 calc PR B 1
C6A C 0.5464(8) 0.9679(7) 0.1094(5) 0.070(3) Uani 0.466(8) 1 d P B 2
H6A1 H 0.4541 0.9682 0.0941 0.084 Uiso 0.466(8) 1 calc PR B 2
H6A2 H 0.5741 1.0212 0.1162 0.084 Uiso 0.466(8) 1 calc PR B 2
O4A O 0.6081(4) 0.9354(3) 0.0611(2) 0.0604(18) Uani 0.466(8) 1 d P B 2
C7A C 0.5490(12) 0.8685(7) 0.0332(7) 0.071(3) Uani 0.466(8) 1 d P B 2
H7A1 H 0.5553 0.8284 0.0658 0.085 Uiso 0.466(8) 1 calc PR B 2
H7A2 H 0.4582 0.8790 0.0186 0.085 Uiso 0.466(8) 1 calc PR B 2
C108 C 0.6021(3) 0.8407(2) -0.01866(15) 0.0636(8) Uani 1 1 d . . .
H10U H 0.5591 0.7913 -0.0173 0.076 Uiso 1 1 calc R B 1
H10V H 0.5899 0.8574 -0.0632 0.076 Uiso 1 1 calc R B 1
O105 O 0.7316(2) 0.83130(13) 0.00371(10) 0.0579(5) Uani 1 1 d . B .
C109 C 0.7986(4) 0.80236(19) -0.04282(14) 0.0601(8) Uani 1 1 d . . .
H10W H 0.7858 0.8358 -0.0803 0.072 Uiso 1 1 calc R B .
H10$ H 0.7672 0.7512 -0.0562 0.072 Uiso 1 1 calc R . .
C110 C 0.9357(4) 0.79882(19) -0.01490(15) 0.0629(9) Uani 1 1 d . B .
H11G H 0.9488 0.7635 0.0214 0.075 Uiso 1 1 calc R . .
H11H H 0.9846 0.7799 -0.0468 0.075 Uiso 1 1 calc R . .
O106 O 0.9784(2) 0.87271(12) 0.00547(10) 0.0556(5) Uani 1 1 d . B .
C111 C 1.1099(3) 0.8770(2) 0.02930(18) 0.0711(10) Uani 1 1 d . B .
H11I H 1.1582 0.8684 -0.0054 0.085 Uiso 1 1 calc R . .
H11J H 1.1338 0.8372 0.0616 0.085 Uiso 1 1 calc R . .
C112 C 1.1413(3) 0.9525(3) 0.05763(18) 0.0702(10) Uani 1 1 d . . .
H11K H 1.2339 0.9577 0.0701 0.084 Uiso 1 1 calc R B .
H11L H 1.1110 0.9927 0.0266 0.084 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 1.7668(19) . ?
P1 C1 1.778(2) . ?
C1 O1 1.184(3) . ?
C1 N1 1.501(3) . ?
C2 O2 1.239(3) . ?
C2 N2 1.348(3) . ?
C2 N1 1.386(3) . ?
O2 K1 2.6382(16) . ?
N1 C3 1.433(3) . ?
C3 C4 1.397(3) . ?
C3 C8 1.403(3) . ?
C4 C5 1.397(4) . ?
C4 C9 1.521(3) . ?
C5 C6 1.391(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.380(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(4) . ?
C7 H7 0.9500 . ?
C8 C12 1.518(4) . ?
C9 C11 1.507(4) . ?
C9 C10 1.526(4) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10D 0.9800 . ?
C10 H10E 0.9800 . ?
C10 H10F 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 H11D 0.9800 . ?
C11 H11E 0.9800 . ?
C11 H11F 0.9800 . ?
C12 C13 1.524(4) . ?
C12 C14 1.525(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 H13D 0.9800 . ?
C13 H13E 0.9800 . ?
C13 H13F 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 H14D 0.9800 . ?
C14 H14E 0.9800 . ?
C14 H14F 0.9800 . ?
N2 C15 1.432(3) . ?
C15 C20 1.402(3) . ?
C15 C16 1.409(3) . ?
C16 C17 1.391(4) . ?
C16 C21 1.520(3) . ?
C17 C18 1.381(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.382(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.400(3) . ?
C19 H19 0.9500 . ?
C20 C24 1.517(3) . ?
C21 C22 1.525(4) . ?
C21 C23 1.540(4) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 H22D 0.9800 . ?
C22 H22E 0.9800 . ?
C22 H22F 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 H23D 0.9800 . ?
C23 H23E 0.9800 . ?
C23 H23F 0.9800 . ?
C24 C25 1.516(4) . ?
C24 C26 1.521(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 H25D 0.9800 . ?
C25 H25E 0.9800 . ?
C25 H25F 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26 H26D 0.9800 . ?
C26 H26E 0.9800 . ?
C26 H26F 0.9800 . ?
K1 O101 2.738(2) . ?
K1 O105 2.754(2) . ?
K1 O103 2.811(2) . ?
K1 O102 2.872(2) . ?
K1 O106 2.887(2) . ?
K1 O4A 2.966(5) . ?
K1 O104 3.034(4) . ?
K1 C110 3.399(3) . ?
K1 C111 3.505(4) . ?
O101 C112 1.422(4) . ?
O101 C101 1.434(4) . ?
C101 C102 1.464(5) . ?
C101 H10G 0.9900 . ?
C101 H10H 0.9900 . ?
C102 O102 1.424(4) . ?
C102 H10I 0.9900 . ?
C102 H10J 0.9900 . ?
O102 C103 1.402(4) . ?
C103 C104 1.489(5) . ?
C103 H10K 0.9900 . ?
C103 H10L 0.9900 . ?
C104 O103 1.408(4) . ?
C104 H10M 0.9900 . ?
C104 H10N 0.9900 . ?
O103 C105 1.409(4) . ?
C105 C106 1.266(9) . ?
C105 C6A 1.742(13) . ?
C105 H10O 0.9900 . ?
C105 H10P 0.9900 . ?
C106 O104 1.423(9) . ?
C106 H10Q 0.9900 . ?
C106 H10R 0.9900 . ?
O104 C107 1.416(11) . ?
C107 C108 1.501(12) . ?
C107 H10S 0.9900 . ?
C107 H10T 0.9900 . ?
C6A O4A 1.443(10) . ?
C6A H6A1 0.9900 . ?
C6A H6A2 0.9900 . ?
O4A C7A 1.424(15) . ?
C7A C108 1.424(17) . ?
C7A H7A1 0.9900 . ?
C7A H7A2 0.9900 . ?
C108 O105 1.402(4) . ?
C108 H10U 0.9900 . ?
C108 H10V 0.9900 . ?
O105 C109 1.424(4) . ?
C109 C110 1.494(5) . ?
C109 H10W 0.9900 . ?
C109 H10$ 0.9900 . ?
C110 O106 1.426(4) . ?
C110 H11G 0.9900 . ?
C110 H11H 0.9900 . ?
O106 C111 1.420(4) . ?
C111 C112 1.480(6) . ?
C111 H11I 0.9900 . ?
C111 H11J 0.9900 . ?
C112 H11K 0.9900 . ?
C112 H11L 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 P1 C1 90.70(9) . . ?
O1 C1 N1 119.79(19) . . ?
O1 C1 P1 134.18(19) . . ?
N1 C1 P1 105.90(13) . . ?
O2 C2 N2 125.9(2) . . ?
O2 C2 N1 124.5(2) . . ?
N2 C2 N1 109.66(18) . . ?
C2 O2 K1 162.96(15) . . ?
C2 N1 C3 121.26(18) . . ?
C2 N1 C1 117.00(17) . . ?
C3 N1 C1 120.60(16) . . ?
C4 C3 C8 122.5(2) . . ?
C4 C3 N1 118.5(2) . . ?
C8 C3 N1 119.0(2) . . ?
C5 C4 C3 117.7(2) . . ?
C5 C4 C9 120.6(2) . . ?
C3 C4 C9 121.7(2) . . ?
C6 C5 C4 120.5(2) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C7 C6 C5 120.5(2) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 121.1(3) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C7 C8 C3 117.6(2) . . ?
C7 C8 C12 122.2(2) . . ?
C3 C8 C12 120.2(2) . . ?
C11 C9 C4 112.0(2) . . ?
C11 C9 C10 111.2(3) . . ?
C4 C9 C10 111.7(2) . . ?
C11 C9 H9 107.2 . . ?
C4 C9 H9 107.2 . . ?
C10 C9 H9 107.2 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C10 H10D 109.5 . . ?
H10A C10 H10D 141.1 . . ?
H10B C10 H10D 56.3 . . ?
H10C C10 H10D 56.3 . . ?
C9 C10 H10E 109.5 . . ?
H10A C10 H10E 56.3 . . ?
H10B C10 H10E 141.1 . . ?
H10C C10 H10E 56.3 . . ?
H10D C10 H10E 109.5 . . ?
C9 C10 H10F 109.5 . . ?
H10A C10 H10F 56.3 . . ?
H10B C10 H10F 56.3 . . ?
H10C C10 H10F 141.1 . . ?
H10D C10 H10F 109.5 . . ?
H10E C10 H10F 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C11 H11D 109.5 . . ?
H11A C11 H11D 141.1 . . ?
H11B C11 H11D 56.3 . . ?
H11C C11 H11D 56.3 . . ?
C9 C11 H11E 109.5 . . ?
H11A C11 H11E 56.3 . . ?
H11B C11 H11E 141.1 . . ?
H11C C11 H11E 56.3 . . ?
H11D C11 H11E 109.5 . . ?
C9 C11 H11F 109.5 . . ?
H11A C11 H11F 56.3 . . ?
H11B C11 H11F 56.3 . . ?
H11C C11 H11F 141.1 . . ?
H11D C11 H11F 109.5 . . ?
H11E C11 H11F 109.5 . . ?
C8 C12 C13 114.0(2) . . ?
C8 C12 C14 110.1(3) . . ?
C13 C12 C14 110.0(3) . . ?
C8 C12 H12 107.5 . . ?
C13 C12 H12 107.5 . . ?
C14 C12 H12 107.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C13 H13D 109.5 . . ?
H13A C13 H13D 141.1 . . ?
H13B C13 H13D 56.3 . . ?
H13C C13 H13D 56.3 . . ?
C12 C13 H13E 109.5 . . ?
H13A C13 H13E 56.3 . . ?
H13B C13 H13E 141.1 . . ?
H13C C13 H13E 56.3 . . ?
H13D C13 H13E 109.5 . . ?
C12 C13 H13F 109.5 . . ?
H13A C13 H13F 56.3 . . ?
H13B C13 H13F 56.3 . . ?
H13C C13 H13F 141.1 . . ?
H13D C13 H13F 109.5 . . ?
H13E C13 H13F 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C14 H14D 109.5 . . ?
H14A C14 H14D 141.1 . . ?
H14B C14 H14D 56.3 . . ?
H14C C14 H14D 56.3 . . ?
C12 C14 H14E 109.5 . . ?
H14A C14 H14E 56.3 . . ?
H14B C14 H14E 141.1 . . ?
H14C C14 H14E 56.3 . . ?
H14D C14 H14E 109.5 . . ?
C12 C14 H14F 109.5 . . ?
H14A C14 H14F 56.3 . . ?
H14B C14 H14F 56.3 . . ?
H14C C14 H14F 141.1 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
C2 N2 C15 121.51(18) . . ?
C2 N2 P1 116.69(15) . . ?
C15 N2 P1 121.41(15) . . ?
C20 C15 C16 122.1(2) . . ?
C20 C15 N2 119.0(2) . . ?
C16 C15 N2 118.9(2) . . ?
C17 C16 C15 117.8(2) . . ?
C17 C16 C21 121.1(2) . . ?
C15 C16 C21 121.2(2) . . ?
C18 C17 C16 121.2(2) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 120.3(2) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 121.0(2) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C19 C20 C15 117.6(2) . . ?
C19 C20 C24 120.3(2) . . ?
C15 C20 C24 122.1(2) . . ?
C16 C21 C22 110.6(2) . . ?
C16 C21 C23 113.3(2) . . ?
C22 C21 C23 108.5(2) . . ?
C16 C21 H21 108.1 . . ?
C22 C21 H21 108.1 . . ?
C23 C21 H21 108.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C22 H22D 109.5 . . ?
H22A C22 H22D 141.1 . . ?
H22B C22 H22D 56.3 . . ?
H22C C22 H22D 56.3 . . ?
C21 C22 H22E 109.5 . . ?
H22A C22 H22E 56.3 . . ?
H22B C22 H22E 141.1 . . ?
H22C C22 H22E 56.3 . . ?
H22D C22 H22E 109.5 . . ?
C21 C22 H22F 109.5 . . ?
H22A C22 H22F 56.3 . . ?
H22B C22 H22F 56.3 . . ?
H22C C22 H22F 141.1 . . ?
H22D C22 H22F 109.5 . . ?
H22E C22 H22F 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C23 H23D 109.5 . . ?
H23A C23 H23D 141.1 . . ?
H23B C23 H23D 56.3 . . ?
H23C C23 H23D 56.3 . . ?
C21 C23 H23E 109.5 . . ?
H23A C23 H23E 56.3 . . ?
H23B C23 H23E 141.1 . . ?
H23C C23 H23E 56.3 . . ?
H23D C23 H23E 109.5 . . ?
C21 C23 H23F 109.5 . . ?
H23A C23 H23F 56.3 . . ?
H23B C23 H23F 56.3 . . ?
H23C C23 H23F 141.1 . . ?
H23D C23 H23F 109.5 . . ?
H23E C23 H23F 109.5 . . ?
C25 C24 C20 112.5(2) . . ?
C25 C24 C26 111.8(3) . . ?
C20 C24 C26 111.0(2) . . ?
C25 C24 H24 107.1 . . ?
C20 C24 H24 107.1 . . ?
C26 C24 H24 107.1 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C25 H25D 109.5 . . ?
H25A C25 H25D 141.1 . . ?
H25B C25 H25D 56.3 . . ?
H25C C25 H25D 56.3 . . ?
C24 C25 H25E 109.5 . . ?
H25A C25 H25E 56.3 . . ?
H25B C25 H25E 141.1 . . ?
H25C C25 H25E 56.3 . . ?
H25D C25 H25E 109.5 . . ?
C24 C25 H25F 109.5 . . ?
H25A C25 H25F 56.3 . . ?
H25B C25 H25F 56.3 . . ?
H25C C25 H25F 141.1 . . ?
H25D C25 H25F 109.5 . . ?
H25E C25 H25F 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C26 H26D 109.5 . . ?
H26A C26 H26D 141.1 . . ?
H26B C26 H26D 56.3 . . ?
H26C C26 H26D 56.3 . . ?
C24 C26 H26E 109.5 . . ?
H26A C26 H26E 56.3 . . ?
H26B C26 H26E 141.1 . . ?
H26C C26 H26E 56.3 . . ?
H26D C26 H26E 109.5 . . ?
C24 C26 H26F 109.5 . . ?
H26A C26 H26F 56.3 . . ?
H26B C26 H26F 56.3 . . ?
H26C C26 H26F 141.1 . . ?
H26D C26 H26F 109.5 . . ?
H26E C26 H26F 109.5 . . ?
O2 K1 O101 93.32(6) . . ?
O2 K1 O105 98.99(6) . . ?
O101 K1 O105 115.92(7) . . ?
O2 K1 O103 112.58(7) . . ?
O101 K1 O103 118.91(7) . . ?
O105 K1 O103 113.17(7) . . ?
O2 K1 O102 118.26(6) . . ?
O101 K1 O102 59.37(7) . . ?
O105 K1 O102 142.24(7) . . ?
O103 K1 O102 59.62(7) . . ?
O2 K1 O106 87.30(6) . . ?
O101 K1 O106 59.97(7) . . ?
O105 K1 O106 58.19(7) . . ?
O103 K1 O106 159.91(7) . . ?
O102 K1 O106 114.47(7) . . ?
O2 K1 O4A 140.61(12) . . ?
O101 K1 O4A 123.98(12) . . ?
O105 K1 O4A 55.90(11) . . ?
O103 K1 O4A 62.97(11) . . ?
O102 K1 O4A 93.90(11) . . ?
O106 K1 O4A 100.08(12) . . ?
O2 K1 O104 119.98(9) . . ?
O101 K1 O104 145.99(10) . . ?
O105 K1 O104 56.12(9) . . ?
O103 K1 O104 57.06(9) . . ?
O102 K1 O104 104.95(9) . . ?
O106 K1 O104 111.31(9) . . ?
O4A K1 O104 22.07(12) . . ?
O2 K1 C110 74.03(7) . . ?
O101 K1 C110 81.97(9) . . ?
O105 K1 C110 43.70(8) . . ?
O103 K1 C110 156.49(8) . . ?
O102 K1 C110 138.92(8) . . ?
O106 K1 C110 24.53(8) . . ?
O4A K1 C110 97.13(12) . . ?
O104 K1 C110 99.72(10) . . ?
O2 K1 C111 76.60(7) . . ?
O101 K1 C111 42.05(9) . . ?
O105 K1 C111 80.60(8) . . ?
O103 K1 C111 160.73(9) . . ?
O102 K1 C111 101.18(9) . . ?
O106 K1 C111 23.19(8) . . ?
O4A K1 C111 121.29(13) . . ?
O104 K1 C111 134.47(10) . . ?
C110 K1 C111 40.43(10) . . ?
C112 O101 C101 113.7(3) . . ?
C112 O101 K1 120.0(2) . . ?
C101 O101 K1 120.4(2) . . ?
O101 C101 C102 108.9(3) . . ?
O101 C101 H10G 109.9 . . ?
C102 C101 H10G 109.9 . . ?
O101 C101 H10H 109.9 . . ?
C102 C101 H10H 109.9 . . ?
H10G C101 H10H 108.3 . . ?
O102 C102 C101 109.3(3) . . ?
O102 C102 H10I 109.8 . . ?
C101 C102 H10I 109.8 . . ?
O102 C102 H10J 109.8 . . ?
C101 C102 H10J 109.8 . . ?
H10I C102 H10J 108.3 . . ?
C103 O102 C102 112.4(2) . . ?
C103 O102 K1 109.46(19) . . ?
C102 O102 K1 110.1(2) . . ?
O102 C103 C104 108.7(3) . . ?
O102 C103 H10K 110.0 . . ?
C104 C103 H10K 110.0 . . ?
O102 C103 H10L 110.0 . . ?
C104 C103 H10L 110.0 . . ?
H10K C103 H10L 108.3 . . ?
O103 C104 C103 109.1(3) . . ?
O103 C104 H10M 109.9 . . ?
C103 C104 H10M 109.9 . . ?
O103 C104 H10N 109.9 . . ?
C103 C104 H10N 109.9 . . ?
H10M C104 H10N 108.3 . . ?
C104 O103 C105 111.6(3) . . ?
C104 O103 K1 116.7(2) . . ?
C105 O103 K1 116.3(2) . . ?
C106 C105 O103 122.7(6) . . ?
O103 C105 C6A 103.2(5) . . ?
C106 C105 H10O 106.6 . . ?
O103 C105 H10O 106.6 . . ?
C6A C105 H10O 131.5 . . ?
C106 C105 H10P 106.6 . . ?
O103 C105 H10P 106.6 . . ?
C6A C105 H10P 100.1 . . ?
H10O C105 H10P 106.6 . . ?
C105 C106 O104 110.1(6) . . ?
C105 C106 H10Q 109.6 . . ?
O104 C106 H10Q 109.6 . . ?
C105 C106 H10R 109.6 . . ?
O104 C106 H10R 109.6 . . ?
H10Q C106 H10R 108.2 . . ?
C107 O104 C106 114.4(6) . . ?
C107 O104 K1 108.7(5) . . ?
C106 O104 K1 111.6(4) . . ?
O104 C107 C108 109.4(6) . . ?
O104 C107 H10S 109.8 . . ?
C108 C107 H10S 109.8 . . ?
O104 C107 H10T 109.8 . . ?
C108 C107 H10T 109.8 . . ?
H10S C107 H10T 108.2 . . ?
O4A C6A C105 114.2(7) . . ?
O4A C6A H6A1 108.7 . . ?
C105 C6A H6A1 108.7 . . ?
O4A C6A H6A2 108.7 . . ?
C105 C6A H6A2 108.7 . . ?
H6A1 C6A H6A2 107.6 . . ?
C7A O4A C6A 114.0(9) . . ?
C7A O4A K1 102.8(6) . . ?
C6A O4A K1 110.1(4) . . ?
C108 C7A O4A 113.9(10) . . ?
C108 C7A H7A1 108.8 . . ?
O4A C7A H7A1 108.8 . . ?
C108 C7A H7A2 108.8 . . ?
O4A C7A H7A2 108.8 . . ?
H7A1 C7A H7A2 107.7 . . ?
O105 C108 C7A 106.2(5) . . ?
O105 C108 C107 112.5(5) . . ?
O105 C108 H10U 109.1 . . ?
C7A C108 H10U 91.6 . . ?
C107 C108 H10U 109.1 . . ?
O105 C108 H10V 109.1 . . ?
C7A C108 H10V 130.6 . . ?
C107 C108 H10V 109.1 . . ?
H10U C108 H10V 107.8 . . ?
C108 O105 C109 113.1(2) . . ?
C108 O105 K1 126.74(19) . . ?
C109 O105 K1 119.45(19) . . ?
O105 C109 C110 108.4(2) . . ?
O105 C109 H10W 110.0 . . ?
C110 C109 H10W 110.0 . . ?
O105 C109 H10$ 110.0 . . ?
C110 C109 H10$ 110.0 . . ?
H10W C109 H10$ 108.4 . . ?
O106 C110 C109 109.2(3) . . ?
O106 C110 K1 57.19(14) . . ?
C109 C110 K1 88.23(17) . . ?
O106 C110 H11G 109.8 . . ?
C109 C110 H11G 109.8 . . ?
K1 C110 H11G 68.4 . . ?
O106 C110 H11H 109.8 . . ?
C109 C110 H11H 109.8 . . ?
K1 C110 H11H 161.2 . . ?
H11G C110 H11H 108.3 . . ?
C111 O106 C110 114.1(3) . . ?
C111 O106 K1 103.64(18) . . ?
C110 O106 K1 98.27(17) . . ?
O106 C111 C112 109.8(3) . . ?
O106 C111 K1 53.17(14) . . ?
C112 C111 K1 84.11(19) . . ?
O106 C111 H11I 109.7 . . ?
C112 C111 H11I 109.7 . . ?
K1 C111 H11I 161.9 . . ?
O106 C111 H11J 109.7 . . ?
C112 C111 H11J 109.7 . . ?
K1 C111 H11J 76.5 . . ?
H11I C111 H11J 108.2 . . ?
O101 C112 C111 108.3(3) . . ?
O101 C112 H11K 110.0 . . ?
C111 C112 H11K 110.0 . . ?
O101 C112 H11L 110.0 . . ?
C111 C112 H11L 110.0 . . ?
H11K C112 H11L 108.4 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        76.89
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.063
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pyridine, ether'
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1049374'
_audit_update_record             
;
2015-02-13 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 [K(18-crown-6)][P{(CO)2[N(Dipp)]2}2]
;
_contact_author_fax              '+44 1865 272690'
_chemical_name_common            .
_chemical_melting_point          .
_chemical_formula_moiety         'C12 H24 K O6, C52 H80 N4 O4 P'
_chemical_formula_sum            'C64 H92 K N4 O10 P'
_chemical_formula_weight         1147.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   13.2330(3)
_cell_length_b                   19.9093(4)
_cell_length_c                   13.5733(3)
_cell_angle_alpha                90
_cell_angle_beta                 115.271(3)
_cell_angle_gamma                90
_cell_volume                     3233.79(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6922
_cell_measurement_theta_min      3.5980
_cell_measurement_theta_max      75.8623

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_F_000             1236
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.412
_shelx_estimated_absorpt_T_min   0.908
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_T_min  0.98061
_exptl_absorpt_correction_T_max  1.00000
__exptl_absorpt_process_details  multi-scan

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_reflns_number            19203
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.601
_diffrn_reflns_theta_max         76.045
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11186
_reflns_number_gt                9838
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_max     0.987
_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, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0540P)²+0.6914P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     .
_atom_sites_solution_secondary   .
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.306(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11186
_refine_ls_number_parameters     760
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1168
_refine_ls_wR_factor_gt          0.1096
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.96307(6) 0.71644(4) 0.25402(6) 0.01821(16) Uani 1 1 d . . . . .
N1 N 1.1164(2) 0.73433(17) 0.3542(2) 0.0225(6) Uani 1 1 d . . . . .
N2 N 1.0394(2) 0.72892(16) 0.4739(2) 0.0214(6) Uani 1 1 d . . . . .
C1 C 1.1395(3) 0.72859(18) 0.4600(3) 0.0206(6) Uani 1 1 d . . . . .
C2 C 0.9392(3) 0.72182(18) 0.3823(2) 0.0202(6) Uani 1 1 d . . . . .
O1 O 1.23063(18) 0.72211(15) 0.53806(18) 0.0262(5) Uani 1 1 d . . . . .
O2 O 0.84921(18) 0.72155(16) 0.38633(19) 0.0290(6) Uani 1 1 d . . . . .
N3 N 0.8184(2) 0.81676(15) 0.1467(2) 0.0215(6) Uani 1 1 d . . . . .
N4 N 0.8071(2) 0.70337(14) 0.1556(2) 0.0190(6) Uani 1 1 d . . . . .
C3 C 0.9263(3) 0.80925(19) 0.2270(3) 0.0221(7) Uani 1 1 d . . . . .
C4 C 0.7584(3) 0.75783(18) 0.0963(3) 0.0196(6) Uani 1 1 d . . . . .
O3 O 0.9857(2) 0.85596(14) 0.2733(2) 0.0291(6) Uani 1 1 d . . . . .
O4 O 0.6751(2) 0.76138(14) 0.0084(2) 0.0268(5) Uani 1 1 d . . . . .
C5 C 1.1969(3) 0.7083(3) 0.3180(3) 0.0320(9) Uani 1 1 d . . . . .
C6 C 1.2510(3) 0.7529(3) 0.2776(4) 0.0479(13) Uani 1 1 d . . . . .
C7 C 1.3188(4) 0.7218(5) 0.2300(4) 0.0663(19) Uani 1 1 d . . . . .
H7 H 1.3560 0.7496 0.1990 0.080 Uiso 1 1 calc R U . . .
C8 C 1.3309(5) 0.6534(4) 0.2283(6) 0.0725(19) Uani 1 1 d . . . . .
H8 H 1.3762 0.6348 0.1966 0.087 Uiso 1 1 calc R U . . .
C9 C 1.2799(4) 0.6127(4) 0.2705(5) 0.0602(16) Uani 1 1 d . . . . .
H9 H 1.2906 0.5655 0.2697 0.072 Uiso 1 1 calc R U . . .
C10 C 1.2105(3) 0.6380(3) 0.3163(3) 0.0404(11) Uani 1 1 d . . . . .
C11 C 1.2377(4) 0.8275(3) 0.2852(4) 0.0570(16) Uani 1 1 d . . . . .
H11 H 1.1570 0.8364 0.2652 0.068 Uiso 1 1 calc R U . . .
C12 C 1.3054(5) 0.8539(4) 0.4035(5) 0.0705(19) Uani 1 1 d . . . . .
H12A H 1.2948 0.9026 0.4053 0.106 Uiso 1 1 calc R U . . .
H12B H 1.2791 0.8317 0.4526 0.106 Uiso 1 1 calc R U . . .
H12C H 1.3850 0.8442 0.4269 0.106 Uiso 1 1 calc R U . . .
C13 C 1.2696(6) 0.8679(5) 0.2060(7) 0.087(3) Uani 1 1 d . . . . .
H13A H 1.2593 0.9159 0.2146 0.131 Uiso 1 1 calc R U . . .
H13B H 1.3479 0.8592 0.2220 0.131 Uiso 1 1 calc R U . . .
H13C H 1.2217 0.8542 0.1311 0.131 Uiso 1 1 calc R U . . .
C14 C 1.1559(4) 0.5884(2) 0.3621(4) 0.0404(10) Uani 1 1 d . . . . .
H14 H 1.1042 0.6142 0.3844 0.048 Uiso 1 1 calc R U . . .
C15 C 1.2430(5) 0.5542(3) 0.4647(4) 0.0589(16) Uani 1 1 d . . . . .
H15A H 1.2055 0.5222 0.4929 0.088 Uiso 1 1 calc R U . . .
H15B H 1.2975 0.5303 0.4464 0.088 Uiso 1 1 calc R U . . .
H15C H 1.2815 0.5883 0.5203 0.088 Uiso 1 1 calc R U . . .
C16 C 1.0856(5) 0.5348(3) 0.2792(4) 0.0523(13) Uani 1 1 d . . . . .
H16A H 1.0525 0.5042 0.3139 0.078 Uiso 1 1 calc R U . . .
H16B H 1.0260 0.5568 0.2168 0.078 Uiso 1 1 calc R U . . .
H16C H 1.1336 0.5093 0.2542 0.078 Uiso 1 1 calc R U . . .
C17 C 1.0430(3) 0.7421(2) 0.5799(3) 0.0229(7) Uani 1 1 d . . . . .
C18 C 1.0434(3) 0.8093(2) 0.6108(3) 0.0281(8) Uani 1 1 d . . . . .
C19 C 1.0455(4) 0.8224(2) 0.7131(3) 0.0356(9) Uani 1 1 d . . . . .
H19 H 1.0446 0.8675 0.7356 0.043 Uiso 1 1 calc R U . . .
C20 C 1.0487(4) 0.7705(2) 0.7813(3) 0.0367(9) Uani 1 1 d . . . . .
H20 H 1.0496 0.7801 0.8502 0.044 Uiso 1 1 calc R U . . .
C21 C 1.0508(4) 0.7044(2) 0.7505(3) 0.0344(9) Uani 1 1 d . . . . .
H21 H 1.0543 0.6692 0.7991 0.041 Uiso 1 1 calc R U . . .
C22 C 1.0478(3) 0.6888(2) 0.6491(3) 0.0280(7) Uani 1 1 d . . . . .
C23 C 1.0442(4) 0.8666(2) 0.5374(3) 0.0361(9) Uani 1 1 d . . . . .
H23 H 1.0617 0.8467 0.4787 0.043 Uiso 1 1 calc R U . . .
C24 C 1.1364(5) 0.9178(3) 0.5988(5) 0.0574(14) Uani 1 1 d . . . . .
H24A H 1.2087 0.8948 0.6325 0.086 Uiso 1 1 calc R U . . .
H24B H 1.1388 0.9519 0.5477 0.086 Uiso 1 1 calc R U . . .
H24C H 1.1206 0.9395 0.6555 0.086 Uiso 1 1 calc R U . . .
C25 C 0.9315(5) 0.8969(3) 0.4836(5) 0.0570(13) Uani 1 1 d . . . . .
H25A H 0.9327 0.9338 0.4363 0.085 Uiso 1 1 calc R U . . .
H25B H 0.8777 0.8628 0.4397 0.085 Uiso 1 1 calc R U . . .
H25C H 0.9093 0.9142 0.5391 0.085 Uiso 1 1 calc R U . . .
C26 C 1.0524(4) 0.6155(2) 0.6186(3) 0.0332(9) Uani 1 1 d . . . . .
H26 H 1.0493 0.6139 0.5437 0.040 Uiso 1 1 calc R U . . .
C27 C 1.1616(5) 0.5835(3) 0.6976(5) 0.0568(14) Uani 1 1 d . . . . .
H27A H 1.2247 0.6092 0.6974 0.085 Uiso 1 1 calc R U . . .
H27B H 1.1650 0.5836 0.7712 0.085 Uiso 1 1 calc R U . . .
H27C H 1.1654 0.5372 0.6751 0.085 Uiso 1 1 calc R U . . .
C28 C 0.9542(6) 0.5761(4) 0.6184(7) 0.081(2) Uani 1 1 d . . . . .
H28A H 0.8843 0.5969 0.5674 0.121 Uiso 1 1 calc R U . . .
H28B H 0.9577 0.5297 0.5958 0.121 Uiso 1 1 calc R U . . .
H28C H 0.9573 0.5762 0.6918 0.121 Uiso 1 1 calc R U . . .
C29 C 0.7702(3) 0.88197(19) 0.1093(3) 0.0267(8) Uani 1 1 d . . . . .
C30 C 0.8108(4) 0.9209(2) 0.0480(3) 0.0348(9) Uani 1 1 d . . . . .
C31 C 0.7617(5) 0.9839(2) 0.0104(4) 0.0464(12) Uani 1 1 d . . . . .
H31 H 0.7888 1.0116 -0.0300 0.056 Uiso 1 1 calc R U . . .
C32 C 0.6746(5) 1.0055(3) 0.0320(4) 0.0535(14) Uani 1 1 d . . . . .
H32 H 0.6417 1.0481 0.0061 0.064 Uiso 1 1 calc R U . . .
C33 C 0.6343(4) 0.9661(3) 0.0905(4) 0.0460(11) Uani 1 1 d . . . . .
H33 H 0.5729 0.9817 0.1029 0.055 Uiso 1 1 calc R U . . .
C34 C 0.6815(3) 0.9032(2) 0.1326(3) 0.0330(9) Uani 1 1 d . . . . .
C35 C 0.9010(4) 0.8968(2) 0.0158(4) 0.0375(9) Uani 1 1 d . . . . .
H35 H 0.9329 0.8544 0.0570 0.045 Uiso 1 1 calc R U . . .
C36 C 0.9962(6) 0.9466(4) 0.0439(7) 0.078(2) Uani 1 1 d . . . . .
H36A H 1.0518 0.9284 0.0213 0.117 Uiso 1 1 calc R U . . .
H36B H 0.9670 0.9891 0.0059 0.117 Uiso 1 1 calc R U . . .
H36C H 1.0311 0.9545 0.1227 0.117 Uiso 1 1 calc R U . . .
C37 C 0.8499(5) 0.8798(3) -0.1052(4) 0.0560(14) Uani 1 1 d . . . . .
H37A H 0.9086 0.8642 -0.1256 0.084 Uiso 1 1 calc R U . . .
H37B H 0.7939 0.8443 -0.1203 0.084 Uiso 1 1 calc R U . . .
H37C H 0.8142 0.9199 -0.1477 0.084 Uiso 1 1 calc R U . . .
C38 C 0.6365(4) 0.8612(2) 0.1965(4) 0.0398(10) Uani 1 1 d . . . . .
H38 H 0.6853 0.8208 0.2254 0.048 Uiso 1 1 calc R U . . .
C39 C 0.6286(5) 0.8988(3) 0.2923(4) 0.0562(14) Uani 1 1 d . . . . .
H39A H 0.5987 0.8686 0.3304 0.084 Uiso 1 1 calc R U . . .
H39B H 0.7032 0.9142 0.3430 0.084 Uiso 1 1 calc R U . . .
H39C H 0.5789 0.9377 0.2644 0.084 Uiso 1 1 calc R U . . .
C40 C 0.5178(5) 0.8380(4) 0.1203(6) 0.0686(18) Uani 1 1 d . . . . .
H40A H 0.4876 0.8105 0.1613 0.103 Uiso 1 1 calc R U . . .
H40B H 0.4699 0.8773 0.0904 0.103 Uiso 1 1 calc R U . . .
H40C H 0.5203 0.8114 0.0607 0.103 Uiso 1 1 calc R U . . .
C41 C 0.7822(3) 0.63929(18) 0.1009(3) 0.0207(6) Uani 1 1 d . . . . .
C42 C 0.8207(3) 0.62471(19) 0.0218(3) 0.0239(7) Uani 1 1 d . . . . .
C43 C 0.8008(3) 0.5601(2) -0.0243(3) 0.0305(8) Uani 1 1 d . . . . .
H43 H 0.8256 0.5493 -0.0785 0.037 Uiso 1 1 calc R U . . .
C44 C 0.7456(4) 0.5119(2) 0.0081(4) 0.0360(9) Uani 1 1 d . . . . .
H44 H 0.7337 0.4682 -0.0229 0.043 Uiso 1 1 calc R U . . .
C45 C 0.7079(4) 0.5278(2) 0.0857(3) 0.0328(9) Uani 1 1 d . . . . .
H45 H 0.6705 0.4944 0.1077 0.039 Uiso 1 1 calc R U . . .
C46 C 0.7233(3) 0.5913(2) 0.1323(3) 0.0264(7) Uani 1 1 d . . . . .
C47 C 0.8798(3) 0.6760(2) -0.0191(3) 0.0275(8) Uani 1 1 d . . . . .
H47 H 0.8876 0.7185 0.0227 0.033 Uiso 1 1 calc R U . . .
C48 C 0.9979(4) 0.6527(3) 0.0011(4) 0.0368(9) Uani 1 1 d . . . . .
H48A H 1.0330 0.6868 -0.0261 0.055 Uiso 1 1 calc R U . . .
H48B H 1.0429 0.6463 0.0794 0.055 Uiso 1 1 calc R U . . .
H48C H 0.9930 0.6102 -0.0371 0.055 Uiso 1 1 calc R U . . .
C49 C 0.8108(4) 0.6917(3) -0.1396(3) 0.0402(10) Uani 1 1 d . . . . .
H49A H 0.8506 0.7246 -0.1637 0.060 Uiso 1 1 calc R U . . .
H49B H 0.7993 0.6504 -0.1823 0.060 Uiso 1 1 calc R U . . .
H49C H 0.7382 0.7101 -0.1501 0.060 Uiso 1 1 calc R U . . .
C50 C 0.6757(4) 0.6101(2) 0.2120(3) 0.0360(9) Uani 1 1 d D . . . .
H50 H 0.7344 0.6355 0.2733 0.043 Uiso 1 1 calc R U . A 1
C51 C 0.6351(5) 0.5547(3) 0.2603(5) 0.0411(15) Uani 0.744(8) 1 d . . P B 1
H51A H 0.6066 0.5737 0.3101 0.062 Uiso 0.744(8) 1 calc R U P B 1
H51B H 0.5751 0.5301 0.2019 0.062 Uiso 0.744(8) 1 calc R U P B 1
H51C H 0.6969 0.5239 0.3004 0.062 Uiso 0.744(8) 1 calc R U P B 1
C52 C 0.5700(4) 0.6600(3) 0.1511(4) 0.0309(13) Uani 0.744(8) 1 d . . P B 1
H52A H 0.5926 0.6974 0.1180 0.046 Uiso 0.744(8) 1 calc R U P B 1
H52B H 0.5089 0.6352 0.0943 0.046 Uiso 0.744(8) 1 calc R U P B 1
H52C H 0.5448 0.6776 0.2043 0.046 Uiso 0.744(8) 1 calc R U P B 1
C51A C 0.747(2) 0.5543(10) 0.3122(14) 0.051(6) Uani 0.256(8) 1 d D . P B 2
H51D H 0.8269 0.5648 0.3431 0.076 Uiso 0.256(8) 1 calc R U P B 2
H51E H 0.7205 0.5571 0.3694 0.076 Uiso 0.256(8) 1 calc R U P B 2
H51F H 0.7346 0.5088 0.2818 0.076 Uiso 0.256(8) 1 calc R U P B 2
C52A C 0.5633(13) 0.5902(11) 0.1742(14) 0.045(5) Uani 0.256(8) 1 d D . P B 2
H52D H 0.5351 0.6031 0.2276 0.068 Uiso 0.256(8) 1 calc R U P B 2
H52E H 0.5187 0.6123 0.1045 0.068 Uiso 0.256(8) 1 calc R U P B 2
H52F H 0.5579 0.5414 0.1642 0.068 Uiso 0.256(8) 1 calc R U P B 2
K101 K 0.45735(6) 0.73395(4) 0.60563(6) 0.02904(17) Uani 1 1 d . . . . .
O101 O 0.6195(4) 0.7955(2) 0.5332(4) 0.0590(10) Uani 1 1 d . . . . .
O102 O 0.5735(3) 0.85875(16) 0.6907(3) 0.0379(7) Uani 1 1 d . . . . .
O103 O 0.3948(2) 0.81877(16) 0.7348(2) 0.0327(6) Uani 1 1 d . . . . .
O104 O 0.4291(2) 0.67848(15) 0.7810(2) 0.0314(6) Uani 1 1 d . . . . .
O105 O 0.5574(3) 0.60901(16) 0.6945(3) 0.0391(7) Uani 1 1 d . . . . .
O106 O 0.5789(4) 0.6544(2) 0.5098(4) 0.0660(11) Uani 1 1 d . . . . .
C101 C 0.6875(4) 0.8476(3) 0.5980(5) 0.0574(15) Uani 1 1 d . . . . .
H10A H 0.7227 0.8721 0.5573 0.069 Uiso 1 1 calc R U . . .
H10B H 0.7474 0.8287 0.6649 0.069 Uiso 1 1 calc R U . . .
C102 C 0.6173(4) 0.8935(3) 0.6267(4) 0.0456(11) Uani 1 1 d . . . . .
H10C H 0.6624 0.9323 0.6680 0.055 Uiso 1 1 calc R U . . .
H10D H 0.5554 0.9107 0.5596 0.055 Uiso 1 1 calc R U . . .
C103 C 0.5211(4) 0.9030(2) 0.7373(4) 0.0415(10) Uani 1 1 d . . . . .
H10E H 0.4578 0.9264 0.6790 0.050 Uiso 1 1 calc R U . . .
H10F H 0.5752 0.9372 0.7828 0.050 Uiso 1 1 calc R U . . .
C104 C 0.4799(3) 0.8624(2) 0.8060(3) 0.0354(9) Uani 1 1 d . . . . .
H10G H 0.5419 0.8359 0.8605 0.042 Uiso 1 1 calc R U . . .
H10H H 0.4495 0.8923 0.8450 0.042 Uiso 1 1 calc R U . . .
C105 C 0.3405(3) 0.7808(2) 0.7868(3) 0.0345(9) Uani 1 1 d . . . . .
H10I H 0.2692 0.7631 0.7306 0.041 Uiso 1 1 calc R U . . .
H10J H 0.3223 0.8108 0.8351 0.041 Uiso 1 1 calc R U . . .
C106 C 0.4091(3) 0.7231(3) 0.8528(3) 0.0341(9) Uani 1 1 d . . . . .
H10K H 0.4809 0.7397 0.9094 0.041 Uiso 1 1 calc R U . . .
H10L H 0.3687 0.6994 0.8892 0.041 Uiso 1 1 calc R U . . .
C107 C 0.5017(3) 0.6249(2) 0.8385(3) 0.0353(9) Uani 1 1 d . . . . .
H10M H 0.4727 0.6020 0.8859 0.042 Uiso 1 1 calc R U . . .
H10N H 0.5771 0.6427 0.8849 0.042 Uiso 1 1 calc R U . . .
C108 C 0.5080(4) 0.5764(2) 0.7572(4) 0.0386(10) Uani 1 1 d . . . . .
H10O H 0.5536 0.5370 0.7954 0.046 Uiso 1 1 calc R U . . .
H10P H 0.4321 0.5604 0.7086 0.046 Uiso 1 1 calc R U . . .
C109 C 0.5751(4) 0.5641(3) 0.6227(4) 0.0488(12) Uani 1 1 d . . . . .
H10Q H 0.5025 0.5495 0.5649 0.059 Uiso 1 1 calc R U . . .
H10R H 0.6157 0.5239 0.6631 0.059 Uiso 1 1 calc R U . . .
C110 C 0.6426(5) 0.5994(4) 0.5725(5) 0.0581(15) Uani 1 1 d . . . . .
H11A H 0.7139 0.6158 0.6303 0.070 Uiso 1 1 calc R U . . .
H11B H 0.6599 0.5680 0.5253 0.070 Uiso 1 1 calc R U . . .
C111 C 0.6214(8) 0.6942(5) 0.4501(7) 0.053(2) Uani 0.744(8) 1 d . . P B 3
H11C H 0.5583 0.7136 0.3863 0.063 Uiso 0.744(8) 1 calc R U P B 3
H11D H 0.6647 0.6653 0.4226 0.063 Uiso 0.744(8) 1 calc R U P B 3
C112 C 0.6943(6) 0.7494(4) 0.5161(6) 0.0492(19) Uani 0.744(8) 1 d . . P B 3
H11E H 0.7510 0.7322 0.5864 0.059 Uiso 0.744(8) 1 calc R U P B 3
H11F H 0.7331 0.7715 0.4765 0.059 Uiso 0.744(8) 1 calc R U P B 3
C11A C 0.6873(14) 0.6869(9) 0.5093(15) 0.027(4) Uani 0.256(8) 1 d . . P B 4
H11G H 0.7430 0.6994 0.5833 0.032 Uiso 0.256(8) 1 calc R U P B 4
H11H H 0.7224 0.6579 0.4734 0.032 Uiso 0.256(8) 1 calc R U P B 4
C12A C 0.6285(14) 0.7482(10) 0.4402(13) 0.034(4) Uani 0.256(8) 1 d . . P B 4
H12D H 0.5539 0.7365 0.3827 0.041 Uiso 0.256(8) 1 calc R U P B 4
H12E H 0.6739 0.7694 0.4067 0.041 Uiso 0.256(8) 1 calc R U P B 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C2 1.901(3) . ?
P1 C3 1.906(4) . ?
P1 N1 1.933(3) . ?
P1 N4 1.939(3) . ?
N1 C1 1.340(4) . ?
N1 C5 1.445(4) . ?
N2 C2 1.385(4) . ?
N2 C1 1.416(4) . ?
N2 C17 1.443(4) . ?
C1 O1 1.226(4) . ?
C2 O2 1.215(4) . ?
O1 K101 2.747(2) 1_655 ?
N3 C3 1.386(4) . ?
N3 C4 1.419(4) . ?
N3 C29 1.440(5) . ?
N4 C4 1.340(4) . ?
N4 C41 1.441(4) . ?
C3 O3 1.206(5) . ?
C4 O4 1.233(4) . ?
C5 C6 1.392(6) . ?
C5 C10 1.413(7) . ?
C6 C7 1.449(8) . ?
C6 C11 1.504(9) . ?
C7 C8 1.373(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.331(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.404(6) . ?
C9 H9 0.9500 . ?
C10 C14 1.506(8) . ?
C11 C13 1.537(7) . ?
C11 C12 1.558(9) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.536(6) . ?
C14 C16 1.542(7) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C22 1.401(5) . ?
C17 C18 1.402(6) . ?
C18 C19 1.402(6) . ?
C18 C23 1.516(6) . ?
C19 C20 1.375(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.384(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.396(6) . ?
C21 H21 0.9500 . ?
C22 C26 1.524(6) . ?
C23 C25 1.482(7) . ?
C23 C24 1.535(7) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.516(8) . ?
C26 C27 1.524(6) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.401(6) . ?
C29 C34 1.405(6) . ?
C30 C31 1.403(6) . ?
C30 C35 1.514(7) . ?
C31 C32 1.374(9) . ?
C31 H31 0.9500 . ?
C32 C33 1.376(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.407(6) . ?
C33 H33 0.9500 . ?
C34 C38 1.499(7) . ?
C35 C36 1.518(7) . ?
C35 C37 1.523(7) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C40 1.537(7) . ?
C38 C39 1.543(7) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.403(5) . ?
C41 C46 1.409(5) . ?
C42 C43 1.405(5) . ?
C42 C47 1.527(5) . ?
C43 C44 1.387(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.380(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.390(6) . ?
C45 H45 0.9500 . ?
C46 C50 1.513(6) . ?
C47 C49 1.527(5) . ?
C47 C48 1.538(6) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C52A 1.407(16) . ?
C50 C51 1.495(7) . ?
C50 C52 1.625(7) . ?
C50 C51A 1.696(15) . ?
C50 H50 1.0000 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C51A H51D 0.9800 . ?
C51A H51E 0.9800 . ?
C51A H51F 0.9800 . ?
C52A H52D 0.9800 . ?
C52A H52E 0.9800 . ?
C52A H52F 0.9800 . ?
K101 O1 2.747(2) 1_455 ?
K101 O104 2.790(3) . ?
K101 O103 2.802(3) . ?
K101 O105 2.834(3) . ?
K101 O102 2.890(3) . ?
K101 O106 2.927(4) . ?
K101 O101 2.979(4) . ?
O101 C101 1.407(8) . ?
O101 C112 1.441(7) . ?
O101 C12A 1.620(18) . ?
O102 C102 1.414(6) . ?
O102 C103 1.425(6) . ?
O103 C105 1.421(5) . ?
O103 C104 1.424(5) . ?
O104 C106 1.424(5) . ?
O104 C107 1.425(5) . ?
O105 C109 1.414(6) . ?
O105 C108 1.431(6) . ?
O106 C111 1.411(10) . ?
O106 C110 1.422(8) . ?
O106 C11A 1.576(15) . ?
C101 C102 1.470(8) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C103 C104 1.501(7) . ?
C103 H10E 0.9900 . ?
C103 H10F 0.9900 . ?
C104 H10G 0.9900 . ?
C104 H10H 0.9900 . ?
C105 C106 1.501(6) . ?
C105 H10I 0.9900 . ?
C105 H10J 0.9900 . ?
C106 H10K 0.9900 . ?
C106 H10L 0.9900 . ?
C107 C108 1.494(7) . ?
C107 H10M 0.9900 . ?
C107 H10N 0.9900 . ?
C108 H10O 0.9900 . ?
C108 H10P 0.9900 . ?
C109 C110 1.508(9) . ?
C109 H10Q 0.9900 . ?
C109 H10R 0.9900 . ?
C110 H11A 0.9900 . ?
C110 H11B 0.9900 . ?
C111 C112 1.484(12) . ?
C111 H11C 0.9900 . ?
C111 H11D 0.9900 . ?
C112 H11E 0.9900 . ?
C112 H11F 0.9900 . ?
C11A C12A 1.53(2) . ?
C11A H11G 0.9900 . ?
C11A H11H 0.9900 . ?
C12A H12D 0.9900 . ?
C12A H12E 0.9900 . ?

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 P1 C3 89.62(15) . . ?
C2 P1 N1 83.15(13) . . ?
C3 P1 N1 93.54(15) . . ?
C2 P1 N4 95.42(13) . . ?
C3 P1 N4 83.59(14) . . ?
N1 P1 N4 176.81(14) . . ?
C1 N1 C5 118.0(3) . . ?
C1 N1 P1 115.4(2) . . ?
C5 N1 P1 113.6(2) . . ?
C2 N2 C1 118.1(3) . . ?
C2 N2 C17 121.7(3) . . ?
C1 N2 C17 119.9(3) . . ?
O1 C1 N1 128.7(3) . . ?
O1 C1 N2 121.1(3) . . ?
N1 C1 N2 110.2(3) . . ?
O2 C2 N2 122.8(3) . . ?
O2 C2 P1 126.2(2) . . ?
N2 C2 P1 111.0(2) . . ?
C1 O1 K101 144.2(2) . 1_655 ?
C3 N3 C4 117.8(3) . . ?
C3 N3 C29 121.8(3) . . ?
C4 N3 C29 120.2(3) . . ?
C4 N4 C41 117.5(3) . . ?
C4 N4 P1 113.8(2) . . ?
C41 N4 P1 114.6(2) . . ?
O3 C3 N3 123.3(3) . . ?
O3 C3 P1 126.2(3) . . ?
N3 C3 P1 110.4(3) . . ?
O4 C4 N4 129.0(3) . . ?
O4 C4 N3 120.3(3) . . ?
N4 C4 N3 110.6(3) . . ?
C6 C5 C10 122.4(4) . . ?
C6 C5 N1 118.9(4) . . ?
C10 C5 N1 118.5(4) . . ?
C5 C6 C7 115.0(6) . . ?
C5 C6 C11 120.5(4) . . ?
C7 C6 C11 124.5(5) . . ?
C8 C7 C6 122.1(6) . . ?
C8 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C9 C8 C7 120.8(6) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 121.3(7) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C9 C10 C5 118.4(5) . . ?
C9 C10 C14 117.8(5) . . ?
C5 C10 C14 123.8(4) . . ?
C6 C11 C13 113.1(6) . . ?
C6 C11 C12 111.8(4) . . ?
C13 C11 C12 109.6(5) . . ?
C6 C11 H11 107.3 . . ?
C13 C11 H11 107.3 . . ?
C12 C11 H11 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 C15 111.0(4) . . ?
C10 C14 C16 113.5(4) . . ?
C15 C14 C16 109.9(4) . . ?
C10 C14 H14 107.4 . . ?
C15 C14 H14 107.4 . . ?
C16 C14 H14 107.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 122.0(3) . . ?
C22 C17 N2 120.2(3) . . ?
C18 C17 N2 117.8(3) . . ?
C17 C18 C19 118.0(4) . . ?
C17 C18 C23 121.4(3) . . ?
C19 C18 C23 120.6(4) . . ?
C20 C19 C18 120.6(4) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C20 C21 120.6(4) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C20 C21 C22 121.0(4) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C21 C22 C17 117.7(4) . . ?
C21 C22 C26 119.6(4) . . ?
C17 C22 C26 122.7(3) . . ?
C25 C23 C18 110.0(4) . . ?
C25 C23 C24 113.3(4) . . ?
C18 C23 C24 111.7(4) . . ?
C25 C23 H23 107.2 . . ?
C18 C23 H23 107.2 . . ?
C24 C23 H23 107.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C27 109.8(5) . . ?
C28 C26 C22 111.3(4) . . ?
C27 C26 C22 110.2(4) . . ?
C28 C26 H26 108.5 . . ?
C27 C26 H26 108.5 . . ?
C22 C26 H26 108.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 122.5(4) . . ?
C30 C29 N3 118.9(4) . . ?
C34 C29 N3 118.6(4) . . ?
C29 C30 C31 118.3(5) . . ?
C29 C30 C35 123.0(4) . . ?
C31 C30 C35 118.6(4) . . ?
C32 C31 C30 120.2(5) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 120.7(4) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C32 C33 C34 121.8(5) . . ?
C32 C33 H33 119.1 . . ?
C34 C33 H33 119.1 . . ?
C29 C34 C33 116.4(4) . . ?
C29 C34 C38 122.7(4) . . ?
C33 C34 C38 120.9(4) . . ?
C30 C35 C36 113.0(5) . . ?
C30 C35 C37 109.8(4) . . ?
C36 C35 C37 110.8(5) . . ?
C30 C35 H35 107.6 . . ?
C36 C35 H35 107.6 . . ?
C37 C35 H35 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 C40 108.8(4) . . ?
C34 C38 C39 113.8(4) . . ?
C40 C38 C39 107.2(4) . . ?
C34 C38 H38 109.0 . . ?
C40 C38 H38 109.0 . . ?
C39 C38 H38 109.0 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C46 121.3(3) . . ?
C42 C41 N4 119.9(3) . . ?
C46 C41 N4 118.7(3) . . ?
C41 C42 C43 118.0(3) . . ?
C41 C42 C47 123.4(3) . . ?
C43 C42 C47 118.6(3) . . ?
C44 C43 C42 121.1(4) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C45 C44 C43 119.7(4) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C44 C45 C46 121.7(4) . . ?
C44 C45 H45 119.2 . . ?
C46 C45 H45 119.2 . . ?
C45 C46 C41 118.2(4) . . ?
C45 C46 C50 121.8(4) . . ?
C41 C46 C50 120.0(3) . . ?
C42 C47 C49 111.1(3) . . ?
C42 C47 C48 111.9(3) . . ?
C49 C47 C48 110.5(3) . . ?
C42 C47 H47 107.7 . . ?
C49 C47 H47 107.7 . . ?
C48 C47 H47 107.7 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C52A C50 C46 111.5(8) . . ?
C51 C50 C46 117.9(4) . . ?
C51 C50 C52 106.4(4) . . ?
C46 C50 C52 108.5(3) . . ?
C52A C50 C51A 104.3(13) . . ?
C46 C50 C51A 98.7(7) . . ?
C51 C50 H50 107.9 . . ?
C46 C50 H50 107.9 . . ?
C52 C50 H50 107.9 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C51A H51D 109.5 . . ?
C50 C51A H51E 109.5 . . ?
H51D C51A H51E 109.5 . . ?
C50 C51A H51F 109.5 . . ?
H51D C51A H51F 109.5 . . ?
H51E C51A H51F 109.5 . . ?
C50 C52A H52D 109.5 . . ?
C50 C52A H52E 109.5 . . ?
H52D C52A H52E 109.5 . . ?
C50 C52A H52F 109.5 . . ?
H52D C52A H52F 109.5 . . ?
H52E C52A H52F 109.5 . . ?
O1 K101 O104 74.09(8) 1_455 . ?
O1 K101 O103 71.84(8) 1_455 . ?
O104 K101 O103 61.42(9) . . ?
O1 K101 O105 108.17(9) 1_455 . ?
O104 K101 O105 59.86(9) . . ?
O103 K101 O105 118.14(9) . . ?
O1 K101 O102 121.72(9) 1_455 . ?
O104 K101 O102 103.97(9) . . ?
O103 K101 O102 58.71(9) . . ?
O105 K101 O102 120.82(9) . . ?
O1 K101 O106 122.27(12) 1_455 . ?
O104 K101 O106 117.65(12) . . ?
O103 K101 O106 165.71(12) . . ?
O105 K101 O106 57.93(12) . . ?
O102 K101 O106 110.07(12) . . ?
O1 K101 O101 139.71(11) 1_455 . ?
O104 K101 O101 145.31(11) . . ?
O103 K101 O101 113.91(10) . . ?
O105 K101 O101 103.33(11) . . ?
O102 K101 O101 56.16(10) . . ?
O106 K101 O101 57.75(12) . . ?
C101 O101 C112 105.7(5) . . ?
C101 O101 C12A 132.5(7) . . ?
C101 O101 K101 117.1(3) . . ?
C112 O101 K101 115.6(4) . . ?
C12A O101 K101 108.7(7) . . ?
C102 O102 C103 112.0(4) . . ?
C102 O102 K101 117.6(3) . . ?
C103 O102 K101 115.6(3) . . ?
C105 O103 C104 114.2(3) . . ?
C105 O103 K101 109.7(2) . . ?
C104 O103 K101 115.6(2) . . ?
C106 O104 C107 111.8(3) . . ?
C106 O104 K101 117.9(2) . . ?
C107 O104 K101 117.3(2) . . ?
C109 O105 C108 112.1(4) . . ?
C109 O105 K101 116.5(3) . . ?
C108 O105 K101 113.8(3) . . ?
C111 O106 C110 119.7(6) . . ?
C110 O106 C11A 90.6(8) . . ?
C111 O106 K101 112.4(4) . . ?
C110 O106 K101 116.7(3) . . ?
C11A O106 K101 117.0(6) . . ?
O101 C101 C102 108.4(4) . . ?
O101 C101 H10A 110.0 . . ?
C102 C101 H10A 110.0 . . ?
O101 C101 H10B 110.0 . . ?
C102 C101 H10B 110.0 . . ?
H10A C101 H10B 108.4 . . ?
O102 C102 C101 109.2(4) . . ?
O102 C102 H10C 109.8 . . ?
C101 C102 H10C 109.8 . . ?
O102 C102 H10D 109.8 . . ?
C101 C102 H10D 109.8 . . ?
H10C C102 H10D 108.3 . . ?
O102 C103 C104 108.5(4) . . ?
O102 C103 H10E 110.0 . . ?
C104 C103 H10E 110.0 . . ?
O102 C103 H10F 110.0 . . ?
C104 C103 H10F 110.0 . . ?
H10E C103 H10F 108.4 . . ?
O103 C104 C103 107.4(3) . . ?
O103 C104 H10G 110.2 . . ?
C103 C104 H10G 110.2 . . ?
O103 C104 H10H 110.2 . . ?
C103 C104 H10H 110.2 . . ?
H10G C104 H10H 108.5 . . ?
O103 C105 C106 113.4(3) . . ?
O103 C105 H10I 108.9 . . ?
C106 C105 H10I 108.9 . . ?
O103 C105 H10J 108.9 . . ?
C106 C105 H10J 108.9 . . ?
H10I C105 H10J 107.7 . . ?
O104 C106 C105 108.1(3) . . ?
O104 C106 H10K 110.1 . . ?
C105 C106 H10K 110.1 . . ?
O104 C106 H10L 110.1 . . ?
C105 C106 H10L 110.1 . . ?
H10K C106 H10L 108.4 . . ?
O104 C107 C108 108.5(3) . . ?
O104 C107 H10M 110.0 . . ?
C108 C107 H10M 110.0 . . ?
O104 C107 H10N 110.0 . . ?
C108 C107 H10N 110.0 . . ?
H10M C107 H10N 108.4 . . ?
O105 C108 C107 109.2(4) . . ?
O105 C108 H10O 109.8 . . ?
C107 C108 H10O 109.8 . . ?
O105 C108 H10P 109.8 . . ?
C107 C108 H10P 109.8 . . ?
H10O C108 H10P 108.3 . . ?
O105 C109 C110 108.8(4) . . ?
O105 C109 H10Q 109.9 . . ?
C110 C109 H10Q 109.9 . . ?
O105 C109 H10R 109.9 . . ?
C110 C109 H10R 109.9 . . ?
H10Q C109 H10R 108.3 . . ?
O106 C110 C109 108.4(4) . . ?
O106 C110 H11A 110.0 . . ?
C109 C110 H11A 110.0 . . ?
O106 C110 H11B 110.0 . . ?
C109 C110 H11B 110.0 . . ?
H11A C110 H11B 108.4 . . ?
O106 C111 C112 112.6(6) . . ?
O106 C111 H11C 109.1 . . ?
C112 C111 H11C 109.1 . . ?
O106 C111 H11D 109.1 . . ?
C112 C111 H11D 109.1 . . ?
H11C C111 H11D 107.8 . . ?
O101 C112 C111 104.8(6) . . ?
O101 C112 H11E 110.8 . . ?
C111 C112 H11E 110.8 . . ?
O101 C112 H11F 110.8 . . ?
C111 C112 H11F 110.8 . . ?
H11E C112 H11F 108.9 . . ?
C12A C11A O106 96.0(12) . . ?
C12A C11A H11G 112.6 . . ?
O106 C11A H11G 112.6 . . ?
C12A C11A H11H 112.6 . . ?
O106 C11A H11H 112.6 . . ?
H11G C11A H11H 110.1 . . ?
C11A C12A O101 100.0(11) . . ?
C11A C12A H12D 111.8 . . ?
O101 C12A H12D 111.8 . . ?
C11A C12A H12E 111.8 . . ?
O101 C12A H12E 111.8 . . ?
H12D C12A H12E 109.5 . . ?

_refine_diff_density_max         0.712
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.047

_shelxl_version_number           2014-3


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pyridine, ether'
