# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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_alsn37
_database_code_depnum_ccdc_archive 'CCDC 1032118'
_audit_update_record             
;
2014-12-13 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_audit_creation_date             2014-11-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H55 N2 Np O7 P5'
_chemical_formula_sum            'C66 H55 N2 Np O7 P5'
_chemical_formula_weight         1379.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         Np1O6P4n2C48H40
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'
Np Np -11.4937 4.1493 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   13.61157(19)
_cell_length_b                   16.5891(2)
_cell_length_c                   26.4952(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.6657(13)
_cell_angle_gamma                90
_cell_volume                     5980.21(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    32360
_cell_measurement_temperature    150.03(18)
_cell_measurement_theta_max      28.5360
_cell_measurement_theta_min      3.2960
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51286
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.045
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -11.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454   77.0000   60.0000 104

#__ type_ start__ end____ width___ exp.time_
  2 omega   -3.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454   57.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega   -1.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454  -57.0000 -150.0000 41

#__ type_ start__ end____ width___ exp.time_
  4 omega  -64.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000  120.0000 62

#__ type_ start__ end____ width___ exp.time_
  5 omega  -93.00    8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000 -150.0000 101

#__ type_ start__ end____ width___ exp.time_
  6 omega  -87.00  -62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  178.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
  7 omega  -29.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   37.0000  -30.0000 58

#__ type_ start__ end____ width___ exp.time_
  8 omega  -39.00  -10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   37.0000 -150.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0193922000
_diffrn_orient_matrix_UB_12      -0.0286709000
_diffrn_orient_matrix_UB_13      0.0174704000
_diffrn_orient_matrix_UB_21      -0.0482609000
_diffrn_orient_matrix_UB_22      -0.0090203000
_diffrn_orient_matrix_UB_23      0.0077048000
_diffrn_orient_matrix_UB_31      -0.0039458000
_diffrn_orient_matrix_UB_32      -0.0304202000
_diffrn_orient_matrix_UB_33      -0.0187533000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11200
_reflns_number_total             12137
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.884
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         12137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0231
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0172P)²+5.8268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0523
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Np1 Np 0.52705(2) 0.70031(2) 0.23446(2) 0.01221(3) Uani 1 1 d . . . . .
C1 C 0.64827(18) 0.94597(15) 0.26586(9) 0.0237(5) Uani 1 1 d . . . . .
C2 C 0.6742(2) 1.01861(19) 0.24383(13) 0.0464(8) Uani 1 1 d . . . . .
H2 H 0.7340 1.0231 0.2264 0.056 Uiso 1 1 calc R . . . .
C3 C 0.6124(3) 1.0845(2) 0.24744(17) 0.0691(12) Uani 1 1 d . . . . .
H3 H 0.6303 1.1345 0.2328 0.083 Uiso 1 1 calc R . . . .
C4 C 0.5253(3) 1.0781(2) 0.27195(15) 0.0594(10) Uani 1 1 d . . . . .
H4 H 0.4826 1.1233 0.2736 0.071 Uiso 1 1 calc R . . . .
C5 C 0.4996(2) 1.00714(19) 0.29403(11) 0.0413(7) Uani 1 1 d . . . . .
H5 H 0.4396 1.0033 0.3113 0.050 Uiso 1 1 calc R . . . .
C6 C 0.56071(19) 0.94106(17) 0.29133(10) 0.0303(6) Uani 1 1 d . . . . .
H6 H 0.5428 0.8919 0.3070 0.036 Uiso 1 1 calc R . . . .
C7 C 0.82015(16) 0.87374(14) 0.22046(9) 0.0199(5) Uani 1 1 d . . . . .
C8 C 0.81475(19) 0.82943(18) 0.17626(10) 0.0303(6) Uani 1 1 d . . . . .
H8 H 0.7631 0.7916 0.1708 0.036 Uiso 1 1 calc R . . . .
C9 C 0.8850(2) 0.8402(2) 0.13986(11) 0.0414(8) Uani 1 1 d . . . . .
H9 H 0.8814 0.8101 0.1094 0.050 Uiso 1 1 calc R . . . .
C10 C 0.9603(2) 0.89513(19) 0.14816(11) 0.0389(7) Uani 1 1 d . . . . .
H10 H 1.0085 0.9024 0.1233 0.047 Uiso 1 1 calc R . . . .
C11 C 0.96581(19) 0.93936(17) 0.19210(11) 0.0327(6) Uani 1 1 d . . . . .
H11 H 1.0173 0.9774 0.1973 0.039 Uiso 1 1 calc R . . . .
C12 C 0.89674(18) 0.92858(15) 0.22855(10) 0.0267(6) Uani 1 1 d . . . . .
H12 H 0.9013 0.9584 0.2591 0.032 Uiso 1 1 calc R . . . .
C13 C 0.78142(17) 0.85193(16) 0.32737(9) 0.0232(5) Uani 1 1 d . . . . .
C14 C 0.8159(2) 0.92050(19) 0.35282(11) 0.0360(7) Uani 1 1 d . . . . .
H14 H 0.8084 0.9722 0.3377 0.043 Uiso 1 1 calc R . . . .
C15 C 0.8608(2) 0.9129(2) 0.40007(12) 0.0475(8) Uani 1 1 d . . . . .
H15 H 0.8853 0.9594 0.4171 0.057 Uiso 1 1 calc R . . . .
C16 C 0.8703(2) 0.8385(2) 0.42257(11) 0.0443(8) Uani 1 1 d . . . . .
H16 H 0.9018 0.8338 0.4549 0.053 Uiso 1 1 calc R . . . .
C17 C 0.8342(2) 0.7706(2) 0.39829(11) 0.0368(7) Uani 1 1 d . . . . .
H17 H 0.8396 0.7195 0.4143 0.044 Uiso 1 1 calc R . . . .
C18 C 0.79011(18) 0.77708(17) 0.35046(10) 0.0269(6) Uani 1 1 d . . . . .
H18 H 0.7659 0.7303 0.3336 0.032 Uiso 1 1 calc R . . . .
C19 C 0.52403(19) 0.84744(17) 0.08961(10) 0.0291(6) Uani 1 1 d . . . . .
C20 C 0.4686(2) 0.8670(2) 0.04635(11) 0.0393(7) Uani 1 1 d . . . . .
H20 H 0.4538 0.8267 0.0218 0.047 Uiso 1 1 calc R . . . .
C21 C 0.4346(2) 0.9452(2) 0.03896(15) 0.0546(10) Uani 1 1 d . . . . .
H21 H 0.3972 0.9585 0.0093 0.066 Uiso 1 1 calc R . . . .
C22 C 0.4552(3) 1.0033(2) 0.07458(16) 0.0615(11) Uani 1 1 d . . . . .
H22 H 0.4317 1.0567 0.0695 0.074 Uiso 1 1 calc R . . . .
C23 C 0.5091(3) 0.9849(2) 0.11725(15) 0.0585(10) Uani 1 1 d . . . . .
H23 H 0.5229 1.0256 0.1417 0.070 Uiso 1 1 calc R . . . .
C24 C 0.5441(2) 0.90710(19) 0.12528(12) 0.0427(7) Uani 1 1 d . . . . .
H24 H 0.5816 0.8947 0.1551 0.051 Uiso 1 1 calc R . . . .
C25 C 0.67632(18) 0.73068(17) 0.06737(10) 0.0283(6) Uani 1 1 d . . . . .
C26 C 0.7378(2) 0.66813(19) 0.08334(12) 0.0402(7) Uani 1 1 d . . . . .
H26 H 0.7212 0.6363 0.1117 0.048 Uiso 1 1 calc R . . . .
C27 C 0.8237(2) 0.6521(2) 0.05781(14) 0.0520(9) Uani 1 1 d . . . . .
H27 H 0.8658 0.6096 0.0689 0.062 Uiso 1 1 calc R . . . .
C28 C 0.8478(2) 0.6974(3) 0.01676(13) 0.0550(10) Uani 1 1 d . . . . .
H28 H 0.9063 0.6859 -0.0006 0.066 Uiso 1 1 calc R . . . .
C29 C 0.7885(2) 0.7586(3) 0.00069(12) 0.0538(10) Uani 1 1 d . . . . .
H29 H 0.8055 0.7896 -0.0279 0.065 Uiso 1 1 calc R . . . .
C30 C 0.7021(2) 0.7762(2) 0.02613(11) 0.0405(7) Uani 1 1 d . . . . .
H30 H 0.6613 0.8195 0.0150 0.049 Uiso 1 1 calc R . . . .
C31 C 0.28557(18) 0.67682(16) 0.09668(10) 0.0263(6) Uani 1 1 d . . . . .
C32 C 0.2675(2) 0.71447(19) 0.05106(11) 0.0368(7) Uani 1 1 d . . . . .
H32 H 0.3199 0.7225 0.0287 0.044 Uiso 1 1 calc R . . . .
C33 C 0.1738(2) 0.7409(2) 0.03724(13) 0.0506(9) Uani 1 1 d . . . . .
H33 H 0.1625 0.7672 0.0058 0.061 Uiso 1 1 calc R . . . .
C34 C 0.0980(2) 0.7290(2) 0.06902(17) 0.0587(10) Uani 1 1 d . . . . .
H34 H 0.0339 0.7472 0.0596 0.070 Uiso 1 1 calc R . . . .
C35 C 0.1138(3) 0.6911(2) 0.11411(18) 0.0647(12) Uani 1 1 d . . . . .
H35 H 0.0604 0.6827 0.1358 0.078 Uiso 1 1 calc R . . . .
C36 C 0.2078(2) 0.6645(2) 0.12876(13) 0.0461(8) Uani 1 1 d . . . . .
H36 H 0.2185 0.6382 0.1603 0.055 Uiso 1 1 calc R . . . .
C37 C 0.39927(18) 0.53497(16) 0.09922(10) 0.0270(6) Uani 1 1 d . . . . .
C38 C 0.4049(2) 0.50752(18) 0.05030(11) 0.0363(7) Uani 1 1 d . . . . .
H38 H 0.4192 0.5442 0.0240 0.044 Uiso 1 1 calc R . . . .
C39 C 0.3899(2) 0.4262(2) 0.03919(15) 0.0507(9) Uani 1 1 d . . . . .
H39 H 0.3947 0.4071 0.0055 0.061 Uiso 1 1 calc R . . . .
C40 C 0.3679(2) 0.3735(2) 0.07806(18) 0.0586(11) Uani 1 1 d . . . . .
H40 H 0.3574 0.3180 0.0709 0.070 Uiso 1 1 calc R . . . .
C41 C 0.3614(2) 0.4007(2) 0.12622(17) 0.0572(10) Uani 1 1 d . . . . .
H41 H 0.3458 0.3642 0.1524 0.069 Uiso 1 1 calc R . . . .
C42 C 0.3771(2) 0.4808(2) 0.13729(13) 0.0418(7) Uani 1 1 d . . . . .
H42 H 0.3728 0.4992 0.1711 0.050 Uiso 1 1 calc R . . . .
C43 C 0.22160(17) 0.68848(14) 0.30353(10) 0.0218(5) Uani 1 1 d . . . . .
C44 C 0.2095(2) 0.73498(18) 0.26056(11) 0.0357(7) Uani 1 1 d . . . . .
H44 H 0.2620 0.7402 0.2379 0.043 Uiso 1 1 calc R . . . .
C45 C 0.1212(2) 0.7742(2) 0.25023(14) 0.0479(8) Uani 1 1 d . . . . .
H45 H 0.1137 0.8065 0.2208 0.058 Uiso 1 1 calc R . . . .
C46 C 0.0444(2) 0.76636(19) 0.28256(14) 0.0447(8) Uani 1 1 d . . . . .
H46 H -0.0163 0.7929 0.2753 0.054 Uiso 1 1 calc R . . . .
C47 C 0.0554(2) 0.72032(18) 0.32527(13) 0.0414(8) Uani 1 1 d . . . . .
H47 H 0.0024 0.7150 0.3476 0.050 Uiso 1 1 calc R . . . .
C48 C 0.1435(2) 0.68149(16) 0.33608(11) 0.0316(6) Uani 1 1 d . . . . .
H48 H 0.1507 0.6499 0.3659 0.038 Uiso 1 1 calc R . . . .
C49 C 0.29044(16) 0.53331(14) 0.32885(9) 0.0184(5) Uani 1 1 d . . . . .
C50 C 0.23924(19) 0.49421(16) 0.28950(10) 0.0288(6) Uani 1 1 d . . . . .
H50 H 0.2303 0.5202 0.2578 0.035 Uiso 1 1 calc R . . . .
C51 C 0.2017(2) 0.41814(17) 0.29653(12) 0.0371(7) Uani 1 1 d . . . . .
H51 H 0.1673 0.3916 0.2696 0.044 Uiso 1 1 calc R . . . .
C52 C 0.2142(2) 0.38048(16) 0.34275(12) 0.0376(7) Uani 1 1 d . . . . .
H52 H 0.1875 0.3283 0.3477 0.045 Uiso 1 1 calc R . . . .
C53 C 0.2648(2) 0.41791(17) 0.38146(11) 0.0346(7) Uani 1 1 d . . . . .
H53 H 0.2740 0.3912 0.4130 0.041 Uiso 1 1 calc R . . . .
C54 C 0.30303(18) 0.49503(16) 0.37482(10) 0.0267(6) Uani 1 1 d . . . . .
H54 H 0.3376 0.5211 0.4019 0.032 Uiso 1 1 calc R . . . .
C55 C 0.48912(19) 0.80156(15) 0.39866(9) 0.0243(5) Uani 1 1 d . . . . .
C56 C 0.5722(2) 0.83718(17) 0.42152(10) 0.0298(6) Uani 1 1 d . . . . .
H56 H 0.6317 0.8075 0.4249 0.036 Uiso 1 1 calc R . . . .
C57 C 0.5678(2) 0.91572(18) 0.43924(11) 0.0382(7) Uani 1 1 d . . . . .
H57 H 0.6243 0.9395 0.4551 0.046 Uiso 1 1 calc R . . . .
C58 C 0.4822(2) 0.95930(18) 0.43401(11) 0.0389(7) Uani 1 1 d . . . . .
H58 H 0.4798 1.0131 0.4462 0.047 Uiso 1 1 calc R . . . .
C59 C 0.3998(2) 0.92536(18) 0.41109(11) 0.0377(7) Uani 1 1 d . . . . .
H59 H 0.3409 0.9558 0.4073 0.045 Uiso 1 1 calc R . . . .
C60 C 0.4033(2) 0.84639(17) 0.39354(10) 0.0303(6) Uani 1 1 d . . . . .
H60 H 0.3465 0.8229 0.3779 0.036 Uiso 1 1 calc R . . . .
C61 C 0.56630(18) 0.63791(15) 0.41293(9) 0.0242(5) Uani 1 1 d . . . . .
C62 C 0.6486(2) 0.59902(19) 0.39594(12) 0.0402(7) Uani 1 1 d . . . . .
H62 H 0.6704 0.6091 0.3628 0.048 Uiso 1 1 calc R . . . .
C63 C 0.7000(3) 0.5449(2) 0.42725(15) 0.0561(9) Uani 1 1 d . . . . .
H63 H 0.7566 0.5182 0.4154 0.067 Uiso 1 1 calc R . . . .
C64 C 0.6688(3) 0.5301(2) 0.47520(14) 0.0511(9) Uani 1 1 d . . . . .
H64 H 0.7040 0.4934 0.4965 0.061 Uiso 1 1 calc R . . . .
C65 C 0.5872(2) 0.5683(2) 0.49229(12) 0.0466(8) Uani 1 1 d . . . . .
H65 H 0.5659 0.5582 0.5255 0.056 Uiso 1 1 calc R . . . .
C66 C 0.5357(2) 0.62142(18) 0.46144(10) 0.0359(7) Uani 1 1 d . . . . .
H66 H 0.4786 0.6471 0.4735 0.043 Uiso 1 1 calc R . . . .
N1 N 0.48626(15) 0.68265(13) 0.07980(7) 0.0251(5) Uani 1 1 d . . . . .
N2 N 0.38566(15) 0.66862(13) 0.36696(7) 0.0238(5) Uani 1 1 d . . . . .
O1 O 0.45665(13) 0.78831(11) 0.23570(8) 0.0332(5) Uani 1 1 d . . . . .
O2 O 0.59906(13) 0.61296(10) 0.23337(8) 0.0310(4) Uani 1 1 d . . . . .
O3 O 0.67022(12) 0.78183(10) 0.25280(6) 0.0209(4) Uani 1 1 d . . . . .
O4 O 0.59346(12) 0.73960(12) 0.15699(6) 0.0289(4) Uani 1 1 d . . . . .
O5 O 0.42045(13) 0.64935(13) 0.17058(6) 0.0381(5) Uani 1 1 d . . . . .
O6 O 0.39429(11) 0.63194(10) 0.27024(6) 0.0200(3) Uani 1 1 d . . . . .
O7 O 0.55186(12) 0.70864(12) 0.32267(6) 0.0285(4) Uani 1 1 d . . . . .
P1 P 0.72514(4) 0.85788(4) 0.26521(2) 0.01768(12) Uani 1 1 d . . . . .
P2 P 0.56515(5) 0.74556(4) 0.10167(2) 0.02311(14) Uani 1 1 d . . . . .
P3 P 0.40710(5) 0.64062(4) 0.11437(2) 0.02351(14) Uani 1 1 d . . . . .
P4 P 0.33403(4) 0.63375(4) 0.31707(2) 0.01653(12) Uani 1 1 d . . . . .
P5 P 0.49504(5) 0.70239(4) 0.37068(2) 0.02083(13) 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
Np1 O1 1.7470(17) . ?
Np1 O2 1.7501(17) . ?
Np1 O3 2.4099(16) . ?
Np1 O4 2.3584(17) . ?
Np1 O5 2.3542(17) . ?
Np1 O6 2.3560(15) . ?
Np1 O7 2.3558(16) . ?
C1 C2 1.389(4) . ?
C1 C6 1.389(3) . ?
C1 P1 1.798(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.373(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.364(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.383(4) . ?
C7 C12 1.396(3) . ?
C7 P1 1.799(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.376(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.397(4) . ?
C13 C18 1.388(4) . ?
C13 P1 1.799(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.376(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.380(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.391(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.392(4) . ?
C19 C24 1.390(4) . ?
C19 P2 1.806(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.390(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.372(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.365(6) . ?
C23 H23 0.9500 . ?
C23 C24 1.390(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(4) . ?
C25 C30 1.382(4) . ?
C25 P2 1.805(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.394(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.369(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.358(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.402(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.376(4) . ?
C31 C36 1.391(4) . ?
C31 P3 1.809(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.387(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.365(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.361(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.398(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.378(4) . ?
C37 C42 1.390(4) . ?
C37 P3 1.801(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.395(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.390(5) . ?
C40 H40 0.9500 . ?
C40 C41 1.359(6) . ?
C41 H41 0.9500 . ?
C41 C42 1.376(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.381(4) . ?
C43 C48 1.393(4) . ?
C43 P4 1.806(2) . ?
C44 H44 0.9500 . ?
C44 C45 1.387(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.377(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.370(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.383(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.397(3) . ?
C49 C54 1.380(3) . ?
C49 P4 1.799(2) . ?
C50 H50 0.9500 . ?
C50 C51 1.376(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.381(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.368(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.394(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.398(4) . ?
C55 C60 1.388(4) . ?
C55 P5 1.807(3) . ?
C56 H56 0.9500 . ?
C56 C57 1.387(4) . ?
C57 H57 0.9500 . ?
C57 C58 1.375(4) . ?
C58 H58 0.9500 . ?
C58 C59 1.380(4) . ?
C59 H59 0.9500 . ?
C59 C60 1.392(4) . ?
C60 H60 0.9500 . ?
C61 C62 1.380(4) . ?
C61 C66 1.390(4) . ?
C61 P5 1.810(3) . ?
C62 H62 0.9500 . ?
C62 C63 1.397(5) . ?
C63 H63 0.9500 . ?
C63 C64 1.373(5) . ?
C64 H64 0.9500 . ?
C64 C65 1.367(5) . ?
C65 H65 0.9500 . ?
C65 C66 1.380(4) . ?
C66 H66 0.9500 . ?
N1 P2 1.594(2) . ?
N1 P3 1.595(2) . ?
N2 P4 1.588(2) . ?
N2 P5 1.591(2) . ?
O3 P1 1.4981(17) . ?
O4 P2 1.5080(18) . ?
O5 P3 1.5019(18) . ?
O6 P4 1.5075(16) . ?
O7 P5 1.5112(17) . ?

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 Np1 O2 179.21(8) . . ?
O1 Np1 O3 88.18(7) . . ?
O1 Np1 O4 90.57(8) . . ?
O1 Np1 O5 89.23(9) . . ?
O1 Np1 O6 88.11(7) . . ?
O1 Np1 O7 89.73(9) . . ?
O2 Np1 O3 91.03(7) . . ?
O2 Np1 O4 89.17(8) . . ?
O2 Np1 O5 91.41(8) . . ?
O2 Np1 O6 92.55(7) . . ?
O2 Np1 O7 90.04(8) . . ?
O4 Np1 O3 72.08(6) . . ?
O5 Np1 O3 145.53(6) . . ?
O5 Np1 O4 73.58(6) . . ?
O5 Np1 O6 69.66(6) . . ?
O5 Np1 O7 143.31(6) . . ?
O6 Np1 O3 144.51(5) . . ?
O6 Np1 O4 143.23(5) . . ?
O7 Np1 O3 71.05(6) . . ?
O7 Np1 O4 143.10(6) . . ?
O7 Np1 O6 73.65(5) . . ?
C2 C1 P1 123.1(2) . . ?
C6 C1 C2 119.2(2) . . ?
C6 C1 P1 117.7(2) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.1(3) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C12 119.8(2) . . ?
C8 C7 P1 117.31(18) . . ?
C12 C7 P1 122.84(19) . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.7(3) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.5(3) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.1(2) . . ?
C12 C11 H11 120.0 . . ?
C7 C12 H12 120.0 . . ?
C11 C12 C7 119.9(3) . . ?
C11 C12 H12 120.0 . . ?
C14 C13 P1 121.7(2) . . ?
C18 C13 C14 119.5(2) . . ?
C18 C13 P1 118.77(19) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.8(3) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.5(3) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(3) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 C17 120.0(3) . . ?
C13 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 P2 121.4(2) . . ?
C24 C19 C20 119.0(3) . . ?
C24 C19 P2 119.5(2) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.2(3) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 119.9(3) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.8 . . ?
C23 C22 C21 120.5(4) . . ?
C23 C22 H22 119.8 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.5(4) . . ?
C24 C23 H23 119.7 . . ?
C19 C24 H24 120.1 . . ?
C23 C24 C19 119.8(3) . . ?
C23 C24 H24 120.1 . . ?
C26 C25 P2 117.0(2) . . ?
C30 C25 C26 118.9(3) . . ?
C30 C25 P2 124.0(2) . . ?
C25 C26 H26 120.0 . . ?
C25 C26 C27 120.0(3) . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.3(3) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.4(3) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.3(3) . . ?
C30 C29 H29 119.9 . . ?
C25 C30 C29 120.2(3) . . ?
C25 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C32 C31 C36 118.9(3) . . ?
C32 C31 P3 121.1(2) . . ?
C36 C31 P3 119.9(2) . . ?
C31 C32 H32 119.5 . . ?
C31 C32 C33 121.0(3) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.8(4) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 H34 119.8 . . ?
C35 C34 C33 120.3(3) . . ?
C35 C34 H34 119.8 . . ?
C34 C35 H35 119.7 . . ?
C34 C35 C36 120.6(3) . . ?
C36 C35 H35 119.7 . . ?
C31 C36 C35 119.4(3) . . ?
C31 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
C38 C37 C42 119.2(3) . . ?
C38 C37 P3 121.8(2) . . ?
C42 C37 P3 118.7(2) . . ?
C37 C38 H38 119.8 . . ?
C37 C38 C39 120.4(3) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 120.5 . . ?
C40 C39 C38 119.0(3) . . ?
C40 C39 H39 120.5 . . ?
C39 C40 H40 119.7 . . ?
C41 C40 C39 120.5(3) . . ?
C41 C40 H40 119.7 . . ?
C40 C41 H41 119.8 . . ?
C40 C41 C42 120.5(3) . . ?
C42 C41 H41 119.8 . . ?
C37 C42 H42 119.8 . . ?
C41 C42 C37 120.3(3) . . ?
C41 C42 H42 119.8 . . ?
C44 C43 C48 118.8(2) . . ?
C44 C43 P4 121.6(2) . . ?
C48 C43 P4 119.5(2) . . ?
C43 C44 H44 119.8 . . ?
C43 C44 C45 120.4(3) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 119.9 . . ?
C46 C45 C44 120.2(3) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 C45 119.9(3) . . ?
C47 C46 H46 120.0 . . ?
C46 C47 H47 119.8 . . ?
C46 C47 C48 120.3(3) . . ?
C48 C47 H47 119.8 . . ?
C43 C48 H48 119.8 . . ?
C47 C48 C43 120.3(3) . . ?
C47 C48 H48 119.8 . . ?
C50 C49 P4 117.43(18) . . ?
C54 C49 C50 119.4(2) . . ?
C54 C49 P4 123.11(19) . . ?
C49 C50 H50 119.9 . . ?
C51 C50 C49 120.3(3) . . ?
C51 C50 H50 119.9 . . ?
C50 C51 H51 120.1 . . ?
C50 C51 C52 119.9(3) . . ?
C52 C51 H51 120.1 . . ?
C51 C52 H52 119.8 . . ?
C53 C52 C51 120.4(3) . . ?
C53 C52 H52 119.8 . . ?
C52 C53 H53 119.9 . . ?
C52 C53 C54 120.2(3) . . ?
C54 C53 H53 119.9 . . ?
C49 C54 C53 119.8(3) . . ?
C49 C54 H54 120.1 . . ?
C53 C54 H54 120.1 . . ?
C56 C55 P5 121.2(2) . . ?
C60 C55 C56 118.9(2) . . ?
C60 C55 P5 119.7(2) . . ?
C55 C56 H56 119.9 . . ?
C57 C56 C55 120.1(3) . . ?
C57 C56 H56 119.9 . . ?
C56 C57 H57 119.9 . . ?
C58 C57 C56 120.3(3) . . ?
C58 C57 H57 119.9 . . ?
C57 C58 H58 119.8 . . ?
C57 C58 C59 120.4(3) . . ?
C59 C58 H58 119.8 . . ?
C58 C59 H59 120.1 . . ?
C58 C59 C60 119.7(3) . . ?
C60 C59 H59 120.1 . . ?
C55 C60 C59 120.6(3) . . ?
C55 C60 H60 119.7 . . ?
C59 C60 H60 119.7 . . ?
C62 C61 C66 118.5(3) . . ?
C62 C61 P5 120.0(2) . . ?
C66 C61 P5 121.2(2) . . ?
C61 C62 H62 119.8 . . ?
C61 C62 C63 120.3(3) . . ?
C63 C62 H62 119.8 . . ?
C62 C63 H63 120.0 . . ?
C64 C63 C62 120.1(3) . . ?
C64 C63 H63 120.0 . . ?
C63 C64 H64 120.0 . . ?
C65 C64 C63 120.0(3) . . ?
C65 C64 H64 120.0 . . ?
C64 C65 H65 119.9 . . ?
C64 C65 C66 120.2(3) . . ?
C66 C65 H65 119.9 . . ?
C61 C66 H66 119.6 . . ?
C65 C66 C61 120.8(3) . . ?
C65 C66 H66 119.6 . . ?
P2 N1 P3 122.46(13) . . ?
P4 N2 P5 124.78(13) . . ?
P1 O3 Np1 155.82(10) . . ?
P2 O4 Np1 140.40(10) . . ?
P3 O5 Np1 143.30(10) . . ?
P4 O6 Np1 139.79(9) . . ?
P5 O7 Np1 140.25(10) . . ?
C1 P1 C7 108.50(11) . . ?
C1 P1 C13 105.57(12) . . ?
C13 P1 C7 108.44(11) . . ?
O3 P1 C1 113.56(11) . . ?
O3 P1 C7 110.02(10) . . ?
O3 P1 C13 110.55(11) . . ?
C25 P2 C19 107.40(13) . . ?
N1 P2 C19 110.26(12) . . ?
N1 P2 C25 107.06(12) . . ?
O4 P2 C19 107.60(12) . . ?
O4 P2 C25 106.63(11) . . ?
O4 P2 N1 117.43(10) . . ?
C37 P3 C31 102.57(11) . . ?
N1 P3 C31 109.52(12) . . ?
N1 P3 C37 109.52(12) . . ?
O5 P3 C31 107.95(12) . . ?
O5 P3 C37 108.65(12) . . ?
O5 P3 N1 117.58(10) . . ?
C49 P4 C43 102.60(11) . . ?
N2 P4 C43 109.52(12) . . ?
N2 P4 C49 109.46(11) . . ?
O6 P4 C43 108.95(11) . . ?
O6 P4 C49 108.32(10) . . ?
O6 P4 N2 117.01(10) . . ?
C55 P5 C61 108.28(12) . . ?
N2 P5 C55 107.04(12) . . ?
N2 P5 C61 108.30(12) . . ?
O7 P5 C55 108.23(11) . . ?
O7 P5 C61 106.44(11) . . ?
O7 P5 N2 118.23(10) . . ?

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
Np1 O3 P1 C1 -4.8(3) . . . . ?
Np1 O3 P1 C7 -126.6(2) . . . . ?
Np1 O3 P1 C13 113.7(2) . . . . ?
Np1 O4 P2 C19 95.18(19) . . . . ?
Np1 O4 P2 C25 -149.85(18) . . . . ?
Np1 O4 P2 N1 -29.8(2) . . . . ?
Np1 O5 P3 C31 -129.3(2) . . . . ?
Np1 O5 P3 C37 120.2(2) . . . . ?
Np1 O5 P3 N1 -4.8(3) . . . . ?
Np1 O6 P4 C43 98.04(16) . . . . ?
Np1 O6 P4 C49 -151.06(14) . . . . ?
Np1 O6 P4 N2 -26.8(2) . . . . ?
Np1 O7 P5 C55 -110.53(18) . . . . ?
Np1 O7 P5 C61 133.26(17) . . . . ?
Np1 O7 P5 N2 11.3(2) . . . . ?
C1 C2 C3 C4 -0.9(6) . . . . ?
C2 C1 C6 C5 1.0(4) . . . . ?
C2 C1 P1 C7 -13.2(3) . . . . ?
C2 C1 P1 C13 102.8(3) . . . . ?
C2 C1 P1 O3 -135.9(2) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C3 C4 C5 C6 -0.7(6) . . . . ?
C4 C5 C6 C1 -0.5(5) . . . . ?
C6 C1 C2 C3 -0.3(5) . . . . ?
C6 C1 P1 C7 169.2(2) . . . . ?
C6 C1 P1 C13 -74.8(2) . . . . ?
C6 C1 P1 O3 46.5(2) . . . . ?
C7 C8 C9 C10 0.3(5) . . . . ?
C8 C7 C12 C11 1.1(4) . . . . ?
C8 C7 P1 C1 -109.3(2) . . . . ?
C8 C7 P1 C13 136.5(2) . . . . ?
C8 C7 P1 O3 15.5(2) . . . . ?
C8 C9 C10 C11 -0.3(5) . . . . ?
C9 C10 C11 C12 0.7(5) . . . . ?
C10 C11 C12 C7 -1.1(4) . . . . ?
C12 C7 C8 C9 -0.6(4) . . . . ?
C12 C7 P1 C1 70.1(2) . . . . ?
C12 C7 P1 C13 -44.1(2) . . . . ?
C12 C7 P1 O3 -165.1(2) . . . . ?
C13 C14 C15 C16 -1.1(5) . . . . ?
C14 C13 C18 C17 -1.0(4) . . . . ?
C14 C13 P1 C1 -40.8(2) . . . . ?
C14 C13 P1 C7 75.3(2) . . . . ?
C14 C13 P1 O3 -164.0(2) . . . . ?
C14 C15 C16 C17 -0.5(5) . . . . ?
C15 C16 C17 C18 1.4(4) . . . . ?
C16 C17 C18 C13 -0.7(4) . . . . ?
C18 C13 C14 C15 1.9(4) . . . . ?
C18 C13 P1 C1 138.9(2) . . . . ?
C18 C13 P1 C7 -105.0(2) . . . . ?
C18 C13 P1 O3 15.7(2) . . . . ?
C19 C20 C21 C22 -0.5(5) . . . . ?
C20 C19 C24 C23 -0.3(4) . . . . ?
C20 C19 P2 C25 83.2(2) . . . . ?
C20 C19 P2 N1 -33.1(2) . . . . ?
C20 C19 P2 O4 -162.3(2) . . . . ?
C20 C21 C22 C23 0.2(5) . . . . ?
C21 C22 C23 C24 0.0(6) . . . . ?
C22 C23 C24 C19 0.0(5) . . . . ?
C24 C19 C20 C21 0.5(4) . . . . ?
C24 C19 P2 C25 -99.8(2) . . . . ?
C24 C19 P2 N1 143.9(2) . . . . ?
C24 C19 P2 O4 14.7(2) . . . . ?
C25 C26 C27 C28 -0.5(5) . . . . ?
C26 C25 C30 C29 0.7(4) . . . . ?
C26 C25 P2 C19 159.6(2) . . . . ?
C26 C25 P2 N1 -82.0(2) . . . . ?
C26 C25 P2 O4 44.5(2) . . . . ?
C26 C27 C28 C29 0.4(5) . . . . ?
C27 C28 C29 C30 0.2(5) . . . . ?
C28 C29 C30 C25 -0.8(5) . . . . ?
C30 C25 C26 C27 -0.1(4) . . . . ?
C30 C25 P2 C19 -21.9(3) . . . . ?
C30 C25 P2 N1 96.5(3) . . . . ?
C30 C25 P2 O4 -137.0(2) . . . . ?
C31 C32 C33 C34 -0.5(5) . . . . ?
C32 C31 C36 C35 -0.5(5) . . . . ?
C32 C31 P3 C37 -98.6(2) . . . . ?
C32 C31 P3 N1 17.6(3) . . . . ?
C32 C31 P3 O5 146.8(2) . . . . ?
C32 C33 C34 C35 -0.2(6) . . . . ?
C33 C34 C35 C36 0.5(6) . . . . ?
C34 C35 C36 C31 -0.2(6) . . . . ?
C36 C31 C32 C33 0.9(4) . . . . ?
C36 C31 P3 C37 79.3(3) . . . . ?
C36 C31 P3 N1 -164.4(2) . . . . ?
C36 C31 P3 O5 -35.3(3) . . . . ?
C37 C38 C39 C40 0.8(5) . . . . ?
C38 C37 C42 C41 0.2(4) . . . . ?
C38 C37 P3 C31 78.0(2) . . . . ?
C38 C37 P3 N1 -38.3(3) . . . . ?
C38 C37 P3 O5 -167.9(2) . . . . ?
C38 C39 C40 C41 -0.1(5) . . . . ?
C39 C40 C41 C42 -0.5(5) . . . . ?
C40 C41 C42 C37 0.5(5) . . . . ?
C42 C37 C38 C39 -0.9(4) . . . . ?
C42 C37 P3 C31 -95.5(2) . . . . ?
C42 C37 P3 N1 148.3(2) . . . . ?
C42 C37 P3 O5 18.6(2) . . . . ?
C43 C44 C45 C46 -0.6(5) . . . . ?
C44 C43 C48 C47 0.2(4) . . . . ?
C44 C43 P4 C49 -128.2(2) . . . . ?
C44 C43 P4 N2 115.6(2) . . . . ?
C44 C43 P4 O6 -13.5(3) . . . . ?
C44 C45 C46 C47 0.5(5) . . . . ?
C45 C46 C47 C48 -0.1(5) . . . . ?
C46 C47 C48 C43 -0.3(5) . . . . ?
C48 C43 C44 C45 0.2(4) . . . . ?
C48 C43 P4 C49 49.3(2) . . . . ?
C48 C43 P4 N2 -66.9(2) . . . . ?
C48 C43 P4 O6 164.0(2) . . . . ?
C49 C50 C51 C52 0.4(4) . . . . ?
C50 C49 C54 C53 0.2(4) . . . . ?
C50 C49 P4 C43 61.2(2) . . . . ?
C50 C49 P4 N2 177.47(19) . . . . ?
C50 C49 P4 O6 -53.9(2) . . . . ?
C50 C51 C52 C53 -0.9(4) . . . . ?
C51 C52 C53 C54 1.0(4) . . . . ?
C52 C53 C54 C49 -0.6(4) . . . . ?
C54 C49 C50 C51 0.0(4) . . . . ?
C54 C49 P4 C43 -116.9(2) . . . . ?
C54 C49 P4 N2 -0.7(2) . . . . ?
C54 C49 P4 O6 128.0(2) . . . . ?
C55 C56 C57 C58 -0.6(4) . . . . ?
C56 C55 C60 C59 -0.3(4) . . . . ?
C56 C55 P5 C61 43.2(2) . . . . ?
C56 C55 P5 N2 159.7(2) . . . . ?
C56 C55 P5 O7 -71.8(2) . . . . ?
C56 C57 C58 C59 0.0(4) . . . . ?
C57 C58 C59 C60 0.5(4) . . . . ?
C58 C59 C60 C55 -0.3(4) . . . . ?
C60 C55 C56 C57 0.8(4) . . . . ?
C60 C55 P5 C61 -142.7(2) . . . . ?
C60 C55 P5 N2 -26.1(2) . . . . ?
C60 C55 P5 O7 102.3(2) . . . . ?
C61 C62 C63 C64 -0.1(5) . . . . ?
C62 C61 C66 C65 1.0(4) . . . . ?
C62 C61 P5 C55 -123.1(2) . . . . ?
C62 C61 P5 N2 121.2(2) . . . . ?
C62 C61 P5 O7 -6.9(2) . . . . ?
C62 C63 C64 C65 0.2(5) . . . . ?
C63 C64 C65 C66 0.3(5) . . . . ?
C64 C65 C66 C61 -0.9(5) . . . . ?
C66 C61 C62 C63 -0.5(4) . . . . ?
C66 C61 P5 C55 62.0(2) . . . . ?
C66 C61 P5 N2 -53.7(2) . . . . ?
C66 C61 P5 O7 178.2(2) . . . . ?
P1 C1 C2 C3 -177.9(3) . . . . ?
P1 C1 C6 C5 178.7(2) . . . . ?
P1 C7 C8 C9 178.8(2) . . . . ?
P1 C7 C12 C11 -178.3(2) . . . . ?
P1 C13 C14 C15 -178.4(2) . . . . ?
P1 C13 C18 C17 179.33(19) . . . . ?
P2 C19 C20 C21 177.5(2) . . . . ?
P2 C19 C24 C23 -177.3(2) . . . . ?
P2 C25 C26 C27 178.5(2) . . . . ?
P2 C25 C30 C29 -177.8(2) . . . . ?
P2 N1 P3 C31 112.07(16) . . . . ?
P2 N1 P3 C37 -136.18(16) . . . . ?
P2 N1 P3 O5 -11.6(2) . . . . ?
P3 C31 C32 C33 178.9(2) . . . . ?
P3 C31 C36 C35 -178.5(3) . . . . ?
P3 C37 C38 C39 -174.3(2) . . . . ?
P3 C37 C42 C41 173.9(2) . . . . ?
P3 N1 P2 C19 -98.26(17) . . . . ?
P3 N1 P2 C25 145.21(16) . . . . ?
P3 N1 P2 O4 25.4(2) . . . . ?
P4 C43 C44 C45 177.8(2) . . . . ?
P4 C43 C48 C47 -177.4(2) . . . . ?
P4 C49 C50 C51 -178.3(2) . . . . ?
P4 C49 C54 C53 178.28(19) . . . . ?
P4 N2 P5 C55 127.87(17) . . . . ?
P4 N2 P5 C61 -115.59(17) . . . . ?
P4 N2 P5 O7 5.5(2) . . . . ?
P5 C55 C56 C57 175.0(2) . . . . ?
P5 C55 C60 C59 -174.6(2) . . . . ?
P5 C61 C62 C63 -175.6(2) . . . . ?
P5 C61 C66 C65 176.0(2) . . . . ?
P5 N2 P4 C43 -123.80(17) . . . . ?
P5 N2 P4 C49 124.44(16) . . . . ?
P5 N2 P4 O6 0.8(2) . . . . ?

_olex2_date_sample_data_collection 2013-06-26
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_olsn147
_database_code_depnum_ccdc_archive 'CCDC 1032119'
_audit_update_record             
;
2014-12-13 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_audit_creation_date             2014-11-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
;
_shelxl_version_number           2014/6
_chemical_name_common            '[U(TPIP)2Ph3PO)'
_chemical_name_systematic        2
_chemical_formula_moiety         'C66 H55 N2 O7 P5 U, C H2 Cl2'
_chemical_formula_sum            'C67 H57 Cl2 N2 O7 P5 U'
_chemical_formula_weight         1465.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44.67 H38.67 Cl1.33 N1.33 O4.67 P3.33 U0.67'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   9.7808(5)
_cell_length_b                   23.6970(7)
_cell_length_c                   26.1815(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.334(4)
_cell_angle_gamma                90
_cell_volume                     6042.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9052
_cell_measurement_temperature    101.8(3)
_cell_measurement_theta_max      27.8420
_cell_measurement_theta_min      2.8714
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2920
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22263
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.871
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101.8(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3367
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -70.00  -36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1807 -179.0000   90.0000 34

#__ type_ start__ end____ width___ exp.time_
  2 omega  -17.00  101.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1807   37.0000 -120.0000 118

#__ type_ start__ end____ width___ exp.time_
  3 omega  -35.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1807  -77.0000   60.0000 71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0037946000
_diffrn_orient_matrix_UB_12      0.0282585000
_diffrn_orient_matrix_UB_13      0.0089800000
_diffrn_orient_matrix_UB_21      0.0338476000
_diffrn_orient_matrix_UB_22      -0.0093205000
_diffrn_orient_matrix_UB_23      0.0236198000
_diffrn_orient_matrix_UB_31      0.0643365000
_diffrn_orient_matrix_UB_32      0.0033125000
_diffrn_orient_matrix_UB_33      -0.0101082000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10453
_reflns_number_total             12024
_reflns_odcompleteness_completeness 97.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         3.473
_refine_diff_density_min         -2.377
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         12024
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0374P)²+18.4858P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0898
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 Cl2, C67, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B)
3.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C62(H62), C20(H20), C54(H54), C21(H21), C39(H39), C36(H36),
 C22(H22), C38(H38), C44(H44), C35(H35), C2(H2), C14(H14), C15(H15), C4(H4),
 C27(H27), C16(H16), C17(H17), C26(H26), C48(H48), C18(H18), C6(H6), C40(H40),
 C41(H41), C30(H30), C66(H66), C23(H23), C3(H3), C11(H11), C64(H64), C33(H33),
 C9(H9), C5(H5), C50(H50), C28(H28), C53(H53), C34(H34), C29(H29), C12(H12),
 C10(H10), C24(H24), C60(H60), C46(H46), C45(H45), C56(H56), C32(H32), C65(H65),
  C51(H51), C47(H47), C8(H8), C52(H52), C63(H63), C59(H59), C58(H58), C57(H57)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
U1 U 0.48272(2) 0.68160(2) 0.13797(2) 0.01069(5) Uani 1 1 d . . . . .
P2 P 0.34207(11) 0.54519(5) 0.16861(4) 0.0117(2) Uani 1 1 d . . . . .
P4 P 0.66784(11) 0.80070(5) 0.20332(4) 0.0136(2) Uani 1 1 d . . . . .
P1 P 0.25763(11) 0.67008(5) 0.00832(4) 0.0134(2) Uani 1 1 d . . . . .
P3 P 0.51061(11) 0.59259(5) 0.24999(4) 0.0117(2) Uani 1 1 d . . . . .
P5 P 0.52745(11) 0.83285(5) 0.11070(4) 0.0135(2) Uani 1 1 d . . . . .
O3 O 0.3539(3) 0.67444(13) 0.05620(11) 0.0168(6) Uani 1 1 d . . . . .
O2 O 0.6360(3) 0.66304(14) 0.11134(11) 0.0200(7) Uani 1 1 d . . . . .
O1 O 0.3283(3) 0.69923(14) 0.16405(11) 0.0185(7) Uani 1 1 d . . . . .
O5 O 0.5706(3) 0.63370(12) 0.21382(10) 0.0130(6) Uani 1 1 d . . . . .
O4 O 0.3970(3) 0.58662(12) 0.13127(10) 0.0145(6) Uani 1 1 d . . . . .
O6 O 0.5851(3) 0.74634(13) 0.19936(11) 0.0180(7) Uani 1 1 d . . . . .
O7 O 0.4941(3) 0.77215(12) 0.09508(10) 0.0158(6) Uani 1 1 d . . . . .
N2 N 0.6507(4) 0.84133(15) 0.15464(13) 0.0161(8) Uani 1 1 d . . . . .
N1 N 0.4171(3) 0.54295(15) 0.22538(13) 0.0141(7) Uani 1 1 d . . . . .
C19 C 0.1611(4) 0.55860(18) 0.17186(16) 0.0138(9) Uani 1 1 d . . . . .
C43 C 0.6179(4) 0.83959(19) 0.25801(16) 0.0167(9) Uani 1 1 d . . . . .
C1 C 0.0896(4) 0.69605(19) 0.01943(17) 0.0175(9) Uani 1 1 d . . . . .
C7 C 0.2443(4) 0.59876(19) -0.01579(15) 0.0166(9) Uani 1 1 d . . . . .
C42 C 0.7551(5) 0.59502(19) 0.31307(17) 0.0196(9) Uani 1 1 d . . . . .
H42 H 0.7538 0.6345 0.3069 0.023 Uiso 1 1 calc R . . . .
C31 C 0.4202(4) 0.63231(19) 0.29509(15) 0.0146(9) Uani 1 1 d . . . . .
C37 C 0.6507(4) 0.56083(19) 0.28990(15) 0.0141(9) Uani 1 1 d . . . . .
C25 C 0.3523(4) 0.47467(18) 0.14290(16) 0.0145(9) Uani 1 1 d . . . . .
C62 C 0.7159(5) 0.8797(2) 0.04993(19) 0.0268(11) Uani 1 1 d . . . . .
H62 H 0.7830 0.8620 0.0732 0.032 Uiso 1 1 calc R . . . .
C20 C 0.0919(4) 0.5340(2) 0.21031(17) 0.0200(10) Uani 1 1 d . . . . .
H20 H 0.1400 0.5096 0.2345 0.024 Uiso 1 1 calc R . . . .
C61 C 0.5773(5) 0.87371(18) 0.05686(16) 0.0159(9) Uani 1 1 d . . . . .
C54 C 0.9528(5) 0.8207(2) 0.21054(17) 0.0216(10) Uani 1 1 d . . . . .
H54 H 0.9319 0.8581 0.1992 0.026 Uiso 1 1 calc R . . . .
C21 C -0.0467(4) 0.5447(2) 0.21372(17) 0.0207(10) Uani 1 1 d . . . . .
H21 H -0.0930 0.5278 0.2402 0.025 Uiso 1 1 calc R . . . .
C39 C 0.7614(5) 0.4791(2) 0.33099(17) 0.0231(10) Uani 1 1 d . . . . .
H39 H 0.7637 0.4396 0.3370 0.028 Uiso 1 1 calc R . . . .
C36 C 0.4626(5) 0.68720(19) 0.30846(17) 0.0192(9) Uani 1 1 d . . . . .
H36 H 0.5333 0.7046 0.2915 0.023 Uiso 1 1 calc R . . . .
C22 C -0.1169(5) 0.5802(2) 0.17810(18) 0.0219(10) Uani 1 1 d . . . . .
H22 H -0.2114 0.5880 0.1804 0.026 Uiso 1 1 calc R . . . .
C38 C 0.6554(5) 0.50304(19) 0.29910(16) 0.0179(9) Uani 1 1 d . . . . .
H38 H 0.5851 0.4795 0.2833 0.021 Uiso 1 1 calc R . . . .
C44 C 0.7022(5) 0.8790(2) 0.28405(16) 0.0207(10) Uani 1 1 d . . . . .
H44 H 0.7936 0.8837 0.2753 0.025 Uiso 1 1 calc R . . . .
C49 C 0.8465(4) 0.78219(19) 0.21630(15) 0.0155(9) Uani 1 1 d . . . . .
C35 C 0.4018(5) 0.7163(2) 0.34648(18) 0.0253(11) Uani 1 1 d . . . . .
H35 H 0.4322 0.7533 0.3557 0.030 Uiso 1 1 calc R . . . .
C2 C 0.0702(5) 0.7183(2) 0.06775(17) 0.0191(9) Uani 1 1 d . . . . .
H2 H 0.1449 0.7190 0.0937 0.023 Uiso 1 1 calc R . . . .
C14 C 0.2737(5) 0.7043(2) -0.09354(16) 0.0192(9) Uani 1 1 d . . . . .
H14 H 0.2051 0.6769 -0.1029 0.023 Uiso 1 1 calc R . . . .
C13 C 0.3221(4) 0.71149(18) -0.04220(15) 0.0146(9) Uani 1 1 d . . . . .
C15 C 0.3262(5) 0.7374(2) -0.13106(16) 0.0209(10) Uani 1 1 d . . . . .
H15 H 0.2920 0.7331 -0.1660 0.025 Uiso 1 1 calc R . . . .
C4 C -0.1661(5) 0.7371(2) 0.04132(19) 0.0255(11) Uani 1 1 d . . . . .
H4 H -0.2540 0.7499 0.0490 0.031 Uiso 1 1 calc R . . . .
C27 C 0.4303(5) 0.3777(2) 0.15043(18) 0.0227(10) Uani 1 1 d . . . . .
H27 H 0.4775 0.3487 0.1699 0.027 Uiso 1 1 calc R . . . .
C16 C 0.4278(5) 0.77651(19) -0.11758(17) 0.0203(10) Uani 1 1 d . . . . .
H16 H 0.4651 0.7983 -0.1434 0.024 Uiso 1 1 calc R . . . .
C17 C 0.4755(5) 0.7841(2) -0.06651(17) 0.0207(10) Uani 1 1 d . . . . .
H17 H 0.5444 0.8115 -0.0574 0.025 Uiso 1 1 calc R . . . .
C26 C 0.4191(5) 0.43160(19) 0.17151(17) 0.0198(10) Uani 1 1 d . . . . .
H26 H 0.4574 0.4388 0.2056 0.024 Uiso 1 1 calc R . . . .
C48 C 0.4835(5) 0.8332(2) 0.27186(19) 0.0255(11) Uani 1 1 d . . . . .
H48 H 0.4236 0.8064 0.2545 0.031 Uiso 1 1 calc R . . . .
C18 C 0.4228(4) 0.75177(18) -0.02875(16) 0.0171(9) Uani 1 1 d . . . . .
H18 H 0.4554 0.7571 0.0062 0.021 Uiso 1 1 calc R . . . .
C6 C -0.0218(5) 0.6957(2) -0.01797(18) 0.0242(10) Uani 1 1 d . . . . .
H6 H -0.0108 0.6813 -0.0512 0.029 Uiso 1 1 calc R . . . .
C40 C 0.8636(5) 0.5136(2) 0.35390(17) 0.0242(11) Uani 1 1 d . . . . .
H40 H 0.9362 0.4976 0.3758 0.029 Uiso 1 1 calc R . . . .
C41 C 0.8610(5) 0.5713(2) 0.34515(18) 0.0241(10) Uani 1 1 d . . . . .
H41 H 0.9317 0.5946 0.3611 0.029 Uiso 1 1 calc R . . . .
C30 C 0.2929(5) 0.46261(19) 0.09321(17) 0.0190(9) Uani 1 1 d . . . . .
H30 H 0.2456 0.4914 0.0735 0.023 Uiso 1 1 calc R . . . .
C66 C 0.4802(5) 0.9001(2) 0.02229(17) 0.0244(10) Uani 1 1 d . . . . .
H66 H 0.3851 0.8963 0.0262 0.029 Uiso 1 1 calc R . . . .
C23 C -0.0493(5) 0.6043(2) 0.13940(18) 0.0226(10) Uani 1 1 d . . . . .
H23 H -0.0980 0.6282 0.1149 0.027 Uiso 1 1 calc R . . . .
C3 C -0.0562(5) 0.7393(2) 0.07827(18) 0.0245(11) Uani 1 1 d . . . . .
H3 H -0.0672 0.7552 0.1109 0.029 Uiso 1 1 calc R . . . .
C11 C 0.3689(5) 0.5193(2) -0.04715(19) 0.0289(11) Uani 1 1 d . . . . .
H11 H 0.4531 0.5027 -0.0546 0.035 Uiso 1 1 calc R . . . .
C64 C 0.6607(6) 0.9379(2) -0.02437(19) 0.0349(13) Uani 1 1 d . . . . .
H64 H 0.6892 0.9601 -0.0517 0.042 Uiso 1 1 calc R . . . .
C33 C 0.2531(5) 0.6385(2) 0.35710(19) 0.0315(12) Uani 1 1 d . . . . .
H33 H 0.1801 0.6220 0.3735 0.038 Uiso 1 1 calc R . . . .
C9 C 0.1251(5) 0.5140(2) -0.0442(2) 0.0302(12) Uani 1 1 d . . . . .
H9 H 0.0416 0.4935 -0.0502 0.036 Uiso 1 1 calc R . . . .
C5 C -0.1481(5) 0.7161(2) -0.00695(19) 0.0275(11) Uani 1 1 d . . . . .
H5 H -0.2231 0.7158 -0.0327 0.033 Uiso 1 1 calc R . . . .
C50 C 0.8797(5) 0.7270(2) 0.23174(16) 0.0197(10) Uani 1 1 d . . . . .
H50 H 0.8085 0.7004 0.2353 0.024 Uiso 1 1 calc R . . . .
C28 C 0.3730(5) 0.3668(2) 0.10157(18) 0.0215(10) Uani 1 1 d . . . . .
H28 H 0.3810 0.3302 0.0873 0.026 Uiso 1 1 calc R . . . .
C53 C 1.0887(5) 0.8041(2) 0.22140(18) 0.0274(11) Uani 1 1 d . . . . .
H53 H 1.1607 0.8304 0.2179 0.033 Uiso 1 1 calc R . . . .
C34 C 0.2987(5) 0.6921(2) 0.37079(18) 0.0268(11) Uani 1 1 d . . . . .
H34 H 0.2585 0.7122 0.3970 0.032 Uiso 1 1 calc R . . . .
C29 C 0.3028(5) 0.4091(2) 0.07268(17) 0.0222(10) Uani 1 1 d . . . . .
H29 H 0.2621 0.4012 0.0391 0.027 Uiso 1 1 calc R . . . .
C12 C 0.3663(5) 0.5736(2) -0.02746(19) 0.0276(11) Uani 1 1 d . . . . .
H12 H 0.4498 0.5941 -0.0218 0.033 Uiso 1 1 calc R . . . .
C10 C 0.2470(5) 0.4896(2) -0.05578(17) 0.0251(11) Uani 1 1 d . . . . .
H10 H 0.2470 0.4526 -0.0697 0.030 Uiso 1 1 calc R . . . .
C24 C 0.0893(4) 0.59370(19) 0.13613(16) 0.0182(9) Uani 1 1 d . . . . .
H24 H 0.1351 0.6104 0.1095 0.022 Uiso 1 1 calc R . . . .
C55 C 0.3694(4) 0.86591(19) 0.12575(16) 0.0172(9) Uani 1 1 d . . . . .
C60 C 0.3672(5) 0.9102(2) 0.16071(17) 0.0212(10) Uani 1 1 d . . . . .
H60 H 0.4490 0.9207 0.1808 0.025 Uiso 1 1 calc R . . . .
C46 C 0.5221(6) 0.9049(2) 0.3364(2) 0.0353(13) Uani 1 1 d . . . . .
H46 H 0.4899 0.9271 0.3630 0.042 Uiso 1 1 calc R . . . .
C45 C 0.6552(6) 0.9118(2) 0.32303(19) 0.0308(12) Uani 1 1 d . . . . .
H45 H 0.7141 0.9389 0.3404 0.037 Uiso 1 1 calc R . . . .
C56 C 0.2466(5) 0.8495(2) 0.09775(18) 0.0252(11) Uani 1 1 d . . . . .
H56 H 0.2455 0.8179 0.0754 0.030 Uiso 1 1 calc R . . . .
C32 C 0.3138(5) 0.6087(2) 0.31939(18) 0.0246(11) Uani 1 1 d . . . . .
H32 H 0.2822 0.5718 0.3102 0.029 Uiso 1 1 calc R . . . .
C65 C 0.5231(6) 0.9322(2) -0.01796(18) 0.0291(12) Uani 1 1 d . . . . .
H65 H 0.4568 0.9503 -0.0412 0.035 Uiso 1 1 calc R . . . .
C51 C 1.0150(5) 0.7106(2) 0.24185(18) 0.0271(11) Uani 1 1 d . . . . .
H51 H 1.0366 0.6729 0.2519 0.033 Uiso 1 1 calc R . . . .
C47 C 0.4378(6) 0.8663(2) 0.3112(2) 0.0358(13) Uani 1 1 d . . . . .
H47 H 0.3468 0.8617 0.3204 0.043 Uiso 1 1 calc R . . . .
C8 C 0.1234(5) 0.5682(2) -0.02378(19) 0.0244(10) Uani 1 1 d . . . . .
H8 H 0.0394 0.5842 -0.0153 0.029 Uiso 1 1 calc R . . . .
C52 C 1.1194(5) 0.7494(2) 0.23724(18) 0.0284(12) Uani 1 1 d . . . . .
H52 H 1.2124 0.7384 0.2450 0.034 Uiso 1 1 calc R . . . .
C63 C 0.7570(6) 0.9111(2) 0.0093(2) 0.0379(14) Uani 1 1 d . . . . .
H63 H 0.8519 0.9142 0.0046 0.045 Uiso 1 1 calc R . . . .
C59 C 0.2448(5) 0.9391(2) 0.16631(19) 0.0293(12) Uani 1 1 d . . . . .
H59 H 0.2432 0.9689 0.1905 0.035 Uiso 1 1 calc R . . . .
C58 C 0.1257(5) 0.9241(2) 0.1364(2) 0.0328(12) Uani 1 1 d . . . . .
H58 H 0.0434 0.9447 0.1393 0.039 Uiso 1 1 calc R . . . .
C57 C 0.1260(5) 0.8798(2) 0.1027(2) 0.0316(12) Uani 1 1 d . . . . .
H57 H 0.0437 0.8696 0.0826 0.038 Uiso 1 1 calc R . . . .
Cl1 Cl 0.1104(2) 0.95408(8) -0.04592(8) 0.0673(5) Uani 1 1 d . U . . .
Cl2 Cl 0.0850(2) 0.83248(7) -0.03010(7) 0.0658(5) Uani 1 1 d . U . . .
C67 C 0.1108(10) 0.8837(4) -0.0709(3) 0.080(3) Uani 1 1 d . U . . .
H67A H 0.0390 0.8811 -0.1000 0.096 Uiso 1 1 calc R . . . .
H67B H 0.2004 0.8770 -0.0846 0.096 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
U1 O3 2.387(3) . ?
U1 O2 1.767(3) . ?
U1 O1 1.764(3) . ?
U1 O5 2.378(3) . ?
U1 O4 2.403(3) . ?
U1 O6 2.375(3) . ?
U1 O7 2.429(3) . ?
P2 O4 1.518(3) . ?
P2 N1 1.596(3) . ?
P2 C19 1.808(4) . ?
P2 C25 1.808(4) . ?
P4 O6 1.520(3) . ?
P4 N2 1.594(4) . ?
P4 C43 1.808(4) . ?
P4 C49 1.803(4) . ?
P1 O3 1.500(3) . ?
P1 C1 1.803(5) . ?
P1 C7 1.805(5) . ?
P1 C13 1.807(4) . ?
P3 O5 1.514(3) . ?
P3 N1 1.589(4) . ?
P3 C31 1.805(4) . ?
P3 C37 1.808(4) . ?
P5 O7 1.523(3) . ?
P5 N2 1.600(4) . ?
P5 C61 1.814(4) . ?
P5 C55 1.809(5) . ?
C19 C20 1.393(6) . ?
C19 C24 1.392(6) . ?
C43 C44 1.382(6) . ?
C43 C48 1.404(6) . ?
C1 C2 1.400(6) . ?
C1 C6 1.396(6) . ?
C7 C12 1.393(6) . ?
C7 C8 1.386(6) . ?
C42 H42 0.9500 . ?
C42 C37 1.397(6) . ?
C42 C41 1.391(6) . ?
C31 C36 1.400(6) . ?
C31 C32 1.387(6) . ?
C37 C38 1.390(6) . ?
C25 C26 1.393(6) . ?
C25 C30 1.404(6) . ?
C62 H62 0.9500 . ?
C62 C61 1.391(6) . ?
C62 C63 1.389(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.390(6) . ?
C61 C66 1.397(6) . ?
C54 H54 0.9500 . ?
C54 C49 1.402(6) . ?
C54 C53 1.390(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.391(7) . ?
C39 H39 0.9500 . ?
C39 C38 1.390(6) . ?
C39 C40 1.383(7) . ?
C36 H36 0.9500 . ?
C36 C35 1.389(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.383(7) . ?
C38 H38 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.396(6) . ?
C49 C50 1.399(6) . ?
C35 H35 0.9500 . ?
C35 C34 1.367(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(6) . ?
C14 H14 0.9500 . ?
C14 C13 1.393(6) . ?
C14 C15 1.392(6) . ?
C13 C18 1.393(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.380(7) . ?
C4 H4 0.9500 . ?
C4 C3 1.379(7) . ?
C4 C5 1.384(7) . ?
C27 H27 0.9500 . ?
C27 C26 1.399(6) . ?
C27 C28 1.373(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(6) . ?
C26 H26 0.9500 . ?
C48 H48 0.9500 . ?
C48 C47 1.401(7) . ?
C18 H18 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.382(7) . ?
C40 H40 0.9500 . ?
C40 C41 1.385(7) . ?
C41 H41 0.9500 . ?
C30 H30 0.9500 . ?
C30 C29 1.384(6) . ?
C66 H66 0.9500 . ?
C66 C65 1.395(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(6) . ?
C3 H3 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.388(7) . ?
C11 C10 1.384(7) . ?
C64 H64 0.9500 . ?
C64 C65 1.378(8) . ?
C64 C63 1.383(8) . ?
C33 H33 0.9500 . ?
C33 C34 1.383(7) . ?
C33 C32 1.392(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.384(7) . ?
C9 C8 1.390(7) . ?
C5 H5 0.9500 . ?
C50 H50 0.9500 . ?
C50 C51 1.380(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.397(7) . ?
C53 H53 0.9500 . ?
C53 C52 1.385(8) . ?
C34 H34 0.9500 . ?
C29 H29 0.9500 . ?
C12 H12 0.9500 . ?
C10 H10 0.9500 . ?
C24 H24 0.9500 . ?
C55 C60 1.394(6) . ?
C55 C56 1.402(6) . ?
C60 H60 0.9500 . ?
C60 C59 1.399(7) . ?
C46 H46 0.9500 . ?
C46 C45 1.388(8) . ?
C46 C47 1.361(8) . ?
C45 H45 0.9500 . ?
C56 H56 0.9500 . ?
C56 C57 1.397(7) . ?
C32 H32 0.9500 . ?
C65 H65 0.9500 . ?
C51 H51 0.9500 . ?
C51 C52 1.387(7) . ?
C47 H47 0.9500 . ?
C8 H8 0.9500 . ?
C52 H52 0.9500 . ?
C63 H63 0.9500 . ?
C59 H59 0.9500 . ?
C59 C58 1.388(7) . ?
C58 H58 0.9500 . ?
C58 C57 1.373(8) . ?
C57 H57 0.9500 . ?
Cl1 C67 1.792(8) . ?
Cl2 C67 1.651(8) . ?
C67 H67A 0.9900 . ?
C67 H67B 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
O3 U1 O4 73.52(10) . . ?
O3 U1 O7 72.02(10) . . ?
O2 U1 O3 91.44(12) . . ?
O2 U1 O5 87.53(12) . . ?
O2 U1 O4 92.37(13) . . ?
O2 U1 O6 96.20(13) . . ?
O2 U1 O7 87.74(13) . . ?
O1 U1 O3 87.96(12) . . ?
O1 U1 O2 179.10(15) . . ?
O1 U1 O5 92.61(12) . . ?
O1 U1 O4 86.82(13) . . ?
O1 U1 O6 84.68(12) . . ?
O1 U1 O7 92.71(12) . . ?
O5 U1 O3 146.59(10) . . ?
O5 U1 O4 73.17(9) . . ?
O5 U1 O7 141.19(9) . . ?
O4 U1 O7 145.53(9) . . ?
O6 U1 O3 143.81(10) . . ?
O6 U1 O5 69.28(10) . . ?
O6 U1 O4 140.97(10) . . ?
O6 U1 O7 73.01(10) . . ?
O4 P2 N1 117.49(18) . . ?
O4 P2 C19 108.84(18) . . ?
O4 P2 C25 108.84(18) . . ?
N1 P2 C19 109.23(19) . . ?
N1 P2 C25 106.2(2) . . ?
C19 P2 C25 105.57(19) . . ?
O6 P4 N2 116.23(18) . . ?
O6 P4 C43 107.75(19) . . ?
O6 P4 C49 107.9(2) . . ?
N2 P4 C43 108.0(2) . . ?
N2 P4 C49 109.0(2) . . ?
C49 P4 C43 107.64(19) . . ?
O3 P1 C1 110.62(19) . . ?
O3 P1 C7 112.11(19) . . ?
O3 P1 C13 109.86(19) . . ?
C1 P1 C7 109.8(2) . . ?
C1 P1 C13 108.5(2) . . ?
C7 P1 C13 105.75(19) . . ?
O5 P3 N1 117.68(17) . . ?
O5 P3 C31 108.39(19) . . ?
O5 P3 C37 108.21(18) . . ?
N1 P3 C31 110.64(19) . . ?
N1 P3 C37 107.6(2) . . ?
C31 P3 C37 103.31(19) . . ?
O7 P5 N2 116.12(18) . . ?
O7 P5 C61 111.23(18) . . ?
O7 P5 C55 107.55(19) . . ?
N2 P5 C61 104.6(2) . . ?
N2 P5 C55 113.0(2) . . ?
C55 P5 C61 103.6(2) . . ?
P1 O3 U1 173.03(19) . . ?
P3 O5 U1 134.32(16) . . ?
P2 O4 U1 134.48(16) . . ?
P4 O6 U1 141.44(17) . . ?
P5 O7 U1 136.74(16) . . ?
P4 N2 P5 121.0(2) . . ?
P3 N1 P2 123.4(2) . . ?
C20 C19 P2 120.3(3) . . ?
C24 C19 P2 120.6(3) . . ?
C24 C19 C20 119.1(4) . . ?
C44 C43 P4 122.8(3) . . ?
C44 C43 C48 118.4(4) . . ?
C48 C43 P4 118.5(4) . . ?
C2 C1 P1 118.5(3) . . ?
C6 C1 P1 123.3(4) . . ?
C6 C1 C2 118.3(4) . . ?
C12 C7 P1 116.2(3) . . ?
C8 C7 P1 125.2(4) . . ?
C8 C7 C12 118.6(4) . . ?
C37 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C41 C42 C37 120.0(4) . . ?
C36 C31 P3 119.7(3) . . ?
C32 C31 P3 121.6(4) . . ?
C32 C31 C36 118.6(4) . . ?
C42 C37 P3 119.6(3) . . ?
C38 C37 P3 121.4(3) . . ?
C38 C37 C42 119.0(4) . . ?
C26 C25 P2 121.1(3) . . ?
C26 C25 C30 118.8(4) . . ?
C30 C25 P2 120.1(3) . . ?
C61 C62 H62 119.7 . . ?
C63 C62 H62 119.7 . . ?
C63 C62 C61 120.6(5) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.8(4) . . ?
C21 C20 H20 119.6 . . ?
C62 C61 P5 119.4(3) . . ?
C62 C61 C66 118.8(4) . . ?
C66 C61 P5 121.8(3) . . ?
C49 C54 H54 120.1 . . ?
C53 C54 H54 120.1 . . ?
C53 C54 C49 119.9(5) . . ?
C20 C21 H21 120.3 . . ?
C20 C21 C22 119.4(4) . . ?
C22 C21 H21 120.3 . . ?
C38 C39 H39 120.4 . . ?
C40 C39 H39 120.4 . . ?
C40 C39 C38 119.2(4) . . ?
C31 C36 H36 119.9 . . ?
C35 C36 C31 120.2(4) . . ?
C35 C36 H36 119.9 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.1(4) . . ?
C23 C22 H22 120.0 . . ?
C37 C38 H38 119.5 . . ?
C39 C38 C37 121.1(4) . . ?
C39 C38 H38 119.5 . . ?
C43 C44 H44 119.5 . . ?
C43 C44 C45 121.0(5) . . ?
C45 C44 H44 119.5 . . ?
C54 C49 P4 122.4(3) . . ?
C50 C49 P4 118.5(3) . . ?
C50 C49 C54 119.0(4) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 C36 120.7(5) . . ?
C34 C35 H35 119.7 . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 120.9(4) . . ?
C3 C2 H2 119.5 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C15 C14 C13 119.8(4) . . ?
C14 C13 P1 122.0(3) . . ?
C18 C13 P1 118.3(3) . . ?
C18 C13 C14 119.7(4) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.1(4) . . ?
C16 C15 H15 119.9 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C28 C27 C26 120.0(4) . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.2(4) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.1(4) . . ?
C18 C17 H17 119.9 . . ?
C25 C26 C27 120.4(4) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C43 C48 H48 120.0 . . ?
C47 C48 C43 120.0(5) . . ?
C47 C48 H48 120.0 . . ?
C13 C18 H18 120.0 . . ?
C17 C18 C13 119.9(4) . . ?
C17 C18 H18 120.0 . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.4(4) . . ?
C5 C6 H6 119.8 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.6(4) . . ?
C41 C40 H40 119.7 . . ?
C42 C41 H41 120.0 . . ?
C40 C41 C42 120.0(4) . . ?
C40 C41 H41 120.0 . . ?
C25 C30 H30 119.7 . . ?
C29 C30 C25 120.6(4) . . ?
C29 C30 H30 119.7 . . ?
C61 C66 H66 120.0 . . ?
C65 C66 C61 119.9(5) . . ?
C65 C66 H66 120.0 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.4(4) . . ?
C24 C23 H23 119.8 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 H3 120.0 . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C10 C11 C12 119.1(5) . . ?
C65 C64 H64 120.3 . . ?
C65 C64 C63 119.5(5) . . ?
C63 C64 H64 120.3 . . ?
C34 C33 H33 119.9 . . ?
C34 C33 C32 120.1(5) . . ?
C32 C33 H33 119.9 . . ?
C10 C9 H9 119.6 . . ?
C10 C9 C8 120.7(5) . . ?
C8 C9 H9 119.6 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(4) . . ?
C6 C5 H5 119.7 . . ?
C49 C50 H50 119.7 . . ?
C51 C50 C49 120.7(5) . . ?
C51 C50 H50 119.7 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.4(4) . . ?
C29 C28 H28 119.8 . . ?
C54 C53 H53 119.9 . . ?
C52 C53 C54 120.1(5) . . ?
C52 C53 H53 119.9 . . ?
C35 C34 C33 119.9(4) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C30 C29 C28 119.7(4) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C7 C12 H12 119.2 . . ?
C11 C12 C7 121.6(5) . . ?
C11 C12 H12 119.2 . . ?
C11 C10 C9 119.9(5) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C19 C24 H24 120.0 . . ?
C23 C24 C19 120.1(4) . . ?
C23 C24 H24 120.0 . . ?
C60 C55 P5 122.3(3) . . ?
C60 C55 C56 119.1(4) . . ?
C56 C55 P5 118.3(4) . . ?
C55 C60 H60 119.9 . . ?
C55 C60 C59 120.2(4) . . ?
C59 C60 H60 119.9 . . ?
C45 C46 H46 120.1 . . ?
C47 C46 H46 120.1 . . ?
C47 C46 C45 119.9(5) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 C44 119.9(5) . . ?
C46 C45 H45 120.0 . . ?
C55 C56 H56 120.0 . . ?
C57 C56 C55 120.0(5) . . ?
C57 C56 H56 120.0 . . ?
C31 C32 C33 120.5(5) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C66 C65 H65 119.6 . . ?
C64 C65 C66 120.7(5) . . ?
C64 C65 H65 119.6 . . ?
C50 C51 H51 120.1 . . ?
C50 C51 C52 119.9(5) . . ?
C52 C51 H51 120.1 . . ?
C48 C47 H47 119.6 . . ?
C46 C47 C48 120.8(5) . . ?
C46 C47 H47 119.6 . . ?
C7 C8 C9 120.1(5) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C53 C52 C51 120.4(5) . . ?
C53 C52 H52 119.8 . . ?
C51 C52 H52 119.8 . . ?
C62 C63 H63 119.8 . . ?
C64 C63 C62 120.4(5) . . ?
C64 C63 H63 119.8 . . ?
C60 C59 H59 120.1 . . ?
C58 C59 C60 119.8(5) . . ?
C58 C59 H59 120.1 . . ?
C59 C58 H58 119.8 . . ?
C57 C58 C59 120.4(5) . . ?
C57 C58 H58 119.8 . . ?
C56 C57 H57 119.8 . . ?
C58 C57 C56 120.3(5) . . ?
C58 C57 H57 119.8 . . ?
Cl1 C67 H67A 108.2 . . ?
Cl1 C67 H67B 108.2 . . ?
Cl2 C67 Cl1 116.3(4) . . ?
Cl2 C67 H67A 108.2 . . ?
Cl2 C67 H67B 108.2 . . ?
H67A C67 H67B 107.4 . . ?

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
P2 C19 C20 C21 179.0(4) . . . . ?
P2 C19 C24 C23 -179.1(3) . . . . ?
P2 C25 C26 C27 -177.8(3) . . . . ?
P2 C25 C30 C29 178.5(3) . . . . ?
P4 C43 C44 C45 174.0(4) . . . . ?
P4 C43 C48 C47 -174.5(4) . . . . ?
P4 C49 C50 C51 179.6(3) . . . . ?
P1 C1 C2 C3 179.4(4) . . . . ?
P1 C1 C6 C5 179.9(4) . . . . ?
P1 C7 C12 C11 -178.8(4) . . . . ?
P1 C7 C8 C9 177.9(4) . . . . ?
P1 C13 C18 C17 179.6(3) . . . . ?
P3 C31 C36 C35 -174.2(4) . . . . ?
P3 C31 C32 C33 174.7(4) . . . . ?
P3 C37 C38 C39 -178.2(3) . . . . ?
P5 C61 C66 C65 178.6(4) . . . . ?
P5 C55 C60 C59 171.9(4) . . . . ?
P5 C55 C56 C57 -170.3(4) . . . . ?
O3 P1 C1 C2 2.6(4) . . . . ?
O3 P1 C1 C6 -178.2(4) . . . . ?
O3 P1 C7 C12 -58.3(4) . . . . ?
O3 P1 C7 C8 122.4(4) . . . . ?
O3 P1 C13 C14 163.6(4) . . . . ?
O3 P1 C13 C18 -16.6(4) . . . . ?
O5 P3 N1 P2 -21.5(3) . . . . ?
O5 P3 C31 C36 -28.9(4) . . . . ?
O5 P3 C31 C32 154.9(4) . . . . ?
O5 P3 C37 C42 46.8(4) . . . . ?
O5 P3 C37 C38 -134.7(3) . . . . ?
O4 P2 N1 P3 19.9(3) . . . . ?
O4 P2 C19 C20 -167.6(3) . . . . ?
O4 P2 C19 C24 12.2(4) . . . . ?
O4 P2 C25 C26 126.1(4) . . . . ?
O4 P2 C25 C30 -53.6(4) . . . . ?
O6 P4 N2 P5 14.6(3) . . . . ?
O6 P4 C43 C44 155.8(4) . . . . ?
O6 P4 C43 C48 -29.9(4) . . . . ?
O6 P4 C49 C54 164.9(3) . . . . ?
O6 P4 C49 C50 -13.9(4) . . . . ?
O7 P5 N2 P4 -41.2(3) . . . . ?
O7 P5 C61 C62 -94.9(4) . . . . ?
O7 P5 C61 C66 85.9(4) . . . . ?
O7 P5 C55 C60 151.8(4) . . . . ?
O7 P5 C55 C56 -33.9(4) . . . . ?
N2 P4 O6 U1 25.9(4) . . . . ?
N2 P4 C43 C44 -77.9(4) . . . . ?
N2 P4 C43 C48 96.4(4) . . . . ?
N2 P4 C49 C54 37.8(4) . . . . ?
N2 P4 C49 C50 -140.9(3) . . . . ?
N2 P5 O7 U1 39.0(3) . . . . ?
N2 P5 C61 C62 31.2(4) . . . . ?
N2 P5 C61 C66 -148.0(4) . . . . ?
N2 P5 C55 C60 22.3(4) . . . . ?
N2 P5 C55 C56 -163.5(3) . . . . ?
N1 P2 O4 U1 -39.6(3) . . . . ?
N1 P2 C19 C20 -38.2(4) . . . . ?
N1 P2 C19 C24 141.6(4) . . . . ?
N1 P2 C25 C26 -1.3(4) . . . . ?
N1 P2 C25 C30 179.0(3) . . . . ?
N1 P3 O5 U1 43.5(3) . . . . ?
N1 P3 C31 C36 -159.4(3) . . . . ?
N1 P3 C31 C32 24.5(4) . . . . ?
N1 P3 C37 C42 174.9(3) . . . . ?
N1 P3 C37 C38 -6.6(4) . . . . ?
C19 P2 O4 U1 85.1(3) . . . . ?
C19 P2 N1 P3 -104.6(3) . . . . ?
C19 P2 C25 C26 -117.2(4) . . . . ?
C19 P2 C25 C30 63.1(4) . . . . ?
C19 C20 C21 C22 0.2(7) . . . . ?
C43 P4 O6 U1 147.2(3) . . . . ?
C43 P4 N2 P5 -106.6(3) . . . . ?
C43 P4 C49 C54 -79.1(4) . . . . ?
C43 P4 C49 C50 102.1(4) . . . . ?
C43 C44 C45 C46 0.4(7) . . . . ?
C43 C48 C47 C46 0.1(8) . . . . ?
C1 P1 C7 C12 178.4(3) . . . . ?
C1 P1 C7 C8 -1.0(5) . . . . ?
C1 P1 C13 C14 -75.3(4) . . . . ?
C1 P1 C13 C18 104.4(4) . . . . ?
C1 C2 C3 C4 1.8(7) . . . . ?
C1 C6 C5 C4 -0.2(8) . . . . ?
C7 P1 C1 C2 126.8(4) . . . . ?
C7 P1 C1 C6 -53.9(5) . . . . ?
C7 P1 C13 C14 42.5(4) . . . . ?
C7 P1 C13 C18 -137.8(4) . . . . ?
C42 C37 C38 C39 0.3(6) . . . . ?
C31 P3 O5 U1 -82.9(3) . . . . ?
C31 P3 N1 P2 103.9(3) . . . . ?
C31 P3 C37 C42 -68.0(4) . . . . ?
C31 P3 C37 C38 110.5(4) . . . . ?
C31 C36 C35 C34 -0.9(7) . . . . ?
C37 P3 O5 U1 165.7(2) . . . . ?
C37 P3 N1 P2 -143.9(2) . . . . ?
C37 P3 C31 C36 85.7(4) . . . . ?
C37 P3 C31 C32 -90.4(4) . . . . ?
C37 C42 C41 C40 0.4(7) . . . . ?
C25 P2 O4 U1 -160.3(2) . . . . ?
C25 P2 N1 P3 142.0(2) . . . . ?
C25 P2 C19 C20 75.7(4) . . . . ?
C25 P2 C19 C24 -104.5(4) . . . . ?
C25 C30 C29 C28 -0.2(7) . . . . ?
C62 C61 C66 C65 -0.6(7) . . . . ?
C20 C19 C24 C23 0.7(7) . . . . ?
C20 C21 C22 C23 0.6(7) . . . . ?
C61 P5 O7 U1 158.5(2) . . . . ?
C61 P5 N2 P4 -164.2(3) . . . . ?
C61 P5 C55 C60 -90.3(4) . . . . ?
C61 P5 C55 C56 83.9(4) . . . . ?
C61 C62 C63 C64 1.3(8) . . . . ?
C61 C66 C65 C64 0.5(7) . . . . ?
C54 C49 C50 C51 0.9(6) . . . . ?
C54 C53 C52 C51 0.7(7) . . . . ?
C21 C22 C23 C24 -0.8(7) . . . . ?
C39 C40 C41 C42 0.0(7) . . . . ?
C36 C31 C32 C33 -1.5(7) . . . . ?
C36 C35 C34 C33 -0.8(8) . . . . ?
C22 C23 C24 C19 0.1(7) . . . . ?
C38 C39 C40 C41 -0.2(7) . . . . ?
C44 C43 C48 C47 0.0(7) . . . . ?
C49 P4 O6 U1 -96.8(3) . . . . ?
C49 P4 N2 P5 136.7(3) . . . . ?
C49 P4 C43 C44 39.7(4) . . . . ?
C49 P4 C43 C48 -146.0(4) . . . . ?
C49 C54 C53 C52 0.9(7) . . . . ?
C49 C50 C51 C52 0.7(7) . . . . ?
C2 C1 C6 C5 -0.9(7) . . . . ?
C14 C13 C18 C17 -0.7(7) . . . . ?
C14 C15 C16 C17 -1.7(7) . . . . ?
C13 P1 C1 C2 -118.0(4) . . . . ?
C13 P1 C1 C6 61.2(4) . . . . ?
C13 P1 C7 C12 61.4(4) . . . . ?
C13 P1 C7 C8 -117.9(4) . . . . ?
C13 C14 C15 C16 1.2(7) . . . . ?
C15 C14 C13 P1 179.7(3) . . . . ?
C15 C14 C13 C18 0.0(7) . . . . ?
C15 C16 C17 C18 1.0(7) . . . . ?
C27 C28 C29 C30 1.0(7) . . . . ?
C16 C17 C18 C13 0.2(7) . . . . ?
C26 C25 C30 C29 -1.2(6) . . . . ?
C26 C27 C28 C29 -0.3(7) . . . . ?
C48 C43 C44 C45 -0.3(7) . . . . ?
C6 C1 C2 C3 0.1(7) . . . . ?
C40 C39 C38 C37 0.1(7) . . . . ?
C41 C42 C37 P3 178.0(3) . . . . ?
C41 C42 C37 C38 -0.6(6) . . . . ?
C30 C25 C26 C27 1.9(6) . . . . ?
C3 C4 C5 C6 2.1(8) . . . . ?
C5 C4 C3 C2 -2.9(7) . . . . ?
C50 C51 C52 C53 -1.5(7) . . . . ?
C28 C27 C26 C25 -1.2(7) . . . . ?
C53 C54 C49 P4 179.6(3) . . . . ?
C53 C54 C49 C50 -1.6(6) . . . . ?
C34 C33 C32 C31 -0.2(8) . . . . ?
C12 C7 C8 C9 -1.4(7) . . . . ?
C12 C11 C10 C9 -0.8(7) . . . . ?
C10 C11 C12 C7 0.6(8) . . . . ?
C10 C9 C8 C7 1.2(8) . . . . ?
C24 C19 C20 C21 -0.9(7) . . . . ?
C55 P5 O7 U1 -88.7(3) . . . . ?
C55 P5 N2 P4 83.7(3) . . . . ?
C55 P5 C61 C62 149.8(4) . . . . ?
C55 P5 C61 C66 -29.4(4) . . . . ?
C55 C60 C59 C58 -0.9(7) . . . . ?
C55 C56 C57 C58 -2.6(8) . . . . ?
C60 C55 C56 C57 4.1(7) . . . . ?
C60 C59 C58 C57 2.4(8) . . . . ?
C45 C46 C47 C48 0.0(8) . . . . ?
C56 C55 C60 C59 -2.3(7) . . . . ?
C32 C31 C36 C35 2.0(7) . . . . ?
C32 C33 C34 C35 1.3(8) . . . . ?
C65 C64 C63 C62 -1.4(8) . . . . ?
C47 C46 C45 C44 -0.3(8) . . . . ?
C8 C7 C12 C11 0.6(7) . . . . ?
C8 C9 C10 C11 -0.1(8) . . . . ?
C63 C62 C61 P5 -179.5(4) . . . . ?
C63 C62 C61 C66 -0.2(7) . . . . ?
C63 C64 C65 C66 0.5(8) . . . . ?
C59 C58 C57 C56 -0.6(8) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 4 -36 0.0696 -0.9995 3.9988 -35.9968 -0.2140 -0.9213 0.3128
1 -4 36 0.0513 0.9995 -3.9988 35.9968 0.2140 0.9213 -0.3128
14 3 -6 0.5838 13.9997 3.0013 -6.0026 0.0840 0.3041 0.9713
-14 -2 2 0.5802 -13.9996 -2.0014 2.0031 -0.0917 -0.4079 -0.9276
0 -33 -4 0.0600 -0.0005 -33.0015 -4.0075 -0.9686 0.2129 -0.0688
-1 33 4 0.0140 -0.9995 33.0014 4.0077 0.9648 -0.2468 0.0045

_olex2_date_sample_data_collection 2012-04-20
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
