# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_CCA-28-L-Pro
_database_code_depnum_ccdc_archive 'CCDC 2352908'
loop_
_audit_author_name
_audit_author_address
'Pascal Retailleau'
;ICSN CNRS University Paris Saclay
France
;
_audit_update_record             
;
2024-05-03 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_CCA-28-L-Pro        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:  Very poor crystals diffracting little beyond atomic resolution 
;
_vrf_PLAT089_CCA-28-L-Pro        
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........ 3.88 Note  
RESPONSE: Due to limited resolution data and relatively large structure. 
Rigid-bond restraints throughout the model and other SHELXL commands 
were used to refine the structure anisotropically in a satisfactory 
manner.
;
_vrf_PLAT340_CCA-28-L-Pro        
;
PROBLEM: Low Bond Precision on  C-C Bonds .............  0.03067 Ang.  
RESPONSE: See above
;
_vrf_STRVA01_CCA-28-L-Pro        
;
PROBLEM: Chirality of atom sites is inverted?
RESPONSE: the molecule was synthesized using L-prolin building blocks 
and the absence of anomalous scatterers led us to refine the model as
a 2-component inversion twin without considering the fraction value. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H59 F9 N10 O13, 3(H2 O)'
_chemical_formula_sum            'C47 H65 F9 N10 O16'
_chemical_formula_weight         1197.09

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

_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'

_cell_length_a                   6.7234(16)
_cell_length_b                   10.105(2)
_cell_length_c                   19.638(5)
_cell_angle_alpha                91.057(19)
_cell_angle_beta                 90.07(2)
_cell_angle_gamma                93.418(18)
_cell_volume                     1331.6(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1089
_cell_measurement_theta_min      3.0190
_cell_measurement_theta_max      24.1110

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             626
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.019
_exptl_absorpt_coefficient_mu    0.132
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.121a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      123(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            10538
_diffrn_reflns_av_unetI/netI     0.1726
_diffrn_reflns_av_R_equivalents  0.1186
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.035
_diffrn_reflns_theta_max         21.485
_diffrn_reflns_theta_full        21.485
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             5817
_reflns_number_gt                4033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_max     0.915
_reflns_Friedel_fraction_full    0.915

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro system (CCD 42.75a 64-bit)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0582P)²+9.0585P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   1(4)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         5814
_refine_ls_number_parameters     779
_refine_ls_number_restraints     1240
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.1101
_refine_ls_wR_factor_ref         0.2600
_refine_ls_wR_factor_gt          0.2404
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      0.985
_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
F2 F 1.117(2) 1.0701(14) -0.0252(7) 0.059(4) Uani 1 1 d . U . . .
O2 O 0.744(2) 1.2407(15) 0.2211(9) 0.045(4) Uani 1 1 d . U . . .
N2 N 0.821(3) 1.1282(16) 0.1250(10) 0.038(4) Uani 1 1 d . U . . .
C1 C 0.657(4) 1.630(2) 0.1420(14) 0.058(7) Uani 1 1 d . U . . .
H1A H 0.764333 1.700273 0.146190 0.087 Uiso 1 1 calc R U . . .
H1B H 0.582128 1.625217 0.184717 0.087 Uiso 1 1 calc R U . . .
H1C H 0.567731 1.651020 0.104752 0.087 Uiso 1 1 calc R U . . .
F1 F 1.2169(19) 1.1401(14) 0.0735(8) 0.055(4) Uani 1 1 d . U . . .
O1 O 0.659(2) 1.4146(16) 0.0863(9) 0.051(4) Uani 1 1 d . U . . .
F3 F 1.079(2) 0.9435(13) 0.0605(8) 0.060(4) Uani 1 1 d . U . . .
O3 O 0.723(2) 1.0425(15) 0.0209(9) 0.049(4) Uani 1 1 d . U . . .
N3 N 0.543(2) 0.9281(17) 0.2429(10) 0.033(4) Uani 1 1 d . U . . .
F4 F 1.0546(17) 0.3729(11) 0.4062(8) 0.052(4) Uani 1 1 d . U . . .
F5 F 0.9519(18) 0.1881(12) 0.3575(7) 0.044(3) Uani 1 1 d . U . . .
F6 F 0.9240(16) 0.2115(13) 0.4655(7) 0.045(3) Uani 1 1 d . U . . .
F7 F 0.9031(18) -0.1264(13) 0.7359(9) 0.065(4) Uani 1 1 d . U . . .
O4 O 0.861(2) 0.9296(17) 0.2162(9) 0.053(5) Uani 1 1 d . U . . .
N4 N 0.766(2) 0.7526(16) 0.3832(10) 0.032(4) Uani 1 1 d . U . . .
O5 O 0.566(2) 0.6612(13) 0.3018(9) 0.038(4) Uani 1 1 d . U . . .
O6 O 0.5571(19) 0.6159(13) 0.4869(7) 0.029(3) Uani 1 1 d D U . . .
N5 N 0.649(2) 0.4146(16) 0.4494(9) 0.030(4) Uani 1 1 d . U . . .
N6 N 0.391(2) 0.3931(15) 0.6103(8) 0.017(3) Uani 1 1 d . U . . .
O7 O 0.557(2) 0.2217(13) 0.3951(8) 0.035(3) Uani 1 1 d . U . . .
F8 F 0.762(2) -0.2419(14) 0.6533(9) 0.063(4) Uani 1 1 d . U . . .
F9 F 0.736(2) -0.3067(12) 0.7569(8) 0.059(4) Uani 1 1 d . U . . .
O8 O 0.7078(19) 0.3350(13) 0.5880(8) 0.032(4) Uani 1 1 d D U . . .
O9 O 0.422(2) 0.1539(14) 0.6841(8) 0.039(4) Uani 1 1 d D U . . .
N7 N 0.635(3) 0.2655(15) 0.7569(10) 0.031(4) Uani 1 1 d . U . . .
N8 N 0.517(2) -0.0728(17) 0.7944(9) 0.029(3) Uani 1 1 d . U . . .
N9 N 0.291(3) -0.2832(17) 0.9297(10) 0.039(4) Uani 1 1 d . U . . .
O10 O 0.468(2) 0.1009(15) 0.8645(8) 0.044(4) Uani 1 1 d . U . . .
O11 O 0.386(2) -0.2043(14) 0.7095(8) 0.041(4) Uani 1 1 d . U . . .
O12 O 0.616(2) -0.2408(16) 0.9000(10) 0.054(5) Uani 1 1 d . U . . .
O13 O 0.293(2) -0.5253(16) 0.8732(9) 0.044(4) Uani 1 1 d . U . . .
N10 N 0.408(3) -0.6253(19) 0.9656(12) 0.055(6) Uani 1 1 d . U . . .
H10A H 0.414784 -0.701672 0.943662 0.067 Uiso 1 1 calc R U . . .
H10B H 0.443654 -0.618139 1.008735 0.067 Uiso 1 1 calc R U . . .
N1 N 0.913(3) 1.4707(19) 0.1601(12) 0.051(5) Uani 1 1 d . U . . .
C2 C 0.742(4) 1.504(2) 0.1278(14) 0.047(5) Uani 1 1 d . U . . .
C3 C 1.022(4) 1.556(2) 0.2091(14) 0.055(6) Uani 1 1 d D U . . .
H3A H 0.929254 1.603034 0.238826 0.066 Uiso 0.6 1 calc R U P A 1
H3B H 1.111939 1.621709 0.186068 0.066 Uiso 0.6 1 calc R U P A 1
H3C H 0.945966 1.562178 0.252119 0.066 Uiso 0.4 1 calc R U P B 2
H3D H 1.047108 1.646012 0.190951 0.066 Uiso 0.4 1 calc R U P B 2
C4 C 1.138(6) 1.460(3) 0.2495(18) 0.056(9) Uani 0.6 1 d D U P C 1
H4A H 1.269013 1.500752 0.264311 0.067 Uiso 0.6 1 calc R U P C 1
H4B H 1.062935 1.427743 0.289791 0.067 Uiso 0.6 1 calc R U P C 1
C4B C 1.213(6) 1.491(3) 0.220(4) 0.065(14) Uani 0.4 1 d D U P C 2
H4BA H 1.252631 1.496466 0.268802 0.077 Uiso 0.4 1 calc R U P C 2
H4BB H 1.321183 1.531955 0.192256 0.077 Uiso 0.4 1 calc R U P C 2
C5 C 1.162(4) 1.350(3) 0.1980(14) 0.055(6) Uani 1 1 d D U . . .
H5A H 1.288389 1.366480 0.172809 0.067 Uiso 0.6 1 calc R U P C 1
H5B H 1.167311 1.264599 0.221442 0.067 Uiso 0.6 1 calc R U P C 1
H5C H 1.279243 1.313341 0.175740 0.067 Uiso 0.4 1 calc R U P C 2
H5D H 1.127218 1.296028 0.238222 0.067 Uiso 0.4 1 calc R U P C 2
C6 C 0.992(3) 1.344(2) 0.1498(13) 0.039(4) Uani 1 1 d . U . . .
H6 H 1.039135 1.332775 0.101864 0.046 Uiso 1 1 calc R U . . .
C7 C 0.831(3) 1.240(2) 0.1666(14) 0.039(5) Uani 1 1 d . U . . .
C8 C 0.866(3) 1.125(2) 0.0510(13) 0.036(4) Uani 1 1 d . U . . .
H8 H 0.864120 1.215799 0.031848 0.043 Uiso 1 1 calc R U . . .
C9 C 0.651(5) 0.946(2) 0.0713(14) 0.062(7) Uani 1 1 d . U . . .
H9A H 0.740881 0.873155 0.075413 0.074 Uiso 1 1 calc R U . . .
H9B H 0.514462 0.909443 0.060200 0.074 Uiso 1 1 calc R U . . .
C10 C 0.653(4) 1.032(2) 0.1347(13) 0.043(4) Uani 1 1 d . U . . .
H10 H 0.525525 1.078053 0.139116 0.051 Uiso 1 1 calc R U . . .
C11 C 1.077(3) 1.067(2) 0.0400(13) 0.037(3) Uani 1 1 d . U . . .
C12 C 0.696(3) 0.956(2) 0.2010(13) 0.035(5) Uani 1 1 d . U . . .
C13 C 0.330(3) 0.943(3) 0.2316(12) 0.045(6) Uani 1 1 d D U . . .
H13A H 0.283399 0.896843 0.189085 0.054 Uiso 0.65 1 calc R U P D 3
H13B H 0.300693 1.037767 0.229194 0.054 Uiso 0.65 1 calc R U P D 3
H13C H 0.253057 0.856540 0.227746 0.054 Uiso 0.35 1 calc R U P E 4
H13D H 0.304758 0.996841 0.191178 0.054 Uiso 0.35 1 calc R U P E 4
C15 C 0.373(3) 0.925(2) 0.3489(12) 0.041(5) Uani 1 1 d D U . . .
H15A H 0.354204 0.870296 0.389887 0.049 Uiso 0.65 1 calc R U P F 3
H15B H 0.357850 1.019356 0.361320 0.049 Uiso 0.65 1 calc R U P F 3
H15C H 0.291083 0.840767 0.352548 0.049 Uiso 0.35 1 calc R U P G 4
H15D H 0.388618 0.968100 0.394405 0.049 Uiso 0.35 1 calc R U P G 4
C16 C 0.575(3) 0.9050(18) 0.3147(11) 0.023(4) Uani 1 1 d . U . . .
H16 H 0.677317 0.971840 0.333309 0.028 Uiso 1 1 calc R U . . .
C17 C 0.636(3) 0.7603(19) 0.3316(12) 0.029(4) Uani 1 1 d . U . . .
C18 C 0.862(3) 0.862(2) 0.4255(12) 0.035(5) Uani 1 1 d . U . . .
H18A H 0.760939 0.918956 0.445315 0.042 Uiso 1 1 calc R U . . .
H18B H 0.956656 0.918046 0.398072 0.042 Uiso 1 1 calc R U . . .
C19 C 0.970(3) 0.792(2) 0.4807(13) 0.038(5) Uani 1 1 d . U . . .
H19A H 1.096134 0.842519 0.493443 0.045 Uiso 1 1 calc R U . . .
H19B H 0.885998 0.781518 0.521767 0.045 Uiso 1 1 calc R U . . .
C20 C 1.010(3) 0.662(2) 0.4497(13) 0.039(5) Uani 1 1 d . U . . .
H20A H 1.026470 0.595348 0.485162 0.047 Uiso 1 1 calc R U . . .
H20B H 1.131071 0.668656 0.421134 0.047 Uiso 1 1 calc R U . . .
C21 C 0.822(3) 0.627(2) 0.4058(12) 0.028(4) Uani 1 1 d . U . . .
H21 H 0.857295 0.570142 0.365822 0.033 Uiso 1 1 calc R U . . .
C22 C 0.655(3) 0.554(2) 0.4474(11) 0.026(3) Uani 1 1 d . U . . .
C23 C 0.701(3) 0.3316(19) 0.3942(12) 0.028(3) Uani 1 1 d . U . . .
H23 H 0.700210 0.378827 0.349924 0.034 Uiso 1 1 calc R U . . .
C24 C 0.907(3) 0.269(2) 0.4072(13) 0.037(3) Uani 1 1 d . U . . .
C25 C 0.489(3) 0.211(2) 0.4635(11) 0.032(4) Uani 1 1 d . U . . .
H25A H 0.577677 0.156696 0.490316 0.038 Uiso 1 1 calc R U . . .
H25B H 0.351873 0.169572 0.464949 0.038 Uiso 1 1 calc R U . . .
C26 C 0.495(3) 0.355(2) 0.4913(11) 0.027(4) Uani 1 1 d . U . . .
H26 H 0.365576 0.395206 0.482184 0.032 Uiso 1 1 calc R U . . .
C27 C 0.540(3) 0.3605(18) 0.5674(11) 0.019(3) Uani 1 1 d . U . . .
C28 C 0.191(3) 0.441(2) 0.5883(12) 0.032(5) Uani 1 1 d . U . . .
H28A H 0.206277 0.509148 0.553077 0.038 Uiso 1 1 calc R U . . .
H28B H 0.100499 0.366360 0.571398 0.038 Uiso 1 1 calc R U . . .
C29 C 0.121(3) 0.496(2) 0.6544(11) 0.035(5) Uani 1 1 d . U . . .
H29A H -0.025992 0.492557 0.656128 0.042 Uiso 1 1 calc R U . . .
H29B H 0.172229 0.589916 0.660565 0.042 Uiso 1 1 calc R U . . .
C30 C 0.204(3) 0.411(2) 0.7080(12) 0.030(5) Uani 1 1 d . U . . .
H30A H 0.208701 0.457520 0.752997 0.036 Uiso 1 1 calc R U . . .
H30B H 0.124084 0.326295 0.711776 0.036 Uiso 1 1 calc R U . . .
C31 C 0.408(3) 0.3910(18) 0.6815(10) 0.018(3) Uani 1 1 d . U . . .
H31 H 0.499076 0.467918 0.696728 0.021 Uiso 1 1 calc R U . . .
C32 C 0.493(3) 0.263(2) 0.7070(12) 0.029(4) Uani 1 1 d . U . . .
C33 C 0.726(3) 0.379(2) 0.7943(12) 0.033(5) Uani 1 1 d . U . . .
H33A H 0.624317 0.437105 0.812049 0.040 Uiso 1 1 calc R U . . .
H33B H 0.820680 0.431358 0.765251 0.040 Uiso 1 1 calc R U . . .
C34 C 0.834(3) 0.316(2) 0.8517(13) 0.039(5) Uani 1 1 d . U . . .
H34A H 0.958070 0.368855 0.863956 0.046 Uiso 1 1 calc R U . . .
H34B H 0.748483 0.307686 0.892547 0.046 Uiso 1 1 calc R U . . .
C35 C 0.880(3) 0.183(2) 0.8247(12) 0.037(5) Uani 1 1 d . U . . .
H35A H 0.887451 0.119354 0.862118 0.044 Uiso 1 1 calc R U . . .
H35B H 1.009170 0.187901 0.800290 0.044 Uiso 1 1 calc R U . . .
C36 C 0.712(3) 0.141(2) 0.7765(12) 0.032(4) Uani 1 1 d . U . . .
H36 H 0.762232 0.092396 0.735916 0.038 Uiso 1 1 calc R U . . .
C37 C 0.552(3) 0.058(2) 0.8133(12) 0.034(4) Uani 1 1 d . U . . .
C38 C 0.549(3) -0.120(2) 0.7258(11) 0.030(4) Uani 1 1 d . U . . .
H38 H 0.558054 -0.044039 0.693945 0.036 Uiso 1 1 calc R U . . .
C39 C 0.311(3) -0.263(2) 0.7716(13) 0.039(5) Uani 1 1 d . U . . .
H39A H 0.372816 -0.347216 0.780309 0.047 Uiso 1 1 calc R U . . .
H39B H 0.164391 -0.279416 0.769531 0.047 Uiso 1 1 calc R U . . .
C40 C 0.370(3) -0.158(2) 0.8270(12) 0.034(4) Uani 1 1 d . U . . .
H40 H 0.251656 -0.106472 0.838122 0.041 Uiso 1 1 calc R U . . .
C41 C 0.743(3) -0.203(2) 0.7195(16) 0.047(4) Uani 1 1 d . U . . .
C42 C 0.438(3) -0.221(2) 0.8903(12) 0.040(5) Uani 1 1 d . U . . .
C43 C 0.079(3) -0.274(3) 0.9218(14) 0.047(6) Uani 1 1 d . U . . .
H43A H 0.034448 -0.304400 0.875729 0.057 Uiso 1 1 calc R U . . .
H43B H 0.040868 -0.181578 0.929417 0.057 Uiso 1 1 calc R U . . .
C44 C -0.010(3) -0.365(3) 0.9764(14) 0.055(7) Uani 1 1 d . U . . .
H44A H -0.068259 -0.448755 0.955689 0.066 Uiso 1 1 calc R U . . .
H44B H -0.114686 -0.321463 1.002276 0.066 Uiso 1 1 calc R U . . .
C45 C 0.168(3) -0.392(3) 1.0233(14) 0.049(6) Uani 1 1 d . U . . .
H45A H 0.189638 -0.321923 1.058722 0.058 Uiso 1 1 calc R U . . .
H45B H 0.148326 -0.479263 1.045501 0.058 Uiso 1 1 calc R U . . .
C46 C 0.343(3) -0.392(2) 0.9730(13) 0.039(4) Uani 1 1 d . U . . .
H46 H 0.473391 -0.370800 0.996792 0.046 Uiso 1 1 calc R U . . .
C47 C 0.345(4) -0.520(2) 0.9334(13) 0.039(5) Uani 1 1 d . U . . .
C14 C 0.233(5) 0.879(4) 0.2934(12) 0.047(8) Uani 0.65 1 d D U P H 3
H14A H 0.098325 0.910617 0.301279 0.056 Uiso 0.65 1 calc R U P H 3
H14B H 0.224438 0.781374 0.288749 0.056 Uiso 0.65 1 calc R U P H 3
C14B C 0.288(9) 1.016(5) 0.2976(15) 0.044(10) Uani 0.35 1 d D U P H 4
H14C H 0.357777 1.105132 0.299357 0.053 Uiso 0.35 1 calc R U P H 4
H14D H 0.143748 1.024363 0.304458 0.053 Uiso 0.35 1 calc R U P H 4
O1W O 0.480(3) 0.8948(17) 0.5342(10) 0.054(5) Uani 1 1 d D U . . .
H1W1 H 0.47(2) 0.814(7) 0.524(13) 0.080 Uiso 1 1 d D U . . .
H1W2 H 0.376(19) 0.920(11) 0.552(11) 0.080 Uiso 1 1 d D U . . .
O2W O 0.194(2) 0.0625(17) 0.5748(9) 0.049(5) Uani 1 1 d D U . . .
H2W1 H 0.25(3) 0.09(2) 0.612(6) 0.073 Uiso 1 1 d D U . . .
H2W2 H 0.073(7) 0.074(19) 0.580(10) 0.073 Uiso 1 1 d D U . . .
O3W O 0.786(2) 0.0503(14) 0.6000(9) 0.047(5) Uani 1 1 d D U . . .
H3W1 H 0.77(3) 0.131(6) 0.602(10) 0.070 Uiso 1 1 d D U . . .
H3W2 H 0.70(2) 0.019(16) 0.571(7) 0.070 Uiso 1 1 d D U . . .


_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
F2 C11 1.31(3) . ?
O2 C7 1.22(3) . ?
N2 C7 1.38(3) . ?
N2 C10 1.46(3) . ?
N2 C8 1.49(3) . ?
C1 C2 1.45(3) . ?
F1 C11 1.32(3) . ?
O1 C2 1.31(3) . ?
F3 C11 1.32(3) . ?
O3 C8 1.36(3) . ?
O3 C9 1.46(3) . ?
N3 C12 1.34(3) . ?
N3 C16 1.45(3) . ?
N3 C13 1.47(3) . ?
F4 C24 1.40(2) . ?
F5 C24 1.31(3) . ?
F6 C24 1.30(3) . ?
F7 C41 1.32(3) . ?
O4 C12 1.20(3) . ?
N4 C17 1.35(3) . ?
N4 C21 1.43(3) . ?
N4 C18 1.49(3) . ?
O5 C17 1.22(2) . ?
O6 C22 1.21(2) . ?
N5 C22 1.41(3) . ?
N5 C23 1.42(3) . ?
N5 C26 1.43(3) . ?
N6 C27 1.36(2) . ?
N6 C31 1.40(2) . ?
N6 C28 1.52(2) . ?
O7 C25 1.42(3) . ?
O7 C23 1.43(2) . ?
F8 C41 1.36(3) . ?
F9 C41 1.29(3) . ?
O8 C27 1.24(2) . ?
O9 C32 1.25(2) . ?
N7 C32 1.37(3) . ?
N7 C36 1.44(3) . ?
N7 C33 1.45(3) . ?
N8 C37 1.37(3) . ?
N8 C40 1.44(3) . ?
N8 C38 1.44(3) . ?
N9 C42 1.38(3) . ?
N9 C43 1.45(3) . ?
N9 C46 1.46(3) . ?
O10 C37 1.24(3) . ?
O11 C38 1.38(2) . ?
O11 C39 1.44(3) . ?
O12 C42 1.24(3) . ?
O13 C47 1.23(3) . ?
N10 C47 1.34(3) . ?
N1 C2 1.37(3) . ?
N1 C6 1.43(3) . ?
N1 C3 1.44(3) . ?
C3 C4B 1.49(3) . ?
C3 C4 1.52(3) . ?
C4 C5 1.50(3) . ?
C4B C5 1.50(3) . ?
C5 C6 1.48(3) . ?
C6 C7 1.51(3) . ?
C8 C11 1.58(3) . ?
C9 C10 1.50(4) . ?
C10 C12 1.56(3) . ?
C13 C14B 1.51(3) . ?
C13 C14 1.51(3) . ?
C15 C14 1.49(2) . ?
C15 C14B 1.51(3) . ?
C15 C16 1.54(3) . ?
C16 C17 1.58(3) . ?
C18 C19 1.51(3) . ?
C19 C20 1.48(3) . ?
C20 C21 1.55(3) . ?
C21 C22 1.54(3) . ?
C23 C24 1.58(3) . ?
C25 C26 1.55(3) . ?
C26 C27 1.52(3) . ?
C28 C29 1.49(3) . ?
C29 C30 1.50(3) . ?
C30 C31 1.50(3) . ?
C31 C32 1.54(3) . ?
C33 C34 1.51(3) . ?
C34 C35 1.48(3) . ?
C35 C36 1.51(3) . ?
C36 C37 1.52(3) . ?
C38 C41 1.59(3) . ?
C39 C40 1.54(3) . ?
C40 C42 1.49(3) . ?
C43 C44 1.53(3) . ?
C44 C45 1.55(3) . ?
C45 C46 1.54(3) . ?
C46 C47 1.50(3) . ?

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
C7 N2 C10 117(2) . . ?
C7 N2 C8 125.7(18) . . ?
C10 N2 C8 106.0(18) . . ?
C8 O3 C9 108.0(19) . . ?
C12 N3 C16 121.1(17) . . ?
C12 N3 C13 129.0(19) . . ?
C16 N3 C13 108.6(17) . . ?
C17 N4 C21 120.3(17) . . ?
C17 N4 C18 128.4(17) . . ?
C21 N4 C18 111.2(17) . . ?
C22 N5 C23 124.3(17) . . ?
C22 N5 C26 115.2(16) . . ?
C23 N5 C26 113.0(16) . . ?
C27 N6 C31 123.0(15) . . ?
C27 N6 C28 125.4(16) . . ?
C31 N6 C28 111.6(15) . . ?
C25 O7 C23 106.6(15) . . ?
C32 N7 C36 118.2(18) . . ?
C32 N7 C33 128.8(17) . . ?
C36 N7 C33 113.0(17) . . ?
C37 N8 C40 122.2(19) . . ?
C37 N8 C38 122.4(18) . . ?
C40 N8 C38 109.6(17) . . ?
C42 N9 C43 126(2) . . ?
C42 N9 C46 118.9(18) . . ?
C43 N9 C46 113.3(17) . . ?
C38 O11 C39 108.0(16) . . ?
C2 N1 C6 122(2) . . ?
C2 N1 C3 124(2) . . ?
C6 N1 C3 115(2) . . ?
O1 C2 N1 116(2) . . ?
O1 C2 C1 123(2) . . ?
N1 C2 C1 121(2) . . ?
N1 C3 C4B 105(3) . . ?
N1 C3 C4 103(2) . . ?
C5 C4 C3 102(2) . . ?
C3 C4B C5 103(3) . . ?
C6 C5 C4B 110(3) . . ?
C6 C5 C4 110(2) . . ?
N1 C6 C5 102(2) . . ?
N1 C6 C7 107.9(19) . . ?
C5 C6 C7 114(2) . . ?
O2 C7 N2 121(2) . . ?
O2 C7 C6 122(2) . . ?
N2 C7 C6 116(2) . . ?
O3 C8 N2 106.8(18) . . ?
O3 C8 C11 109.8(19) . . ?
N2 C8 C11 109.0(18) . . ?
O3 C9 C10 101.0(18) . . ?
N2 C10 C9 104(2) . . ?
N2 C10 C12 106.9(19) . . ?
C9 C10 C12 113.6(19) . . ?
F2 C11 F3 109(2) . . ?
F2 C11 F1 109(2) . . ?
F3 C11 F1 108.7(19) . . ?
F2 C11 C8 108.0(19) . . ?
F3 C11 C8 111.5(19) . . ?
F1 C11 C8 110.8(19) . . ?
O4 C12 N3 121(2) . . ?
O4 C12 C10 122(2) . . ?
N3 C12 C10 117.4(19) . . ?
N3 C13 C14B 98(3) . . ?
N3 C13 C14 103(2) . . ?
C14 C15 C16 101(2) . . ?
C14B C15 C16 99(3) . . ?
N3 C16 C15 105.2(16) . . ?
N3 C16 C17 114.7(17) . . ?
C15 C16 C17 107.7(16) . . ?
O5 C17 N4 121.5(18) . . ?
O5 C17 C16 123.0(19) . . ?
N4 C17 C16 115.4(17) . . ?
N4 C18 C19 104.2(16) . . ?
C20 C19 C18 104(2) . . ?
C19 C20 C21 103.7(18) . . ?
N4 C21 C22 112.4(17) . . ?
N4 C21 C20 103.1(17) . . ?
C22 C21 C20 111.8(18) . . ?
O6 C22 N5 120.1(18) . . ?
O6 C22 C21 119.9(19) . . ?
N5 C22 C21 118.6(17) . . ?
N5 C23 O7 104.9(16) . . ?
N5 C23 C24 111.6(18) . . ?
O7 C23 C24 104.7(15) . . ?
F6 C24 F5 110.3(19) . . ?
F6 C24 F4 106.3(18) . . ?
F5 C24 F4 105.4(18) . . ?
F6 C24 C23 115.5(19) . . ?
F5 C24 C23 111.6(19) . . ?
F4 C24 C23 106.9(16) . . ?
O7 C25 C26 104.8(16) . . ?
N5 C26 C27 114.8(16) . . ?
N5 C26 C25 100.2(17) . . ?
C27 C26 C25 110.9(16) . . ?
O8 C27 N6 122.7(19) . . ?
O8 C27 C26 119.8(17) . . ?
N6 C27 C26 117.5(16) . . ?
C29 C28 N6 100.1(16) . . ?
C28 C29 C30 105.3(18) . . ?
C31 C30 C29 101.9(17) . . ?
N6 C31 C30 105.4(16) . . ?
N6 C31 C32 112.8(17) . . ?
C30 C31 C32 112.9(16) . . ?
O9 C32 N7 119.5(18) . . ?
O9 C32 C31 118.8(18) . . ?
N7 C32 C31 121.5(19) . . ?
N7 C33 C34 103.1(16) . . ?
C35 C34 C33 105(2) . . ?
C34 C35 C36 105.8(18) . . ?
N7 C36 C35 103.5(17) . . ?
N7 C36 C37 110.0(18) . . ?
C35 C36 C37 110.3(19) . . ?
O10 C37 N8 119(2) . . ?
O10 C37 C36 121(2) . . ?
N8 C37 C36 119(2) . . ?
O11 C38 N8 106.4(17) . . ?
O11 C38 C41 107.9(17) . . ?
N8 C38 C41 112.3(19) . . ?
O11 C39 C40 104.1(16) . . ?
N8 C40 C42 115.0(17) . . ?
N8 C40 C39 103.6(18) . . ?
C42 C40 C39 111.4(19) . . ?
F9 C41 F7 109(2) . . ?
F9 C41 F8 109(2) . . ?
F7 C41 F8 108(2) . . ?
F9 C41 C38 113(2) . . ?
F7 C41 C38 110.0(19) . . ?
F8 C41 C38 108(2) . . ?
O12 C42 N9 121(2) . . ?
O12 C42 C40 122(2) . . ?
N9 C42 C40 116.2(19) . . ?
N9 C43 C44 104(2) . . ?
C43 C44 C45 104.7(19) . . ?
C46 C45 C44 102(2) . . ?
N9 C46 C47 111(2) . . ?
N9 C46 C45 99.8(18) . . ?
C47 C46 C45 111.2(19) . . ?
O13 C47 N10 122(2) . . ?
O13 C47 C46 120(2) . . ?
N10 C47 C46 117(2) . . ?
C15 C14 C13 102(2) . . ?
C15 C14B C13 101(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C2 O1 -1(3) . . . . ?
C3 N1 C2 O1 -178(2) . . . . ?
C6 N1 C2 C1 176(2) . . . . ?
C3 N1 C2 C1 -1(4) . . . . ?
C2 N1 C3 C4B -170(4) . . . . ?
C6 N1 C3 C4B 13(4) . . . . ?
C2 N1 C3 C4 158(3) . . . . ?
C6 N1 C3 C4 -19(3) . . . . ?
N1 C3 C4 C5 28(3) . . . . ?
N1 C3 C4B C5 -21(5) . . . . ?
C3 C4B C5 C6 24(6) . . . . ?
C3 C4 C5 C6 -29(4) . . . . ?
C2 N1 C6 C5 -176(2) . . . . ?
C3 N1 C6 C5 1(3) . . . . ?
C2 N1 C6 C7 -56(3) . . . . ?
C3 N1 C6 C7 121(2) . . . . ?
C4B C5 C6 N1 -16(4) . . . . ?
C4 C5 C6 N1 18(3) . . . . ?
C4B C5 C6 C7 -132(4) . . . . ?
C4 C5 C6 C7 -98(3) . . . . ?
C10 N2 C7 O2 22(3) . . . . ?
C8 N2 C7 O2 161(2) . . . . ?
C10 N2 C7 C6 -173.2(19) . . . . ?
C8 N2 C7 C6 -34(3) . . . . ?
N1 C6 C7 O2 -54(3) . . . . ?
C5 C6 C7 O2 59(3) . . . . ?
N1 C6 C7 N2 142(2) . . . . ?
C5 C6 C7 N2 -106(3) . . . . ?
C9 O3 C8 N2 -27(2) . . . . ?
C9 O3 C8 C11 91(2) . . . . ?
C7 N2 C8 O3 -137(2) . . . . ?
C10 N2 C8 O3 5(2) . . . . ?
C7 N2 C8 C11 104(2) . . . . ?
C10 N2 C8 C11 -113.4(19) . . . . ?
C8 O3 C9 C10 38(3) . . . . ?
C7 N2 C10 C9 164(2) . . . . ?
C8 N2 C10 C9 18(2) . . . . ?
C7 N2 C10 C12 -75(2) . . . . ?
C8 N2 C10 C12 138.4(18) . . . . ?
O3 C9 C10 N2 -33(2) . . . . ?
O3 C9 C10 C12 -149(2) . . . . ?
O3 C8 C11 F2 66(2) . . . . ?
N2 C8 C11 F2 -177.5(18) . . . . ?
O3 C8 C11 F3 -54(3) . . . . ?
N2 C8 C11 F3 63(2) . . . . ?
O3 C8 C11 F1 -174.9(19) . . . . ?
N2 C8 C11 F1 -58(2) . . . . ?
C16 N3 C12 O4 19(3) . . . . ?
C13 N3 C12 O4 -175(2) . . . . ?
C16 N3 C12 C10 -156.3(19) . . . . ?
C13 N3 C12 C10 9(3) . . . . ?
N2 C10 C12 O4 -36(3) . . . . ?
C9 C10 C12 O4 79(3) . . . . ?
N2 C10 C12 N3 140(2) . . . . ?
C9 C10 C12 N3 -106(3) . . . . ?
C12 N3 C13 C14B -131(3) . . . . ?
C16 N3 C13 C14B 36(3) . . . . ?
C12 N3 C13 C14 173(2) . . . . ?
C16 N3 C13 C14 -20(3) . . . . ?
C12 N3 C16 C15 161.0(19) . . . . ?
C13 N3 C16 C15 -7(2) . . . . ?
C12 N3 C16 C17 -81(2) . . . . ?
C13 N3 C16 C17 110.8(19) . . . . ?
C14 C15 C16 N3 32(2) . . . . ?
C14B C15 C16 N3 -25(3) . . . . ?
C14 C15 C16 C17 -91(2) . . . . ?
C14B C15 C16 C17 -148(2) . . . . ?
C21 N4 C17 O5 -2(3) . . . . ?
C18 N4 C17 O5 -179(2) . . . . ?
C21 N4 C17 C16 175.8(17) . . . . ?
C18 N4 C17 C16 -1(3) . . . . ?
N3 C16 C17 O5 -38(3) . . . . ?
C15 C16 C17 O5 79(3) . . . . ?
N3 C16 C17 N4 144.4(18) . . . . ?
C15 C16 C17 N4 -99(2) . . . . ?
C17 N4 C18 C19 173(2) . . . . ?
C21 N4 C18 C19 -4(2) . . . . ?
N4 C18 C19 C20 26(2) . . . . ?
C18 C19 C20 C21 -37(2) . . . . ?
C17 N4 C21 C22 -74(3) . . . . ?
C18 N4 C21 C22 103(2) . . . . ?
C17 N4 C21 C20 165.0(19) . . . . ?
C18 N4 C21 C20 -18(2) . . . . ?
C19 C20 C21 N4 34(2) . . . . ?
C19 C20 C21 C22 -87(2) . . . . ?
C23 N5 C22 O6 158(2) . . . . ?
C26 N5 C22 O6 11(3) . . . . ?
C23 N5 C22 C21 -35(3) . . . . ?
C26 N5 C22 C21 177.5(18) . . . . ?
N4 C21 C22 O6 -39(3) . . . . ?
C20 C21 C22 O6 76(3) . . . . ?
N4 C21 C22 N5 154.2(19) . . . . ?
C20 C21 C22 N5 -90(2) . . . . ?
C22 N5 C23 O7 -140.1(18) . . . . ?
C26 N5 C23 O7 8(2) . . . . ?
C22 N5 C23 C24 107(2) . . . . ?
C26 N5 C23 C24 -104.6(19) . . . . ?
C25 O7 C23 N5 -26(2) . . . . ?
C25 O7 C23 C24 91.4(19) . . . . ?
N5 C23 C24 F6 50(2) . . . . ?
O7 C23 C24 F6 -62(2) . . . . ?
N5 C23 C24 F5 177.5(17) . . . . ?
O7 C23 C24 F5 65(2) . . . . ?
N5 C23 C24 F4 -68(2) . . . . ?
O7 C23 C24 F4 179.5(17) . . . . ?
C23 O7 C25 C26 33(2) . . . . ?
C22 N5 C26 C27 -78(2) . . . . ?
C23 N5 C26 C27 130.2(18) . . . . ?
C22 N5 C26 C25 162.6(17) . . . . ?
C23 N5 C26 C25 11(2) . . . . ?
O7 C25 C26 N5 -27(2) . . . . ?
O7 C25 C26 C27 -148.5(16) . . . . ?
C31 N6 C27 O8 -5(3) . . . . ?
C28 N6 C27 O8 172.6(18) . . . . ?
C31 N6 C27 C26 174.6(16) . . . . ?
C28 N6 C27 C26 -8(3) . . . . ?
N5 C26 C27 O8 -44(2) . . . . ?
C25 C26 C27 O8 69(2) . . . . ?
N5 C26 C27 N6 136.7(17) . . . . ?
C25 C26 C27 N6 -110.6(19) . . . . ?
C27 N6 C28 C29 -164.2(17) . . . . ?
C31 N6 C28 C29 14(2) . . . . ?
N6 C28 C29 C30 -33(2) . . . . ?
C28 C29 C30 C31 41(2) . . . . ?
C27 N6 C31 C30 -171.1(17) . . . . ?
C28 N6 C31 C30 11(2) . . . . ?
C27 N6 C31 C32 -47(2) . . . . ?
C28 N6 C31 C32 134.6(17) . . . . ?
C29 C30 C31 N6 -31(2) . . . . ?
C29 C30 C31 C32 -154.6(18) . . . . ?
C36 N7 C32 O9 6(3) . . . . ?
C33 N7 C32 O9 -175(2) . . . . ?
C36 N7 C32 C31 -178.1(18) . . . . ?
C33 N7 C32 C31 1(3) . . . . ?
N6 C31 C32 O9 -48(3) . . . . ?
C30 C31 C32 O9 71(3) . . . . ?
N6 C31 C32 N7 136(2) . . . . ?
C30 C31 C32 N7 -104(2) . . . . ?
C32 N7 C33 C34 168(2) . . . . ?
C36 N7 C33 C34 -13(2) . . . . ?
N7 C33 C34 C35 27(2) . . . . ?
C33 C34 C35 C36 -32(2) . . . . ?
C32 N7 C36 C35 172.9(19) . . . . ?
C33 N7 C36 C35 -6(2) . . . . ?
C32 N7 C36 C37 -69(2) . . . . ?
C33 N7 C36 C37 112(2) . . . . ?
C34 C35 C36 N7 24(2) . . . . ?
C34 C35 C36 C37 -94(2) . . . . ?
C40 N8 C37 O10 7(3) . . . . ?
C38 N8 C37 O10 158(2) . . . . ?
C40 N8 C37 C36 179.5(19) . . . . ?
C38 N8 C37 C36 -30(3) . . . . ?
N7 C36 C37 O10 -56(3) . . . . ?
C35 C36 C37 O10 58(3) . . . . ?
N7 C36 C37 N8 132(2) . . . . ?
C35 C36 C37 N8 -114(2) . . . . ?
C39 O11 C38 N8 -29(2) . . . . ?
C39 O11 C38 C41 92(2) . . . . ?
C37 N8 C38 O11 -135.6(18) . . . . ?
C40 N8 C38 O11 18(2) . . . . ?
C37 N8 C38 C41 107(2) . . . . ?
C40 N8 C38 C41 -100(2) . . . . ?
C38 O11 C39 C40 28(2) . . . . ?
C37 N8 C40 C42 -85(3) . . . . ?
C38 N8 C40 C42 121(2) . . . . ?
C37 N8 C40 C39 153.1(19) . . . . ?
C38 N8 C40 C39 -1(2) . . . . ?
O11 C39 C40 N8 -16(2) . . . . ?
O11 C39 C40 C42 -140.2(18) . . . . ?
O11 C38 C41 F9 -57(3) . . . . ?
N8 C38 C41 F9 60(3) . . . . ?
O11 C38 C41 F7 -179(2) . . . . ?
N8 C38 C41 F7 -62(3) . . . . ?
O11 C38 C41 F8 64(2) . . . . ?
N8 C38 C41 F8 -179.3(16) . . . . ?
C43 N9 C42 O12 -177(2) . . . . ?
C46 N9 C42 O12 -13(3) . . . . ?
C43 N9 C42 C40 -11(3) . . . . ?
C46 N9 C42 C40 154(2) . . . . ?
N8 C40 C42 O12 -26(3) . . . . ?
C39 C40 C42 O12 92(2) . . . . ?
N8 C40 C42 N9 168(2) . . . . ?
C39 C40 C42 N9 -75(3) . . . . ?
C42 N9 C43 C44 178(2) . . . . ?
C46 N9 C43 C44 13(3) . . . . ?
N9 C43 C44 C45 14(3) . . . . ?
C43 C44 C45 C46 -33(3) . . . . ?
C42 N9 C46 C47 -82(2) . . . . ?
C43 N9 C46 C47 84(2) . . . . ?
C42 N9 C46 C45 160(2) . . . . ?
C43 N9 C46 C45 -33(2) . . . . ?
C44 C45 C46 N9 39(2) . . . . ?
C44 C45 C46 C47 -79(2) . . . . ?
N9 C46 C47 O13 -4(3) . . . . ?
C45 C46 C47 O13 106(3) . . . . ?
N9 C46 C47 N10 173.8(19) . . . . ?
C45 C46 C47 N10 -76(3) . . . . ?
C16 C15 C14 C13 -44(3) . . . . ?
N3 C13 C14 C15 40(3) . . . . ?
C16 C15 C14B C13 48(4) . . . . ?
N3 C13 C14B C15 -52(4) . . . . ?

_refine_diff_density_max         0.516
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.092




_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
