# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_structure_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1520676'
_audit_update_record             
;
2017-05-19 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_structure_1_sq      
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Given formula calculated on the presquezzed cell contents, expected calculated on the post squeeze model.
;
_vrf_PLAT058_structure_1_sq      
;
PROBLEM: Maximum Transmission Factor Missing ............          ?
RESPONSE: Value not supplied by XDS
;
_vrf_PLAT059_structure_1_sq      
;
PROBLEM: Minimum Transmission Factor Missing ............          ?
RESPONSE: Value not supplied by XDS
;
_vrf_PLAT184_structure_1_sq      
;
PROBLEM: Missing _cell_measurement_theta_min value ......     Please Do !
RESPONSE: Value not supplied by XDS
;
_vrf_PLAT185_structure_1_sq      
;
PROBLEM: Missing _cell_measurement_theta_max value ......     Please Do !
RESPONSE: Value not supplied by XDS
;
_vrf_THETM01_structure_1_sq      
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Low resolution weakly diffracting small needles. Best resolution available with a microfocus synchrotron beamline.
;
_vrf_PLAT340_structure_1_sq      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01255 Ang.
RESPONSE: Low resolution weakly diffracting small needles. Best resolution available with a microfocus synchrotron beamline.
;
_vrf_PLAT430_structure_1_sq      
;
PROBLEM: Short Inter D...A Contact  O2A    ..  O32     ..       2.56 Ang.
RESPONSE: Unresolved disorder due to low resolution data and an appropriate donor acceptor model could not be found
;
# Added during the CSD deposition process: Friday 19 May 2017 07:41 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H78 N10 O12, 18(H2 O)'
_chemical_formula_sum            'C44 H114 N10 O30'
_chemical_formula_weight         1263.45

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

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

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

_cell_length_a                   25.256(5)
_cell_length_b                   26.729(5)
_cell_length_c                   9.5380(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6439(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2469
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_F_000             2752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.001
_exptl_absorpt_coefficient_mu    0.109
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?


_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_diffrn_measurement_method       'Phi Scan'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36610
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_av_R_equivalents  0.1257
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.109
_diffrn_reflns_theta_max         23.327
_diffrn_reflns_theta_full        23.327
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             9053
_reflns_number_gt                5139
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_max     0.967
_reflns_Friedel_fraction_full    0.967

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


_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXLE (Hübschle, 2011)'
_computing_publication_material  'enCIFer (Allen, 2004)'

_refine_special_details          ', SQUEEZE, SQUEEZE'

# SQUEEZE RESULTS (Version = 301214)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.023 254 95 ' '
2 0.500 0.000 -0.018 655 262 ' '
3 1.000 0.500 -0.102 654 262 ' '
4 0.500 0.500 -0.035 253 95 ' '
5 0.788 0.166 0.051 9 0 ' '
6 0.212 0.834 0.051 9 0 ' '
7 0.288 0.334 0.949 9 0 ' '
8 0.712 0.666 0.949 8 0 ' '
# Missing Reflections Below sin(th)/lambda= 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
2 0 0 1.613
0 0 2 4.273
3 0 4 8.911
0 1 4 8.605
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          )
# Solvent Accessible Volume =    1899.4
# Electrons Found in S.A.V. =     715.6
# Note: Atoms in Void as Cxxx and Qxxx all others




_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1208P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1635 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.5(10)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         9053
_refine_ls_number_parameters     672
_refine_ls_number_restraints     604
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.2103
_refine_ls_wR_factor_gt          0.1768
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_restrained_S_all      0.956
_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
O1 O 0.4975(2) 0.3176(3) 0.9254(5) 0.089(2) Uani 1 1 d . U . . .
N1 N 0.5914(2) 0.3487(2) 0.7810(6) 0.0586(15) Uani 1 1 d . U . . .
H1 H 0.5935 0.3518 0.8726 0.070 Uiso 1 1 calc R U . . .
C1 C 0.5529(3) 0.3136(3) 0.7247(7) 0.0599(18) Uani 1 1 d . U . . .
H1A H 0.5490 0.3186 0.6214 0.072 Uiso 1 1 calc R U . . .
C19 C 0.2737(4) 0.6643(4) 0.8411(11) 0.106(3) Uani 1 1 d . U . . .
H19A H 0.2970 0.6897 0.7975 0.127 Uiso 1 1 calc R U . . .
H19B H 0.2852 0.6602 0.9397 0.127 Uiso 1 1 calc R U . . .
O6 O 0.3766(2) 0.6238(2) 0.5736(5) 0.0801(17) Uani 1 1 d . U . . .
C6 C 0.5009(3) 0.3238(3) 0.7976(7) 0.061(2) Uani 1 1 d . U . . .
C5 C 0.5309(5) 0.2185(5) 0.5415(11) 0.125(4) Uani 1 1 d . U . . .
H5A H 0.5191 0.2517 0.5113 0.188 Uiso 1 1 calc R U . . .
H5B H 0.5054 0.1932 0.5100 0.188 Uiso 1 1 calc R U . . .
H5C H 0.5657 0.2113 0.5008 0.188 Uiso 1 1 calc R U . . .
C52 C 0.6686(3) 0.4842(3) 0.2997(7) 0.0499(17) Uani 1 1 d . U . . .
O5 O 0.3160(2) 0.5061(2) 0.9315(5) 0.0727(15) Uani 1 1 d . U . . .
O4 O 0.3916(2) 0.3992(2) 0.5790(5) 0.0771(17) Uani 1 1 d . U . . .
N4 N 0.3320(2) 0.5437(2) 0.7226(6) 0.0537(14) Uani 1 1 d . U . . .
H4 H 0.3370 0.5396 0.6321 0.064 Uiso 1 1 calc R U . . .
C4 C 0.5553(6) 0.1673(4) 0.7507(16) 0.163(6) Uani 1 1 d . U . . .
H4A H 0.5317 0.1406 0.7179 0.244 Uiso 1 1 calc R U . . .
H4B H 0.5564 0.1671 0.8534 0.244 Uiso 1 1 calc R U . . .
H4C H 0.5910 0.1618 0.7135 0.244 Uiso 1 1 calc R U . . .
C49 C 0.7562(3) 0.4048(3) 0.3401(7) 0.072(2) Uani 1 1 d . U . . .
H49A H 0.7341 0.3796 0.3884 0.086 Uiso 1 1 calc R U . . .
H49B H 0.7589 0.4345 0.4016 0.086 Uiso 1 1 calc R U . . .
N3 N 0.3528(2) 0.4187(2) 0.7848(6) 0.0556(15) Uani 1 1 d . U . . .
H3 H 0.3554 0.4158 0.8765 0.067 Uiso 1 1 calc R U . . .
C8A C 0.3651(14) 0.3055(8) 0.754(3) 0.086(6) Uani 0.65 1 d D U P A 1
H8A1 H 0.3356 0.3130 0.8192 0.103 Uiso 0.65 1 calc R U P A 1
H8A2 H 0.3512 0.3092 0.6578 0.103 Uiso 0.65 1 calc R U P A 1
O2A O 0.3994(5) 0.2293(5) 0.6770(12) 0.122(4) Uani 0.65 1 d D U P A 1
O3A O 0.3719(7) 0.2351(6) 0.8847(16) 0.127(5) Uani 0.65 1 d D U P A 1
C9A C 0.3792(11) 0.2546(7) 0.773(2) 0.107(5) Uani 0.65 1 d D U P A 1
O34A O 0.4962(17) 0.3492(14) 0.421(2) 0.077(10) Uani 0.5 1 d . U P B 1
C51A C 0.8469(12) 0.3827(14) 0.453(4) 0.104(11) Uani 0.5 1 d . U P C 1
H51A H 0.8465 0.4161 0.4975 0.125 Uiso 0.5 1 calc R U P C 1
H51B H 0.8330 0.3579 0.5202 0.125 Uiso 0.5 1 calc R U P C 1
N35A N 0.9011(11) 0.3694(13) 0.411(4) 0.138(14) Uani 0.5 1 d . U P C 1
H35A H 0.9143 0.3463 0.4716 0.208 Uiso 0.5 1 calc R U P C 1
H35B H 0.9218 0.3972 0.4122 0.208 Uiso 0.5 1 calc R U P C 1
H35C H 0.9007 0.3563 0.3226 0.208 Uiso 0.5 1 calc R U P C 1
C8B C 0.367(3) 0.2982(16) 0.730(6) 0.091(9) Uani 0.35 1 d D U P A 2
H8B1 H 0.3302 0.3101 0.7284 0.109 Uiso 0.35 1 calc R U P A 2
H8B2 H 0.3765 0.2863 0.6350 0.109 Uiso 0.35 1 calc R U P A 2
C9B C 0.372(3) 0.2582(13) 0.827(4) 0.121(9) Uani 0.35 1 d D U P A 2
O3B O 0.3608(18) 0.2536(14) 0.949(3) 0.166(10) Uani 0.35 1 d D U P A 2
O2B O 0.3844(16) 0.2149(11) 0.805(4) 0.168(10) Uani 0.35 1 d D U P A 2
O34B O 0.5006(16) 0.3667(14) 0.398(2) 0.069(8) Uani 0.5 1 d . U P B 2
C51B C 0.8316(11) 0.3587(14) 0.454(3) 0.102(12) Uani 0.5 1 d . U P C 2
H51C H 0.8087 0.3300 0.4787 0.122 Uiso 0.5 1 calc R U P C 2
H51D H 0.8303 0.3833 0.5311 0.122 Uiso 0.5 1 calc R U P C 2
N35B N 0.8896(11) 0.3407(14) 0.431(5) 0.158(19) Uani 0.5 1 d . U P C 2
H35D H 0.8934 0.3293 0.3411 0.237 Uiso 0.5 1 calc R U P C 2
H35E H 0.8971 0.3155 0.4916 0.237 Uiso 0.5 1 calc R U P C 2
H35F H 0.9123 0.3666 0.4453 0.237 Uiso 0.5 1 calc R U P C 2
C3 C 0.5348(4) 0.2172(4) 0.7004(11) 0.094(3) Uani 1 1 d . U . . .
H3A H 0.4985 0.2224 0.7401 0.113 Uiso 1 1 calc R U . . .
N2 N 0.4593(2) 0.3348(2) 0.7158(6) 0.0543(15) Uani 1 1 d . U . . .
H2 H 0.4634 0.3357 0.6242 0.065 Uiso 1 1 calc R U . . .
C2 C 0.5712(3) 0.2589(3) 0.7556(10) 0.086(3) Uani 1 1 d . U . . .
H2A H 0.6068 0.2541 0.7144 0.103 Uiso 1 1 calc R U . . .
H2B H 0.5746 0.2549 0.8584 0.103 Uiso 1 1 calc R U . . .
C7 C 0.4074(3) 0.3454(3) 0.7753(8) 0.0618(19) Uani 1 1 d . U . . .
H7 H 0.4114 0.3522 0.8779 0.074 Uiso 1 1 calc R U . A 1
C18 C 0.2813(3) 0.6197(4) 0.7728(9) 0.083(2) Uani 1 1 d . U . . .
H18A H 0.2734 0.6253 0.6724 0.100 Uiso 1 1 calc R U . . .
H18B H 0.2544 0.5959 0.8084 0.100 Uiso 1 1 calc R U . . .
C12 C 0.2578(3) 0.4323(3) 0.7622(9) 0.076(2) Uani 1 1 d . U . . .
H12A H 0.2529 0.4011 0.7078 0.091 Uiso 1 1 calc R U . . .
H12B H 0.2566 0.4232 0.8628 0.091 Uiso 1 1 calc R U . . .
C11 C 0.3143(3) 0.4534(3) 0.7290(8) 0.0605(19) Uani 1 1 d . U . . .
H11 H 0.3192 0.4574 0.6255 0.073 Uiso 1 1 calc R U . . .
C10 C 0.3847(3) 0.3908(3) 0.7054(7) 0.0583(18) Uani 1 1 d . U . . .
C14 C 0.1615(5) 0.4415(6) 0.7764(17) 0.177(6) Uani 1 1 d . U . . .
H14A H 0.1662 0.4260 0.8688 0.265 Uiso 1 1 calc R U . . .
H14B H 0.1517 0.4157 0.7080 0.265 Uiso 1 1 calc R U . . .
H14C H 0.1333 0.4667 0.7815 0.265 Uiso 1 1 calc R U . . .
C13 C 0.2122(4) 0.4660(4) 0.7320(14) 0.116(3) Uani 1 1 d . U . . .
H13 H 0.2167 0.4992 0.7787 0.139 Uiso 1 1 calc R U . . .
C15 C 0.2088(5) 0.4714(7) 0.5805(16) 0.179(7) Uani 1 1 d . U . . .
H15A H 0.2444 0.4765 0.5419 0.269 Uiso 1 1 calc R U . . .
H15B H 0.1866 0.5003 0.5575 0.269 Uiso 1 1 calc R U . . .
H15C H 0.1933 0.4411 0.5399 0.269 Uiso 1 1 calc R U . . .
C16 C 0.3212(3) 0.5037(3) 0.8032(8) 0.0591(18) Uani 1 1 d . U . . .
C17 C 0.3357(3) 0.5934(3) 0.7814(8) 0.0579(18) Uani 1 1 d . U . . .
H17 H 0.3467 0.5909 0.8818 0.069 Uiso 1 1 calc R U . . .
C50 C 0.8118(3) 0.3831(4) 0.3153(9) 0.091(3) Uani 1 1 d . U . . .
H50A H 0.8299 0.4032 0.2424 0.109 Uiso 1 1 calc R U . C 1
H50B H 0.8084 0.3485 0.2796 0.109 Uiso 1 1 calc R U . C 1
C48 C 0.7304(3) 0.4193(3) 0.2060(7) 0.0637(19) Uani 1 1 d . U . . .
H48A H 0.7320 0.3905 0.1411 0.076 Uiso 1 1 calc R U . . .
H48B H 0.7511 0.4468 0.1631 0.076 Uiso 1 1 calc R U . . .
C47 C 0.6721(3) 0.4364(3) 0.2190(7) 0.0535(17) Uani 1 1 d . U . . .
H47 H 0.6586 0.4430 0.1222 0.064 Uiso 1 1 calc R U . . .
C46 C 0.6169(2) 0.3625(3) 0.2002(7) 0.0466(15) Uani 1 1 d . U . . .
C45 C 0.6986(5) 0.2225(4) 0.1983(13) 0.130(4) Uani 1 1 d . U . . .
H45A H 0.6958 0.2249 0.0960 0.195 Uiso 1 1 calc R U . . .
H45B H 0.6802 0.1924 0.2308 0.195 Uiso 1 1 calc R U . . .
H45C H 0.7360 0.2207 0.2252 0.195 Uiso 1 1 calc R U . . .
C44 C 0.6845(4) 0.2704(4) 0.4206(9) 0.089(3) Uani 1 1 d . U . . .
H44A H 0.7228 0.2695 0.4366 0.133 Uiso 1 1 calc R U . . .
H44B H 0.6680 0.2415 0.4664 0.133 Uiso 1 1 calc R U . . .
H44C H 0.6698 0.3013 0.4598 0.133 Uiso 1 1 calc R U . . .
C43 C 0.6735(3) 0.2685(4) 0.2648(9) 0.081(2) Uani 1 1 d . U . . .
H43 H 0.6908 0.2985 0.2220 0.097 Uiso 1 1 calc R U . . .
C42 C 0.6151(3) 0.2711(3) 0.2290(7) 0.0605(18) Uani 1 1 d . U . . .
H42A H 0.5967 0.2431 0.2762 0.073 Uiso 1 1 calc R U . . .
H42B H 0.6110 0.2663 0.1266 0.073 Uiso 1 1 calc R U . . .
C41 C 0.5874(2) 0.3206(3) 0.2708(7) 0.0500(16) Uani 1 1 d . U . . .
H41 H 0.5886 0.3250 0.3748 0.060 Uiso 1 1 calc R U . . .
C40 C 0.4930(3) 0.3398(3) 0.2934(7) 0.0568(18) Uani 1 1 d . U . . .
C39 C 0.4120(4) 0.2579(4) 0.3343(10) 0.089(3) Uani 1 1 d . U . . .
O33 O 0.4000(3) 0.2109(3) 0.3328(7) 0.125(3) Uani 1 1 d . U . . .
O32 O 0.4165(4) 0.2798(3) 0.4530(7) 0.124(3) Uani 1 1 d . U . . .
C38 C 0.4194(3) 0.2828(3) 0.2071(9) 0.076(2) Uani 1 1 d . U . . .
H38A H 0.3852 0.2834 0.1563 0.091 Uiso 1 1 calc R U . . .
H38B H 0.4447 0.2633 0.1496 0.091 Uiso 1 1 calc R U . . .
C37 C 0.4403(3) 0.3377(3) 0.2196(8) 0.0599(18) Uani 1 1 d . U . . .
H37 H 0.4463 0.3500 0.1219 0.072 Uiso 1 1 calc R U . . .
C36 C 0.3677(3) 0.3943(3) 0.2016(7) 0.0469(16) Uani 1 1 d . U . . .
C34 C 0.2147(4) 0.3234(5) 0.2230(12) 0.123(4) Uani 1 1 d . U . . .
H34A H 0.2128 0.3271 0.1209 0.185 Uiso 1 1 calc R U . . .
H34B H 0.1855 0.3420 0.2664 0.185 Uiso 1 1 calc R U . . .
H34C H 0.2119 0.2879 0.2478 0.185 Uiso 1 1 calc R U . . .
C33 C 0.2670(3) 0.3439(3) 0.2753(9) 0.076(2) Uani 1 1 d . U . . .
H33 H 0.2961 0.3268 0.2226 0.091 Uiso 1 1 calc R U . . .
C32 C 0.2702(3) 0.4004(3) 0.2431(8) 0.0633(19) Uani 1 1 d . U . . .
H32A H 0.2624 0.4058 0.1425 0.076 Uiso 1 1 calc R U . . .
H32B H 0.2427 0.4181 0.2981 0.076 Uiso 1 1 calc R U . . .
C31 C 0.3242(3) 0.4234(3) 0.2767(7) 0.0493(16) Uani 1 1 d . U . . .
H31 H 0.3305 0.4235 0.3802 0.059 Uiso 1 1 calc R U . . .
O36 O 0.6614(2) 0.48501(19) 0.4281(5) 0.0669(15) Uani 1 1 d . U . . .
O35 O 0.62025(19) 0.3644(2) 0.0707(5) 0.0627(14) Uani 1 1 d . U . . .
C35 C 0.2741(4) 0.3325(4) 0.4286(9) 0.093(3) Uani 1 1 d . U . . .
H35G H 0.2438 0.3457 0.4813 0.139 Uiso 1 1 calc R U . . .
H35H H 0.3067 0.3483 0.4624 0.139 Uiso 1 1 calc R U . . .
H35I H 0.2764 0.2963 0.4420 0.139 Uiso 1 1 calc R U . . .
N34 N 0.6394(2) 0.3975(2) 0.2806(5) 0.0486(13) Uani 1 1 d . U . . .
H24 H 0.6343 0.3970 0.3718 0.058 Uiso 1 1 calc R U . . .
N32 N 0.40205(19) 0.3696(2) 0.2808(5) 0.0479(13) Uani 1 1 d . U . . .
H22 H 0.4010 0.3731 0.3725 0.057 Uiso 1 1 calc R U . . .
C22 C 0.3759(3) 0.6233(3) 0.7022(8) 0.0591(19) Uani 1 1 d . U . . .
N33 N 0.5331(2) 0.3211(2) 0.2228(6) 0.0549(15) Uani 1 1 d . U . . .
H23 H 0.5263 0.3079 0.1402 0.066 Uiso 1 1 calc R U . . .
C20 C 0.2156(5) 0.6846(5) 0.8406(13) 0.130(4) Uani 1 1 d . U . . .
H20A H 0.2131 0.7146 0.9011 0.156 Uiso 1 1 calc R U . . .
H20B H 0.2054 0.6944 0.7441 0.156 Uiso 1 1 calc R U . . .
O31 O 0.36722(19) 0.39129(19) 0.0720(5) 0.0641(14) Uani 1 1 d . U . . .
N31 N 0.3249(2) 0.4745(2) 0.2212(6) 0.0524(14) Uani 1 1 d . U . . .
H21 H 0.3209 0.4784 0.1303 0.063 Uiso 1 1 calc R U . . .
C21 C 0.1783(5) 0.6445(5) 0.8941(14) 0.127(4) Uani 1 1 d . U . . .
H21A H 0.1922 0.6310 0.9836 0.152 Uiso 1 1 calc R U . . .
H21B H 0.1773 0.6166 0.8257 0.152 Uiso 1 1 calc R U . . .
N5 N 0.1189(4) 0.6651(4) 0.9187(10) 0.137(4) Uani 1 1 d . U . . .
H5D H 0.1036 0.6719 0.8344 0.206 Uiso 1 1 calc R U . . .
H5E H 0.1201 0.6935 0.9712 0.206 Uiso 1 1 calc R U . . .
H5F H 0.0995 0.6415 0.9644 0.206 Uiso 1 1 calc R 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
O1 C6 1.234(7) . ?
N1 C22 1.345(9) 2_665 ?
N1 C1 1.453(9) . ?
N1 H1 0.8800 . ?
C1 C6 1.512(10) . ?
C1 C2 1.560(12) . ?
C1 H1A 1.0000 . ?
C19 C18 1.371(12) . ?
C19 C20 1.566(15) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
O6 C22 1.226(8) . ?
C6 N2 1.342(9) . ?
C5 C3 1.518(13) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C52 O36 1.238(7) . ?
C52 N31 1.343(9) 2_665 ?
C52 C47 1.494(10) . ?
O5 C16 1.233(7) . ?
O4 C10 1.238(8) . ?
N4 C16 1.345(9) . ?
N4 C17 1.443(9) . ?
N4 H4 0.8800 . ?
C4 C3 1.509(15) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C49 C48 1.487(10) . ?
C49 C50 1.536(11) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
N3 C10 1.333(9) . ?
N3 C11 1.447(9) . ?
N3 H3 0.8800 . ?
C8A C9A 1.42(2) . ?
C8A C7 1.52(3) . ?
C8A H8A1 0.9900 . ?
C8A H8A2 0.9900 . ?
O2A C9A 1.250(16) . ?
O3A C9A 1.198(15) . ?
O34A C40 1.24(2) . ?
C51A N35A 1.47(3) . ?
C51A C50 1.58(3) . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
N35A H35A 0.9100 . ?
N35A H35B 0.9100 . ?
N35A H35C 0.9100 . ?
C8B C9B 1.42(3) . ?
C8B C7 1.67(6) . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
C9B O3B 1.21(2) . ?
C9B O2B 1.22(2) . ?
O3B O2B 1.82(5) . ?
O34B C40 1.24(3) . ?
C51B C50 1.56(3) . ?
C51B N35B 1.56(3) . ?
C51B H51C 0.9900 . ?
C51B H51D 0.9900 . ?
N35B H35D 0.9100 . ?
N35B H35E 0.9100 . ?
N35B H35F 0.9100 . ?
C3 C2 1.538(13) . ?
C3 H3A 1.0000 . ?
N2 C7 1.454(9) . ?
N2 H2 0.8800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C7 C10 1.500(10) . ?
C7 H7 1.0000 . ?
C18 C17 1.545(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C12 C13 1.492(13) . ?
C12 C11 1.567(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C11 C16 1.529(11) . ?
C11 H11 1.0000 . ?
C14 C13 1.500(16) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 C15 1.455(16) . ?
C13 H13 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 C22 1.498(11) . ?
C17 H17 1.0000 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C48 C47 1.547(10) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C47 N34 1.453(9) . ?
C47 H47 1.0000 . ?
C46 O35 1.239(7) . ?
C46 N34 1.337(8) . ?
C46 C41 1.505(10) . ?
C45 C43 1.521(13) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C44 C43 1.512(12) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C43 C42 1.516(11) . ?
C43 H43 1.0000 . ?
C42 C41 1.547(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C41 N33 1.447(8) . ?
C41 H41 1.0000 . ?
C40 N33 1.314(9) . ?
C40 C37 1.506(10) . ?
C39 O32 1.279(11) . ?
C39 O33 1.292(12) . ?
C39 C38 1.396(12) . ?
C38 C37 1.564(11) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C37 N32 1.416(8) . ?
C37 H37 1.0000 . ?
C36 O31 1.238(7) . ?
C36 N32 1.327(8) . ?
C36 C31 1.525(9) . ?
C34 C33 1.515(12) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C33 C35 1.504(11) . ?
C33 C32 1.544(11) . ?
C33 H33 1.0000 . ?
C32 C31 1.529(10) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C31 N31 1.465(9) . ?
C31 H31 1.0000 . ?
C35 H35G 0.9800 . ?
C35 H35H 0.9800 . ?
C35 H35I 0.9800 . ?
N34 H24 0.8800 . ?
N32 H22 0.8800 . ?
C22 N1 1.345(9) 2_665 ?
N33 H23 0.8800 . ?
C20 C21 1.516(17) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
N31 C52 1.343(9) 2_665 ?
N31 H21 0.8800 . ?
C21 N5 1.617(13) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
N5 H5D 0.9100 . ?
N5 H5E 0.9100 . ?
N5 H5F 0.9100 . ?

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
C22 N1 C1 124.3(6) 2_665 . ?
C22 N1 H1 117.8 2_665 . ?
C1 N1 H1 117.8 . . ?
N1 C1 C6 107.1(6) . . ?
N1 C1 C2 109.7(6) . . ?
C6 C1 C2 109.9(7) . . ?
N1 C1 H1A 110.0 . . ?
C6 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
C18 C19 C20 115.5(10) . . ?
C18 C19 H19A 108.4 . . ?
C20 C19 H19A 108.4 . . ?
C18 C19 H19B 108.4 . . ?
C20 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
O1 C6 N2 123.4(7) . . ?
O1 C6 C1 119.4(7) . . ?
N2 C6 C1 117.0(6) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O36 C52 N31 123.7(7) . 2_665 ?
O36 C52 C47 122.2(7) . . ?
N31 C52 C47 114.1(6) 2_665 . ?
C16 N4 C17 121.5(6) . . ?
C16 N4 H4 119.3 . . ?
C17 N4 H4 119.3 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C48 C49 C50 111.5(6) . . ?
C48 C49 H49A 109.3 . . ?
C50 C49 H49A 109.3 . . ?
C48 C49 H49B 109.3 . . ?
C50 C49 H49B 109.3 . . ?
H49A C49 H49B 108.0 . . ?
C10 N3 C11 123.8(6) . . ?
C10 N3 H3 118.1 . . ?
C11 N3 H3 118.1 . . ?
C9A C8A C7 119(3) . . ?
C9A C8A H8A1 107.7 . . ?
C7 C8A H8A1 107.7 . . ?
C9A C8A H8A2 107.7 . . ?
C7 C8A H8A2 107.7 . . ?
H8A1 C8A H8A2 107.1 . . ?
O3A C9A O2A 118.6(18) . . ?
O3A C9A C8A 119(2) . . ?
O2A C9A C8A 122(2) . . ?
N35A C51A C50 107(3) . . ?
N35A C51A H51A 110.2 . . ?
C50 C51A H51A 110.2 . . ?
N35A C51A H51B 110.2 . . ?
C50 C51A H51B 110.2 . . ?
H51A C51A H51B 108.5 . . ?
C51A N35A H35A 109.5 . . ?
C51A N35A H35B 109.5 . . ?
H35A N35A H35B 109.5 . . ?
C51A N35A H35C 109.5 . . ?
H35A N35A H35C 109.5 . . ?
H35B N35A H35C 109.5 . . ?
C9B C8B C7 110(4) . . ?
C9B C8B H8B1 109.6 . . ?
C7 C8B H8B1 109.6 . . ?
C9B C8B H8B2 109.6 . . ?
C7 C8B H8B2 109.6 . . ?
H8B1 C8B H8B2 108.1 . . ?
O3B C9B O2B 97(3) . . ?
O3B C9B C8B 133(4) . . ?
O2B C9B C8B 129(4) . . ?
C9B O3B O2B 41.6(18) . . ?
C9B O2B O3B 41.2(19) . . ?
C50 C51B N35B 108(2) . . ?
C50 C51B H51C 110.1 . . ?
N35B C51B H51C 110.1 . . ?
C50 C51B H51D 110.1 . . ?
N35B C51B H51D 110.1 . . ?
H51C C51B H51D 108.4 . . ?
C51B N35B H35D 109.5 . . ?
C51B N35B H35E 109.5 . . ?
H35D N35B H35E 109.5 . . ?
C51B N35B H35F 109.5 . . ?
H35D N35B H35F 109.5 . . ?
H35E N35B H35F 109.5 . . ?
C4 C3 C5 111.1(11) . . ?
C4 C3 C2 109.0(8) . . ?
C5 C3 C2 111.3(9) . . ?
C4 C3 H3A 108.4 . . ?
C5 C3 H3A 108.4 . . ?
C2 C3 H3A 108.4 . . ?
C6 N2 C7 121.4(6) . . ?
C6 N2 H2 119.3 . . ?
C7 N2 H2 119.3 . . ?
C3 C2 C1 115.9(7) . . ?
C3 C2 H2A 108.3 . . ?
C1 C2 H2A 108.3 . . ?
C3 C2 H2B 108.3 . . ?
C1 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
N2 C7 C10 109.2(6) . . ?
N2 C7 C8A 116.4(13) . . ?
C10 C7 C8A 103.8(10) . . ?
N2 C7 C8B 107(2) . . ?
C10 C7 C8B 105.2(15) . . ?
N2 C7 H7 109.1 . . ?
C10 C7 H7 109.1 . . ?
C8A C7 H7 109.1 . . ?
C19 C18 C17 119.6(8) . . ?
C19 C18 H18A 107.4 . . ?
C17 C18 H18A 107.4 . . ?
C19 C18 H18B 107.4 . . ?
C17 C18 H18B 107.4 . . ?
H18A C18 H18B 106.9 . . ?
C13 C12 C11 116.5(7) . . ?
C13 C12 H12A 108.2 . . ?
C11 C12 H12A 108.2 . . ?
C13 C12 H12B 108.2 . . ?
C11 C12 H12B 108.2 . . ?
H12A C12 H12B 107.3 . . ?
N3 C11 C16 108.6(6) . . ?
N3 C11 C12 107.8(6) . . ?
C16 C11 C12 109.1(6) . . ?
N3 C11 H11 110.4 . . ?
C16 C11 H11 110.4 . . ?
C12 C11 H11 110.4 . . ?
O4 C10 N3 122.5(7) . . ?
O4 C10 C7 121.7(7) . . ?
N3 C10 C7 115.6(6) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C13 C12 107.3(11) . . ?
C15 C13 C14 105.9(12) . . ?
C12 C13 C14 109.9(10) . . ?
C15 C13 H13 111.2 . . ?
C12 C13 H13 111.2 . . ?
C14 C13 H13 111.2 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O5 C16 N4 123.2(7) . . ?
O5 C16 C11 119.5(7) . . ?
N4 C16 C11 117.3(6) . . ?
N4 C17 C22 109.8(6) . . ?
N4 C17 C18 110.0(6) . . ?
C22 C17 C18 109.5(6) . . ?
N4 C17 H17 109.2 . . ?
C22 C17 H17 109.2 . . ?
C18 C17 H17 109.2 . . ?
C49 C50 C51B 108.8(14) . . ?
C49 C50 C51A 112.8(15) . . ?
C49 C50 H50A 109.0 . . ?
C51A C50 H50A 109.0 . . ?
C49 C50 H50B 109.0 . . ?
C51A C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?
C49 C48 C47 115.2(6) . . ?
C49 C48 H48A 108.5 . . ?
C47 C48 H48A 108.5 . . ?
C49 C48 H48B 108.5 . . ?
C47 C48 H48B 108.5 . . ?
H48A C48 H48B 107.5 . . ?
N34 C47 C52 111.7(5) . . ?
N34 C47 C48 111.3(6) . . ?
C52 C47 C48 110.5(6) . . ?
N34 C47 H47 107.7 . . ?
C52 C47 H47 107.7 . . ?
C48 C47 H47 107.7 . . ?
O35 C46 N34 120.9(7) . . ?
O35 C46 C41 120.7(6) . . ?
N34 C46 C41 118.4(6) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C44 C43 C42 113.5(7) . . ?
C44 C43 C45 111.1(8) . . ?
C42 C43 C45 110.5(8) . . ?
C44 C43 H43 107.1 . . ?
C42 C43 H43 107.1 . . ?
C45 C43 H43 107.1 . . ?
C43 C42 C41 114.9(7) . . ?
C43 C42 H42A 108.5 . . ?
C41 C42 H42A 108.5 . . ?
C43 C42 H42B 108.5 . . ?
C41 C42 H42B 108.5 . . ?
H42A C42 H42B 107.5 . . ?
N33 C41 C46 108.7(5) . . ?
N33 C41 C42 110.8(6) . . ?
C46 C41 C42 107.3(5) . . ?
N33 C41 H41 110.0 . . ?
C46 C41 H41 110.0 . . ?
C42 C41 H41 110.0 . . ?
O34B C40 N33 121(2) . . ?
O34A C40 N33 122(2) . . ?
O34B C40 C37 122(2) . . ?
O34A C40 C37 121(2) . . ?
N33 C40 C37 115.2(6) . . ?
O32 C39 O33 118.3(9) . . ?
O32 C39 C38 122.7(10) . . ?
O33 C39 C38 119.0(9) . . ?
C39 C38 C37 115.2(7) . . ?
C39 C38 H38A 108.5 . . ?
C37 C38 H38A 108.5 . . ?
C39 C38 H38B 108.5 . . ?
C37 C38 H38B 108.5 . . ?
H38A C38 H38B 107.5 . . ?
N32 C37 C40 112.8(6) . . ?
N32 C37 C38 111.5(6) . . ?
C40 C37 C38 111.7(6) . . ?
N32 C37 H37 106.8 . . ?
C40 C37 H37 106.8 . . ?
C38 C37 H37 106.8 . . ?
O31 C36 N32 122.9(6) . . ?
O31 C36 C31 119.7(6) . . ?
N32 C36 C31 117.2(6) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 C33 C34 110.6(8) . . ?
C35 C33 C32 112.6(7) . . ?
C34 C33 C32 109.5(8) . . ?
C35 C33 H33 108.0 . . ?
C34 C33 H33 108.0 . . ?
C32 C33 H33 108.0 . . ?
C31 C32 C33 113.4(6) . . ?
C31 C32 H32A 108.9 . . ?
C33 C32 H32A 108.9 . . ?
C31 C32 H32B 108.9 . . ?
C33 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
N31 C31 C36 107.2(5) . . ?
N31 C31 C32 108.0(6) . . ?
C36 C31 C32 109.9(6) . . ?
N31 C31 H31 110.5 . . ?
C36 C31 H31 110.5 . . ?
C32 C31 H31 110.5 . . ?
C33 C35 H35G 109.5 . . ?
C33 C35 H35H 109.5 . . ?
H35G C35 H35H 109.5 . . ?
C33 C35 H35I 109.5 . . ?
H35G C35 H35I 109.5 . . ?
H35H C35 H35I 109.5 . . ?
C46 N34 C47 120.7(5) . . ?
C46 N34 H24 119.6 . . ?
C47 N34 H24 119.6 . . ?
C36 N32 C37 120.7(6) . . ?
C36 N32 H22 119.6 . . ?
C37 N32 H22 119.6 . . ?
O6 C22 N1 122.9(7) . 2_665 ?
O6 C22 C17 121.4(7) . . ?
N1 C22 C17 115.6(6) 2_665 . ?
C40 N33 C41 124.9(6) . . ?
C40 N33 H23 117.5 . . ?
C41 N33 H23 117.5 . . ?
C21 C20 C19 109.6(10) . . ?
C21 C20 H20A 109.8 . . ?
C19 C20 H20A 109.8 . . ?
C21 C20 H20B 109.8 . . ?
C19 C20 H20B 109.8 . . ?
H20A C20 H20B 108.2 . . ?
C52 N31 C31 124.5(6) 2_665 . ?
C52 N31 H21 117.7 2_665 . ?
C31 N31 H21 117.7 . . ?
C20 C21 N5 112.5(9) . . ?
C20 C21 H21A 109.1 . . ?
N5 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
N5 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C21 N5 H5D 109.5 . . ?
C21 N5 H5E 109.5 . . ?
H5D N5 H5E 109.5 . . ?
C21 N5 H5F 109.5 . . ?
H5D N5 H5F 109.5 . . ?
H5E N5 H5F 109.5 . . ?

_refine_diff_density_max         0.442
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.045




_chemical_properties_physical    ', Air-sensitive,radiation damage'
####################################################################### 
# 
# 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_c2_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1520675'
_audit_update_record             
;
2017-05-19 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_c2_a_sq             
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Given formula calculated on the presqueezed cell contents, expected calculated on the post squeeze model.
;
_vrf_THETM01_c2_a_sq             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Low resolution weakly diffracting small needles. Best resolution available with a microfocus synchrotron beamline.
;
_vrf_PLAT184_c2_a_sq             
;
PROBLEM: Missing _cell_measurement_theta_min value ......     Please Do !
RESPONSE: Value not supplied by XDS
;
_vrf_PLAT185_c2_a_sq             
;
PROBLEM: Missing _cell_measurement_theta_max value ......     Please Do !
RESPONSE: Value not supplied by XDS
;
_vrf_PLAT029_c2_a_sq             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.950 Note
RESPONSE: Low resolution weakly diffracting small needles. Best resolution available with a microfocus synchrotron beamline.
;
_vrf_PLAT089_c2_a_sq             
;
PROBLEM: Poor Data / Parameter Ratio (Zmax &lt; 18) ........       5.29 Note
RESPONSE: Low resolution weakly diffracting small needles. Best resolution available with a microfocus synchrotron beamline.
;
_vrf_PLAT340_c2_a_sq             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01514 Ang.
RESPONSE: Low resolution weakly diffracting small needles. Best resolution available with a microfocus synchrotron beamline.
;
_vrf_PLAT430_c2_a_sq             
;
PROBLEM: Short Inter D...A Contact  O33    ..  O33     ..       2.71 Ang.
RESPONSE: Well located solvent water with half occupancy, Hydrogens unable to be determined.
;
_vrf_PLAT430_c2_a_sq_2           
;
PROBLEM: Short Inter D...A Contact  O33    ..  O33     ..       2.71 Ang.
RESPONSE: W
;
# Added during the CSD deposition process: Friday 19 May 2017 07:52 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H48 N10 O12, 2(C3F6O1H1), 4(H2O)'
_chemical_formula_sum            'C38 H66 F18 N10 O15'
_chemical_formula_weight         1245.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0070 0.0030 '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 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0210 0.0120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0330 0.0200 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

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

_cell_length_a                   29.780(6)
_cell_length_b                   4.7000(9)
_cell_length_c                   20.220(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.38(3)
_cell_angle_gamma                90
_cell_volume                     2783.8(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    826
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.004
_exptl_crystal_size_min          0.002
_exptl_absorpt_coefficient_mu    0.321
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7616
_exptl_absorpt_correction_T_max  0.8543
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.95369
_diffrn_radiation_type           synchrotron
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14129
_diffrn_reflns_av_unetI/netI     0.1109
_diffrn_reflns_av_R_equivalents  0.1269
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.374
_diffrn_reflns_theta_max         30.227
_diffrn_reflns_theta_full        30.227
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measured_fraction_theta_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_point_group_measured_fraction_full 0.939
_reflns_number_total             3194
_reflns_number_gt                2765
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_max     0.923
_reflns_Friedel_fraction_full    0.923

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

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXLE (Hübschle, 2011)'
_computing_publication_material  'enCIFer (Allen, 2004)'

_refine_special_details          'SQUEEZE, SQUEEZE'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 961 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(4)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         3194
_refine_ls_number_parameters     352
_refine_ls_number_restraints     251
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.1068
_refine_ls_wR_factor_ref         0.2918
_refine_ls_wR_factor_gt          0.2794
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_restrained_S_all      1.191
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001

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
O33 O 0.2695(9) 0.405(8) 0.4879(12) 0.160(13) Uani 0.5 1 d . U P . .
N1 N 0.6511(3) 0.7334(18) -0.0099(3) 0.054(2) Uani 1 1 d . U . . .
H1A H 0.6494 0.5478 -0.0156 0.064 Uiso 1 1 calc R U . . .
C1 C 0.6585(3) 0.845(2) 0.0598(4) 0.056(2) Uani 1 1 d . U . . .
H1B H 0.6520 1.0541 0.0583 0.067 Uiso 1 1 calc R U . . .
O2 O 0.6682(3) 0.310(2) 0.2227(4) 0.080(2) Uani 1 1 d . U . . .
N2 N 0.6165(2) 0.8354(17) 0.1500(3) 0.0488(17) Uani 1 1 d . U . . .
H2 H 0.6243 1.0155 0.1555 0.059 Uiso 1 1 calc R U . . .
C2 C 0.7081(4) 0.797(4) 0.0934(5) 0.098(5) Uani 1 1 d . U . . .
H2A H 0.7142 0.8983 0.1364 0.148 Uiso 1 1 calc R U . . .
H2B H 0.7284 0.8685 0.0641 0.148 Uiso 1 1 calc R U . . .
H2C H 0.7134 0.5929 0.1012 0.148 Uiso 1 1 calc R U . . .
O3 O 0.7023(3) 0.563(2) 0.3103(5) 0.105(3) Uani 1 1 d . U . . .
N3 N 0.5180(2) 0.6918(17) 0.2223(3) 0.0431(16) Uani 1 1 d . U . . .
H3 H 0.5210 0.5055 0.2232 0.052 Uiso 1 1 calc R U . . .
C3 C 0.6250(4) 0.696(2) 0.0979(5) 0.060(2) Uani 1 1 d D U . . .
C6 C 0.6693(4) 0.502(3) 0.2662(6) 0.078(3) Uani 1 1 d . U . . .
C5 C 0.6246(3) 0.695(3) 0.2658(5) 0.064(2) Uani 1 1 d . U . . .
H5A H 0.6074 0.6198 0.2996 0.076 Uiso 1 1 calc R U . . .
H5B H 0.6340 0.8918 0.2788 0.076 Uiso 1 1 calc R U . . .
N5 N 0.2447(3) 0.573(3) 0.3531(5) 0.097(3) Uani 1 1 d . U . . .
H5C H 0.2263 0.4501 0.3257 0.146 Uiso 1 1 calc R U . . .
H5D H 0.2320 0.7496 0.3493 0.146 Uiso 1 1 calc R U . . .
H5E H 0.2478 0.5125 0.3964 0.146 Uiso 1 1 calc R U . . .
C4 C 0.5944(3) 0.697(2) 0.1984(4) 0.048(2) Uani 1 1 d . U . . .
H4 H 0.5873 0.4963 0.1837 0.058 Uiso 1 1 calc R U . . .
N4 N 0.4029(2) 0.8496(17) 0.1691(3) 0.0445(17) Uani 1 1 d . U . . .
H4A H 0.4066 1.0339 0.1756 0.053 Uiso 1 1 calc R U . . .
C7 C 0.5500(3) 0.848(3) 0.2053(5) 0.061(2) Uani 1 1 d D U . . .
C8 C 0.4775(2) 0.817(2) 0.2397(4) 0.050(2) Uani 1 1 d . U . . .
H8 H 0.4771 1.0270 0.2312 0.060 Uiso 1 1 calc R U . . .
C9 C 0.4757(4) 0.759(3) 0.3129(5) 0.081(4) Uani 1 1 d . U . . .
H9A H 0.5032 0.8350 0.3413 0.121 Uiso 1 1 calc R U . . .
H9B H 0.4741 0.5529 0.3200 0.121 Uiso 1 1 calc R U . . .
H9C H 0.4487 0.8501 0.3247 0.121 Uiso 1 1 calc R U . . .
C10 C 0.4360(3) 0.676(2) 0.1963(4) 0.051(2) Uani 1 1 d D U . . .
C11 C 0.3607(3) 0.747(2) 0.1291(4) 0.046(2) Uani 1 1 d . U . . .
H11 H 0.3637 0.5375 0.1225 0.055 Uiso 1 1 calc R U . . .
C14 C 0.2840(5) 0.670(5) 0.2609(6) 0.103(5) Uani 1 1 d . U . . .
H14A H 0.2619 0.5389 0.2340 0.123 Uiso 1 1 calc R U . . .
H14B H 0.2705 0.8633 0.2564 0.123 Uiso 1 1 calc R U . . .
C16 C 0.3528(3) 0.888(2) 0.0613(4) 0.051(2) Uani 1 1 d D U . . .
C21 C 0.3785(5) 0.211(4) 0.4936(5) 0.089(4) Uani 1 1 d . U . . .
H21 H 0.3727 0.4208 0.4911 0.107 Uiso 1 1 calc R U . . .
O21 O 0.3391(5) 0.082(5) 0.4728(5) 0.173(7) Uani 1 1 d . U . . .
H21A H 0.3325 -0.0184 0.5041 0.259 Uiso 1 1 calc R U . . .
C22 C 0.3962(5) 0.138(4) 0.5660(10) 0.130(6) Uiso 1 1 d D . . . .
C23 C 0.4089(6) 0.142(5) 0.4456(8) 0.112(5) Uiso 1 1 d . . . . .
C15 C 0.2904(4) 0.583(4) 0.3330(6) 0.089(4) Uani 1 1 d . U . . .
H15A H 0.3050 0.3930 0.3390 0.107 Uiso 1 1 calc R U . . .
H15B H 0.3102 0.7210 0.3614 0.107 Uiso 1 1 calc R U . . .
C13 C 0.3264(3) 0.671(3) 0.2331(5) 0.071(3) Uani 1 1 d . U . . .
H13A H 0.3374 0.4729 0.2312 0.085 Uiso 1 1 calc R U . . .
H13B H 0.3500 0.7798 0.2635 0.085 Uiso 1 1 calc R U . . .
C12 C 0.3201(3) 0.799(3) 0.1637(4) 0.061(3) Uani 1 1 d . U . . .
H12A H 0.3153 1.0067 0.1671 0.073 Uiso 1 1 calc R U . . .
H12B H 0.2924 0.7174 0.1358 0.073 Uiso 1 1 calc R U . . .
F21 F 0.4085(4) -0.140(2) 0.5753(5) 0.142(4) Uani 1 1 d D . . . .
F22 F 0.4335(5) 0.284(3) 0.5913(7) 0.202(8) Uani 1 1 d D U . . .
F23 F 0.3643(6) 0.198(3) 0.6020(4) 0.176(6) Uani 1 1 d D U . . .
F24 F 0.4495(4) 0.243(4) 0.4593(10) 0.201(7) Uani 1 1 d . . . . .
F25 F 0.4155(6) -0.124(3) 0.4398(7) 0.182(6) Uani 1 1 d . U . . .
F26 F 0.3934(4) 0.244(3) 0.3838(4) 0.144(4) Uani 1 1 d . . . . .
O1A O 0.6060(3) 0.4692(15) 0.0762(3) 0.056(2) Uani 0.864(13) 1 d D U P A 1
O4A O 0.5395(3) 1.094(2) 0.1785(6) 0.052(2) Uani 0.580(10) 1 d D U P B 1
O5A O 0.4316(5) 0.406(2) 0.2048(8) 0.045(3) Uani 0.563(17) 1 d D U P C 1
O6A O 0.3717(10) 1.134(4) 0.0548(10) 0.054(3) Uani 0.301(14) 1 d D U P D 1
O1B O 0.6461(15) 0.462(7) 0.115(2) 0.056(2) Uani 0.136(13) 1 d D U P A 2
O4B O 0.5547(5) 1.106(3) 0.2307(8) 0.052(2) Uani 0.420(10) 1 d D U P B 2
O5B O 0.4365(7) 0.415(3) 0.1732(10) 0.045(3) Uani 0.437(17) 1 d D U P C 2
O6B O 0.3418(4) 1.1496(19) 0.0583(4) 0.054(3) Uani 0.699(14) 1 d D U P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C16 1.255(12) 2_655 ?
N1 C1 1.483(12) . ?
N1 H1A 0.8800 . ?
C1 C2 1.527(16) . ?
C1 C3 1.535(14) . ?
C1 H1B 1.0000 . ?
O2 C6 1.259(16) . ?
N2 C3 1.304(13) . ?
N2 C4 1.429(11) . ?
N2 H2 0.8800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C6 1.236(15) . ?
N3 C7 1.298(13) . ?
N3 C8 1.443(12) . ?
N3 H3 0.8800 . ?
C3 O1A 1.250(12) . ?
C3 O1B 1.28(3) . ?
C6 C5 1.607(17) . ?
C5 C4 1.493(13) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N5 C15 1.488(17) . ?
N5 H5C 0.9100 . ?
N5 H5D 0.9100 . ?
N5 H5E 0.9100 . ?
C4 C7 1.526(14) . ?
C4 H4 1.0000 . ?
N4 C10 1.319(12) . ?
N4 C11 1.448(10) . ?
N4 H4A 0.8800 . ?
C7 O4A 1.294(15) . ?
C7 O4B 1.315(18) . ?
C8 C9 1.515(15) . ?
C8 C10 1.531(12) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 O5A 1.292(15) . ?
C10 O5B 1.314(17) . ?
C11 C16 1.502(13) . ?
C11 C12 1.523(13) . ?
C11 H11 1.0000 . ?
C14 C13 1.473(18) . ?
C14 C15 1.493(18) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 N1 1.255(12) 2_655 ?
C16 O6B 1.272(13) . ?
C16 O6A 1.30(2) . ?
C21 O21 1.321(19) . ?
C21 C23 1.48(2) . ?
C21 C22 1.50(2) . ?
C21 H21 1.0000 . ?
O21 H21A 0.8400 . ?
C22 F23 1.328(16) . ?
C22 F22 1.329(17) . ?
C22 F21 1.360(17) . ?
C23 F25 1.28(2) . ?
C23 F24 1.28(2) . ?
C23 F26 1.341(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C13 C12 1.507(15) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 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
C16 N1 C1 123.8(9) 2_655 . ?
C16 N1 H1A 118.1 2_655 . ?
C1 N1 H1A 118.1 . . ?
N1 C1 C2 109.7(9) . . ?
N1 C1 C3 108.5(8) . . ?
C2 C1 C3 111.8(9) . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
C3 C1 H1B 108.9 . . ?
C3 N2 C4 120.4(9) . . ?
C3 N2 H2 119.8 . . ?
C4 N2 H2 119.8 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C7 N3 C8 121.4(9) . . ?
C7 N3 H3 119.3 . . ?
C8 N3 H3 119.3 . . ?
O1A C3 N2 124.8(9) . . ?
O1B C3 N2 112(2) . . ?
O1A C3 C1 120.5(9) . . ?
O1B C3 C1 101(2) . . ?
N2 C3 C1 114.6(9) . . ?
O3 C6 O2 125.9(12) . . ?
O3 C6 C5 115.1(12) . . ?
O2 C6 C5 119.0(10) . . ?
C4 C5 C6 111.8(9) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
C15 N5 H5C 109.5 . . ?
C15 N5 H5D 109.5 . . ?
H5C N5 H5D 109.5 . . ?
C15 N5 H5E 109.5 . . ?
H5C N5 H5E 109.5 . . ?
H5D N5 H5E 109.5 . . ?
N2 C4 C5 110.6(7) . . ?
N2 C4 C7 111.4(8) . . ?
C5 C4 C7 108.0(8) . . ?
N2 C4 H4 108.9 . . ?
C5 C4 H4 108.9 . . ?
C7 C4 H4 108.9 . . ?
C10 N4 C11 122.3(8) . . ?
C10 N4 H4A 118.8 . . ?
C11 N4 H4A 118.8 . . ?
O4A C7 N3 118.8(9) . . ?
N3 C7 O4B 116.6(10) . . ?
O4A C7 C4 121.7(9) . . ?
N3 C7 C4 116.9(10) . . ?
O4B C7 C4 115.6(10) . . ?
N3 C8 C9 110.0(7) . . ?
N3 C8 C10 107.9(7) . . ?
C9 C8 C10 108.4(8) . . ?
N3 C8 H8 110.2 . . ?
C9 C8 H8 110.2 . . ?
C10 C8 H8 110.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5A C10 N4 125.2(10) . . ?
O5B C10 N4 118.9(11) . . ?
O5A C10 C8 116.1(10) . . ?
O5B C10 C8 123.3(11) . . ?
N4 C10 C8 115.9(9) . . ?
N4 C11 C16 110.0(7) . . ?
N4 C11 C12 111.7(7) . . ?
C16 C11 C12 110.0(7) . . ?
N4 C11 H11 108.4 . . ?
C16 C11 H11 108.4 . . ?
C12 C11 H11 108.4 . . ?
C13 C14 C15 114.0(11) . . ?
C13 C14 H14A 108.8 . . ?
C15 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.6 . . ?
N1 C16 O6B 122.4(9) 2_655 . ?
N1 C16 O6A 114.1(12) 2_655 . ?
N1 C16 C11 118.4(9) 2_655 . ?
O6B C16 C11 117.8(8) . . ?
O6A C16 C11 118.9(11) . . ?
O21 C21 C23 107.6(13) . . ?
O21 C21 C22 109.9(13) . . ?
C23 C21 C22 116.1(13) . . ?
O21 C21 H21 107.6 . . ?
C23 C21 H21 107.6 . . ?
C22 C21 H21 107.6 . . ?
C21 O21 H21A 109.5 . . ?
F23 C22 F22 108.0(18) . . ?
F23 C22 F21 109.2(15) . . ?
F22 C22 F21 105.1(15) . . ?
F23 C22 C21 109.0(13) . . ?
F22 C22 C21 112.2(15) . . ?
F21 C22 C21 113.2(14) . . ?
F25 C23 F24 103(2) . . ?
F25 C23 F26 107.3(17) . . ?
F24 C23 F26 102.9(17) . . ?
F25 C23 C21 113.4(16) . . ?
F24 C23 C21 116.3(17) . . ?
F26 C23 C21 112.7(15) . . ?
N5 C15 C14 108.2(10) . . ?
N5 C15 H15A 110.1 . . ?
C14 C15 H15A 110.1 . . ?
N5 C15 H15B 110.1 . . ?
C14 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
C14 C13 C12 112.7(9) . . ?
C14 C13 H13A 109.0 . . ?
C12 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C13 C12 C11 112.9(8) . . ?
C13 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?

_refine_diff_density_max         0.394
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.081




_chemical_properties_physical    ', Air-sensitive,radiation damage'
