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

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

data_zlcul2-b
_database_code_depnum_ccdc_archive 'CCDC 1015477'
_audit_update_record             
;
2014-07-22 deposited with the CCDC.
2015-01-20 downloaded from the CCDC.
;

_audit_creation_date             2011-12-02T11:06:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
;
        C24 H32 Cu N6 O4, 5(H2 O)
;
_chemical_formula_sum            'C24 H42 Cu N6 O9'
_chemical_formula_weight         622.18
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121
_symmetry_space_group_name_Hall  P2ac2ab
_symmetry_Int_Tables_number      19
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.2042(7)
_cell_length_b                   16.8211(11)
_cell_length_c                   16.8403(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2890.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    4265
_cell_measurement_theta_min      3.1278
_cell_measurement_theta_max      31.6979

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       
;
        truncated triangle, main faces {0 1 1}
;
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.43
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -1 0.01
-1 1 0 0.025
1 -1 0 0.0494
1 0 1 0.065
-1 0 -1 0.03
-1 -1 0 0.03
1 1 0 0.055
0 -1 1 0.03
0 1 -1 0.065
0 1 1 0.03

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_T_max  0.970

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'sealed X-ray tube'
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          X-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_orient_matrix_ub_11      0.0369989275
_diffrn_orient_matrix_ub_12      -0.0229092152
_diffrn_orient_matrix_ub_13      -0.0272955363
_diffrn_orient_matrix_ub_21      -0.043599363
_diffrn_orient_matrix_ub_22      0.0109732361
_diffrn_orient_matrix_ub_23      -0.0308618761
_diffrn_orient_matrix_ub_31      0.0394993655
_diffrn_orient_matrix_ub_32      0.0336066113
_diffrn_orient_matrix_ub_33      -0.0084996108
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_unetI/netI     0.1448
_diffrn_reflns_number            22452
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             5901
_reflns_number_gt                3242
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1980-2002)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0385P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5901
_refine_ls_number_parameters     387
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.0907
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
Flack H D (1983), Acta Cryst. A39, 876-881
2585 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.010(19)
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.059

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O5 O 0.5018(6) 0.0774(3) 0.6216(3) 0.0856(17) Uani 1 1 d D . .
O6 O 0.1620(6) 0.0375(4) 0.1987(5) 0.123(2) Uani 1 1 d D . .
O7 O 0.8809(6) 0.0591(3) 0.0597(3) 0.0734(14) Uani 1 1 d D . .
O8 O 0.7310(4) -0.1592(3) 0.4474(3) 0.0570(13) Uani 1 1 d D . .
O9 O 0.9072(5) -0.3405(2) 0.4173(3) 0.0683(14) Uani 1 1 d D . .
H5E H 0.474(6) 0.113(4) 0.591(4) 0.102 Uiso 1 1 d D . .
H5F H 0.575(5) 0.064(4) 0.597(4) 0.102 Uiso 1 1 d D . .
H6E H 0.109(6) 0.075(3) 0.193(5) 0.102 Uiso 1 1 d D . .
H6F H 0.128(7) 0.000(3) 0.230(4) 0.102 Uiso 1 1 d D . .
H7E H 0.845(6) 0.084(4) 0.021(3) 0.102 Uiso 1 1 d D . .
H7F H 0.951(4) 0.087(4) 0.064(4) 0.102 Uiso 1 1 d D . .
H8E H 0.811(3) -0.162(4) 0.442(5) 0.102 Uiso 1 1 d D . .
H8F H 0.701(6) -0.195(3) 0.477(4) 0.102 Uiso 1 1 d D . .
H9E H 0.949(6) -0.297(3) 0.420(4) 0.102 Uiso 1 1 d D . .
H9F H 0.845(5) -0.337(4) 0.450(4) 0.102 Uiso 1 1 d D . .
C1 C 0.5638(6) 0.0596(4) 0.1529(3) 0.0482(17) Uani 1 1 d DU . .
H1A H 0.6555 0.0464 0.1452 0.058 Uiso 1 1 calc R . .
H1B H 0.5182 0.0505 0.1032 0.058 Uiso 1 1 calc R . .
C2 C 0.5073(6) 0.0082(4) 0.2156(3) 0.0504(18) Uani 1 1 d DU A .
H2A H 0.4146 0.0198 0.2204 0.06 Uiso 1 1 calc R . .
H2B H 0.5157 -0.0469 0.1993 0.06 Uiso 1 1 calc R . .
C3A C 0.7194(9) -0.0198(7) 0.2919(7) 0.021(3) Uiso 0.5 1 d PDU A 1
H3A1 H 0.7341 -0.0481 0.3414 0.025 Uiso 0.5 1 calc PR A 1
H3A2 H 0.7215 -0.059 0.2497 0.025 Uiso 0.5 1 calc PR A 1
C4A C 0.8296(10) 0.0341(7) 0.2800(7) 0.028(3) Uiso 0.5 1 d PDU A 1
H4A1 H 0.9119 0.0076 0.2913 0.034 Uiso 0.5 1 calc PR A 1
H4A2 H 0.8313 0.0537 0.2259 0.034 Uiso 0.5 1 calc PR A 1
C5A C 0.9048(9) 0.1703(5) 0.3241(6) 0.019(2) Uiso 0.5 1 d PDU A 1
H5A1 H 0.9222 0.1933 0.3758 0.022 Uiso 0.5 1 calc PR A 1
H5A2 H 0.9874 0.1515 0.3026 0.022 Uiso 0.5 1 calc PR A 1
C6A C 0.8601(12) 0.2224(9) 0.2798(9) 0.055(5) Uiso 0.5 1 d PDU A 1
H6A1 H 0.8898 0.2094 0.2266 0.066 Uiso 0.5 1 calc PR A 1
H6A2 H 0.9037 0.2715 0.2944 0.066 Uiso 0.5 1 calc PR A 1
C3B C 0.6679(13) -0.0369(8) 0.3113(11) 0.071(5) Uiso 0.5 1 d PDU A 2
H3B1 H 0.6622 -0.0827 0.2765 0.085 Uiso 0.5 1 calc PR A 2
H3B2 H 0.6642 -0.0546 0.3661 0.085 Uiso 0.5 1 calc PR A 2
C4B C 0.7864(17) 0.0090(8) 0.2960(11) 0.083(6) Uiso 0.5 1 d PDU A 2
H4B1 H 0.7938 0.0147 0.2388 0.1 Uiso 0.5 1 calc PR A 2
H4B2 H 0.86 -0.0234 0.313 0.1 Uiso 0.5 1 calc PR A 2
C5B C 0.8873(15) 0.1384(8) 0.2802(9) 0.084(4) Uiso 0.5 1 d PDU A 2
H5B1 H 0.8991 0.1039 0.2346 0.101 Uiso 0.5 1 calc PR A 2
H5B2 H 0.9725 0.1435 0.3051 0.101 Uiso 0.5 1 calc PR A 2
C6B C 0.8542(12) 0.2163(8) 0.2492(9) 0.044(4) Uiso 0.5 1 d PDU A 2
H6B1 H 0.8603 0.2154 0.1917 0.053 Uiso 0.5 1 calc PR A 2
H6B2 H 0.9171 0.2549 0.2687 0.053 Uiso 0.5 1 calc PR A 2
C7 C 0.6667(6) 0.2673(3) 0.1952(4) 0.0518(17) Uani 1 1 d DU A .
H7A H 0.7287 0.3034 0.1707 0.062 Uiso 1 1 calc R . .
H7B H 0.5858 0.2963 0.2039 0.062 Uiso 1 1 calc R . .
C8 C 0.6407(7) 0.2004(4) 0.1398(3) 0.0580(18) Uani 1 1 d DU . .
H8A H 0.6025 0.2208 0.0912 0.07 Uiso 1 1 calc R . .
H8B H 0.7227 0.1744 0.1264 0.07 Uiso 1 1 calc R . .
C9 C 0.4169(5) 0.1720(3) 0.1736(3) 0.0433(16) Uani 1 1 d U . .
H9A H 0.3597 0.1289 0.1576 0.052 Uiso 1 1 calc R . .
H9B H 0.4109 0.2132 0.1334 0.052 Uiso 1 1 calc R . .
C10 C 0.3684(7) 0.2048(3) 0.2499(3) 0.0342(14) Uani 1 1 d U A .
C11 C 0.2525(6) 0.2486(4) 0.2536(4) 0.0484(18) Uani 1 1 d U . .
H11 H 0.205 0.2595 0.2078 0.058 Uiso 1 1 calc R . .
C12 C 0.2102(6) 0.2750(4) 0.3256(4) 0.0519(17) Uani 1 1 d U . .
H12 H 0.1335 0.3046 0.3292 0.062 Uiso 1 1 calc R . .
C13 C 0.2810(6) 0.2579(3) 0.3930(4) 0.0418(16) Uani 1 1 d U . .
H13 H 0.2523 0.2756 0.4424 0.05 Uiso 1 1 calc R . .
C14 C 0.3937(6) 0.2147(3) 0.3866(3) 0.0294(13) Uani 1 1 d U A .
C15 C 0.4795(6) 0.1936(3) 0.4573(3) 0.0351(15) Uani 1 1 d U A .
C16 C 0.8304(5) 0.0795(4) 0.4187(3) 0.0375(15) Uani 1 1 d U A .
H16A H 0.7631 0.0429 0.4367 0.045 Uiso 1 1 calc R . .
H16B H 0.8196 0.1285 0.4483 0.045 Uiso 1 1 calc R . .
C17 C 0.9613(6) 0.0448(4) 0.4395(3) 0.0350(15) Uani 1 1 d U . .
C18 C 1.0626(6) 0.0933(4) 0.4664(4) 0.0502(18) Uani 1 1 d U . .
H18 H 1.0512 0.1481 0.47 0.06 Uiso 1 1 calc R . .
C19 C 1.1795(6) 0.0591(4) 0.4875(4) 0.0485(18) Uani 1 1 d U . .
H19 H 1.2491 0.0901 0.5051 0.058 Uiso 1 1 calc R . .
C20 C 1.1916(6) -0.0220(4) 0.4822(4) 0.0430(16) Uani 1 1 d U . .
H20 H 1.2696 -0.0467 0.4965 0.052 Uiso 1 1 calc R . .
C21 C 1.0866(5) -0.0668(3) 0.4552(3) 0.0293(13) Uani 1 1 d U . .
C22 C 1.0953(6) -0.1570(3) 0.4518(3) 0.0383(15) Uani 1 1 d U . .
C23A C 0.5074(13) -0.0139(8) 0.3643(7) 0.040(3) Uiso 0.5 1 d PDU A 1
H23A H 0.5603 -0.0029 0.4101 0.059 Uiso 0.5 1 calc PR A 1
H23B H 0.4971 -0.0703 0.3585 0.059 Uiso 0.5 1 calc PR A 1
H23C H 0.4228 0.0104 0.3707 0.059 Uiso 0.5 1 calc PR A 1
C23B C 0.4492(15) -0.0021(11) 0.3440(10) 0.094(7) Uiso 0.5 1 d PDU A 2
H23D H 0.3803 0.0348 0.3317 0.141 Uiso 0.5 1 calc PR A 2
H23E H 0.4703 0.0016 0.3995 0.141 Uiso 0.5 1 calc PR A 2
H23F H 0.4208 -0.0551 0.3319 0.141 Uiso 0.5 1 calc PR A 2
C24 C 0.7072(6) 0.3078(4) 0.3297(4) 0.064(2) Uani 1 1 d DU A .
H24A H 0.6163 0.3199 0.3378 0.095 Uiso 1 1 calc R . .
H24B H 0.7512 0.3538 0.309 0.095 Uiso 1 1 calc R . .
H24C H 0.7463 0.2929 0.3794 0.095 Uiso 1 1 calc R . .
N1 N 0.5515(4) 0.1425(3) 0.1756(3) 0.0361(10) Uani 1 1 d DU . .
N2 N 0.5697(5) 0.0178(3) 0.2950(3) 0.0535(15) Uani 1 1 d DU . .
N3 N 0.8071(5) 0.0966(3) 0.3342(3) 0.0513(15) Uani 1 1 d DU . .
N4 N 0.7195(4) 0.2416(3) 0.2728(3) 0.0429(13) Uani 1 1 d DU . .
N5 N 0.4389(4) 0.1901(2) 0.3145(3) 0.0309(10) Uani 1 1 d U . .
N6 N 0.9724(4) -0.0338(3) 0.4339(3) 0.0312(11) Uani 1 1 d U . .
O1 O 0.5868(4) 0.1614(2) 0.4403(2) 0.0473(12) Uani 1 1 d U . .
O2 O 0.4373(4) 0.2096(2) 0.5240(2) 0.0499(12) Uani 1 1 d U . .
O3 O 1.0038(4) -0.1924(2) 0.4181(3) 0.0640(14) Uani 1 1 d U . .
O4 O 1.1929(4) -0.1884(2) 0.4825(2) 0.0526(12) Uani 1 1 d U . .
Cu1 Cu 0.62103(6) 0.13949(4) 0.31313(4) 0.03330(18) Uani 1 1 d U A .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O5 H5E 0.84(2) . ?
O5 H5F 0.88(2) . ?
O6 H6E 0.84(2) . ?
O6 H6F 0.89(2) . ?
O7 H7E 0.85(2) . ?
O7 H7F 0.86(2) . ?
O8 H8E 0.82(2) . ?
O8 H8F 0.83(2) . ?
O9 H9E 0.85(2) . ?
O9 H9F 0.84(2) . ?
C1 N1 1.453(6) . ?
C1 C2 1.482(7) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 N2 1.490(7) . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C3A C4A 1.458(13) . ?
C3A N2 1.654(10) . ?
C3A H3A1 0.97 . ?
C3A H3A2 0.97 . ?
C4A N3 1.412(10) . ?
C4A H4A1 0.97 . ?
C4A H4A2 0.97 . ?
C5A C6A 1.238(11) . ?
C5A N3 1.600(9) . ?
C5A H5A1 0.97 . ?
C5A H5A2 0.97 . ?
C6A N4 1.475(12) . ?
C6A H6A1 0.97 . ?
C6A H6A2 0.97 . ?
C3B N2 1.387(12) . ?
C3B C4B 1.457(14) . ?
C3B H3B1 0.97 . ?
C3B H3B2 0.97 . ?
C4B N3 1.623(13) . ?
C4B H4B1 0.97 . ?
C4B H4B2 0.97 . ?
C5B N3 1.410(12) . ?
C5B C6B 1.451(14) . ?
C5B H5B1 0.97 . ?
C5B H5B2 0.97 . ?
C6B N4 1.493(11) . ?
C6B H6B1 0.97 . ?
C6B H6B2 0.97 . ?
C7 N4 1.477(7) . ?
C7 C8 1.486(7) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 N1 1.462(7) . ?
C8 H8A 0.97 . ?
C8 H8B 0.97 . ?
C9 N1 1.460(6) . ?
C9 C10 1.483(7) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 N5 1.326(7) . ?
C10 C11 1.395(8) . ?
C11 C12 1.362(8) . ?
C11 H11 0.93 . ?
C12 C13 1.375(8) . ?
C12 H12 0.93 . ?
C13 C14 1.365(8) . ?
C13 H13 0.93 . ?
C14 N5 1.363(6) . ?
C14 C15 1.520(8) . ?
C15 O2 1.233(6) . ?
C15 O1 1.254(6) . ?
C16 N3 1.472(7) . ?
C16 C17 1.499(7) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C17 N6 1.330(7) . ?
C17 C18 1.393(8) . ?
C18 C19 1.371(8) . ?
C18 H18 0.93 . ?
C19 C20 1.373(8) . ?
C19 H19 0.93 . ?
C20 C21 1.386(7) . ?
C20 H20 0.93 . ?
C21 N6 1.340(6) . ?
C21 C22 1.520(8) . ?
C22 O4 1.240(7) . ?
C22 O3 1.245(7) . ?
C23A N2 1.432(10) . ?
C23A H23A 0.96 . ?
C23A H23B 0.96 . ?
C23A H23C 0.96 . ?
C23B N2 1.518(13) . ?
C23B H23D 0.96 . ?
C23B H23E 0.96 . ?
C23B H23F 0.96 . ?
C24 N4 1.476(7) . ?
C24 H24A 0.96 . ?
C24 H24B 0.96 . ?
C24 H24C 0.96 . ?
N1 Cu1 2.423(4) . ?
N2 Cu1 2.135(5) . ?
N3 Cu1 2.062(5) . ?
N4 Cu1 2.102(5) . ?
N5 Cu1 2.045(4) . ?
O1 Cu1 2.201(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H5E O5 H5F 100(5) . . ?
H6E O6 H6F 110(5) . . ?
H7E O7 H7F 99(5) . . ?
H8E O8 H8F 112(5) . . ?
H9E O9 H9F 106(5) . . ?
N1 C1 C2 109.8(5) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 C1 114.2(5) . . ?
N2 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
N2 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4A C3A N2 118.6(8) . . ?
C4A C3A H3A1 107.7 . . ?
N2 C3A H3A1 107.7 . . ?
C4A C3A H3A2 107.7 . . ?
N2 C3A H3A2 107.7 . . ?
H3A1 C3A H3A2 107.1 . . ?
N3 C4A C3A 104.4(8) . . ?
N3 C4A H4A1 110.9 . . ?
C3A C4A H4A1 110.9 . . ?
N3 C4A H4A2 110.9 . . ?
C3A C4A H4A2 110.9 . . ?
H4A1 C4A H4A2 108.9 . . ?
C6A C5A N3 112.5(10) . . ?
C6A C5A H5A1 109.1 . . ?
N3 C5A H5A1 109.1 . . ?
C6A C5A H5A2 109.1 . . ?
N3 C5A H5A2 109.1 . . ?
H5A1 C5A H5A2 107.8 . . ?
C5A C6A N4 124.1(12) . . ?
C5A C6A H6A1 106.3 . . ?
N4 C6A H6A1 106.3 . . ?
C5A C6A H6A2 106.3 . . ?
N4 C6A H6A2 106.3 . . ?
H6A1 C6A H6A2 106.4 . . ?
N2 C3B C4B 102.3(11) . . ?
N2 C3B H3B1 111.3 . . ?
C4B C3B H3B1 111.3 . . ?
N2 C3B H3B2 111.3 . . ?
C4B C3B H3B2 111.3 . . ?
H3B1 C3B H3B2 109.2 . . ?
C3B C4B N3 121.2(12) . . ?
C3B C4B H4B1 107 . . ?
N3 C4B H4B1 107 . . ?
C3B C4B H4B2 107 . . ?
N3 C4B H4B2 107 . . ?
H4B1 C4B H4B2 106.8 . . ?
N3 C5B C6B 123.1(12) . . ?
N3 C5B H5B1 106.5 . . ?
C6B C5B H5B1 106.5 . . ?
N3 C5B H5B2 106.5 . . ?
C6B C5B H5B2 106.5 . . ?
H5B1 C5B H5B2 106.5 . . ?
C5B C6B N4 112.1(11) . . ?
C5B C6B H6B1 109.2 . . ?
N4 C6B H6B1 109.2 . . ?
C5B C6B H6B2 109.2 . . ?
N4 C6B H6B2 109.2 . . ?
H6B1 C6B H6B2 107.9 . . ?
N4 C7 C8 113.5(5) . . ?
N4 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
N4 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
N1 C8 C7 110.9(5) . . ?
N1 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N1 C9 C10 114.8(5) . . ?
N1 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N1 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.5 . . ?
N5 C10 C11 121.4(5) . . ?
N5 C10 C9 117.4(5) . . ?
C11 C10 C9 121.2(5) . . ?
C12 C11 C10 118.8(6) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
C11 C12 C13 120.0(6) . . ?
C11 C12 H12 120 . . ?
C13 C12 H12 120 . . ?
C14 C13 C12 119.2(6) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
N5 C14 C13 121.1(5) . . ?
N5 C14 C15 115.6(5) . . ?
C13 C14 C15 123.3(5) . . ?
O2 C15 O1 127.4(6) . . ?
O2 C15 C14 117.5(5) . . ?
O1 C15 C14 115.2(5) . . ?
N3 C16 C17 116.5(5) . . ?
N3 C16 H16A 108.2 . . ?
C17 C16 H16A 108.2 . . ?
N3 C16 H16B 108.2 . . ?
C17 C16 H16B 108.2 . . ?
H16A C16 H16B 107.3 . . ?
N6 C17 C18 122.8(5) . . ?
N6 C17 C16 116.5(5) . . ?
C18 C17 C16 120.7(5) . . ?
C19 C18 C17 118.9(6) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 118.6(6) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
C19 C20 C21 119.5(6) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
N6 C21 C20 122.3(5) . . ?
N6 C21 C22 117.1(5) . . ?
C20 C21 C22 120.6(5) . . ?
O4 C22 O3 126.1(6) . . ?
O4 C22 C21 117.2(6) . . ?
O3 C22 C21 116.8(6) . . ?
N2 C23A H23A 109.5 . . ?
N2 C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
N2 C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
N2 C23B H23D 109.5 . . ?
N2 C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
N2 C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
N4 C24 H24A 109.5 . . ?
N4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C1 N1 C8 118.5(5) . . ?
C1 N1 C9 113.7(4) . . ?
C8 N1 C9 110.5(5) . . ?
C1 N1 Cu1 101.9(3) . . ?
C8 N1 Cu1 103.0(3) . . ?
C9 N1 Cu1 107.7(3) . . ?
C3B N2 C23A 85.0(9) . . ?
C3B N2 C2 114.5(9) . . ?
C23A N2 C2 120.0(7) . . ?
C3B N2 C23B 109.4(10) . . ?
C23A N2 C23B 27.8(8) . . ?
C2 N2 C23B 96.7(8) . . ?
C3B N2 C3A 23.9(7) . . ?
C23A N2 C3A 107.1(8) . . ?
C2 N2 C3A 109.0(5) . . ?
C23B N2 C3A 132.9(9) . . ?
C3B N2 Cu1 115.5(7) . . ?
C23A N2 Cu1 110.5(6) . . ?
C2 N2 Cu1 109.7(4) . . ?
C23B N2 Cu1 109.4(7) . . ?
C3A N2 Cu1 98.3(4) . . ?
C4A N3 C5B 82.0(8) . . ?
C4A N3 C16 116.9(6) . . ?
C5B N3 C16 128.9(8) . . ?
C4A N3 C5A 114.1(7) . . ?
C5B N3 C5A 35.3(7) . . ?
C16 N3 C5A 98.9(5) . . ?
C4A N3 C4B 24.1(7) . . ?
C5B N3 C4B 105.8(10) . . ?
C16 N3 C4B 103.0(8) . . ?
C5A N3 C4B 138.0(8) . . ?
C4A N3 Cu1 107.4(5) . . ?
C5B N3 Cu1 104.4(7) . . ?
C16 N3 Cu1 112.5(3) . . ?
C5A N3 Cu1 106.5(4) . . ?
C4B N3 Cu1 97.5(7) . . ?
C7 N4 C24 108.8(5) . . ?
C7 N4 C6A 119.2(7) . . ?
C24 N4 C6A 101.3(7) . . ?
C7 N4 C6B 100.6(7) . . ?
C24 N4 C6B 117.7(7) . . ?
C6A N4 C6B 20.5(8) . . ?
C7 N4 Cu1 110.5(3) . . ?
C24 N4 Cu1 111.5(4) . . ?
C6A N4 Cu1 105.1(6) . . ?
C6B N4 Cu1 107.1(6) . . ?
C10 N5 C14 119.4(4) . . ?
C10 N5 Cu1 124.1(4) . . ?
C14 N5 Cu1 116.3(4) . . ?
C17 N6 C21 117.9(5) . . ?
C15 O1 Cu1 115.6(4) . . ?
N5 Cu1 N3 168.8(2) . . ?
N5 Cu1 N4 95.61(18) . . ?
N3 Cu1 N4 84.31(19) . . ?
N5 Cu1 N2 100.27(19) . . ?
N3 Cu1 N2 85.1(2) . . ?
N4 Cu1 N2 148.68(19) . . ?
N5 Cu1 O1 76.99(17) . . ?
N3 Cu1 O1 92.16(17) . . ?
N4 Cu1 O1 104.67(17) . . ?
N2 Cu1 O1 105.12(16) . . ?
N5 Cu1 N1 74.66(17) . . ?
N3 Cu1 N1 116.20(17) . . ?
N4 Cu1 N1 79.27(17) . . ?
N2 Cu1 N1 79.17(17) . . ?
O1 Cu1 N1 151.64(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5E O2 0.84(2) 2.02(3) 2.843(7) 168(8) .
O5 H5F O7 0.88(2) 2.21(6) 2.791(7) 123(6) 2_655
O6 H6E O9 0.84(2) 2.34(6) 2.920(8) 126(7) 3_655
O6 H6F O5 0.89(2) 2.61(8) 2.867(10) 98(6) 2_554
O7 H7E O8 0.85(2) 1.94(3) 2.777(7) 168(8) 2_654
O7 H7F O9 0.86(2) 1.91(3) 2.770(7) 172(8) 3_755
O8 H8E O3 0.82(2) 2.08(3) 2.882(6) 168(8) .
O8 H8F O4 0.83(2) 2.08(4) 2.849(6) 153(7) 4_446
O9 H9E O3 0.85(2) 1.85(3) 2.679(6) 166(8) .
O9 H9F O4 0.84(2) 1.97(3) 2.805(7) 171(8) 4_446

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1017211'
_audit_update_record             
;
2014-07-31 deposited with the CCDC.
2015-01-20 downloaded from the CCDC.
;

_audit_creation_date             2014-05-19T13:29:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C24 H36 N6 O4 Na1,  3(C2 F3 O2), (C2 H1 F3 O2)'
_chemical_formula_sum            'C32 H37 F12 N6 Na O12'
_chemical_formula_weight         948.66

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.412(2)
_cell_length_b                   9.4077(10)
_cell_length_c                   21.531(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.241(6)
_cell_angle_gamma                90
_cell_volume                     4055.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1954
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      26.27
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.14
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1944
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        SADABS Version 2008/1 (Sheldrick, Bruker AXS Inc.)
;
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_T_max  0.998
_shelx_estimated_absorpt_T_min   0.941
_shelx_estimated_absorpt_T_max   0.978

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_number            45414
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.929
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_number_total             8301
_reflns_number_gt                6136
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_reduction        XPREP
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0787P)²+6.3150P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8301
_refine_ls_number_parameters     695
_refine_ls_number_restraints     78
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1827
_refine_ls_wR_factor_gt          0.164
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.073

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.02649(5) -0.62161(12) -0.04479(5) 0.0251(3) Uani 1 d . .
C1 C 0.11035(13) 0.1303(3) 0.05372(13) 0.0225(6) Uani 1 d . .
C2 C 0.10484(13) 0.0125(3) 0.09927(12) 0.0198(6) Uani 1 d . .
C3 C 0.04150(14) -0.0326(3) 0.10433(13) 0.0243(6) Uani 1 d . .
H3 H 0.003 0.0074 0.0783 0.029 Uiso 1 calc . .
C4 C 0.03559(14) -0.1371(3) 0.14812(14) 0.0268(6) Uani 1 d . .
H4 H -0.0071 -0.1685 0.1537 0.032 Uiso 1 calc . .
C5 C 0.09265(14) -0.1942(3) 0.18332(14) 0.0245(6) Uani 1 d . .
H5 H 0.09 -0.2654 0.214 0.029 Uiso 1 calc . .
C6 C 0.15522(13) -0.1468(3) 0.17371(12) 0.0200(6) Uani 1 d . .
C7 C 0.21647(13) -0.2248(3) 0.20849(13) 0.0214(6) Uani 1 d . .
H7A H 0.2171 -0.2196 0.2545 0.026 Uiso 1 calc . .
H7B H 0.2127 -0.3262 0.1961 0.026 Uiso 1 calc . .
C8 C 0.30169(14) -0.0469(3) 0.23744(13) 0.0236(6) Uani 1 d . .
H8A H 0.3306 -0.0798 0.2772 0.028 Uiso 1 calc . .
H8B H 0.2623 0.0011 0.2484 0.028 Uiso 1 calc . .
C9 C 0.33985(13) 0.0568(3) 0.20437(13) 0.0230(6) Uani 1 d . .
H9A H 0.3625 0.1277 0.2352 0.028 Uiso 1 calc . .
H9B H 0.3744 0.0053 0.1868 0.028 Uiso 1 calc . .
C10 C 0.32829(14) 0.1985(3) 0.10454(14) 0.0242(6) Uani 1 d . .
H10A H 0.3595 0.2712 0.1264 0.029 Uiso 1 calc . .
H10B H 0.2947 0.2481 0.0725 0.029 Uiso 1 calc . .
C11 C 0.36698(14) 0.0969(3) 0.07070(15) 0.0249(6) Uani 1 d . .
H11A H 0.386 0.1505 0.0388 0.03 Uiso 1 calc . .
H11B H 0.4047 0.057 0.1018 0.03 Uiso 1 calc . .
C12 C 0.36977(14) -0.1370(3) 0.02571(14) 0.0240(6) Uani 1 d . .
H12A H 0.4125 -0.0973 0.0184 0.029 Uiso 1 calc . .
H12B H 0.3481 -0.1879 -0.0131 0.029 Uiso 1 calc . .
C13 C 0.38319(13) -0.2399(3) 0.08085(14) 0.0215(6) Uani 1 d . .
H13A H 0.418 -0.3087 0.0745 0.026 Uiso 1 calc . .
H13B H 0.3999 -0.1871 0.1205 0.026 Uiso 1 calc . .
C14 C 0.32349(13) -0.3846(3) 0.15037(12) 0.0193(6) Uani 1 d . .
H14A H 0.3612 -0.4525 0.1584 0.023 Uiso 1 calc . .
H14B H 0.2819 -0.4394 0.1495 0.023 Uiso 1 calc . .
C15 C 0.33178(14) -0.2794(3) 0.20494(13) 0.0211(6) Uani 1 d . .
H15A H 0.331 -0.3319 0.2446 0.025 Uiso 1 calc . .
H15B H 0.3759 -0.2328 0.2094 0.025 Uiso 1 calc . .
C16 C 0.28159(14) 0.0251(3) -0.01939(13) 0.0239(6) Uani 1 d . .
H16A H 0.3078 0.0322 -0.0534 0.029 Uiso 1 calc . .
H16B H 0.2648 0.1215 -0.0126 0.029 Uiso 1 calc . .
C17 C 0.22252(13) -0.0713(3) -0.04173(13) 0.0207(6) Uani 1 d . .
C18 C 0.18410(16) -0.0482(3) -0.10226(14) 0.0314(7) Uani 1 d . .
H18 H 0.197 0.0224 -0.1291 0.038 Uiso 1 calc . .
C19 C 0.12777(16) -0.1280(4) -0.12268(15) 0.0361(8) Uani 1 d . .
H19 H 0.1017 -0.1137 -0.1639 0.043 Uiso 1 calc . .
C20 C 0.10913(15) -0.2293(4) -0.08291(14) 0.0292(7) Uani 1 d . .
H20 H 0.07 -0.2851 -0.0957 0.035 Uiso 1 calc . .
C21 C 0.14973(13) -0.2464(3) -0.02359(13) 0.0200(6) Uani 1 d . .
C22 C 0.12785(13) -0.3522(3) 0.02024(13) 0.0197(6) Uani 1 d . .
C23 C 0.25472(14) 0.2429(3) 0.17884(15) 0.0264(6) Uani 1 d . .
H23A H 0.2279 0.1985 0.2066 0.04 Uiso 1 calc . .
H23B H 0.2252 0.2925 0.1442 0.04 Uiso 1 calc . .
H23C H 0.2858 0.311 0.2032 0.04 Uiso 1 calc . .
C24 C 0.30668(14) -0.4319(3) 0.03682(13) 0.0219(6) Uani 1 d . .
H24A H 0.3026 -0.389 -0.0053 0.033 Uiso 1 calc . .
H24B H 0.2649 -0.4803 0.0398 0.033 Uiso 1 calc . .
H24C H 0.3434 -0.5007 0.0436 0.033 Uiso 1 calc . .
N1 N 0.16175(11) -0.0429(2) 0.13311(10) 0.0174(5) Uani 1 d . .
N2 N 0.27973(11) -0.1697(2) 0.19650(10) 0.0182(5) Uani 1 d . .
N3 N 0.29319(11) 0.1309(2) 0.15208(11) 0.0189(5) Uani 1 d . .
H3N H 0.2675(11) 0.074(2) 0.1342(8) 0.023 Uiso 1 calc . .
N4 N 0.32616(11) -0.0208(2) 0.03896(11) 0.0199(5) Uani 1 d . .
N5 N 0.32057(11) -0.3180(2) 0.08625(10) 0.0176(5) Uani 1 d . .
H5N H 0.2864(12) -0.256(2) 0.0793(3) 0.021 Uiso 1 calc . .
N6 N 0.20629(11) -0.1705(2) -0.00286(10) 0.0188(5) Uani 1 d . .
O1 O 0.17118(9) 0.1622(2) 0.04844(10) 0.0233(4) Uani 1 d . .
H1 H 0.17036(14) 0.221(4) 0.0250(18) 0.035 Uiso 1 calc . .
O2 O 0.06052(10) 0.1909(2) 0.02471(11) 0.0348(5) Uani 1 d . .
O3 O 0.16889(9) -0.3714(2) 0.07376(9) 0.0210(4) Uani 1 d . .
H3B H 0.1463(10) -0.445(4) 0.1036(11) 0.031 Uiso 1 calc . .
O4 O 0.07387(10) -0.4142(2) 0.00533(10) 0.0282(5) Uani 1 d . .
C28 C 0.07216(13) -0.6656(3) 0.21220(13) 0.0230(6) Uani 1 d . .
C27 C 0.07672(14) -0.5646(3) 0.15684(14) 0.0232(6) Uani 1 d . .
O5 O 0.02405(10) -0.5162(2) 0.12792(11) 0.0345(5) Uani 1 d . .
O6 O 0.13594(9) -0.5391(2) 0.15079(10) 0.0255(5) Uani 1 d . .
F1A F 0.01082(10) -0.7104(3) 0.21290(10) 0.0494(6) Uani 1 d A 1
F2A F 0.10752(11) -0.7845(2) 0.20988(10) 0.0472(5) Uani 1 d B 1
F3A F 0.09644(13) -0.6068(2) 0.26734(9) 0.0548(6) Uani 1 d C 1
C26 C 0.20348(16) 0.0842(4) 0.36699(15) 0.0313(7) Uani 1 d . .
C25 C 0.16447(14) 0.1429(3) 0.41551(14) 0.0238(6) Uani 1 d . .
O8 O 0.19813(10) 0.1549(2) 0.47054(10) 0.0314(5) Uani 1 d . .
O7 O 0.10569(10) 0.1742(3) 0.39548(10) 0.0371(6) Uani 1 d . .
F4 F 0.16388(12) 0.0273(3) 0.31592(10) 0.0618(7) Uani 1 d . .
F5 F 0.23515(14) 0.1860(3) 0.34325(13) 0.0716(8) Uani 1 d . .
F6 F 0.24511(13) -0.0184(3) 0.38838(10) 0.0739(9) Uani 1 d . .
C29B C 0.489(3) 0.897(10) 0.362(2) 0.025(3) Uani 0.432(6) d D 2
C30B C 0.4486(6) 0.8465(12) 0.4080(6) 0.0319(18) Uani 0.432(6) d D 2
O9B O 0.4526(5) 0.893(2) 0.3069(8) 0.043(3) Uani 0.432(6) d D 2
H90B H 0.4743 0.9251 0.2805 0.065 Uiso 0.432(6) calc D 2
O10B O 0.5437(12) 0.941(3) 0.3805(9) 0.036(4) Uani 0.432(6) d D 2
F7B F 0.3989(6) 0.7627(14) 0.3837(5) 0.093(4) Uani 0.432(6) d D 2
F8B F 0.4822(6) 0.7947(19) 0.4604(5) 0.115(6) Uani 0.432(6) d D 2
F9B F 0.4193(8) 0.9570(16) 0.4286(8) 0.149(7) Uani 0.432(6) d D 2
C29A C 0.494(2) 0.904(7) 0.3715(17) 0.025(3) Uani 0.568(6) d D 1
C30A C 0.4401(4) 0.9049(10) 0.4139(4) 0.0319(18) Uani 0.568(6) d D 1
F7A F 0.4201(5) 1.0365(8) 0.4206(6) 0.120(4) Uani 0.568(6) d D 1
F8A F 0.4644(4) 0.8525(11) 0.4686(3) 0.073(3) Uani 0.568(6) d D 1
F9A F 0.3868(3) 0.8357(7) 0.3925(3) 0.0472(16) Uani 0.568(6) d D 1
O9A O 0.4738(4) 0.877(2) 0.3124(6) 0.053(3) Uani 0.568(6) d D 1
H90A H 0.5067 0.8737 0.2944 0.079 Uiso 0.568(6) calc D 1
O10A O 0.5507(8) 0.925(2) 0.3972(6) 0.034(3) Uani 0.568(6) d D 1
C31A C 0.5462(16) 0.910(4) 0.1966(14) 0.030(4) Uani 0.568(6) d D 1
C32A C 0.5955(4) 0.8796(9) 0.1547(3) 0.0500(16) Uani 0.568(6) d D 1
F10A F 0.5743(3) 0.9008(7) 0.09475(17) 0.0694(14) Uani 0.57 d D 1
F11A F 0.6525(2) 0.9471(9) 0.1731(3) 0.085(2) Uani 0.57 d D 1
F12A F 0.6131(3) 0.7422(7) 0.1544(3) 0.108(2) Uani 0.57 d D 1
O11A O 0.4904(2) 0.9465(5) 0.1711(3) 0.0418(13) Uani 0.568(6) d D 1
O12A O 0.5680(3) 0.8759(6) 0.2532(3) 0.0452(14) Uani 0.568(6) d D 1
C31B C 0.5556(16) 0.909(5) 0.2083(16) 0.026(6) Uani 0.432(6) d D 2
C32B C 0.5702(4) 0.9416(11) 0.1406(4) 0.0500(16) Uani 0.432(6) d D 2
F10B F 0.5327(4) 1.0453(13) 0.1095(4) 0.076(4) Uani 0.28 d D 2
F11B F 0.6298(4) 0.9968(15) 0.1409(4) 0.059(4) Uani 0.28 d D 2
F12B F 0.5558(8) 0.8181(13) 0.1095(7) 0.090(4) Uiso 0.28 d D 2
O12B O 0.6037(3) 0.8808(6) 0.2493(3) 0.0249(13) Uani 0.432(6) d D 2
O11B O 0.4957(2) 0.9318(7) 0.2116(3) 0.0331(15) Uani 0.432(6) d D 2
F10C F 0.6312(6) 0.893(2) 0.1417(11) 0.060(5) Uiso 0.15 d E 3
F11C F 0.5299(7) 0.8701(17) 0.0953(7) 0.053(4) Uiso 0.15 d F 3
F12C F 0.5626(13) 1.0741(14) 0.1215(14) 0.126(12) Uiso 0.15 d G 3



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Na1 O5 2.287(2) 3_545 y
Na1 O7 2.307(2) 4 y
Na1 O2 2.330(2) 1_545 y
Na1 O4 2.345(2) . y
Na1 O4 2.390(2) 3_545 y
Na1 C25 3.105(3) 4 y
Na1 Na1 3.307(2) 3_545 y
C1 O2 1.226(3) . ?
C1 O1 1.304(3) . ?
C1 C2 1.499(4) . ?
C2 N1 1.350(3) . ?
C2 C3 1.385(4) . ?
C3 C4 1.384(4) . ?
C3 H3 0.95 . ?
C4 C5 1.369(4) . ?
C4 H4 0.95 . ?
C5 C6 1.405(4) . ?
C5 H5 0.95 . ?
C6 N1 1.335(4) . ?
C6 C7 1.516(4) . ?
C7 N2 1.460(3) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 N2 1.469(4) . ?
C8 C9 1.510(4) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 N3 1.497(3) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C10 N3 1.501(4) . ?
C10 C11 1.514(4) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C11 N4 1.471(4) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 N4 1.473(3) . ?
C12 C13 1.515(4) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C13 N5 1.499(3) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 N5 1.507(3) . ?
C14 C15 1.520(4) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 N2 1.467(3) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 N4 1.465(4) . ?
C16 C17 1.510(4) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 N6 1.338(4) . ?
C17 C18 1.401(4) . ?
C18 C19 1.372(5) . ?
C18 H18 0.95 . ?
C19 C20 1.383(5) . ?
C19 H19 0.95 . ?
C20 C21 1.390(4) . ?
C20 H20 0.95 . ?
C21 N6 1.357(3) . ?
C21 C22 1.498(4) . ?
C22 O4 1.233(3) . ?
C22 O3 1.298(3) . ?
C23 N3 1.495(3) . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 N5 1.497(3) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
N3 H3N 0.79(3) . ?
N5 H5N 0.90(3) . ?
O1 H1 0.74(4) . ?
O2 Na1 2.330(2) 1_565 ?
O3 H3B 1.10(3) . ?
O4 Na1 2.390(2) 3_545 ?
C28 F3A 1.316(3) . ?
C28 F1A 1.324(3) . ?
C28 F2A 1.337(3) . ?
C28 C27 1.541(4) . ?
C27 O5 1.221(3) . ?
C27 O6 1.264(3) . ?
O5 Na1 2.287(2) 3_545 ?
C26 F6 1.309(4) . ?
C26 F5 1.314(4) . ?
C26 F4 1.343(4) . ?
C26 C25 1.535(4) . ?
C25 O7 1.229(3) . ?
C25 O8 1.253(4) . ?
C25 Na1 3.105(3) 4_556 ?
O7 Na1 2.307(2) 4_556 ?
C29B O10B 1.19(6) . ?
C29B O9B 1.27(4) . ?
C29B C30B 1.48(7) . ?
C30B F8B 1.295(13) . ?
C30B F7B 1.311(13) . ?
C30B F9B 1.318(11) . ?
O9B H90B 0.84 . ?
C29A O10A 1.20(4) . ?
C29A O9A 1.28(3) . ?
C29A C30A 1.56(5) . ?
C30A F9A 1.275(10) . ?
C30A F8A 1.284(10) . ?
C30A F7A 1.320(10) . ?
O9A H90A 0.84 . ?
C31A O11A 1.21(3) . ?
C31A O12A 1.25(3) . ?
C31A C32A 1.50(4) . ?
C32A F10A 1.295(8) . ?
C32A F11A 1.318(9) . ?
C32A F12A 1.341(9) . ?
C31B O12B 1.21(3) . ?
C31B O11B 1.26(4) . ?
C31B C32B 1.57(3) . ?
C32B F11B 1.321(11) . ?
C32B F10B 1.336(12) . ?
C32B F12B 1.345(13) . ?

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
O5 Na1 O7 86.75(9) 3_545 4 y
O5 Na1 O2 164.69(10) 3_545 1_545 y
O7 Na1 O2 92.42(9) 4 1_545 y
O5 Na1 O4 88.35(9) 3_545 . y
O7 Na1 O4 99.43(9) 4 . y
O2 Na1 O4 106.84(9) 1_545 . y
O5 Na1 O4 84.90(8) 3_545 3_545 y
O7 Na1 O4 166.13(9) 4 3_545 y
O2 Na1 O4 92.72(8) 1_545 3_545 y
O4 Na1 O4 91.38(8) . 3_545 y
O5 Na1 C25 96.67(8) 3_545 4 y
O7 Na1 C25 20.11(8) 4 4 y
O2 Na1 C25 87.43(8) 1_545 4 y
O4 Na1 C25 82.27(8) . 4 y
O4 Na1 C25 173.40(9) 3_545 4 y
O5 Na1 Na1 85.14(8) 3_545 3_545 y
O7 Na1 Na1 144.85(9) 4 3_545 y
O2 Na1 Na1 103.87(8) 1_545 3_545 y
O4 Na1 Na1 46.25(6) . 3_545 y
O4 Na1 Na1 45.14(6) 3_545 3_545 y
C25 Na1 Na1 128.49(7) 4 3_545 y
O2 C1 O1 123.9(3) . . ?
O2 C1 C2 121.1(2) . . ?
O1 C1 C2 114.9(2) . . ?
N1 C2 C3 123.9(3) . . ?
N1 C2 C1 118.2(2) . . ?
C3 C2 C1 117.9(2) . . ?
C4 C3 C2 118.5(3) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 118.6(3) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
N1 C6 C5 122.5(3) . . ?
N1 C6 C7 120.0(2) . . ?
C5 C6 C7 117.4(2) . . ?
N2 C7 C6 114.4(2) . . ?
N2 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N2 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N2 C8 C9 110.5(2) . . ?
N2 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
N2 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
N3 C9 C8 110.1(2) . . ?
N3 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N3 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N3 C10 C11 115.1(2) . . ?
N3 C10 H10A 108.5 . . ?
C11 C10 H10A 108.5 . . ?
N3 C10 H10B 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
N4 C11 C10 113.4(2) . . ?
N4 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
N4 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N4 C12 C13 110.3(2) . . ?
N4 C12 H12A 109.6 . . ?
C13 C12 H12A 109.6 . . ?
N4 C12 H12B 109.6 . . ?
C13 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N5 C13 C12 110.3(2) . . ?
N5 C13 H13A 109.6 . . ?
C12 C13 H13A 109.6 . . ?
N5 C13 H13B 109.6 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
N5 C14 C15 114.6(2) . . ?
N5 C14 H14A 108.6 . . ?
C15 C14 H14A 108.6 . . ?
N5 C14 H14B 108.6 . . ?
C15 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
N2 C15 C14 113.2(2) . . ?
N2 C15 H15A 108.9 . . ?
C14 C15 H15A 108.9 . . ?
N2 C15 H15B 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.8 . . ?
N4 C16 C17 114.8(2) . . ?
N4 C16 H16A 108.6 . . ?
C17 C16 H16A 108.6 . . ?
N4 C16 H16B 108.6 . . ?
C17 C16 H16B 108.6 . . ?
H16A C16 H16B 107.5 . . ?
N6 C17 C18 121.9(3) . . ?
N6 C17 C16 120.0(2) . . ?
C18 C17 C16 118.1(3) . . ?
C19 C18 C17 119.7(3) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 119.5(3) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C19 C20 C21 117.5(3) . . ?
C19 C20 H20 121.2 . . ?
C21 C20 H20 121.2 . . ?
N6 C21 C20 123.9(3) . . ?
N6 C21 C22 118.8(2) . . ?
C20 C21 C22 117.3(2) . . ?
O4 C22 O3 123.7(3) . . ?
O4 C22 C21 120.8(2) . . ?
O3 C22 C21 115.6(2) . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N5 C24 H24A 109.5 . . ?
N5 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N5 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C6 N1 C2 116.8(2) . . ?
C7 N2 C15 111.9(2) . . ?
C7 N2 C8 110.5(2) . . ?
C15 N2 C8 110.5(2) . . ?
C23 N3 C9 110.1(2) . . ?
C23 N3 C10 108.7(2) . . ?
C9 N3 C10 113.1(2) . . ?
C23 N3 H3N 108.3 . . ?
C9 N3 H3N 108.3 . . ?
C10 N3 H3N 108.3 . . ?
C16 N4 C11 112.2(2) . . ?
C16 N4 C12 110.5(2) . . ?
C11 N4 C12 109.9(2) . . ?
C24 N5 C13 110.0(2) . . ?
C24 N5 C14 108.8(2) . . ?
C13 N5 C14 113.2(2) . . ?
C24 N5 H5N 108.3 . . ?
C13 N5 H5N 108.3 . . ?
C14 N5 H5N 108.3 . . ?
C17 N6 C21 117.4(2) . . ?
C1 O1 H1 109.5 . . ?
C1 O2 Na1 142.5(2) . 1_565 ?
C22 O3 H3B 109.5 . . ?
C22 O4 Na1 141.37(19) . . ?
C22 O4 Na1 128.69(18) . 3_545 ?
Na1 O4 Na1 88.61(8) . 3_545 ?
F3A C28 F1A 108.3(2) . . ?
F3A C28 F2A 105.9(2) . . ?
F1A C28 F2A 104.6(2) . . ?
F3A C28 C27 111.7(2) . . ?
F1A C28 C27 113.9(2) . . ?
F2A C28 C27 111.8(2) . . ?
O5 C27 O6 129.9(3) . . ?
O5 C27 C28 116.4(2) . . ?
O6 C27 C28 113.6(2) . . ?
C27 O5 Na1 146.0(2) . 3_545 ?
F6 C26 F5 109.9(3) . . ?
F6 C26 F4 103.9(3) . . ?
F5 C26 F4 103.6(3) . . ?
F6 C26 C25 114.4(3) . . ?
F5 C26 C25 111.3(3) . . ?
F4 C26 C25 113.1(3) . . ?
O7 C25 O8 128.9(3) . . ?
O7 C25 C26 116.6(3) . . ?
O8 C25 C26 114.5(3) . . ?
O7 C25 Na1 40.21(14) . 4_556 ?
O8 C25 Na1 96.04(18) . 4_556 ?
C26 C25 Na1 141.5(2) . 4_556 ?
C25 O7 Na1 119.7(2) . 4_556 ?
O10B C29B O9B 131(6) . . ?
O10B C29B C30B 120(4) . . ?
O9B C29B C30B 109(4) . . ?
F8B C30B F7B 111.0(12) . . ?
F8B C30B F9B 101.7(12) . . ?
F7B C30B F9B 104.0(12) . . ?
F8B C30B C29B 116(2) . . ?
F7B C30B C29B 114(2) . . ?
F9B C30B C29B 109(4) . . ?
C29B O9B H90B 109.5 . . ?
O10A C29A O9A 126(5) . . ?
O10A C29A C30A 117(3) . . ?
O9A C29A C30A 117(3) . . ?
F9A C30A F8A 106.7(8) . . ?
F9A C30A F7A 105.0(8) . . ?
F8A C30A F7A 109.4(9) . . ?
F9A C30A C29A 115.8(16) . . ?
F8A C30A C29A 110.1(18) . . ?
F7A C30A C29A 110(3) . . ?
C29A O9A H90A 109.5 . . ?
O11A C31A O12A 129(3) . . ?
O11A C31A C32A 117(2) . . ?
O12A C31A C32A 112(2) . . ?
F10A C32A F11A 109.2(7) . . ?
F10A C32A F12A 100.4(6) . . ?
F11A C32A F12A 104.2(7) . . ?
F10A C32A C31A 115.9(12) . . ?
F11A C32A C31A 112.5(15) . . ?
F12A C32A C31A 113.6(16) . . ?
O12B C31B O11B 131(3) . . ?
O12B C31B C32B 116(2) . . ?
O11B C31B C32B 112(2) . . ?
F11B C32B F10B 98.8(9) . . ?
F11B C32B F12B 117.0(11) . . ?
F10B C32B F12B 109.5(10) . . ?
F11B C32B C31B 114.3(14) . . ?
F10B C32B C31B 114.4(16) . . ?
F12B C32B C31B 103(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
O2 C1 C2 N1 -175.3(3) . . . . ?
O1 C1 C2 N1 4.1(4) . . . . ?
O2 C1 C2 C3 4.4(4) . . . . ?
O1 C1 C2 C3 -176.2(2) . . . . ?
N1 C2 C3 C4 2.4(4) . . . . ?
C1 C2 C3 C4 -177.3(3) . . . . ?
C2 C3 C4 C5 -1.8(4) . . . . ?
C3 C4 C5 C6 -0.7(4) . . . . ?
C4 C5 C6 N1 2.9(4) . . . . ?
C4 C5 C6 C7 -173.3(3) . . . . ?
N1 C6 C7 N2 3.9(4) . . . . ?
C5 C6 C7 N2 -179.8(2) . . . . ?
N2 C8 C9 N3 71.4(3) . . . . ?
N3 C10 C11 N4 55.3(3) . . . . ?
N4 C12 C13 N5 68.1(3) . . . . ?
N5 C14 C15 N2 56.0(3) . . . . ?
N4 C16 C17 N6 13.8(4) . . . . ?
N4 C16 C17 C18 -169.4(2) . . . . ?
N6 C17 C18 C19 0.6(5) . . . . ?
C16 C17 C18 C19 -176.1(3) . . . . ?
C17 C18 C19 C20 0.7(5) . . . . ?
C18 C19 C20 C21 -0.8(5) . . . . ?
C19 C20 C21 N6 -0.4(4) . . . . ?
C19 C20 C21 C22 177.6(3) . . . . ?
N6 C21 C22 O4 173.6(2) . . . . ?
C20 C21 C22 O4 -4.5(4) . . . . ?
N6 C21 C22 O3 -5.7(4) . . . . ?
C20 C21 C22 O3 176.1(2) . . . . ?
C5 C6 N1 C2 -2.4(4) . . . . ?
C7 C6 N1 C2 173.8(2) . . . . ?
C3 C2 N1 C6 -0.3(4) . . . . ?
C1 C2 N1 C6 179.4(2) . . . . ?
C6 C7 N2 C15 -153.4(2) . . . . ?
C6 C7 N2 C8 83.1(3) . . . . ?
C14 C15 N2 C7 75.8(3) . . . . ?
C14 C15 N2 C8 -160.7(2) . . . . ?
C9 C8 N2 C7 -148.1(2) . . . . ?
C9 C8 N2 C15 87.6(3) . . . . ?
C8 C9 N3 C23 76.7(3) . . . . ?
C8 C9 N3 C10 -161.5(2) . . . . ?
C11 C10 N3 C23 -177.2(2) . . . . ?
C11 C10 N3 C9 60.3(3) . . . . ?
C17 C16 N4 C11 -159.2(2) . . . . ?
C17 C16 N4 C12 77.8(3) . . . . ?
C10 C11 N4 C16 75.1(3) . . . . ?
C10 C11 N4 C12 -161.6(2) . . . . ?
C13 C12 N4 C16 -145.7(2) . . . . ?
C13 C12 N4 C11 90.0(3) . . . . ?
C12 C13 N5 C24 76.9(3) . . . . ?
C12 C13 N5 C14 -161.2(2) . . . . ?
C15 C14 N5 C24 -175.3(2) . . . . ?
C15 C14 N5 C13 62.1(3) . . . . ?
C18 C17 N6 C21 -1.7(4) . . . . ?
C16 C17 N6 C21 174.9(2) . . . . ?
C20 C21 N6 C17 1.7(4) . . . . ?
C22 C21 N6 C17 -176.3(2) . . . . ?
O1 C1 O2 Na1 -4.2(5) . . . 1_565 ?
C2 C1 O2 Na1 175.1(2) . . . 1_565 ?
O3 C22 O4 Na1 -89.6(4) . . . . ?
C21 C22 O4 Na1 91.1(3) . . . . ?
O3 C22 O4 Na1 72.7(3) . . . 3_545 ?
C21 C22 O4 Na1 -106.6(3) . . . 3_545 ?
F3A C28 C27 O5 -109.5(3) . . . . ?
F1A C28 C27 O5 13.6(4) . . . . ?
F2A C28 C27 O5 131.9(3) . . . . ?
F3A C28 C27 O6 66.9(3) . . . . ?
F1A C28 C27 O6 -170.0(3) . . . . ?
F2A C28 C27 O6 -51.7(3) . . . . ?
O6 C27 O5 Na1 7.4(6) . . . 3_545 ?
C28 C27 O5 Na1 -176.9(3) . . . 3_545 ?
F6 C26 C25 O7 -141.5(3) . . . . ?
F5 C26 C25 O7 93.2(4) . . . . ?
F4 C26 C25 O7 -22.9(4) . . . . ?
F6 C26 C25 O8 39.9(4) . . . . ?
F5 C26 C25 O8 -85.3(3) . . . . ?
F4 C26 C25 O8 158.6(3) . . . . ?
F6 C26 C25 Na1 -99.5(4) . . . 4_556 ?
F5 C26 C25 Na1 135.3(3) . . . 4_556 ?
F4 C26 C25 Na1 19.2(5) . . . 4_556 ?
O8 C25 O7 Na1 -41.8(4) . . . 4_556 ?
C26 C25 O7 Na1 139.8(2) . . . 4_556 ?
O10B C29B C30B F8B -30(9) . . . . ?
O9B C29B C30B F8B 155(4) . . . . ?
O10B C29B C30B F7B -161(6) . . . . ?
O9B C29B C30B F7B 25(7) . . . . ?
O10B C29B C30B F9B 84(8) . . . . ?
O9B C29B C30B F9B -91(6) . . . . ?
O10A C29A C30A F9A -156(4) . . . . ?
O9A C29A C30A F9A 22(6) . . . . ?
O10A C29A C30A F8A -35(6) . . . . ?
O9A C29A C30A F8A 143(4) . . . . ?
O10A C29A C30A F7A 85(5) . . . . ?
O9A C29A C30A F7A -97(5) . . . . ?
O11A C31A C32A F10A 3(4) . . . . ?
O12A C31A C32A F10A 174.2(19) . . . . ?
O11A C31A C32A F11A 129(3) . . . . ?
O12A C31A C32A F11A -59(3) . . . . ?
O11A C31A C32A F12A -113(3) . . . . ?
O12A C31A C32A F12A 59(3) . . . . ?
O12B C31B C32B F11B -29(4) . . . . ?
O11B C31B C32B F11B 144(3) . . . . ?
O12B C31B C32B F10B -142(3) . . . . ?
O11B C31B C32B F10B 31(4) . . . . ?
O12B C31B C32B F12B 99(3) . . . . ?
O11B C31B C32B F12B -88(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3N N1 0.79 2.42 3.100(3) 144.7 .
N3 H3N N2 0.79 2.64 3.015(3) 110.5 .
N3 H3N O1 0.79 2.56 3.017(3) 118.2 .
N5 H5N N6 0.9 2.31 3.050(3) 139.8 .
N5 H5N O3 0.9 2.62 3.096(3) 114.3 .
O1 H1 O8 0.74 1.82 2.537(3) 160.3 4_565
O3 H3B O6 1.1 1.39 2.475(3) 164 .
O6 H3B O4 1.39 2.35 3.354(3) 125.1 .
O9B H90B O11B 0.84 1.63 2.413(19) 154.1 .
O9A H90A O12A 0.84 1.67 2.506(13) 174.8 .


# END of CIF
