# 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_az117b
_database_code_depnum_ccdc_archive 'CCDC 1413939'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
#==============================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;                                                                             
 ?                                                                             
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H52 Cu2 I8 N12'
_chemical_formula_weight         1723.12

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   12.918(3)
_cell_length_b                   13.050(3)
_cell_length_c                   16.184(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.66(3)
_cell_angle_gamma                90.00
_cell_volume                     2517.7(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.07
_cell_measurement_theta_max      30.99

_exptl_crystal_description       'box shaped'
_exptl_crystal_colour            'metallic black'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.55
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596
_exptl_absorpt_coefficient_mu    5.784
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;                                                                               
 ?                                                                              
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29520
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         30.99
_reflns_number_total             15877
_reflns_number_gt                15138
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;                                                                               
 Refinement of F² against ALL reflections.  The weighted R-factor wR and      
 goodness of fit S are based on F², conventional R-factors R are based        
 on F, with F set to zero for negative F². The threshold expression of        
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is     
 not relevant to the choice of reflections for refinement.  R-factors based     
 on F² are statistically about twice as large as those based on F, and R-     
 factors based on ALL data will be even larger.                                 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0201P)²+2.7853P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(12)
_refine_ls_number_reflns         15877
_refine_ls_number_parameters     485
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0561
_refine_ls_wR_factor_gt          0.0551
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.676094(19) 0.832808(18) 0.623993(14) 0.02018(5) Uani 1 1 d . . .
I2 I 0.80983(2) 0.63102(2) -0.123337(15) 0.02636(5) Uani 1 1 d . . .
I3 I 0.96325(2) 0.320507(19) 0.582685(16) 0.02473(5) Uani 1 1 d . . .
I4 I 0.842319(19) 0.282402(17) 0.386855(16) 0.02074(4) Uani 1 1 d . . .
I5 I 0.72198(2) 0.233458(19) 0.199953(17) 0.02640(5) Uani 1 1 d . . .
I6 I 0.47363(2) 0.64106(2) 0.034476(18) 0.02924(6) Uani 1 1 d . . .
I7 I 0.37110(2) 0.706534(18) 0.158361(16) 0.02340(5) Uani 1 1 d . . .
I8 I 0.25798(2) 0.76566(2) 0.275629(18) 0.02803(5) Uani 1 1 d . . .
Cu1 Cu 0.69701(4) 0.80910(3) 0.48275(3) 0.01764(8) Uani 1 1 d . . .
Cu2 Cu 0.78759(4) 0.67027(3) 0.01545(3) 0.01855(8) Uani 1 1 d . . .
N1 N 0.7241(2) 0.6832(2) 0.42907(19) 0.0159(5) Uani 1 1 d . . .
N2 N 0.7998(3) 0.5863(2) 0.56071(19) 0.0185(6) Uani 1 1 d . . .
N3 N 0.6294(3) 0.5379(2) 0.4497(2) 0.0186(6) Uani 1 1 d . . .
N4 N 0.8078(2) 0.5952(2) 0.12472(18) 0.0155(5) Uani 1 1 d . . .
N5 N 0.9636(2) 0.4849(2) 0.1851(2) 0.0182(6) Uani 1 1 d . . .
N6 N 0.8049(2) 0.4322(2) 0.0640(2) 0.0171(5) Uani 1 1 d . . .
N7 N 0.7641(2) 0.7964(2) 0.07059(18) 0.0160(5) Uani 1 1 d . . .
N8 N 0.7124(3) 0.8958(3) -0.0598(2) 0.0220(6) Uani 1 1 d . . .
N9 N 0.8727(3) 0.9383(2) 0.0638(2) 0.0212(6) Uani 1 1 d . . .
N10 N 0.6945(3) 0.8886(2) 0.38102(19) 0.0156(5) Uani 1 1 d . . .
N11 N 0.5610(3) 1.0219(2) 0.3348(2) 0.0192(6) Uani 1 1 d . . .
N12 N 0.7305(3) 1.0450(2) 0.4566(2) 0.0199(6) Uani 1 1 d . . .
C1 C 0.7406(3) 0.6711(3) 0.3529(2) 0.0143(6) Uani 1 1 d . . .
C2 C 0.7711(3) 0.5704(3) 0.3344(2) 0.0192(7) Uani 1 1 d . . .
H2 H 0.7772 0.5179 0.3749 0.023 Uiso 1 1 calc R . .
C3 C 0.7912(3) 0.5494(2) 0.2606(2) 0.0182(6) Uani 1 1 d . . .
H3 H 0.8080 0.4823 0.2509 0.022 Uiso 1 1 calc R . .
C4 C 0.7876(3) 0.6260(2) 0.1965(2) 0.0141(5) Uani 1 1 d . . .
C5 C 0.7580(3) 0.7294(2) 0.2108(2) 0.0133(5) Uani 1 1 d . . .
C6 C 0.7511(3) 0.8105(2) 0.1487(2) 0.0151(6) Uani 1 1 d . . .
C7 C 0.7244(3) 0.9122(3) 0.1687(2) 0.0189(6) Uani 1 1 d . . .
H7 H 0.7173 0.9645 0.1278 0.023 Uiso 1 1 calc R . .
C8 C 0.7094(3) 0.9340(3) 0.2438(2) 0.0186(6) Uani 1 1 d . . .
H8 H 0.6975 1.0018 0.2553 0.022 Uiso 1 1 calc R . .
C9 C 0.7110(3) 0.8571(2) 0.3074(2) 0.0141(6) Uani 1 1 d . . .
C10 C 0.7342(3) 0.7527(2) 0.2911(2) 0.0140(6) Uani 1 1 d . . .
C11 C 0.7184(3) 0.5998(2) 0.4797(2) 0.0151(6) Uani 1 1 d . . .
C12 C 0.9085(3) 0.6370(3) 0.5832(3) 0.0252(7) Uani 1 1 d . . .
H12A H 0.9173 0.6568 0.5292 0.038 Uiso 1 1 calc R . .
H12B H 0.9676 0.5907 0.6166 0.038 Uiso 1 1 calc R . .
H12C H 0.9118 0.6968 0.6187 0.038 Uiso 1 1 calc R . .
C13 C 0.7792(4) 0.5455(3) 0.6371(3) 0.0270(8) Uani 1 1 d . . .
H13A H 0.7000 0.5377 0.6211 0.041 Uiso 1 1 calc R . .
H13B H 0.8089 0.5919 0.6867 0.041 Uiso 1 1 calc R . .
H13C H 0.8153 0.4801 0.6537 0.041 Uiso 1 1 calc R . .
C14 C 0.6335(3) 0.4302(3) 0.4785(3) 0.0256(8) Uani 1 1 d . . .
H14A H 0.7099 0.4111 0.5127 0.038 Uiso 1 1 calc R . .
H14B H 0.6032 0.3868 0.4268 0.038 Uiso 1 1 calc R . .
H14C H 0.5901 0.4226 0.5148 0.038 Uiso 1 1 calc R . .
C15 C 0.5308(3) 0.5663(3) 0.3719(3) 0.0249(8) Uani 1 1 d . . .
H15A H 0.5178 0.6386 0.3733 0.037 Uiso 1 1 calc R . .
H15B H 0.4668 0.5294 0.3726 0.037 Uiso 1 1 calc R . .
H15C H 0.5426 0.5497 0.3184 0.037 Uiso 1 1 calc R . .
C16 C 0.8584(3) 0.5014(3) 0.1260(2) 0.0161(6) Uani 1 1 d . . .
C17 C 1.0045(3) 0.3825(3) 0.2200(3) 0.0239(7) Uani 1 1 d . . .
H17A H 0.9425 0.3356 0.2031 0.036 Uiso 1 1 calc R . .
H17B H 1.0403 0.3853 0.2841 0.036 Uiso 1 1 calc R . .
H17C H 1.0575 0.3596 0.1956 0.036 Uiso 1 1 calc R . .
C18 C 1.0357(3) 0.5696(3) 0.2316(3) 0.0284(8) Uani 1 1 d . . .
H18A H 1.0212 0.6275 0.1922 0.043 Uiso 1 1 calc R . .
H18B H 1.1128 0.5494 0.2499 0.043 Uiso 1 1 calc R . .
H18C H 1.0205 0.5876 0.2833 0.043 Uiso 1 1 calc R . .
C19 C 0.8634(3) 0.3610(3) 0.0269(3) 0.0237(7) Uani 1 1 d . . .
H19A H 0.9423 0.3755 0.0519 0.036 Uiso 1 1 calc R . .
H19B H 0.8352 0.3687 -0.0370 0.036 Uiso 1 1 calc R . .
H19C H 0.8509 0.2919 0.0414 0.036 Uiso 1 1 calc R . .
C20 C 0.6829(3) 0.4368(3) 0.0165(2) 0.0203(7) Uani 1 1 d . . .
H20A H 0.6506 0.4743 0.0517 0.031 Uiso 1 1 calc R . .
H20B H 0.6529 0.3685 0.0066 0.031 Uiso 1 1 calc R . .
H20C H 0.6651 0.4705 -0.0401 0.031 Uiso 1 1 calc R . .
C21 C 0.7825(3) 0.8794(3) 0.0252(2) 0.0170(6) Uani 1 1 d . . .
C22 C 0.7540(5) 0.9301(3) -0.1273(3) 0.0345(10) Uani 1 1 d . . .
H22A H 0.8340 0.9384 -0.1001 0.052 Uiso 1 1 calc R . .
H22B H 0.7198 0.9945 -0.1518 0.052 Uiso 1 1 calc R . .
H22C H 0.7356 0.8801 -0.1743 0.052 Uiso 1 1 calc R . .
C23 C 0.5990(4) 0.8536(3) -0.0947(3) 0.0315(9) Uani 1 1 d . . .
H23A H 0.5969 0.7933 -0.1293 0.047 Uiso 1 1 calc R . .
H23B H 0.5477 0.9036 -0.1319 0.047 Uiso 1 1 calc R . .
H23C H 0.5779 0.8360 -0.0457 0.047 Uiso 1 1 calc R . .
C24 C 0.8728(4) 1.0479(3) 0.0417(3) 0.0303(9) Uani 1 1 d . . .
H24A H 0.8016 1.0659 -0.0037 0.045 Uiso 1 1 calc R . .
H24B H 0.9312 1.0609 0.0201 0.045 Uiso 1 1 calc R . .
H24C H 0.8858 1.0882 0.0944 0.045 Uiso 1 1 calc R . .
C25 C 0.9669(3) 0.9046(3) 0.1431(3) 0.0301(9) Uani 1 1 d . . .
H25A H 0.9520 0.9196 0.1955 0.045 Uiso 1 1 calc R . .
H25B H 1.0337 0.9398 0.1465 0.045 Uiso 1 1 calc R . .
H25C H 0.9772 0.8321 0.1396 0.045 Uiso 1 1 calc R . .
C26 C 0.6617(3) 0.9875(3) 0.3894(2) 0.0164(6) Uani 1 1 d . . .
C27 C 0.5331(3) 1.1316(3) 0.3192(3) 0.0276(8) Uani 1 1 d . . .
H27A H 0.4830 1.1505 0.3477 0.041 Uiso 1 1 calc R . .
H27B H 0.4977 1.1442 0.2561 0.041 Uiso 1 1 calc R . .
H27C H 0.6006 1.1715 0.3439 0.041 Uiso 1 1 calc R . .
C28 C 0.4767(3) 0.9523(3) 0.2759(3) 0.0279(8) Uani 1 1 d . . .
H28A H 0.4828 0.9499 0.2186 0.042 Uiso 1 1 calc R . .
H28B H 0.4033 0.9762 0.2684 0.042 Uiso 1 1 calc R . .
H28C H 0.4883 0.8850 0.3018 0.042 Uiso 1 1 calc R . .
C29 C 0.6891(4) 1.1126(3) 0.5097(3) 0.0291(8) Uani 1 1 d . . .
H29A H 0.6094 1.1044 0.4908 0.044 Uiso 1 1 calc R . .
H29B H 0.7058 1.1825 0.5012 0.044 Uiso 1 1 calc R . .
H29C H 0.7250 1.0951 0.5720 0.044 Uiso 1 1 calc R . .
C30 C 0.8484(3) 1.0180(3) 0.5006(3) 0.0249(8) Uani 1 1 d . . .
H30A H 0.8581 0.9730 0.5500 0.037 Uiso 1 1 calc R . .
H30B H 0.8919 1.0790 0.5222 0.037 Uiso 1 1 calc R . .
H30C H 0.8728 0.9841 0.4587 0.037 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.4228(7) . ?
I2 Cu2 2.4265(7) . ?
I3 I4 2.9861(10) . ?
I4 I5 2.8897(10) . ?
I6 I7 2.9241(7) . ?
I7 I8 2.9103(7) . ?
Cu1 N10 1.935(3) . ?
Cu1 N1 1.952(3) . ?
Cu2 N4 1.949(3) . ?
Cu2 N7 1.951(3) . ?
N1 C1 1.339(4) . ?
N1 C11 1.381(4) . ?
N2 C11 1.340(4) . ?
N2 C13 1.462(5) . ?
N2 C12 1.465(5) . ?
N3 C11 1.335(4) . ?
N3 C15 1.452(5) . ?
N3 C14 1.475(5) . ?
N4 C4 1.347(4) . ?
N4 C16 1.384(4) . ?
N5 C16 1.344(4) . ?
N5 C18 1.454(5) . ?
N5 C17 1.467(5) . ?
N6 C16 1.329(4) . ?
N6 C19 1.465(4) . ?
N6 C20 1.465(4) . ?
N7 C6 1.350(4) . ?
N7 C21 1.379(4) . ?
N8 C21 1.341(5) . ?
N8 C23 1.460(5) . ?
N8 C22 1.462(5) . ?
N9 C21 1.334(5) . ?
N9 C25 1.456(5) . ?
N9 C24 1.474(5) . ?
N10 C9 1.353(4) . ?
N10 C26 1.382(4) . ?
N11 C26 1.337(5) . ?
N11 C28 1.456(5) . ?
N11 C27 1.474(5) . ?
N12 C26 1.339(5) . ?
N12 C30 1.454(5) . ?
N12 C29 1.469(5) . ?
C1 C2 1.436(5) . ?
C1 C10 1.442(4) . ?
C2 C3 1.345(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.428(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.445(4) . ?
C5 C6 1.439(4) . ?
C5 C10 1.478(4) . ?
C6 C7 1.439(5) . ?
C7 C8 1.333(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.432(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.440(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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
I5 I4 I3 176.576(11) . . ?
I8 I7 I6 176.860(12) . . ?
N10 Cu1 N1 91.11(12) . . ?
N10 Cu1 I1 139.71(9) . . ?
N1 Cu1 I1 129.18(8) . . ?
N4 Cu2 N7 89.95(12) . . ?
N4 Cu2 I2 135.35(9) . . ?
N7 Cu2 I2 134.13(8) . . ?
C1 N1 C11 121.1(3) . . ?
C1 N1 Cu1 129.0(2) . . ?
C11 N1 Cu1 109.9(2) . . ?
C11 N2 C13 123.1(3) . . ?
C11 N2 C12 120.0(3) . . ?
C13 N2 C12 115.0(3) . . ?
C11 N3 C15 120.4(3) . . ?
C11 N3 C14 122.7(3) . . ?
C15 N3 C14 115.5(3) . . ?
C4 N4 C16 119.9(3) . . ?
C4 N4 Cu2 129.1(2) . . ?
C16 N4 Cu2 110.9(2) . . ?
C16 N5 C18 121.1(3) . . ?
C16 N5 C17 122.4(3) . . ?
C18 N5 C17 115.4(3) . . ?
C16 N6 C19 122.7(3) . . ?
C16 N6 C20 120.7(3) . . ?
C19 N6 C20 115.5(3) . . ?
C6 N7 C21 120.0(3) . . ?
C6 N7 Cu2 129.8(2) . . ?
C21 N7 Cu2 109.3(2) . . ?
C21 N8 C23 121.1(3) . . ?
C21 N8 C22 121.3(4) . . ?
C23 N8 C22 115.5(3) . . ?
C21 N9 C25 121.4(3) . . ?
C21 N9 C24 121.9(3) . . ?
C25 N9 C24 115.4(3) . . ?
C9 N10 C26 121.9(3) . . ?
C9 N10 Cu1 129.0(2) . . ?
C26 N10 Cu1 108.8(2) . . ?
C26 N11 C28 121.0(3) . . ?
C26 N11 C27 123.4(3) . . ?
C28 N11 C27 115.0(3) . . ?
C26 N12 C30 120.2(3) . . ?
C26 N12 C29 122.3(3) . . ?
C30 N12 C29 114.1(3) . . ?
N1 C1 C2 117.0(3) . . ?
N1 C1 C10 124.4(3) . . ?
C2 C1 C10 118.6(3) . . ?
C3 C2 C1 122.3(3) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 122.6(3) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
N4 C4 C3 117.1(3) . . ?
N4 C4 C5 124.6(3) . . ?
C3 C4 C5 118.3(3) . . ?
C6 C5 C4 121.6(3) . . ?
C6 C5 C10 119.0(3) . . ?
C4 C5 C10 119.4(3) . . ?
N7 C6 C5 123.9(3) . . ?
N7 C6 C7 117.6(3) . . ?
C5 C6 C7 118.5(3) . . ?
C8 C7 C6 122.2(3) . . ?
C8 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C7 C8 C9 122.6(3) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
N10 C9 C8 117.2(3) . . ?
N10 C9 C10 124.3(3) . . ?
C8 C9 C10 118.5(3) . . ?
C9 C10 C1 122.1(3) . . ?
C9 C10 C5 119.0(3) . . ?
C1 C10 C5 118.8(3) . . ?
N3 C11 N2 121.2(3) . . ?
N3 C11 N1 119.8(3) . . ?
N2 C11 N1 118.9(3) . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 H14A 109.5 . . ?
N3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 N5 121.1(3) . . ?
N6 C16 N4 119.0(3) . . ?
N5 C16 N4 119.7(3) . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N6 C19 H19A 109.5 . . ?
N6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 H20A 109.5 . . ?
N6 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N6 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N9 C21 N8 120.7(3) . . ?
N9 C21 N7 120.2(3) . . ?
N8 C21 N7 119.0(3) . . ?
N8 C22 H22A 109.5 . . ?
N8 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N8 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N8 C23 H23A 109.5 . . ?
N8 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N8 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N9 C24 H24A 109.5 . . ?
N9 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N9 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N9 C25 H25A 109.5 . . ?
N9 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N9 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N11 C26 N12 121.4(3) . . ?
N11 C26 N10 120.4(3) . . ?
N12 C26 N10 118.1(3) . . ?
N11 C27 H27A 109.5 . . ?
N11 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N11 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N11 C28 H28A 109.5 . . ?
N11 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N11 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N12 C29 H29A 109.5 . . ?
N12 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N12 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N12 C30 H30A 109.5 . . ?
N12 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N12 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

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
N10 Cu1 N1 C1 3.9(3) . . . . ?
I1 Cu1 N1 C1 -176.7(2) . . . . ?
N10 Cu1 N1 C11 -172.8(2) . . . . ?
I1 Cu1 N1 C11 6.6(3) . . . . ?
N7 Cu2 N4 C4 11.2(3) . . . . ?
I2 Cu2 N4 C4 -176.9(2) . . . . ?
N7 Cu2 N4 C16 -163.3(2) . . . . ?
I2 Cu2 N4 C16 8.5(3) . . . . ?
N4 Cu2 N7 C6 -8.9(3) . . . . ?
I2 Cu2 N7 C6 179.0(2) . . . . ?
N4 Cu2 N7 C21 160.0(2) . . . . ?
I2 Cu2 N7 C21 -12.0(3) . . . . ?
N1 Cu1 N10 C9 -2.0(3) . . . . ?
I1 Cu1 N10 C9 178.7(2) . . . . ?
N1 Cu1 N10 C26 172.4(2) . . . . ?
I1 Cu1 N10 C26 -6.9(3) . . . . ?
C11 N1 C1 C2 -10.4(5) . . . . ?
Cu1 N1 C1 C2 173.2(3) . . . . ?
C11 N1 C1 C10 172.2(3) . . . . ?
Cu1 N1 C1 C10 -4.1(5) . . . . ?
N1 C1 C2 C3 -179.1(4) . . . . ?
C10 C1 C2 C3 -1.6(5) . . . . ?
C1 C2 C3 C4 2.2(6) . . . . ?
C16 N4 C4 C3 -16.7(5) . . . . ?
Cu2 N4 C4 C3 169.2(3) . . . . ?
C16 N4 C4 C5 166.1(3) . . . . ?
Cu2 N4 C4 C5 -8.0(5) . . . . ?
C2 C3 C4 N4 -179.2(3) . . . . ?
C2 C3 C4 C5 -1.8(5) . . . . ?
N4 C4 C5 C6 -2.0(5) . . . . ?
C3 C4 C5 C6 -179.2(3) . . . . ?
N4 C4 C5 C10 178.0(3) . . . . ?
C3 C4 C5 C10 0.8(5) . . . . ?
C21 N7 C6 C5 -164.8(3) . . . . ?
Cu2 N7 C6 C5 3.2(5) . . . . ?
C21 N7 C6 C7 17.8(5) . . . . ?
Cu2 N7 C6 C7 -174.3(3) . . . . ?
C4 C5 C6 N7 4.4(5) . . . . ?
C10 C5 C6 N7 -175.6(3) . . . . ?
C4 C5 C6 C7 -178.2(3) . . . . ?
C10 C5 C6 C7 1.8(5) . . . . ?
N7 C6 C7 C8 179.7(3) . . . . ?
C5 C6 C7 C8 2.2(5) . . . . ?
C6 C7 C8 C9 -4.4(6) . . . . ?
C26 N10 C9 C8 9.0(5) . . . . ?
Cu1 N10 C9 C8 -177.2(2) . . . . ?
C26 N10 C9 C10 -173.5(3) . . . . ?
Cu1 N10 C9 C10 0.3(5) . . . . ?
C7 C8 C9 N10 -179.8(4) . . . . ?
C7 C8 C9 C10 2.5(5) . . . . ?
N10 C9 C10 C1 0.7(5) . . . . ?
C8 C9 C10 C1 178.2(3) . . . . ?
N10 C9 C10 C5 -176.0(3) . . . . ?
C8 C9 C10 C5 1.5(5) . . . . ?
N1 C1 C10 C9 1.3(5) . . . . ?
C2 C1 C10 C9 -176.1(3) . . . . ?
N1 C1 C10 C5 178.0(3) . . . . ?
C2 C1 C10 C5 0.6(5) . . . . ?
C6 C5 C10 C9 -3.5(4) . . . . ?
C4 C5 C10 C9 176.5(3) . . . . ?
C6 C5 C10 C1 179.7(3) . . . . ?
C4 C5 C10 C1 -0.3(4) . . . . ?
C15 N3 C11 N2 166.0(3) . . . . ?
C14 N3 C11 N2 -28.3(5) . . . . ?
C15 N3 C11 N1 -9.9(5) . . . . ?
C14 N3 C11 N1 155.8(3) . . . . ?
C13 N2 C11 N3 -31.9(5) . . . . ?
C12 N2 C11 N3 164.5(3) . . . . ?
C13 N2 C11 N1 144.0(3) . . . . ?
C12 N2 C11 N1 -19.6(5) . . . . ?
C1 N1 C11 N3 -71.0(4) . . . . ?
Cu1 N1 C11 N3 106.0(3) . . . . ?
C1 N1 C11 N2 113.0(4) . . . . ?
Cu1 N1 C11 N2 -70.0(3) . . . . ?
C19 N6 C16 N5 -29.0(5) . . . . ?
C20 N6 C16 N5 163.2(3) . . . . ?
C19 N6 C16 N4 145.8(3) . . . . ?
C20 N6 C16 N4 -22.0(5) . . . . ?
C18 N5 C16 N6 158.8(3) . . . . ?
C17 N5 C16 N6 -33.9(5) . . . . ?
C18 N5 C16 N4 -15.9(5) . . . . ?
C17 N5 C16 N4 151.4(3) . . . . ?
C4 N4 C16 N6 121.4(4) . . . . ?
Cu2 N4 C16 N6 -63.5(4) . . . . ?
C4 N4 C16 N5 -63.8(4) . . . . ?
Cu2 N4 C16 N5 111.3(3) . . . . ?
C25 N9 C21 N8 -160.4(4) . . . . ?
C24 N9 C21 N8 33.4(5) . . . . ?
C25 N9 C21 N7 15.3(5) . . . . ?
C24 N9 C21 N7 -150.9(4) . . . . ?
C23 N8 C21 N9 -162.1(3) . . . . ?
C22 N8 C21 N9 35.4(5) . . . . ?
C23 N8 C21 N7 22.1(5) . . . . ?
C22 N8 C21 N7 -140.3(4) . . . . ?
C6 N7 C21 N9 60.7(4) . . . . ?
Cu2 N7 C21 N9 -109.5(3) . . . . ?
C6 N7 C21 N8 -123.5(4) . . . . ?
Cu2 N7 C21 N8 66.3(3) . . . . ?
C28 N11 C26 N12 -165.6(3) . . . . ?
C27 N11 C26 N12 24.1(5) . . . . ?
C28 N11 C26 N10 10.4(5) . . . . ?
C27 N11 C26 N10 -159.9(3) . . . . ?
C30 N12 C26 N11 -164.6(3) . . . . ?
C29 N12 C26 N11 37.3(5) . . . . ?
C30 N12 C26 N10 19.3(5) . . . . ?
C29 N12 C26 N10 -138.8(3) . . . . ?
C9 N10 C26 N11 65.5(5) . . . . ?
Cu1 N10 C26 N11 -109.5(3) . . . . ?
C9 N10 C26 N12 -118.4(4) . . . . ?
Cu1 N10 C26 N12 66.6(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.576
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.118
####################################################################### 
# 
# 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_hi_az4
_database_code_depnum_ccdc_archive 'CCDC 1413940'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             
;
'Fri May 03 17:03:45 2013'
;

_audit_block_code                hi_az4
_audit_block_refno               1761
_audit_block_usercomment         'hi_az117c, needle, red'

_vrf_DIFMX01_hi_az4              
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: Residual electron density in between parallel layers of molecules
          (stacking distance 3.355 A) is not assignable to atoms.
;
# start Validation Reply Form
_vrf_PLAT097_hi_az4              
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       1.10 eA-3
RESPONSE: see _vrf_DIFMX01_hi_az4
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C16 H16 N6'
_chemical_formula_sum            'C16 H16 N6'
_chemical_formula_weight         292.35
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            red
_diffrn_ambient_temperature      110(1)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.2045(5)
_cell_length_b                   4.3265(2)
_cell_length_c                   15.5492(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.654(5)
_cell_angle_gamma                90
_cell_volume                     678.68(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4494
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.5710
_cell_measurement_theta_min      4.3780
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.2669
_exptl_crystal_size_mid          0.0694
_exptl_crystal_size_min          0.0300
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13964
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.912
_diffrn_reflns_theta_min         4.383
_diffrn_detector_area_resol_mean 15.9241
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1146
_reflns_number_total             1306
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1306
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0881
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1837P)²+0.4102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2313
_refine_ls_wR_factor_ref         0.2414
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
N1 N 0.14548(17) 0.1019(4) 0.14329(11) 0.0200(6) Uani 1 1 d . . . . .
N2 N 0.24224(17) 0.0913(4) 0.00955(11) 0.0207(6) Uani 1 1 d . . . . .
N3 N 0.33183(19) -0.1887(5) 0.13114(12) 0.0286(6) Uani 1 1 d . . . . .
C12 C 0.0522(2) 0.2949(5) 0.10574(13) 0.0173(6) Uani 1 1 d . . . . .
C13 C -0.0491(2) 0.4148(5) 0.15307(13) 0.0200(6) Uani 1 1 d . . . . .
H13 H -0.0492 0.3527 0.2117 0.024 Uiso 1 1 calc R U . . .
C14 C -0.1433(2) 0.6131(5) 0.11565(13) 0.0205(6) Uani 1 1 d . . . . .
H14 H -0.2081 0.6866 0.1486 0.025 Uiso 1 1 calc R U . . .
C15 C -0.1481(2) 0.7159(5) 0.02669(13) 0.0174(6) Uani 1 1 d . . . . .
C16 C 0.0490(2) 0.3973(5) 0.01949(13) 0.0181(6) Uani 1 1 d . . . . .
C17 C 0.2364(2) 0.0087(5) 0.09315(13) 0.0204(6) Uani 1 1 d . . . . .
C18 C 0.3368(2) -0.2819(6) 0.22100(14) 0.0247(6) Uani 1 1 d . . . . .
H18A H 0.3369 -0.0978 0.2577 0.037 Uiso 1 1 calc R U . . .
H18B H 0.4176 -0.4017 0.2393 0.037 Uiso 1 1 calc R U . . .
H18C H 0.2591 -0.4091 0.2267 0.037 Uiso 1 1 calc R U . . .
C19 C 0.4387(2) -0.2877(6) 0.08537(14) 0.0253(6) Uani 1 1 d . . . . .
H19A H 0.4067 -0.2948 0.0227 0.038 Uiso 1 1 calc R U . . .
H19B H 0.4689 -0.4938 0.1057 0.038 Uiso 1 1 calc R U . . .
H19C H 0.5125 -0.1414 0.0968 0.038 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
N1 C12 1.333(3) . ?
N1 C17 1.360(3) . ?
N2 C15 1.332(3) 3_565 ?
N2 C17 1.358(3) . ?
N3 C17 1.361(3) . ?
N3 C18 1.448(3) . ?
N3 C19 1.453(3) . ?
C12 C13 1.452(3) . ?
C12 C16 1.408(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.353(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.447(3) . ?
C15 N2 1.332(3) 3_565 ?
C15 C16 1.413(3) 3_565 ?
C16 C15 1.413(3) 3_565 ?
C16 C16 1.405(4) 3_565 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 N1 C17 116.00(18) . . ?
C15 N2 C17 115.90(18) 3_565 . ?
C17 N3 C18 120.80(18) . . ?
C17 N3 C19 120.86(18) . . ?
C18 N3 C19 118.08(18) . . ?
N1 C12 C13 121.18(19) . . ?
N1 C12 C16 121.82(19) . . ?
C16 C12 C13 117.0(2) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 C12 121.52(19) . . ?
C14 C13 H13 119.2 . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.69(18) . . ?
C15 C14 H14 119.2 . . ?
N2 C15 C14 121.01(18) 3_565 . ?
N2 C15 C16 121.9(2) 3_565 3_565 ?
C16 C15 C14 117.1(2) 3_565 . ?
C12 C16 C15 117.3(2) . 3_565 ?
C16 C16 C12 121.5(2) 3_565 . ?
C16 C16 C15 121.1(2) 3_565 3_565 ?
N1 C17 N3 116.26(18) . . ?
N2 C17 N1 127.1(2) . . ?
N2 C17 N3 116.65(19) . . ?
N3 C18 H18A 109.5 . . ?
N3 C18 H18B 109.5 . . ?
N3 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

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
N1 C12 C13 C14 179.38(19) . . . . ?
N1 C12 C16 C15 0.8(3) . . . 3_565 ?
N1 C12 C16 C16 -179.5(2) . . . 3_565 ?
C12 N1 C17 N2 0.1(3) . . . . ?
C12 N1 C17 N3 -179.96(18) . . . . ?
C12 C13 C14 C15 0.0(3) . . . . ?
C13 C12 C16 C15 179.36(16) . . . 3_565 ?
C13 C12 C16 C16 -0.9(4) . . . 3_565 ?
C13 C14 C15 N2 179.32(19) . . . 3_565 ?
C13 C14 C15 C16 -0.6(3) . . . 3_565 ?
C15 N2 C17 N1 -0.2(3) 3_565 . . . ?
C15 N2 C17 N3 179.91(18) 3_565 . . . ?
C16 C12 C13 C14 0.8(3) . . . . ?
C17 N1 C12 C13 -178.96(17) . . . . ?
C17 N1 C12 C16 -0.4(3) . . . . ?
C18 N3 C17 N1 -2.1(3) . . . . ?
C18 N3 C17 N2 177.84(19) . . . . ?
C19 N3 C17 N1 -176.13(19) . . . . ?
C19 N3 C17 N2 3.8(3) . . . . ?

_shelx_estimated_absorpt_T_max   0.930
_shelx_estimated_absorpt_T_min   0.930
_cell_oxdiff_length_a            10.2032(6)
_cell_oxdiff_length_b            4.3248(2)
_cell_oxdiff_length_c            15.5555(7)
_cell_oxdiff_angle_alpha         89.941(4)
_cell_oxdiff_angle_beta          98.611(4)
_cell_oxdiff_angle_gamma         90.037(4)
_cell_oxdiff_volume              678.68(6)
_cell_oxdiff_measurement_reflns_used 4494
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2 2 3 0.0363 2.0046 1.9973 3.0099 -0.0167 -0.4017 -0.7460
5 -1 5 0.1231 5.0017 -1.0019 5.0179 -0.0564 0.7867 -0.6756
-5 1 -5 0.1231 -5.0017 1.0019 -5.0179 0.0564 -0.7867 0.6756
-2 -2 -3 0.0293 -2.0046 -1.9973 -3.0099 0.0167 0.4017 0.7460
-4 0 9 0.0111 -4.0093 -0.0020 8.9911 -1.0054 -0.0750 -0.0664
4 0 -9 0.0189 4.0093 0.0020 -8.9911 1.0054 0.0750 0.0664
_diffrn_radiation_monochromator  mirror
_diffrn_orient_matrix_UB_11      0.0745766000
_diffrn_orient_matrix_UB_12      0.0351786000
_diffrn_orient_matrix_UB_13      -0.0785573000
_diffrn_orient_matrix_UB_21      0.0717683000
_diffrn_orient_matrix_UB_22      -0.3087149000
_diffrn_orient_matrix_UB_23      0.0235977000
_diffrn_orient_matrix_UB_31      -0.1122843000
_diffrn_orient_matrix_UB_32      -0.1741968000
_diffrn_orient_matrix_UB_33      -0.0574902000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -17.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   50.0000   60.0000 66

#__ type_ start__ end____ width___ exp.time_
  2 omega  -71.00  -24.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -64.0000   30.0000 47

#__ type_ start__ end____ width___ exp.time_
  3 omega  -24.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000  -90.0000 34

#__ type_ start__ end____ width___ exp.time_
  4 omega  -18.00   18.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -64.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
  5 omega   19.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   79.0000   61.1425 28

#__ type_ start__ end____ width___ exp.time_
  6 omega    4.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   78.0000  150.5895 31

#__ type_ start__ end____ width___ exp.time_
  7 omega    8.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -64.3191 25

#__ type_ start__ end____ width___ exp.time_
  8 omega   11.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000  -48.5502 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   86.00  112.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   75.0000   83.3012 26

#__ type_ start__ end____ width___ exp.time_
 10 omega   13.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   75.0000   83.3012 42

#__ type_ start__ end____ width___ exp.time_
 11 omega   10.00   38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  178.4690 28

#__ type_ start__ end____ width___ exp.time_
 12 omega   24.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   74.0000 -101.3982 25

#__ type_ start__ end____ width___ exp.time_
 13 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -165.1476 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   19.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000  -33.8966 36

#__ type_ start__ end____ width___ exp.time_
 15 omega   19.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -149.2094 26

#__ type_ start__ end____ width___ exp.time_
 16 omega    3.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -70.0000  158.8291 70

#__ type_ start__ end____ width___ exp.time_
 17 omega   41.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000 -134.0792 32

#__ type_ start__ end____ width___ exp.time_
 18 omega   30.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -25.5250 27

#__ type_ start__ end____ width___ exp.time_
 19 omega   34.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   82.4637 27

#__ type_ start__ end____ width___ exp.time_
 20 omega   29.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -60.4871 48

#__ type_ start__ end____ width___ exp.time_
 21 omega   79.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -60.4871 49

#__ type_ start__ end____ width___ exp.time_
 22 omega  102.00  129.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000    2.8067 27

#__ type_ start__ end____ width___ exp.time_
 23 omega   42.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000    2.8067 27

#__ type_ start__ end____ width___ exp.time_
 24 omega   34.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  128.3496 27

#__ type_ start__ end____ width___ exp.time_
 25 omega   88.00  127.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  128.3496 39

#__ type_ start__ end____ width___ exp.time_
 26 omega   42.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   59.0000  -21.4811 28

#__ type_ start__ end____ width___ exp.time_
 27 omega  107.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000 -100.4329 27

#__ type_ start__ end____ width___ exp.time_
 28 omega   38.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000 -100.4329 26

#__ type_ start__ end____ width___ exp.time_
 29 omega  108.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   62.0000   27.0901 26

#__ type_ start__ end____ width___ exp.time_
 30 omega   46.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   62.0000   27.0901 27

#__ type_ start__ end____ width___ exp.time_
 31 omega  113.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   44.0000  -13.2844 27

#__ type_ start__ end____ width___ exp.time_
 32 omega   47.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   44.0000  -13.2844 27

#__ type_ start__ end____ width___ exp.time_
 33 omega   93.00  130.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   59.0000 -163.3023 37

#__ type_ start__ end____ width___ exp.time_
 34 omega   50.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   52.0000  164.2735 29

#__ type_ start__ end____ width___ exp.time_
 35 omega   51.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   59.0000 -163.3023 34

#__ type_ start__ end____ width___ exp.time_
 36 omega   59.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   56.0000  -78.4888 26

#__ type_ start__ end____ width___ exp.time_
 37 omega    0.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   -4.7996 102

#__ type_ start__ end____ width___ exp.time_
 38 omega  107.00  144.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000   37.7927 37

#__ type_ start__ end____ width___ exp.time_
 39 omega  114.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   43.0000   89.1703 32

#__ type_ start__ end____ width___ exp.time_
 40 omega   47.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000   37.7927 29

#__ type_ start__ end____ width___ exp.time_
 41 omega   56.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   67.0000  171.4556 26

#__ type_ start__ end____ width___ exp.time_
 42 omega   56.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000   33.5688 26

#__ type_ start__ end____ width___ exp.time_
 43 omega   59.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   68.0000   96.6377 32

#__ type_ start__ end____ width___ exp.time_
 44 omega   58.00   94.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000 -129.5061 36

#__ type_ start__ end____ width___ exp.time_
 45 omega   71.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   37.0000 -127.5342 27

#__ type_ start__ end____ width___ exp.time_
 46 omega  109.00  154.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000 -129.5061 45

#__ type_ start__ end____ width___ exp.time_
 47 omega  122.00  153.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   68.0000   68.8909 31

#__ type_ start__ end____ width___ exp.time_
 48 omega   70.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   68.0000   68.8909 26

#__ type_ start__ end____ width___ exp.time_
 49 omega   81.00  126.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 45

#__ type_ start__ end____ width___ exp.time_
 50 omega   79.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 95

#__ type_ start__ end____ width___ exp.time_
 51 omega   80.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 52 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 53 omega   37.00   80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   60.0000 43

#__ type_ start__ end____ width___ exp.time_
 54 omega  126.00  166.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 40

#__ type_ start__ end____ width___ exp.time_
 55 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 56 omega  123.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 51

#__ type_ start__ end____ width___ exp.time_
 57 omega   78.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 32

#__ type_ start__ end____ width___ exp.time_
 58 omega  119.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 59

#__ type_ start__ end____ width___ exp.time_
 59 omega  122.00  147.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 60 omega   86.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 29

#__ type_ start__ end____ width___ exp.time_
 61 omega   39.00  128.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -150.0000 89

#__ type_ start__ end____ width___ exp.time_
 62 omega  135.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 41

#__ type_ start__ end____ width___ exp.time_
 63 omega   83.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000    0.0000 56

#__ type_ start__ end____ width___ exp.time_
 64 omega   59.00  100.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -180.0000 41

#__ type_ start__ end____ width___ exp.time_
 65 omega  141.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -116.7706 27

#__ type_ start__ end____ width___ exp.time_
 66 omega   84.00  131.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 47

#__ type_ start__ end____ width___ exp.time_
 67 omega   80.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -116.7706 27

#__ type_ start__ end____ width___ exp.time_
 68 omega   88.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 69 omega   56.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -78.0000   74.2293 40

#__ type_ start__ end____ width___ exp.time_
 70 omega   85.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 83

#__ type_ start__ end____ width___ exp.time_
 71 omega  145.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 30

#__ type_ start__ end____ width___ exp.time_
 72 omega   79.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 73 omega   82.00  135.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -132.0000 53

#__ type_ start__ end____ width___ exp.time_
 74 omega   86.00  124.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 38

#__ type_ start__ end____ width___ exp.time_
 75 omega   47.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   30.0000 63

#__ type_ start__ end____ width___ exp.time_
 76 omega  140.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 38

#__ type_ start__ end____ width___ exp.time_
 77 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 78 omega   86.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 79 omega   57.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  120.0000 56

#__ type_ start__ end____ width___ exp.time_
 80 omega   85.00  161.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 76

#__ type_ start__ end____ width___ exp.time_
 81 omega   61.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -42.3472 43

#__ type_ start__ end____ width___ exp.time_
 82 omega   98.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
 83 omega  114.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 63

#__ type_ start__ end____ width___ exp.time_
 84 omega   82.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
 85 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 86 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 87 omega  -72.00   18.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -57.0000  -60.0000 90

#__ type_ start__ end____ width___ exp.time_
 88 omega   -6.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000   39.4225 52

#__ type_ start__ end____ width___ exp.time_
 89 omega    3.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   78.0000  105.7911 46

#__ type_ start__ end____ width___ exp.time_
 90 omega    7.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  104.8334 40

#__ type_ start__ end____ width___ exp.time_
 91 omega   19.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -149.2094 28

#__ type_ start__ end____ width___ exp.time_
 92 omega  -15.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -70.0000  158.8291 95

#__ type_ start__ end____ width___ exp.time_
 93 omega   31.00  127.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000 -134.0792 96

#__ type_ start__ end____ width___ exp.time_
 94 omega   28.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -60.4871 100

#__ type_ start__ end____ width___ exp.time_
 95 omega   34.00  132.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  128.3496 98

#__ type_ start__ end____ width___ exp.time_
 96 omega   38.00  130.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000    2.8067 92

#__ type_ start__ end____ width___ exp.time_
 97 omega   44.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   62.0000   27.0901 90

#__ type_ start__ end____ width___ exp.time_
 98 omega   49.00  130.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   52.0000  164.2735 81

#__ type_ start__ end____ width___ exp.time_
 99 omega   50.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   59.0000 -163.3023 88

#__ type_ start__ end____ width___ exp.time_
100 omega   -1.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   -4.7996 103

#__ type_ start__ end____ width___ exp.time_
101 omega   46.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000 -112.1281 92

#__ type_ start__ end____ width___ exp.time_
102 omega   47.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   34.0000  -67.5575 100

#__ type_ start__ end____ width___ exp.time_
103 omega   46.00  144.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000   37.7927 98

#__ type_ start__ end____ width___ exp.time_
104 omega   56.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000   33.5688 92

#__ type_ start__ end____ width___ exp.time_
105 omega   56.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   50.0000  102.6818 92

#__ type_ start__ end____ width___ exp.time_
106 omega   54.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   67.0000  171.4556 92

;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent EOS'
_diffrn_measurement_specimen_support 'polyimid foil'


####################################################################### 
# 
# 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_aztw24as
_database_code_depnum_ccdc_archive 'CCDC 1413941'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
#==============================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;                                                                              
 ?                                                                             
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H58 Br4 Cu2 N14'
_chemical_formula_weight         1109.66

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   12.416(3)
_cell_length_b                   15.494(3)
_cell_length_c                   12.116(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.09(3)
_cell_angle_gamma                90.00
_cell_volume                     2279.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      30.10

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1116
_exptl_absorpt_coefficient_mu    4.481
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1741
_exptl_absorpt_correction_T_max  0.4677
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;                                                                               
 ?                                                                              
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39633
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         30.10
_reflns_number_total             6694
_reflns_number_gt                5188
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;                                                                               
 Refinement of F² against ALL reflections.  The weighted R-factor wR and      
 goodness of fit S are based on F², conventional R-factors R are based        
 on F, with F set to zero for negative F². The threshold expression of        
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is     
 not relevant to the choice of reflections for refinement.  R-factors based     
 on F² are statistically about twice as large as those based on F, and R-     
 factors based on ALL data will be even larger.                                 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0540P)²+1.1332P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6694
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1094
_refine_ls_wR_factor_gt          0.1010
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.02187(3) 0.11563(2) 0.75670(3) 0.03020(9) Uani 1 1 d . . .
Br2 Br 0.34500(3) 0.204512(18) 0.77956(2) 0.03003(9) Uani 1 1 d . . .
Cu1 Cu 0.21556(3) 0.09885(2) 0.83214(3) 0.02159(9) Uani 1 1 d . . .
N1 N 0.28235(19) -0.02135(14) 0.82269(18) 0.0188(4) Uani 1 1 d . . .
N2 N 0.2286(2) -0.16565(14) 0.78093(19) 0.0231(5) Uani 1 1 d . . .
N3 N 0.1745(2) -0.05889(15) 0.64771(19) 0.0222(5) Uani 1 1 d . . .
N4 N 0.26966(19) 0.07615(14) 1.00052(18) 0.0187(4) Uani 1 1 d . . .
N5 N 0.1353(2) 0.16300(15) 1.0544(2) 0.0242(5) Uani 1 1 d . . .
N6 N 0.2050(2) 0.04643(15) 1.1655(2) 0.0241(5) Uani 1 1 d . . .
C1 C 0.3902(2) -0.03363(16) 0.8730(2) 0.0172(5) Uani 1 1 d . . .
C2 C 0.4417(2) 0.00629(15) 0.9779(2) 0.0164(5) Uani 1 1 d . . .
C3 C 0.3788(2) 0.05956(16) 1.0385(2) 0.0177(5) Uani 1 1 d . . .
C4 C 0.4348(2) 0.09993(17) 1.1405(2) 0.0209(5) Uani 1 1 d . . .
H4 H 0.3962 0.1376 1.1779 0.025 Uiso 1 1 calc R . .
C5 C 0.5424(2) 0.08463(17) 1.1838(2) 0.0209(5) Uani 1 1 d . . .
H5 H 0.5740 0.1083 1.2536 0.025 Uiso 1 1 calc R . .
C6 C 0.2309(2) -0.08134(17) 0.7497(2) 0.0192(5) Uani 1 1 d . . .
C7 C 0.2363(3) -0.23545(18) 0.7016(3) 0.0316(7) Uani 1 1 d . . .
H7A H 0.2433 -0.2114 0.6304 0.047 Uiso 1 1 calc R . .
H7B H 0.1711 -0.2704 0.6912 0.047 Uiso 1 1 calc R . .
H7C H 0.2996 -0.2704 0.7311 0.047 Uiso 1 1 calc R . .
C8 C 0.2534(3) -0.19004(19) 0.8998(2) 0.0289(6) Uani 1 1 d . . .
H8A H 0.3311 -0.1995 0.9241 0.043 Uiso 1 1 calc R . .
H8B H 0.2145 -0.2421 0.9097 0.043 Uiso 1 1 calc R . .
H8C H 0.2308 -0.1446 0.9439 0.043 Uiso 1 1 calc R . .
C9 C 0.2009(3) 0.01948(19) 0.5921(2) 0.0274(6) Uani 1 1 d . . .
H9A H 0.1441 0.0616 0.5916 0.041 Uiso 1 1 calc R . .
H9B H 0.2058 0.0063 0.5159 0.041 Uiso 1 1 calc R . .
H9C H 0.2700 0.0421 0.6322 0.041 Uiso 1 1 calc R . .
C10 C 0.0748(3) -0.10326(19) 0.5896(3) 0.0297(6) Uani 1 1 d . . .
H10A H 0.0571 -0.1486 0.6367 0.045 Uiso 1 1 calc R . .
H10B H 0.0869 -0.1274 0.5202 0.045 Uiso 1 1 calc R . .
H10C H 0.0149 -0.0629 0.5735 0.045 Uiso 1 1 calc R . .
C11 C 0.2057(2) 0.09656(16) 1.0744(2) 0.0193(5) Uani 1 1 d . . .
C12 C 0.1619(3) 0.24087(18) 0.9973(3) 0.0305(7) Uani 1 1 d . . .
H12A H 0.2352 0.2363 0.9841 0.046 Uiso 1 1 calc R . .
H12B H 0.1572 0.2903 1.0438 0.046 Uiso 1 1 calc R . .
H12C H 0.1106 0.2471 0.9265 0.046 Uiso 1 1 calc R . .
C13 C 0.0251(3) 0.1602(2) 1.0786(3) 0.0385(8) Uani 1 1 d . . .
H13A H 0.0107 0.1032 1.1032 0.058 Uiso 1 1 calc R . .
H13B H -0.0282 0.1743 1.0115 0.058 Uiso 1 1 calc R . .
H13C H 0.0203 0.2011 1.1368 0.058 Uiso 1 1 calc R . .
C14 C 0.1817(3) 0.0807(2) 1.2703(3) 0.0306(7) Uani 1 1 d . . .
H14A H 0.1776 0.1425 1.2660 0.046 Uiso 1 1 calc R . .
H14B H 0.2394 0.0640 1.3325 0.046 Uiso 1 1 calc R . .
H14C H 0.1127 0.0580 1.2814 0.046 Uiso 1 1 calc R . .
C15 C 0.2476(3) -0.04105(18) 1.1738(3) 0.0306(7) Uani 1 1 d . . .
H15A H 0.2444 -0.0637 1.0994 0.046 Uiso 1 1 calc R . .
H15B H 0.2040 -0.0765 1.2126 0.046 Uiso 1 1 calc R . .
H15C H 0.3226 -0.0409 1.2149 0.046 Uiso 1 1 calc R . .
N21 N 0.3500(4) -0.1068(2) 0.4752(4) 0.0641(11) Uani 1 1 d . . .
C21 C 0.4395(3) -0.1202(2) 0.4768(3) 0.0349(7) Uani 1 1 d . . .
C22 C 0.5538(3) -0.1399(3) 0.4811(4) 0.0514(10) Uani 1 1 d . . .
H22A H 0.5789 -0.1814 0.5396 0.077 Uiso 1 1 calc R . .
H22B H 0.5968 -0.0881 0.4966 0.077 Uiso 1 1 calc R . .
H22C H 0.5617 -0.1632 0.4098 0.077 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Cu1 2.4011(8) . ?
Br2 Cu1 2.4694(6) . ?
Cu1 N4 2.040(2) . ?
Cu1 N1 2.052(2) . ?
N1 C6 1.348(3) . ?
N1 C1 1.363(3) . ?
N2 C6 1.362(3) . ?
N2 C8 1.458(4) . ?
N2 C7 1.464(4) . ?
N3 C6 1.333(3) . ?
N3 C9 1.459(4) . ?
N3 C10 1.461(4) . ?
N4 C11 1.352(3) . ?
N4 C3 1.361(3) . ?
N5 C11 1.339(3) . ?
N5 C13 1.458(4) . ?
N5 C12 1.463(4) . ?
N6 C11 1.352(3) . ?
N6 C15 1.451(4) . ?
N6 C14 1.460(4) . ?
C1 C5 1.428(4) 3_657 ?
C1 C2 1.437(3) . ?
C2 C3 1.439(3) . ?
C2 C2 1.448(5) 3_657 ?
C3 C4 1.428(4) . ?
C4 C5 1.351(4) . ?
C4 H4 0.9300 . ?
C5 C1 1.428(4) 3_657 ?
C5 H5 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N21 C21 1.126(5) . ?
C21 C22 1.442(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

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
N4 Cu1 N1 81.20(9) . . ?
N4 Cu1 Br1 119.54(7) . . ?
N1 Cu1 Br1 117.47(7) . . ?
N4 Cu1 Br2 106.06(7) . . ?
N1 Cu1 Br2 107.15(7) . . ?
Br1 Cu1 Br2 118.95(2) . . ?
C6 N1 C1 118.9(2) . . ?
C6 N1 Cu1 121.41(18) . . ?
C1 N1 Cu1 118.18(17) . . ?
C6 N2 C8 120.7(2) . . ?
C6 N2 C7 121.2(2) . . ?
C8 N2 C7 115.3(2) . . ?
C6 N3 C9 121.3(2) . . ?
C6 N3 C10 123.5(2) . . ?
C9 N3 C10 114.7(2) . . ?
C11 N4 C3 120.1(2) . . ?
C11 N4 Cu1 120.35(18) . . ?
C3 N4 Cu1 117.82(17) . . ?
C11 N5 C13 123.0(3) . . ?
C11 N5 C12 121.1(2) . . ?
C13 N5 C12 115.7(3) . . ?
C11 N6 C15 121.9(2) . . ?
C11 N6 C14 122.6(2) . . ?
C15 N6 C14 114.5(2) . . ?
N1 C1 C5 118.8(2) . 3_657 ?
N1 C1 C2 123.3(2) . . ?
C5 C1 C2 117.9(2) 3_657 . ?
C1 C2 C3 120.7(2) . . ?
C1 C2 C2 119.6(3) . 3_657 ?
C3 C2 C2 119.7(3) . 3_657 ?
N4 C3 C4 118.6(2) . . ?
N4 C3 C2 122.9(2) . . ?
C4 C3 C2 118.4(2) . . ?
C5 C4 C3 121.4(2) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C1 122.8(2) . 3_657 ?
C4 C5 H5 118.6 . . ?
C1 C5 H5 118.6 3_657 . ?
N3 C6 N1 120.9(2) . . ?
N3 C6 N2 118.0(2) . . ?
N1 C6 N2 120.9(2) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 N6 118.2(2) . . ?
N5 C11 N4 120.8(2) . . ?
N6 C11 N4 120.8(2) . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N21 C21 C22 178.2(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

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
N4 Cu1 N1 C6 138.1(2) . . . . ?
Br1 Cu1 N1 C6 19.3(2) . . . . ?
Br2 Cu1 N1 C6 -117.68(19) . . . . ?
N4 Cu1 N1 C1 -56.12(19) . . . . ?
Br1 Cu1 N1 C1 -174.92(16) . . . . ?
Br2 Cu1 N1 C1 48.07(19) . . . . ?
N1 Cu1 N4 C11 -137.3(2) . . . . ?
Br1 Cu1 N4 C11 -20.6(2) . . . . ?
Br2 Cu1 N4 C11 117.27(19) . . . . ?
N1 Cu1 N4 C3 57.75(19) . . . . ?
Br1 Cu1 N4 C3 174.42(16) . . . . ?
Br2 Cu1 N4 C3 -47.68(19) . . . . ?
C6 N1 C1 C5 26.7(3) . . . 3_657 ?
Cu1 N1 C1 C5 -139.4(2) . . . 3_657 ?
C6 N1 C1 C2 -156.9(2) . . . . ?
Cu1 N1 C1 C2 37.0(3) . . . . ?
N1 C1 C2 C3 2.7(4) . . . . ?
C5 C1 C2 C3 179.1(2) 3_657 . . . ?
N1 C1 C2 C2 -176.4(3) . . . 3_657 ?
C5 C1 C2 C2 0.0(4) 3_657 . . 3_657 ?
C11 N4 C3 C4 -28.4(3) . . . . ?
Cu1 N4 C3 C4 136.6(2) . . . . ?
C11 N4 C3 C2 154.6(2) . . . . ?
Cu1 N4 C3 C2 -40.4(3) . . . . ?
C1 C2 C3 N4 -0.9(4) . . . . ?
C2 C2 C3 N4 178.1(3) 3_657 . . . ?
C1 C2 C3 C4 -178.0(2) . . . . ?
C2 C2 C3 C4 1.1(4) 3_657 . . . ?
N4 C3 C4 C5 178.6(2) . . . . ?
C2 C3 C4 C5 -4.2(4) . . . . ?
C3 C4 C5 C1 5.4(4) . . . 3_657 ?
C9 N3 C6 N1 25.9(4) . . . . ?
C10 N3 C6 N1 -146.2(3) . . . . ?
C9 N3 C6 N2 -158.6(2) . . . . ?
C10 N3 C6 N2 29.3(4) . . . . ?
C1 N1 C6 N3 -129.7(3) . . . . ?
Cu1 N1 C6 N3 36.0(3) . . . . ?
C1 N1 C6 N2 55.1(3) . . . . ?
Cu1 N1 C6 N2 -139.3(2) . . . . ?
C8 N2 C6 N3 -158.2(3) . . . . ?
C7 N2 C6 N3 41.5(4) . . . . ?
C8 N2 C6 N1 17.2(4) . . . . ?
C7 N2 C6 N1 -143.1(3) . . . . ?
C13 N5 C11 N6 -34.8(4) . . . . ?
C12 N5 C11 N6 150.6(3) . . . . ?
C13 N5 C11 N4 140.1(3) . . . . ?
C12 N5 C11 N4 -34.5(4) . . . . ?
C15 N6 C11 N5 158.4(3) . . . . ?
C14 N6 C11 N5 -33.7(4) . . . . ?
C15 N6 C11 N4 -16.5(4) . . . . ?
C14 N6 C11 N4 151.4(3) . . . . ?
C3 N4 C11 N5 133.9(3) . . . . ?
Cu1 N4 C11 N5 -30.7(3) . . . . ?
C3 N4 C11 N6 -51.3(4) . . . . ?
Cu1 N4 C11 N6 144.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.017
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.188
####################################################################### 
# 
# 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_hi_az7
_database_code_depnum_ccdc_archive 'CCDC 1413942'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             
;
'Wed Dec 04 15:27:56 2013'
;

_audit_block_code                hi_az7
_audit_block_refno               1923
_audit_block_usercomment         'hi_aztk1, irregular, black'


_shelxl_version_number           2013-4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C23 H34 Cu I N9, I3'
_chemical_formula_sum            'C23 H34 Cu I4 N9'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         1007.73
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            black
_diffrn_ambient_temperature      110(1)
_chemical_oxdiff_formula         'C23 H34 Cu1 I4 N9'
_chemical_oxdiff_usercomment     'hi_aztk1, irregular, black'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   12.27369(16)
_cell_length_b                   12.65803(14)
_cell_length_c                   20.9347(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3252.43(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21476
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.2970
_cell_measurement_theta_min      4.1500
_shelx_estimated_absorpt_T_max   0.148
_shelx_estimated_absorpt_T_min   0.148
_exptl_absorpt_coefficient_mu    30.982
_exptl_absorpt_correction_T_max  0.193
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.2386
_exptl_crystal_size_mid          0.1494
_exptl_crystal_size_min          0.1077
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.180
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            84894
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.823
_diffrn_reflns_theta_min         4.081
_diffrn_detector_area_resol_mean 7.9621
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0629575000
_diffrn_orient_matrix_UB_12      -0.0920469000
_diffrn_orient_matrix_UB_13      -0.0310303000
_diffrn_orient_matrix_UB_21      0.0369060000
_diffrn_orient_matrix_UB_22      -0.0737103000
_diffrn_orient_matrix_UB_23      0.0543771000
_diffrn_orient_matrix_UB_31      -0.1020948000
_diffrn_orient_matrix_UB_32      0.0300344000
_diffrn_orient_matrix_UB_33      0.0387189000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3087
_reflns_number_total             3277
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         4.856
_refine_diff_density_min         -2.181
_refine_diff_density_rms         0.276
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0659
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1098P)²+21.0922P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1768
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
I1 I 0.05993(6) 0.2500 0.70997(3) 0.0364(2) Uani 1 2 d S T P . .
I2 I 0.47287(6) 0.7500 0.70786(4) 0.0418(3) Uani 1 2 d S T P . .
I3 I 0.53838(8) 0.7500 0.57245(5) 0.0514(3) Uani 1 2 d S T P . .
I4 I 0.41398(10) 0.7500 0.84252(4) 0.0597(3) Uani 1 2 d S T P . .
Cu Cu 0.24803(12) 0.2500 0.67608(7) 0.0298(4) Uani 1 2 d S T P . .
N1 N 0.3495(5) 0.3610(5) 0.6523(3) 0.0262(12) Uani 1 1 d . . . . .
N2 N 0.2728(5) 0.4994(5) 0.7104(3) 0.0317(14) Uani 1 1 d . . . . .
N3 N 0.2677(5) 0.5024(5) 0.5986(3) 0.0294(13) Uani 1 1 d . . . . .
N4 N 0.9280(8) 0.2500 0.5361(5) 0.035(2) Uani 1 2 d S T P . .
N7 N 0.7792(5) 0.3455(5) 0.5727(3) 0.0298(13) Uani 1 1 d . . . . .
C1 C 0.4520(6) 0.3507(5) 0.6310(3) 0.0245(13) Uani 1 1 d . . . . .
C2 C 0.5167(6) 0.4452(6) 0.6217(3) 0.0303(15) Uani 1 1 d . . . . .
H2 H 0.4835 0.5119 0.6289 0.036 Uiso 1 1 calc R . . . .
C3 C 0.6214(6) 0.4427(6) 0.6035(3) 0.0294(14) Uani 1 1 d . . . . .
H3 H 0.6606 0.5069 0.5983 0.035 Uiso 1 1 calc R . . . .
C4 C 0.6745(6) 0.3440(6) 0.5919(3) 0.0291(14) Uani 1 1 d . . . . .
C5 C 0.6160(9) 0.2500 0.6007(5) 0.030(2) Uani 1 2 d S T P . .
C6 C 0.5010(8) 0.2500 0.6204(5) 0.028(2) Uani 1 2 d S T P . .
C7 C 0.8242(9) 0.2500 0.5620(5) 0.032(2) Uani 1 2 d S T P . .
C8 C 0.2973(6) 0.4579(5) 0.6539(3) 0.0274(14) Uani 1 1 d . . . . .
C9 C 0.3273(7) 0.4606(7) 0.7678(4) 0.0392(17) Uani 1 1 d . . . . .
H9A H 0.2835 0.4042 0.7871 0.059 Uiso 1 1 calc GR . . . .
H9B H 0.3355 0.5186 0.7984 0.059 Uiso 1 1 calc GR . . . .
H9C H 0.3993 0.4329 0.7565 0.059 Uiso 1 1 calc GR . . . .
C10 C 0.1732(7) 0.5613(7) 0.7226(4) 0.0398(18) Uani 1 1 d . . . . .
H10A H 0.1930 0.6346 0.7322 0.060 Uiso 1 1 calc GR . . . .
H10B H 0.1340 0.5310 0.7590 0.060 Uiso 1 1 calc GR . . . .
H10C H 0.1264 0.5596 0.6847 0.060 Uiso 1 1 calc GR . . . .
C11 C 0.2771(7) 0.4444(7) 0.5383(4) 0.0357(16) Uani 1 1 d . . . . .
H11A H 0.3496 0.4561 0.5199 0.054 Uiso 1 1 calc GR . . . .
H11B H 0.2214 0.4695 0.5083 0.054 Uiso 1 1 calc GR . . . .
H11C H 0.2666 0.3688 0.5462 0.054 Uiso 1 1 calc GR . . . .
C12 C 0.2461(7) 0.6163(6) 0.5924(4) 0.0398(18) Uani 1 1 d . . . . .
H12A H 0.1692 0.6273 0.5817 0.060 Uiso 1 1 calc GR . . . .
H12B H 0.2919 0.6457 0.5584 0.060 Uiso 1 1 calc GR . . . .
H12C H 0.2627 0.6516 0.6328 0.060 Uiso 1 1 calc GR . . . .
C13 C 0.9898(7) 0.3474(7) 0.5312(4) 0.0373(17) Uani 1 1 d . . . . .
H13A H 1.0317 0.3473 0.4914 0.056 Uiso 1 1 calc GR . . . .
H13B H 1.0396 0.3531 0.5677 0.056 Uiso 1 1 calc GR . . . .
H13C H 0.9397 0.4077 0.5314 0.056 Uiso 1 1 calc GR . . . .


_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
I1 Cu 2.4152(16) . ?
I2 I3 2.9467(12) . ?
I2 I4 2.9103(13) . ?
Cu N1 1.943(6) 8_565 ?
Cu N1 1.943(6) . ?
N1 C1 1.341(9) . ?
N1 C8 1.384(9) . ?
N2 C8 1.330(9) . ?
N2 C9 1.460(10) . ?
N2 C10 1.475(10) . ?
N3 C8 1.338(9) . ?
N3 C11 1.465(10) . ?
N3 C12 1.471(9) . ?
N4 C7 1.384(15) . ?
N4 C13 1.452(9) 8_565 ?
N4 C13 1.452(9) . ?
N7 C4 1.347(10) . ?
N7 C7 1.348(8) . ?
C1 C2 1.448(10) . ?
C1 C6 1.427(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.341(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.430(10) . ?
C4 C5 1.401(9) . ?
C5 C4 1.401(9) 8_565 ?
C5 C6 1.472(15) . ?
C6 C1 1.427(8) 8_565 ?
C7 N7 1.348(8) 8_565 ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I4 I2 I3 178.54(4) . . ?
N1 Cu I1 133.48(18) 8_565 . ?
N1 Cu I1 133.48(18) . . ?
N1 Cu N1 92.7(4) . 8_565 ?
C1 N1 Cu 128.1(5) . . ?
C1 N1 C8 121.9(6) . . ?
C8 N1 Cu 109.7(4) . . ?
C8 N2 C9 119.8(6) . . ?
C8 N2 C10 123.5(7) . . ?
C9 N2 C10 114.6(6) . . ?
C8 N3 C11 120.9(6) . . ?
C8 N3 C12 122.6(6) . . ?
C11 N3 C12 115.4(6) . . ?
C7 N4 C13 120.6(5) . 8_565 ?
C7 N4 C13 120.6(5) . . ?
C13 N4 C13 116.4(9) . 8_565 ?
C4 N7 C7 115.3(7) . . ?
N1 C1 C2 118.6(6) . . ?
N1 C1 C6 122.2(7) . . ?
C6 C1 C2 119.1(7) . . ?
C1 C2 H2 118.5 . . ?
C3 C2 C1 123.0(7) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.3(7) . . ?
C4 C3 H3 119.8 . . ?
N7 C4 C3 118.2(7) . . ?
N7 C4 C5 122.7(7) . . ?
C5 C4 C3 119.1(7) . . ?
C4 C5 C4 116.2(10) 8_565 . ?
C4 C5 C6 121.9(5) . . ?
C4 C5 C6 121.9(5) 8_565 . ?
C1 C6 C1 126.7(9) 8_565 . ?
C1 C6 C5 116.6(5) . . ?
C1 C6 C5 116.6(5) 8_565 . ?
N7 C7 N4 116.2(5) . . ?
N7 C7 N4 116.2(5) 8_565 . ?
N7 C7 N7 127.5(10) . 8_565 ?
N2 C8 N1 118.4(6) . . ?
N2 C8 N3 122.9(6) . . ?
N3 C8 N1 118.6(6) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
N4 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

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
Cu N1 C1 C2 -174.3(5) . . . . ?
Cu N1 C1 C6 2.2(10) . . . . ?
Cu N1 C8 N2 72.6(7) . . . . ?
Cu N1 C8 N3 -103.3(6) . . . . ?
N1 C1 C2 C3 176.7(7) . . . . ?
N1 C1 C6 C1 -0.7(15) . . . 8_565 ?
N1 C1 C6 C5 -176.4(8) . . . . ?
N7 C4 C5 C4 3.6(14) . . . 8_565 ?
N7 C4 C5 C6 -178.8(8) . . . . ?
C1 N1 C8 N2 -113.3(8) . . . . ?
C1 N1 C8 N3 70.7(9) . . . . ?
C1 C2 C3 C4 0.3(11) . . . . ?
C2 C1 C6 C1 175.8(7) . . . 8_565 ?
C2 C1 C6 C5 0.1(12) . . . . ?
C2 C3 C4 N7 179.0(7) . . . . ?
C2 C3 C4 C5 -0.9(11) . . . . ?
C3 C4 C5 C4 -176.6(5) . . . 8_565 ?
C3 C4 C5 C6 1.1(13) . . . . ?
C4 N7 C7 N4 173.7(8) . . . . ?
C4 N7 C7 N7 -5.3(15) . . . 8_565 ?
C4 C5 C6 C1 -0.7(14) . . . . ?
C4 C5 C6 C1 176.9(8) 8_565 . . . ?
C4 C5 C6 C1 0.7(14) 8_565 . . 8_565 ?
C4 C5 C6 C1 -176.9(8) . . . 8_565 ?
C6 C1 C2 C3 0.1(11) . . . . ?
C7 N7 C4 C3 -179.4(7) . . . . ?
C7 N7 C4 C5 0.4(11) . . . . ?
C8 N1 C1 C2 12.8(10) . . . . ?
C8 N1 C1 C6 -170.7(7) . . . . ?
C9 N2 C8 N1 17.8(10) . . . . ?
C9 N2 C8 N3 -166.4(7) . . . . ?
C10 N2 C8 N1 -144.4(7) . . . . ?
C10 N2 C8 N3 31.3(11) . . . . ?
C11 N3 C8 N1 7.9(10) . . . . ?
C11 N3 C8 N2 -167.8(7) . . . . ?
C12 N3 C8 N1 -159.2(7) . . . . ?
C12 N3 C8 N2 25.1(11) . . . . ?
C13 N4 C7 N7 171.1(8) 8_565 . . . ?
C13 N4 C7 N7 9.8(14) . . . . ?
C13 N4 C7 N7 -171.1(8) . . . 8_565 ?
C13 N4 C7 N7 -9.8(14) 8_565 . . 8_565 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-8 -2 3 0.0538 -8.0000 -2.0000 3.0000 0.5947 0.0153 0.8728
-7 4 1 0.0721 -7.0000 4.0000 0.9999 0.0415 -0.4988 0.8735
7 4 0 0.0655 7.0000 4.0000 -0.0000 -0.8089 -0.0365 -0.5945
-2 6 9 0.0786 -2.0000 6.0000 8.9999 -0.7056 -0.0267 0.7329
-2 -1 13 0.0863 -2.0000 -1.0000 13.0000 -0.1854 0.7068 0.6775
7 -4 -1 0.0630 7.0000 -4.0000 -0.9999 -0.0415 0.4988 -0.8735
1 -4 -11 0.0706 1.0000 -4.0000 -10.9999 0.6466 -0.2664 -0.6481
8 2 -3 0.0538 8.0000 2.0000 -3.0000 -0.5947 -0.0153 -0.8728
-1 3 -13 0.1133 -1.0000 3.0000 -13.0000 0.1902 -0.9649 -0.3111
-1 -6 8 0.0769 -1.0000 -6.0000 8.0001 0.3670 0.8404 0.2316
-2 8 -2 0.1000 -2.0000 8.0000 -2.0001 -0.5484 -0.7723 0.3670
-6 -5 4 0.0504 -6.0000 -5.0000 4.0000 0.7139 0.3646 0.6173
-7 2 -6 0.0841 -7.0000 2.0000 -6.0000 0.4428 -0.7320 0.5424
7 -1 -4 0.0447 7.0000 -1.0000 -4.0000 -0.2245 0.1145 -0.8996
3 -5 -9 0.0502 3.0000 -5.0000 -8.9999 0.5506 -0.0101 -0.8049
-3 -1 -13 0.0933 -3.0000 -1.0000 -13.0000 0.6843 -0.7439 -0.2271
0 8 1 0.0894 -0.0000 8.0000 0.9999 -0.7674 -0.5353 0.2790
-2 8 4 0.0805 -2.0000 8.0000 3.9999 -0.7346 -0.4460 0.5993
-2 6 8 0.0707 -2.0000 6.0000 7.9999 -0.6746 -0.0811 0.6941
-1 4 11 0.0706 -1.0000 4.0000 10.9999 -0.6466 0.2664 0.6481
_cell_oxdiff_length_a            12.2759(3)
_cell_oxdiff_length_b            12.6600(3)
_cell_oxdiff_length_c            20.9278(5)
_cell_oxdiff_angle_alpha         90.0703(19)
_cell_oxdiff_angle_beta          90.046(2)
_cell_oxdiff_angle_gamma         90.031(2)
_cell_oxdiff_volume              3252.43(14)
_cell_oxdiff_measurement_reflns_used 21476
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -13.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 34

#__ type_ start__ end____ width___ exp.time_
  2 omega  -69.00  -19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 50

#__ type_ start__ end____ width___ exp.time_
  3 omega  -58.00  -33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
  4 omega  -25.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega  -12.00   17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 29

#__ type_ start__ end____ width___ exp.time_
  6 omega  -29.00   11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   79.0000    1.0000 40

#__ type_ start__ end____ width___ exp.time_
  7 omega   18.00   61.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 43

#__ type_ start__ end____ width___ exp.time_
  8 omega  -69.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
  9 omega   -3.00   34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   79.0000   80.6249 37

#__ type_ start__ end____ width___ exp.time_
 10 omega  -10.00   15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   80.0000  -57.8676 25

#__ type_ start__ end____ width___ exp.time_
 11 omega    6.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000 -162.9454 25

#__ type_ start__ end____ width___ exp.time_
 12 omega   11.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000   86.7515 25

#__ type_ start__ end____ width___ exp.time_
 13 omega   13.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000   36.9300 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   10.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -119.7007 25

#__ type_ start__ end____ width___ exp.time_
 15 omega   10.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -68.8246 26

#__ type_ start__ end____ width___ exp.time_
 16 omega   15.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -23.4109 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000 -173.4093 25

#__ type_ start__ end____ width___ exp.time_
 18 omega   15.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -86.3998 25

#__ type_ start__ end____ width___ exp.time_
 19 omega   15.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   99.8763 25

#__ type_ start__ end____ width___ exp.time_
 20 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -55.9195 25

#__ type_ start__ end____ width___ exp.time_
 21 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -89.9033 25

#__ type_ start__ end____ width___ exp.time_
 22 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  122.9424 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -156.7237 25

#__ type_ start__ end____ width___ exp.time_
 24 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  112.3714 25

#__ type_ start__ end____ width___ exp.time_
 25 omega   34.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 26 omega   -6.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -180.0000 52

#__ type_ start__ end____ width___ exp.time_
 27 omega   69.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000   78.6628 27

#__ type_ start__ end____ width___ exp.time_
 28 omega   27.00   53.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 29 omega   24.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 28

#__ type_ start__ end____ width___ exp.time_
 30 omega   24.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -67.8439 31

#__ type_ start__ end____ width___ exp.time_
 31 omega   24.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 32 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  140.2373 25

#__ type_ start__ end____ width___ exp.time_
 33 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   29.8151 25

#__ type_ start__ end____ width___ exp.time_
 34 omega   24.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -19.6440 31

#__ type_ start__ end____ width___ exp.time_
 35 omega   34.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 36 omega   25.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000   78.6628 26

#__ type_ start__ end____ width___ exp.time_
 37 omega   27.00   53.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   30.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 39 omega   28.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -109.5457 26

#__ type_ start__ end____ width___ exp.time_
 40 omega  -13.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000  -63.7532 86

#__ type_ start__ end____ width___ exp.time_
 41 omega   34.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000   99.6399 26

#__ type_ start__ end____ width___ exp.time_
 42 omega   49.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   64.0000  130.9714 34

#__ type_ start__ end____ width___ exp.time_
 43 omega   31.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -77.4238 26

#__ type_ start__ end____ width___ exp.time_
 44 omega   31.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -179.4980 26

#__ type_ start__ end____ width___ exp.time_
 45 omega   35.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -152.0344 26

#__ type_ start__ end____ width___ exp.time_
 46 omega   34.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000   17.2126 26

#__ type_ start__ end____ width___ exp.time_
 47 omega   -8.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000 -162.4377 101

#__ type_ start__ end____ width___ exp.time_
 48 omega   83.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -152.0344 26

#__ type_ start__ end____ width___ exp.time_
 49 omega   33.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000 -111.0061 39

#__ type_ start__ end____ width___ exp.time_
 50 omega   35.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000  102.7951 26

#__ type_ start__ end____ width___ exp.time_
 51 omega   52.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000  175.7256 27

#__ type_ start__ end____ width___ exp.time_
 52 omega   39.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000   72.3957 26

#__ type_ start__ end____ width___ exp.time_
 53 omega   38.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000  -17.3604 31

#__ type_ start__ end____ width___ exp.time_
 54 omega   52.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000 -153.1087 27

#__ type_ start__ end____ width___ exp.time_
 55 omega   47.00   78.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   69.0000   93.5793 31

#__ type_ start__ end____ width___ exp.time_
 56 omega   -5.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   10.3730 103

#__ type_ start__ end____ width___ exp.time_
 57 omega   39.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   72.0000   70.4458 25

#__ type_ start__ end____ width___ exp.time_
 58 omega   90.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   64.0000  -59.1921 37

#__ type_ start__ end____ width___ exp.time_
 59 omega   44.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   64.0000  -59.1921 42

#__ type_ start__ end____ width___ exp.time_
 60 omega   44.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000   -0.1924 27

#__ type_ start__ end____ width___ exp.time_
 61 omega   41.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000 -174.2409 26

#__ type_ start__ end____ width___ exp.time_
 62 omega   25.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -78.0000  126.6710 55

#__ type_ start__ end____ width___ exp.time_
 63 omega   53.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000 -105.8589 27

#__ type_ start__ end____ width___ exp.time_
 64 omega   55.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   62.0000   57.4960 45

#__ type_ start__ end____ width___ exp.time_
 65 omega   89.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  -25.1615 25

#__ type_ start__ end____ width___ exp.time_
 66 omega   45.00   84.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  -25.1615 39

#__ type_ start__ end____ width___ exp.time_
 67 omega   77.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000  106.3776 26

#__ type_ start__ end____ width___ exp.time_
 68 omega   46.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000 -135.4169 25

#__ type_ start__ end____ width___ exp.time_
 69 omega   44.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000 -105.2724 50

#__ type_ start__ end____ width___ exp.time_
 70 omega   48.00   78.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   70.0000  143.1806 30

#__ type_ start__ end____ width___ exp.time_
 71 omega   45.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  -49.5511 37

#__ type_ start__ end____ width___ exp.time_
 72 omega   56.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000   94.3996 43

#__ type_ start__ end____ width___ exp.time_
 73 omega   55.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000    8.4906 44

#__ type_ start__ end____ width___ exp.time_
 74 omega   49.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  149.1831 25

#__ type_ start__ end____ width___ exp.time_
 75 omega   56.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   62.0000 -145.2785 88

#__ type_ start__ end____ width___ exp.time_
 76 omega   58.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   59.0000  126.4098 84

#__ type_ start__ end____ width___ exp.time_
 77 omega   48.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -64.2598 29

#__ type_ start__ end____ width___ exp.time_
 78 omega   49.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000   19.1058 27

#__ type_ start__ end____ width___ exp.time_
 79 omega   59.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -14.9632 50

#__ type_ start__ end____ width___ exp.time_
 80 omega   58.00   85.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000 -112.4939 27

#__ type_ start__ end____ width___ exp.time_
 81 omega   59.00   85.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   65.0000  120.5519 26

#__ type_ start__ end____ width___ exp.time_
 82 omega   57.00   92.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   69.0000   12.7188 35

#__ type_ start__ end____ width___ exp.time_
 83 omega   67.00  150.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   60.0000  -92.7238 83

#__ type_ start__ end____ width___ exp.time_
 84 omega   52.00   83.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   77.0000  -33.9608 31

#__ type_ start__ end____ width___ exp.time_
 85 omega   61.00  118.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   58.0000   57.2156 57

#__ type_ start__ end____ width___ exp.time_
 86 omega   60.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   62.0000  174.0146 47

#__ type_ start__ end____ width___ exp.time_
 87 omega   63.00   90.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   64.0000 -168.8069 27

#__ type_ start__ end____ width___ exp.time_
 88 omega   57.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000   58.3131 56

#__ type_ start__ end____ width___ exp.time_
 89 omega   67.00  129.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   64.0000   28.2884 62

#__ type_ start__ end____ width___ exp.time_
 90 omega   58.00   86.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000 -132.0726 28

#__ type_ start__ end____ width___ exp.time_
 91 omega   56.00   82.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000 -153.7099 26

#__ type_ start__ end____ width___ exp.time_
 92 omega   66.00  102.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000   48.0709 36

#__ type_ start__ end____ width___ exp.time_
 93 omega   67.00   98.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000 -141.1740 31

#__ type_ start__ end____ width___ exp.time_
 94 omega   75.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   68.0000   66.8296 28

#__ type_ start__ end____ width___ exp.time_
 95 omega   75.00  163.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   67.0000   65.7577 88

#__ type_ start__ end____ width___ exp.time_
 96 omega   74.00  167.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   74.0000  -46.8541 93

#__ type_ start__ end____ width___ exp.time_
 97 omega   68.00  125.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   77.0000  124.0280 57

#__ type_ start__ end____ width___ exp.time_
 98 omega  143.00  168.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   68.0000  -95.4358 25

#__ type_ start__ end____ width___ exp.time_
 99 omega   80.00  116.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   68.0000  -95.4358 36

#__ type_ start__ end____ width___ exp.time_
100 omega   71.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  123.5120 34

#__ type_ start__ end____ width___ exp.time_
101 omega   85.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 89

#__ type_ start__ end____ width___ exp.time_
102 omega   38.00  119.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   28.5121 81

#__ type_ start__ end____ width___ exp.time_
103 omega   79.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
104 omega   79.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
105 omega   86.00  134.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 48

#__ type_ start__ end____ width___ exp.time_
106 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
107 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
108 omega   38.00  139.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -122.0000 101

#__ type_ start__ end____ width___ exp.time_
109 omega  119.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
110 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
111 omega   78.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 98

#__ type_ start__ end____ width___ exp.time_
112 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
113 omega   78.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 99

#__ type_ start__ end____ width___ exp.time_
114 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
115 omega  115.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 62

#__ type_ start__ end____ width___ exp.time_
116 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
117 omega   78.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 100

#__ type_ start__ end____ width___ exp.time_
118 omega   78.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 98

#__ type_ start__ end____ width___ exp.time_
119 omega   85.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 89

#__ type_ start__ end____ width___ exp.time_
120 omega  127.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 51

#__ type_ start__ end____ width___ exp.time_
121 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
122 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
123 omega   78.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -31.5981 25

#__ type_ start__ end____ width___ exp.time_
124 omega   85.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
125 omega   94.00  153.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   69.0000 -166.8411 59

#__ type_ start__ end____ width___ exp.time_
126 omega   86.00  171.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 85

#__ type_ start__ end____ width___ exp.time_
127 omega   75.00  102.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -15.5020 27

#__ type_ start__ end____ width___ exp.time_
128 omega   74.00  117.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -74.9177 43

#__ type_ start__ end____ width___ exp.time_
129 omega   37.00   69.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -74.9177 32

#__ type_ start__ end____ width___ exp.time_
130 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -127.1676 26

#__ type_ start__ end____ width___ exp.time_
131 omega   87.00  166.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   60.0000  116.6129 79

#__ type_ start__ end____ width___ exp.time_
132 omega   83.00  110.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   70.0000  146.4754 27

#__ type_ start__ end____ width___ exp.time_
133 omega   72.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  106.0079 68

#__ type_ start__ end____ width___ exp.time_
134 omega   49.00  127.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  178.5600 78

#__ type_ start__ end____ width___ exp.time_
135 omega  113.00  139.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -56.3966 26

#__ type_ start__ end____ width___ exp.time_
136 omega   82.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -56.3966 25

#__ type_ start__ end____ width___ exp.time_
137 omega   43.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   69.7155 68

#__ type_ start__ end____ width___ exp.time_
138 omega   83.00  117.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 34

#__ type_ start__ end____ width___ exp.time_
139 omega   85.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 89

#__ type_ start__ end____ width___ exp.time_
140 omega   90.00  141.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 51

;
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_h-m   'P n m a'
_symmetry_int_tables_number      62
_chemical_absolute_configuration .
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent EOS'
_diffrn_measurement_specimen_support 'polyimid foil'


####################################################################### 
# 
# 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_hi_az12_5
_database_code_depnum_ccdc_archive 'CCDC 1413943'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Apr 15 11:39:03 2015'
;

_audit_block_code                hi_az12
_audit_block_refno               2403
_audit_block_usercomment         'hi_az240, needle light blue'


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C38 H64 Cu2 N12 O8, 4(C2 H3 N)'
_chemical_formula_sum            'C46 H76 Cu2 N16 O8'
_chemical_formula_weight         1108.30
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            'light blue'
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C46 H76 Cu2 N16 O8'
_chemical_oxdiff_usercomment     'hi_az240, needle light blue'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.3650(4)
_cell_length_b                   12.5243(5)
_cell_length_c                   20.2731(6)
_cell_angle_alpha                85.405(3)
_cell_angle_beta                 78.567(3)
_cell_angle_gamma                63.473(3)
_cell_volume                     2753.18(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26388
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6050
_cell_measurement_theta_min      4.0140
_shelx_estimated_absorpt_T_max   0.866
_shelx_estimated_absorpt_T_min   0.866
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            156958
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.920
_diffrn_reflns_theta_min         3.945
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -8.00   19.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -37.00   73.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000  -60.0000 110

#__ type_ start__ end____ width___ exp.time_
  3 omega  -65.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 48

#__ type_ start__ end____ width___ exp.time_
  4 omega  -13.00   68.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   71.0000   90.4468 81

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   42.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000  -75.0000  -56.3832 92

#__ type_ start__ end____ width___ exp.time_
  6 omega   -6.00   42.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   79.0000 -106.7781 48

#__ type_ start__ end____ width___ exp.time_
  7 omega    3.00   28.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   79.0000 -110.1131 25

#__ type_ start__ end____ width___ exp.time_
  8 omega    6.00   31.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -87.3739 25

#__ type_ start__ end____ width___ exp.time_
  9 omega   10.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -13.4418 30

#__ type_ start__ end____ width___ exp.time_
 10 omega   11.00   36.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000   57.3528 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   10.00   35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  153.2762 25

#__ type_ start__ end____ width___ exp.time_
 12 omega   10.00   35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  116.4630 25

#__ type_ start__ end____ width___ exp.time_
 13 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  168.6758 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   29.8311 25

#__ type_ start__ end____ width___ exp.time_
 15 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   69.2885 25

#__ type_ start__ end____ width___ exp.time_
 16 omega   14.00   39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -74.2967 25

#__ type_ start__ end____ width___ exp.time_
 17 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -163.8144 25

#__ type_ start__ end____ width___ exp.time_
 18 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -138.1272 25

#__ type_ start__ end____ width___ exp.time_
 19 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   -7.4846 25

#__ type_ start__ end____ width___ exp.time_
 20 omega   24.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 21 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 22 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000  142.8992 27

#__ type_ start__ end____ width___ exp.time_
 23 omega   27.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
 24 omega  -17.00   85.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -80.0000   68.6488 102

#__ type_ start__ end____ width___ exp.time_
 25 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 26 omega   23.00   48.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -102.5566 25

#__ type_ start__ end____ width___ exp.time_
 27 omega   26.00   53.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 28 omega   26.00   53.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
 29 omega   26.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000  116.2096 25

#__ type_ start__ end____ width___ exp.time_
 30 omega   28.00   55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 31 omega  -16.00   84.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -150.0000 100

#__ type_ start__ end____ width___ exp.time_
 32 omega   32.00   59.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 33 omega   26.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   74.9624 25

#__ type_ start__ end____ width___ exp.time_
 34 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
 35 omega   31.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -16.8160 43

#__ type_ start__ end____ width___ exp.time_
 36 omega   31.00   56.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  157.5927 25

#__ type_ start__ end____ width___ exp.time_
 37 omega   29.00   55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   39.6624 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   32.00   59.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -175.4152 27

#__ type_ start__ end____ width___ exp.time_
 39 omega  -12.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000  147.0972 84

#__ type_ start__ end____ width___ exp.time_
 40 omega   35.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -52.9777 27

#__ type_ start__ end____ width___ exp.time_
 41 omega   35.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000   75.4356 27

#__ type_ start__ end____ width___ exp.time_
 42 omega   40.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -96.9302 27

#__ type_ start__ end____ width___ exp.time_
 43 omega   29.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -120.6436 25

#__ type_ start__ end____ width___ exp.time_
 44 omega   36.00   61.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -62.5651 25

#__ type_ start__ end____ width___ exp.time_
 45 omega    9.00   82.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000  -42.7898 73

#__ type_ start__ end____ width___ exp.time_
 46 omega   36.00   63.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  169.4725 27

#__ type_ start__ end____ width___ exp.time_
 47 omega   35.00   61.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000 -145.4414 26

#__ type_ start__ end____ width___ exp.time_
 48 omega   34.00   59.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -24.1646 25

#__ type_ start__ end____ width___ exp.time_
 49 omega   41.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000  -86.0367 27

#__ type_ start__ end____ width___ exp.time_
 50 omega   43.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000   61.8586 25

#__ type_ start__ end____ width___ exp.time_
 51 omega   46.00   73.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   65.0000  104.6077 27

#__ type_ start__ end____ width___ exp.time_
 52 omega   43.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000  -63.2980 25

#__ type_ start__ end____ width___ exp.time_
 53 omega   38.00   65.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000   74.8605 27

#__ type_ start__ end____ width___ exp.time_
 54 omega   59.00   86.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   49.0000  -80.5202 27

#__ type_ start__ end____ width___ exp.time_
 55 omega   58.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -102.5694 25

#__ type_ start__ end____ width___ exp.time_
 56 omega  103.00  133.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000 -121.1015 30

#__ type_ start__ end____ width___ exp.time_
 57 omega   46.00   73.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000 -121.1015 27

#__ type_ start__ end____ width___ exp.time_
 58 omega   37.00   64.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  118.9133 27

#__ type_ start__ end____ width___ exp.time_
 59 omega   36.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   10.3735 26

#__ type_ start__ end____ width___ exp.time_
 60 omega   37.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  145.2330 25

#__ type_ start__ end____ width___ exp.time_
 61 omega   48.00   97.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000 -127.5289 49

#__ type_ start__ end____ width___ exp.time_
 62 omega   45.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000   31.9328 26

#__ type_ start__ end____ width___ exp.time_
 63 omega   49.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   61.0000   80.3515 30

#__ type_ start__ end____ width___ exp.time_
 64 omega   45.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   71.0000  -70.9242 26

#__ type_ start__ end____ width___ exp.time_
 65 omega   48.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000  151.8414 27

#__ type_ start__ end____ width___ exp.time_
 66 omega   43.00   89.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -57.2078 46

#__ type_ start__ end____ width___ exp.time_
 67 omega   53.00   78.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000   95.2710 25

#__ type_ start__ end____ width___ exp.time_
 68 omega   48.00  108.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  163.6336 60

#__ type_ start__ end____ width___ exp.time_
 69 omega   53.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   51.0000   -1.4443 59

#__ type_ start__ end____ width___ exp.time_
 70 omega   51.00  100.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000  130.5663 49

#__ type_ start__ end____ width___ exp.time_
 71 omega   53.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   62.0000   38.1969 26

#__ type_ start__ end____ width___ exp.time_
 72 omega   52.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000   67.0622 27

#__ type_ start__ end____ width___ exp.time_
 73 omega   48.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -10.2780 26

#__ type_ start__ end____ width___ exp.time_
 74 omega   55.00  149.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   42.0000  -57.2975 94

#__ type_ start__ end____ width___ exp.time_
 75 omega   60.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   61.0000  153.2456 28

#__ type_ start__ end____ width___ exp.time_
 76 omega   55.00  117.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   72.0000 -176.7349 62

#__ type_ start__ end____ width___ exp.time_
 77 omega   95.00  126.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   74.3815 31

#__ type_ start__ end____ width___ exp.time_
 78 omega   55.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   74.3815 35

#__ type_ start__ end____ width___ exp.time_
 79 omega   63.00   88.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000 -140.0754 25

#__ type_ start__ end____ width___ exp.time_
 80 omega   57.00   87.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000  -75.7343 30

#__ type_ start__ end____ width___ exp.time_
 81 omega   55.00   82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000  146.3827 27

#__ type_ start__ end____ width___ exp.time_
 82 omega   65.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   55.0000   23.9426 28

#__ type_ start__ end____ width___ exp.time_
 83 omega   62.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   68.0000  106.1133 30

#__ type_ start__ end____ width___ exp.time_
 84 omega   60.00  155.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   71.0000   81.5281 95

#__ type_ start__ end____ width___ exp.time_
 85 omega   63.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   77.0000 -138.4419 27

#__ type_ start__ end____ width___ exp.time_
 86 omega   68.00  111.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   64.0000  142.8403 43

#__ type_ start__ end____ width___ exp.time_
 87 omega   62.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.0000   73.1092 30

#__ type_ start__ end____ width___ exp.time_
 88 omega   67.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   66.0000  -12.6719 45

#__ type_ start__ end____ width___ exp.time_
 89 omega   62.00   99.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   74.0000  117.7472 37

#__ type_ start__ end____ width___ exp.time_
 90 omega   78.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   51.0000  -38.3688 25

#__ type_ start__ end____ width___ exp.time_
 91 omega   64.00   97.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   70.0000   21.5637 33

#__ type_ start__ end____ width___ exp.time_
 92 omega   62.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.0000 -149.3997 31

#__ type_ start__ end____ width___ exp.time_
 93 omega   63.00  147.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   71.0000   38.9755 84

#__ type_ start__ end____ width___ exp.time_
 94 omega   73.00  100.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   49.0000  -52.1947 27

#__ type_ start__ end____ width___ exp.time_
 95 omega   74.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   55.0000 -162.5347 33

#__ type_ start__ end____ width___ exp.time_
 96 omega   68.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   72.0000  148.6443 83

#__ type_ start__ end____ width___ exp.time_
 97 omega   69.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   75.0000 -153.1977 41

#__ type_ start__ end____ width___ exp.time_
 98 omega   69.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   77.0000   96.4146 29

#__ type_ start__ end____ width___ exp.time_
 99 omega   86.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
100 omega   86.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
101 omega  121.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -60.0000 54

#__ type_ start__ end____ width___ exp.time_
102 omega   86.00  118.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -60.0000 32

#__ type_ start__ end____ width___ exp.time_
103 omega   81.00  129.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 48

#__ type_ start__ end____ width___ exp.time_
104 omega   80.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
105 omega   78.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
106 omega   79.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 98

#__ type_ start__ end____ width___ exp.time_
107 omega  112.00  166.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 54

#__ type_ start__ end____ width___ exp.time_
108 omega   79.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 28

#__ type_ start__ end____ width___ exp.time_
109 omega   81.00  137.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   89.6706 56

#__ type_ start__ end____ width___ exp.time_
110 omega   79.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 25

#__ type_ start__ end____ width___ exp.time_
111 omega  143.00  170.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
112 omega   79.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
113 omega   79.00  167.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 88

#__ type_ start__ end____ width___ exp.time_
114 omega  108.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 69

#__ type_ start__ end____ width___ exp.time_
115 omega   79.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
116 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 100

#__ type_ start__ end____ width___ exp.time_
117 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
118 omega  142.00  169.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
119 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
120 omega   87.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -180.0000 89

#__ type_ start__ end____ width___ exp.time_
121 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   60.0000 90

#__ type_ start__ end____ width___ exp.time_
122 omega   69.00  123.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -122.2753 54

#__ type_ start__ end____ width___ exp.time_
123 omega  125.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   70.0000  103.2333 51

#__ type_ start__ end____ width___ exp.time_
124 omega   84.00  122.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   70.0000  103.2333 38

#__ type_ start__ end____ width___ exp.time_
125 omega   42.00  123.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -40.5377 81

#__ type_ start__ end____ width___ exp.time_
126 omega   85.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   71.0000  133.3029 27

#__ type_ start__ end____ width___ exp.time_
127 omega   88.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000  -24.0144 89

#__ type_ start__ end____ width___ exp.time_
128 omega   76.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  105.1003 28

#__ type_ start__ end____ width___ exp.time_
129 omega   71.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   69.6561 68

#__ type_ start__ end____ width___ exp.time_
130 omega   80.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -127.6946 26

#__ type_ start__ end____ width___ exp.time_
131 omega   37.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000    1.5913 103

#__ type_ start__ end____ width___ exp.time_
132 omega   37.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   69.6561 26

#__ type_ start__ end____ width___ exp.time_
133 omega   37.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -143.9925 53

#__ type_ start__ end____ width___ exp.time_
134 omega   64.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -57.9241 27

#__ type_ start__ end____ width___ exp.time_
135 omega   37.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -57.9241 26

#__ type_ start__ end____ width___ exp.time_
136 omega   48.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  150.3644 91

#__ type_ start__ end____ width___ exp.time_
137 omega   83.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
138 omega   87.00  117.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  150.0000 30

#__ type_ start__ end____ width___ exp.time_
139 omega   89.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  120.0000 86

#__ type_ start__ end____ width___ exp.time_
140 omega   48.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -78.2762 57

#__ type_ start__ end____ width___ exp.time_
141 omega  -72.00   26.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  -30.0000 98

#__ type_ start__ end____ width___ exp.time_
142 omega  -44.00   73.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000   30.0000 117

#__ type_ start__ end____ width___ exp.time_
143 omega  -26.00   72.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -180.0000 98

#__ type_ start__ end____ width___ exp.time_
144 omega  -15.00   84.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   76.0000 -162.9406 99

#__ type_ start__ end____ width___ exp.time_
145 omega   -7.00   92.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   76.0000  -40.2728 99

#__ type_ start__ end____ width___ exp.time_
146 omega   -6.00   46.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000   97.5411 52

#__ type_ start__ end____ width___ exp.time_
147 omega   -4.00   96.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000  -89.7379 100

#__ type_ start__ end____ width___ exp.time_
148 omega   10.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  116.4630 36

#__ type_ start__ end____ width___ exp.time_
149 omega   15.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   29.8311 32

#__ type_ start__ end____ width___ exp.time_
150 omega   14.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -74.2967 32

#__ type_ start__ end____ width___ exp.time_
151 omega   19.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   -7.4846 28

#__ type_ start__ end____ width___ exp.time_
152 omega   19.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -163.8144 30

#__ type_ start__ end____ width___ exp.time_
153 omega   19.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -138.1272 28

#__ type_ start__ end____ width___ exp.time_
154 omega   24.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
155 omega  -15.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 90

#__ type_ start__ end____ width___ exp.time_
156 omega  -18.00   80.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
157 omega   30.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -16.8160 98

#__ type_ start__ end____ width___ exp.time_
158 omega   28.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -120.6436 100

#__ type_ start__ end____ width___ exp.time_
159 omega   30.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  157.5927 98

#__ type_ start__ end____ width___ exp.time_
160 omega   33.00  132.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -24.1646 99

#__ type_ start__ end____ width___ exp.time_
161 omega   39.00  129.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000  -86.0367 90

#__ type_ start__ end____ width___ exp.time_
162 omega   34.00  131.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000 -145.4414 97

#__ type_ start__ end____ width___ exp.time_
163 omega   -9.00   93.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000  -42.7898 102

#__ type_ start__ end____ width___ exp.time_
164 omega   39.00  129.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000   61.8586 90

#__ type_ start__ end____ width___ exp.time_
165 omega   35.00  131.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -62.5651 96

#__ type_ start__ end____ width___ exp.time_
166 omega   43.00  134.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   65.0000  104.6077 91

#__ type_ start__ end____ width___ exp.time_
167 omega   36.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  145.2330 100

#__ type_ start__ end____ width___ exp.time_
168 omega   42.00  134.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000  -63.2980 92

#__ type_ start__ end____ width___ exp.time_
169 omega   -5.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -102.5694 103

#__ type_ start__ end____ width___ exp.time_
170 omega   37.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  118.9133 99

#__ type_ start__ end____ width___ exp.time_
171 omega   47.00  137.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000 -127.5289 90

#__ type_ start__ end____ width___ exp.time_
172 omega   41.00  140.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -57.2078 99

#__ type_ start__ end____ width___ exp.time_
173 omega   48.00  138.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   61.0000   80.3515 90

#__ type_ start__ end____ width___ exp.time_
174 omega   43.00  139.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   71.0000  -70.9242 96

#__ type_ start__ end____ width___ exp.time_
175 omega   52.00  144.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   51.0000   -1.4443 92

#__ type_ start__ end____ width___ exp.time_
176 omega   52.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   62.0000   38.1969 90

#__ type_ start__ end____ width___ exp.time_
177 omega   46.00  143.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  163.6336 97

#__ type_ start__ end____ width___ exp.time_
178 omega   50.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000   95.2710 92

#__ type_ start__ end____ width___ exp.time_
179 omega   51.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000  130.5663 90

#__ type_ start__ end____ width___ exp.time_
180 omega   52.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   63.0000   50.1555 90

#__ type_ start__ end____ width___ exp.time_
181 omega   48.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -10.2780 100

#__ type_ start__ end____ width___ exp.time_
182 omega   56.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   61.0000  153.2456 90

#__ type_ start__ end____ width___ exp.time_
183 omega   51.00  147.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000   67.0622 96

#__ type_ start__ end____ width___ exp.time_
184 omega    7.00  109.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000  160.5231 102

#__ type_ start__ end____ width___ exp.time_
185 omega   54.00  150.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   42.0000  -57.2975 96

#__ type_ start__ end____ width___ exp.time_
186 omega   57.00  147.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   56.0000 -157.1409 90

#__ type_ start__ end____ width___ exp.time_
187 omega   56.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   62.0000   13.8303 90

#__ type_ start__ end____ width___ exp.time_
188 omega   45.00  151.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   26.0000  -92.5536 106

#__ type_ start__ end____ width___ exp.time_
189 omega   55.00  149.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   48.0000  -50.2314 94

#__ type_ start__ end____ width___ exp.time_
190 omega   55.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   72.0000 -176.7349 96

#__ type_ start__ end____ width___ exp.time_
191 omega   57.00  156.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000  -75.7343 99

#__ type_ start__ end____ width___ exp.time_
192 omega   67.00  157.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   64.0000  142.8403 90

#__ type_ start__ end____ width___ exp.time_
193 omega   64.00  159.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   70.0000   21.5637 95

#__ type_ start__ end____ width___ exp.time_
194 omega   67.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   66.0000  -12.6719 91

#__ type_ start__ end____ width___ exp.time_
195 omega   60.00  160.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   77.0000 -138.4419 100

#__ type_ start__ end____ width___ exp.time_
196 omega   67.00  163.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   72.0000  148.6443 96

#__ type_ start__ end____ width___ exp.time_
197 omega   73.00  163.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   55.0000 -162.5347 90

#__ type_ start__ end____ width___ exp.time_
198 omega   68.00  168.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   77.0000   96.4146 100

#__ type_ start__ end____ width___ exp.time_
199 omega   37.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   69.6561 103

#__ type_ start__ end____ width___ exp.time_
200 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  120.0000 90

#__ type_ start__ end____ width___ exp.time_
201 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
202 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   90.0000 90

#__ type_ start__ end____ width___ exp.time_
203 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
204 omega   35.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000 -120.0000 143

#__ type_ start__ end____ width___ exp.time_
205 omega   37.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  150.3644 102

#__ type_ start__ end____ width___ exp.time_
206 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
207 phi      0.00  120.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
 108.0000  108.0000   20.0000     -     120

#__ type_ start__ end____ width___ exp.time_
208 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 58

#__ type_ start__ end____ width___ exp.time_
209 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 58

#__ type_ start__ end____ width___ exp.time_
210 omega   37.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000    1.5913 103

#__ type_ start__ end____ width___ exp.time_
211 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 58

#__ type_ start__ end____ width___ exp.time_
212 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 58

#__ type_ start__ end____ width___ exp.time_
213 omega   80.00  118.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -127.6946 38

#__ type_ start__ end____ width___ exp.time_
214 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   60.0000 90

#__ type_ start__ end____ width___ exp.time_
215 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 100

#__ type_ start__ end____ width___ exp.time_
216 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 100

#__ type_ start__ end____ width___ exp.time_
217 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 100

#__ type_ start__ end____ width___ exp.time_
218 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
219 omega   37.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -98.6655 102

#__ type_ start__ end____ width___ exp.time_
220 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 100

#__ type_ start__ end____ width___ exp.time_
221 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 100

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      0.0198751000
_diffrn_orient_matrix_UB_12      -0.0094996000
_diffrn_orient_matrix_UB_13      -0.0771688000
_diffrn_orient_matrix_UB_21      0.1351797000
_diffrn_orient_matrix_UB_22      -0.0904992000
_diffrn_orient_matrix_UB_23      -0.0014196000
_diffrn_orient_matrix_UB_31      -0.0372449000
_diffrn_orient_matrix_UB_32      -0.1030618000
_diffrn_orient_matrix_UB_33      0.0073659000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.5869 51870 107765
2 0.4131 0 107765
_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10602
_reflns_number_total             12848
_reflns_special_details          
;
 _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.
 2-component twin. hkl data include singles and 
 composites from the first component (see *_oxdiff_twin_*).
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         12848
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      0.973
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0632P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0992
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5853(8) 0.4147(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C52(H52A,H52B,H52C), C62(H62A,H62B,H62C),
 C72(H72A,H72B,H72C), C42(H42A,H42B,H42C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
Cu1 Cu 0.25175(4) 0.74072(4) 1.04455(2) 0.01309(10) Uani 1 1 d . . . . .
Cu2 Cu 0.38336(4) 0.74400(4) 0.62472(2) 0.01503(10) Uani 1 1 d . . . . .
O1 O 0.15444(18) 0.68901(19) 1.11698(9) 0.0189(4) Uani 1 1 d . . . . .
O2 O -0.00406(19) 0.7682(2) 1.06250(11) 0.0279(5) Uani 1 1 d . . . . .
O3 O 0.29736(18) 0.79639(19) 1.11731(9) 0.0187(4) Uani 1 1 d . . . . .
O4 O 0.48894(18) 0.7398(2) 1.06018(10) 0.0244(5) Uani 1 1 d . . . . .
O5 O 0.52438(18) 0.67862(19) 0.55117(10) 0.0217(5) Uani 1 1 d . . . . .
O6 O 0.6004(3) 0.7895(3) 0.58690(14) 0.0457(7) Uani 1 1 d . . . . .
O7 O 0.27184(18) 0.8146(2) 0.55952(10) 0.0212(5) Uani 1 1 d . . . . .
O8 O 0.1966(2) 0.6876(2) 0.60357(11) 0.0270(5) Uani 1 1 d . . . . .
N1 N 0.24942(19) 0.8623(2) 0.97684(10) 0.0115(5) Uani 1 1 d . . . . .
N2 N 0.2886(2) 0.6253(2) 0.97463(11) 0.0119(5) Uani 1 1 d . . . . .
N3 N 0.17636(19) 1.0196(2) 1.05250(11) 0.0135(5) Uani 1 1 d . . . . .
N4 N 0.34257(19) 0.9944(2) 0.96891(11) 0.0143(5) Uani 1 1 d . . . . .
N5 N 0.2806(2) 0.4685(2) 1.04122(11) 0.0142(5) Uani 1 1 d . . . . .
N6 N 0.1680(2) 0.5304(2) 0.95545(12) 0.0155(5) Uani 1 1 d . . . . .
N7 N 0.4500(2) 0.6237(2) 0.69228(11) 0.0135(5) Uani 1 1 d . . . . .
N8 N 0.2787(2) 0.8658(2) 0.69409(11) 0.0149(5) Uani 1 1 d . . . . .
N9 N 0.5766(2) 0.4572(2) 0.62319(12) 0.0181(5) Uani 1 1 d . . . . .
N10 N 0.6561(2) 0.5029(2) 0.70480(11) 0.0167(5) Uani 1 1 d . . . . .
N11 N 0.1925(2) 1.0347(2) 0.62977(13) 0.0236(6) Uani 1 1 d . . . . .
N12 N 0.0631(2) 0.9743(2) 0.70398(12) 0.0202(6) Uani 1 1 d . . . . .
C1 C 0.2569(2) 0.8557(2) 0.90658(13) 0.0111(5) Uani 1 1 d . . . . .
C2 C 0.3061(2) 0.7453(3) 0.87084(12) 0.0107(5) Uani 1 1 d . . . . .
C3 C 0.3298(2) 0.6339(2) 0.90471(13) 0.0110(5) Uani 1 1 d . . . . .
C4 C 0.3917(2) 0.5291(2) 0.86747(13) 0.0134(6) Uani 1 1 d . . . . .
H4 H 0.4099 0.4553 0.8900 0.016 Uiso 1 1 calc R . . . .
C5 C 0.4280(2) 0.5285(3) 0.79812(13) 0.0140(6) Uani 1 1 d . . . . .
H5 H 0.4721 0.4542 0.7748 0.017 Uiso 1 1 calc R . . . .
C6 C 0.4020(2) 0.6326(3) 0.76197(13) 0.0132(6) Uani 1 1 d . . . . .
C7 C 0.3301(2) 0.7449(3) 0.79804(12) 0.0118(5) Uani 1 1 d . . . . .
C8 C 0.2789(2) 0.8565(3) 0.76391(13) 0.0128(6) Uani 1 1 d . . . . .
C9 C 0.2243(2) 0.9607(3) 0.80168(13) 0.0142(6) Uani 1 1 d . . . . .
H9 H 0.1925 1.0350 0.7793 0.017 Uiso 1 1 calc R . . . .
C10 C 0.2143(2) 0.9605(3) 0.87107(13) 0.0130(6) Uani 1 1 d . . . . .
H10 H 0.1771 1.0344 0.8947 0.016 Uiso 1 1 calc R . . . .
C11 C 0.2471(2) 0.5421(2) 0.98969(13) 0.0128(6) Uani 1 1 d . . . . .
C12 C 0.3882(3) 0.4517(3) 1.06812(14) 0.0185(6) Uani 1 1 d . . . . .
H12A H 0.4476 0.4639 1.0323 0.028 Uiso 1 1 calc GR . . . .
H12B H 0.4263 0.3705 1.0855 0.028 Uiso 1 1 calc GR . . . .
H12C H 0.3630 0.5093 1.1047 0.028 Uiso 1 1 calc GR . . . .
C13 C 0.2038(3) 0.4183(3) 1.08109(15) 0.0237(7) Uani 1 1 d . . . . .
H13A H 0.1225 0.4551 1.0683 0.036 Uiso 1 1 calc GR . . . .
H13B H 0.1952 0.4339 1.1289 0.036 Uiso 1 1 calc GR . . . .
H13C H 0.2417 0.3320 1.0730 0.036 Uiso 1 1 calc GR . . . .
C14 C 0.0912(3) 0.6327(3) 0.91879(15) 0.0198(6) Uani 1 1 d . . . . .
H14A H 0.0658 0.7063 0.9439 0.030 Uiso 1 1 calc GR . . . .
H14B H 0.0183 0.6243 0.9136 0.030 Uiso 1 1 calc GR . . . .
H14C H 0.1381 0.6360 0.8743 0.030 Uiso 1 1 calc GR . . . .
C15 C 0.1900(3) 0.4133(3) 0.93359(16) 0.0241(7) Uani 1 1 d . . . . .
H15A H 0.2614 0.3517 0.9505 0.036 Uiso 1 1 calc GR . . . .
H15B H 0.2061 0.4097 0.8843 0.036 Uiso 1 1 calc GR . . . .
H15C H 0.1175 0.3997 0.9512 0.036 Uiso 1 1 calc GR . . . .
C16 C 0.2551(2) 0.9585(2) 0.99836(13) 0.0117(5) Uani 1 1 d . . . . .
C17 C 0.2065(3) 1.0813(3) 1.09890(15) 0.0214(7) Uani 1 1 d . . . . .
H17A H 0.1989 1.0479 1.1440 0.032 Uiso 1 1 calc GR . . . .
H17B H 0.1497 1.1665 1.1002 0.032 Uiso 1 1 calc GR . . . .
H17C H 0.2909 1.0708 1.0836 0.032 Uiso 1 1 calc GR . . . .
C18 C 0.0631(2) 1.0089(3) 1.07751(14) 0.0183(6) Uani 1 1 d . . . . .
H18A H 0.0481 0.9677 1.0438 0.027 Uiso 1 1 calc GR . . . .
H18B H -0.0055 1.0886 1.0863 0.027 Uiso 1 1 calc GR . . . .
H18C H 0.0704 0.9631 1.1193 0.027 Uiso 1 1 calc GR . . . .
C19 C 0.3096(3) 1.1201(3) 0.95447(16) 0.0217(6) Uani 1 1 d . . . . .
H19A H 0.3165 1.1325 0.9058 0.033 Uiso 1 1 calc GR . . . .
H19B H 0.3654 1.1432 0.9712 0.033 Uiso 1 1 calc GR . . . .
H19C H 0.2249 1.1690 0.9768 0.033 Uiso 1 1 calc GR . . . .
C20 C 0.4557(2) 0.9103(3) 0.92857(14) 0.0197(6) Uani 1 1 d . . . . .
H20A H 0.4796 0.8305 0.9479 0.029 Uiso 1 1 calc GR . . . .
H20B H 0.5209 0.9348 0.9281 0.029 Uiso 1 1 calc GR . . . .
H20C H 0.4432 0.9089 0.8825 0.029 Uiso 1 1 calc GR . . . .
C21 C 0.0427(3) 0.7195(3) 1.11183(14) 0.0181(6) Uani 1 1 d . . . . .
C22 C -0.0337(3) 0.6921(3) 1.17273(16) 0.0294(7) Uani 1 1 d . . . . .
H22A H -0.0132 0.6069 1.1728 0.044 Uiso 1 1 calc GR . . . .
H22B H -0.1212 0.7392 1.1710 0.044 Uiso 1 1 calc GR . . . .
H22C H -0.0161 0.7125 1.2138 0.044 Uiso 1 1 calc GR . . . .
C23 C 0.4088(3) 0.7815(3) 1.11046(14) 0.0176(6) Uani 1 1 d . . . . .
C24 C 0.4386(3) 0.8211(3) 1.17064(16) 0.0273(7) Uani 1 1 d . . . . .
H24A H 0.4366 0.9000 1.1620 0.041 Uiso 1 1 calc GR . . . .
H24B H 0.5206 0.7636 1.1780 0.041 Uiso 1 1 calc GR . . . .
H24C H 0.3776 0.8252 1.2107 0.041 Uiso 1 1 calc GR . . . .
C25 C 0.5592(2) 0.5286(3) 0.67394(13) 0.0150(6) Uani 1 1 d . . . . .
C26 C 0.6958(3) 0.3926(3) 0.58011(16) 0.0286(8) Uani 1 1 d . . . . .
H26A H 0.7560 0.4144 0.5925 0.043 Uiso 1 1 calc GR . . . .
H26B H 0.6886 0.4133 0.5330 0.043 Uiso 1 1 calc GR . . . .
H26C H 0.7228 0.3065 0.5859 0.043 Uiso 1 1 calc GR . . . .
C27 C 0.4725(3) 0.4589(3) 0.59852(16) 0.0260(7) Uani 1 1 d . . . . .
H27A H 0.3995 0.4886 0.6342 0.039 Uiso 1 1 calc GR . . . .
H27B H 0.4916 0.3778 0.5854 0.039 Uiso 1 1 calc GR . . . .
H27C H 0.4567 0.5113 0.5594 0.039 Uiso 1 1 calc GR . . . .
C28 C 0.6613(3) 0.5979(3) 0.73868(15) 0.0228(7) Uani 1 1 d . . . . .
H28A H 0.6191 0.6739 0.7166 0.034 Uiso 1 1 calc GR . . . .
H28B H 0.7473 0.5811 0.7364 0.034 Uiso 1 1 calc GR . . . .
H28C H 0.6210 0.6028 0.7859 0.034 Uiso 1 1 calc GR . . . .
C29 C 0.7366(3) 0.3812(3) 0.72202(16) 0.0270(7) Uani 1 1 d . . . . .
H29A H 0.7097 0.3257 0.7075 0.041 Uiso 1 1 calc GR . . . .
H29B H 0.7331 0.3756 0.7708 0.041 Uiso 1 1 calc GR . . . .
H29C H 0.8212 0.3607 0.6993 0.041 Uiso 1 1 calc GR . . . .
C30 C 0.1781(3) 0.9582(3) 0.67659(13) 0.0172(6) Uani 1 1 d . . . . .
C31 C 0.3098(3) 1.0408(3) 0.61208(18) 0.0343(8) Uani 1 1 d . . . . .
H31A H 0.3515 1.0177 0.6509 0.052 Uiso 1 1 calc GR . . . .
H31B H 0.2954 1.1225 0.5991 0.052 Uiso 1 1 calc GR . . . .
H31C H 0.3614 0.9863 0.5743 0.052 Uiso 1 1 calc GR . . . .
C32 C 0.1078(3) 1.0934(3) 0.58266(17) 0.0328(8) Uani 1 1 d . . . . .
H32A H 0.0419 1.0681 0.5917 0.049 Uiso 1 1 calc GR . . . .
H32B H 0.1525 1.0712 0.5364 0.049 Uiso 1 1 calc GR . . . .
H32C H 0.0722 1.1801 0.5884 0.049 Uiso 1 1 calc GR . . . .
C33 C 0.0418(3) 0.8767(3) 0.73657(16) 0.0261(7) Uani 1 1 d . . . . .
H33A H 0.1068 0.8009 0.7168 0.039 Uiso 1 1 calc GR . . . .
H33B H -0.0381 0.8849 0.7303 0.039 Uiso 1 1 calc GR . . . .
H33C H 0.0423 0.8781 0.7848 0.039 Uiso 1 1 calc GR . . . .
C34 C -0.0400(3) 1.0935(3) 0.71906(18) 0.0330(9) Uani 1 1 d . . . . .
H34A H -0.0727 1.1010 0.7675 0.050 Uiso 1 1 calc GR . . . .
H34B H -0.1049 1.1042 0.6945 0.050 Uiso 1 1 calc GR . . . .
H34C H -0.0112 1.1545 0.7052 0.050 Uiso 1 1 calc GR . . . .
C35 C 0.6052(3) 0.7165(3) 0.54796(15) 0.0261(7) Uani 1 1 d . . . . .
C36 C 0.7140(3) 0.6635(4) 0.49018(18) 0.0391(9) Uani 1 1 d . . . . .
H36A H 0.7616 0.5782 0.4979 0.059 Uiso 1 1 calc GR . . . .
H36B H 0.7665 0.7042 0.4877 0.059 Uiso 1 1 calc GR . . . .
H36C H 0.6839 0.6741 0.4478 0.059 Uiso 1 1 calc GR . . . .
C37 C 0.1938(3) 0.7717(3) 0.56664(14) 0.0208(7) Uani 1 1 d . . . . .
C38 C 0.0900(3) 0.8326(3) 0.52622(16) 0.0254(7) Uani 1 1 d . . . . .
H38A H 0.0148 0.8859 0.5559 0.038 Uiso 1 1 calc GR . . . .
H38B H 0.0753 0.7719 0.5070 0.038 Uiso 1 1 calc GR . . . .
H38C H 0.1133 0.8790 0.4899 0.038 Uiso 1 1 calc GR . . . .
N51 N 0.0282(5) 0.5645(5) 0.3889(3) 0.0968(19) Uani 1 1 d . . . . .
C51 C 0.0495(5) 0.4685(7) 0.3881(3) 0.0683(15) Uani 1 1 d . . . . .
C52 C 0.0781(7) 0.3417(6) 0.3862(4) 0.110(3) Uani 1 1 d . . . . .
H52A H 0.0947 0.3160 0.3394 0.165 Uiso 1 1 calc GR . . . .
H52B H 0.0080 0.3298 0.4113 0.165 Uiso 1 1 calc GR . . . .
H52C H 0.1507 0.2947 0.4066 0.165 Uiso 1 1 calc GR . . . .
N61 N 0.6630(4) 0.7312(4) 0.2913(2) 0.0652(11) Uani 1 1 d . . . . .
C61 C 0.7314(4) 0.6318(5) 0.28633(19) 0.0472(11) Uani 1 1 d . . . . .
C62 C 0.8187(4) 0.5044(4) 0.2789(2) 0.0520(11) Uani 1 1 d . . . . .
H62A H 0.7956 0.4664 0.2473 0.078 Uiso 1 1 calc GR . . . .
H62B H 0.8166 0.4656 0.3228 0.078 Uiso 1 1 calc GR . . . .
H62C H 0.9018 0.4964 0.2617 0.078 Uiso 1 1 calc GR . . . .
N71 N 0.2584(4) 0.1946(3) 0.21447(19) 0.0515(9) Uani 1 1 d . . . . .
C71 C 0.3431(4) 0.1390(4) 0.23925(18) 0.0383(9) Uani 1 1 d . . . . .
C72 C 0.4508(3) 0.0709(4) 0.27037(18) 0.0377(9) Uani 1 1 d . . . . .
H72A H 0.5204 0.0838 0.2456 0.057 Uiso 1 1 calc GR . . . .
H72B H 0.4714 -0.0142 0.2693 0.057 Uiso 1 1 calc GR . . . .
H72C H 0.4329 0.0973 0.3172 0.057 Uiso 1 1 calc GR . . . .
N41 N 0.2222(4) 0.9649(5) 0.3728(2) 0.0787(15) Uani 1 1 d . . . . .
C41 C 0.3071(4) 0.9396(4) 0.39566(19) 0.0440(10) Uani 1 1 d . . . . .
C42 C 0.4139(3) 0.9087(4) 0.42569(18) 0.0389(9) Uani 1 1 d . . . . .
H42A H 0.4880 0.8566 0.3948 0.058 Uiso 1 1 calc GR . . . .
H42B H 0.4064 0.8669 0.4681 0.058 Uiso 1 1 calc GR . . . .
H42C H 0.4198 0.9815 0.4346 0.058 Uiso 1 1 calc GR . . . .


_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
Cu1 O1 1.966(2) . ?
Cu1 O3 1.9559(19) . ?
Cu1 N1 1.961(2) . ?
Cu1 N2 1.947(2) . ?
Cu2 O5 1.956(2) . ?
Cu2 O7 1.9691(19) . ?
Cu2 N7 1.957(2) . ?
Cu2 N8 1.959(2) . ?
O1 C21 1.283(4) . ?
O2 C21 1.234(4) . ?
O3 C23 1.285(4) . ?
O4 C23 1.231(4) . ?
O5 C35 1.273(4) . ?
O6 C35 1.230(4) . ?
O7 C37 1.279(4) . ?
O8 C37 1.234(4) . ?
N1 C1 1.416(3) . ?
N1 C16 1.349(4) . ?
N2 C3 1.421(3) . ?
N2 C11 1.343(4) . ?
N3 C16 1.335(3) . ?
N3 C17 1.460(4) . ?
N3 C18 1.453(4) . ?
N4 C16 1.365(4) . ?
N4 C19 1.460(4) . ?
N4 C20 1.450(3) . ?
N5 C11 1.338(3) . ?
N5 C12 1.459(3) . ?
N5 C13 1.449(4) . ?
N6 C11 1.369(4) . ?
N6 C14 1.461(3) . ?
N6 C15 1.457(4) . ?
N7 C6 1.412(3) . ?
N7 C25 1.348(3) . ?
N8 C8 1.411(3) . ?
N8 C30 1.355(3) . ?
N9 C25 1.339(4) . ?
N9 C26 1.458(4) . ?
N9 C27 1.462(4) . ?
N10 C25 1.360(4) . ?
N10 C28 1.452(4) . ?
N10 C29 1.460(4) . ?
N11 C30 1.338(4) . ?
N11 C31 1.458(5) . ?
N11 C32 1.465(4) . ?
N12 C30 1.350(4) . ?
N12 C33 1.446(4) . ?
N12 C34 1.471(4) . ?
C1 C2 1.428(4) . ?
C1 C10 1.378(4) . ?
C2 C3 1.438(4) . ?
C2 C7 1.447(3) . ?
C3 C4 1.382(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.381(4) . ?
C6 C7 1.446(4) . ?
C7 C8 1.436(4) . ?
C8 C9 1.384(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.387(4) . ?
C10 H10 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.514(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.519(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.525(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.531(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N51 C51 1.112(7) . ?
C51 C52 1.466(9) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
N61 C61 1.149(6) . ?
C61 C62 1.473(7) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
N71 C71 1.155(5) . ?
C71 C72 1.460(5) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
N41 C41 1.135(5) . ?
C41 C42 1.446(5) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cu1 O1 85.29(8) . . ?
O3 Cu1 N1 99.96(9) . . ?
N1 Cu1 O1 146.29(9) . . ?
N2 Cu1 O1 100.13(9) . . ?
N2 Cu1 O3 151.28(9) . . ?
N2 Cu1 N1 91.06(9) . . ?
O5 Cu2 O7 90.48(8) . . ?
O5 Cu2 N7 97.91(9) . . ?
O5 Cu2 N8 150.88(10) . . ?
N7 Cu2 O7 150.64(10) . . ?
N7 Cu2 N8 91.95(8) . . ?
N8 Cu2 O7 94.21(9) . . ?
C21 O1 Cu1 116.61(18) . . ?
C23 O3 Cu1 118.05(18) . . ?
C35 O5 Cu2 115.8(2) . . ?
C37 O7 Cu2 110.80(18) . . ?
C1 N1 Cu1 127.99(19) . . ?
C16 N1 Cu1 116.15(16) . . ?
C16 N1 C1 115.4(2) . . ?
C3 N2 Cu1 126.83(19) . . ?
C11 N2 Cu1 117.63(17) . . ?
C11 N2 C3 113.9(2) . . ?
C16 N3 C17 123.6(2) . . ?
C16 N3 C18 121.5(2) . . ?
C18 N3 C17 113.8(2) . . ?
C16 N4 C19 120.8(2) . . ?
C16 N4 C20 119.8(2) . . ?
C20 N4 C19 115.3(2) . . ?
C11 N5 C12 120.5(2) . . ?
C11 N5 C13 123.3(2) . . ?
C13 N5 C12 115.4(2) . . ?
C11 N6 C14 119.1(2) . . ?
C11 N6 C15 120.6(2) . . ?
C15 N6 C14 116.4(2) . . ?
C6 N7 Cu2 126.14(17) . . ?
C25 N7 Cu2 118.81(17) . . ?
C25 N7 C6 114.6(2) . . ?
C8 N8 Cu2 127.28(18) . . ?
C30 N8 Cu2 116.67(17) . . ?
C30 N8 C8 114.4(2) . . ?
C25 N9 C26 123.0(3) . . ?
C25 N9 C27 121.1(2) . . ?
C26 N9 C27 114.7(2) . . ?
C25 N10 C28 119.2(2) . . ?
C25 N10 C29 122.4(3) . . ?
C28 N10 C29 116.1(2) . . ?
C30 N11 C31 120.1(2) . . ?
C30 N11 C32 123.0(3) . . ?
C31 N11 C32 115.1(3) . . ?
C30 N12 C33 120.5(2) . . ?
C30 N12 C34 122.5(3) . . ?
C33 N12 C34 115.0(3) . . ?
N1 C1 C2 123.0(2) . . ?
C10 C1 N1 118.5(2) . . ?
C10 C1 C2 118.5(2) . . ?
C1 C2 C3 122.2(2) . . ?
C1 C2 C7 119.5(3) . . ?
C3 C2 C7 118.3(2) . . ?
N2 C3 C2 123.5(2) . . ?
C4 C3 N2 117.6(2) . . ?
C4 C3 C2 118.9(2) . . ?
C3 C4 H4 119.0 . . ?
C3 C4 C5 122.0(3) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 H5 119.0 . . ?
C6 C5 C4 122.0(3) . . ?
C6 C5 H5 119.0 . . ?
N7 C6 C7 123.6(2) . . ?
C5 C6 N7 118.3(2) . . ?
C5 C6 C7 118.1(2) . . ?
C6 C7 C2 119.3(2) . . ?
C8 C7 C2 118.5(2) . . ?
C8 C7 C6 122.1(2) . . ?
N8 C8 C7 123.7(2) . . ?
C9 C8 N8 118.0(2) . . ?
C9 C8 C7 118.3(2) . . ?
C8 C9 H9 118.8 . . ?
C8 C9 C10 122.3(3) . . ?
C10 C9 H9 118.9 . . ?
C1 C10 C9 121.7(3) . . ?
C1 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
N2 C11 N6 122.8(2) . . ?
N5 C11 N2 119.9(2) . . ?
N5 C11 N6 117.3(3) . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C16 N4 122.7(2) . . ?
N3 C16 N1 119.8(2) . . ?
N3 C16 N4 117.3(3) . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 H18A 109.5 . . ?
N3 C18 H18B 109.5 . . ?
N3 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 H19A 109.5 . . ?
N4 C19 H19B 109.5 . . ?
N4 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
N4 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C21 C22 114.9(3) . . ?
O2 C21 O1 125.1(3) . . ?
O2 C21 C22 120.0(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 C24 114.8(3) . . ?
O4 C23 O3 125.4(3) . . ?
O4 C23 C24 119.8(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N7 C25 N10 121.8(3) . . ?
N9 C25 N7 120.6(2) . . ?
N9 C25 N10 117.6(2) . . ?
N9 C26 H26A 109.5 . . ?
N9 C26 H26B 109.5 . . ?
N9 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N9 C27 H27A 109.5 . . ?
N9 C27 H27B 109.5 . . ?
N9 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N10 C28 H28A 109.5 . . ?
N10 C28 H28B 109.5 . . ?
N10 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N10 C29 H29A 109.5 . . ?
N10 C29 H29B 109.5 . . ?
N10 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N11 C30 N8 119.4(3) . . ?
N11 C30 N12 118.6(3) . . ?
N12 C30 N8 121.9(3) . . ?
N11 C31 H31A 109.5 . . ?
N11 C31 H31B 109.5 . . ?
N11 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N11 C32 H32A 109.5 . . ?
N11 C32 H32B 109.5 . . ?
N11 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N12 C33 H33A 109.5 . . ?
N12 C33 H33B 109.5 . . ?
N12 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N12 C34 H34A 109.5 . . ?
N12 C34 H34B 109.5 . . ?
N12 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O5 C35 C36 114.5(3) . . ?
O6 C35 O5 125.2(3) . . ?
O6 C35 C36 120.4(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O7 C37 C38 115.8(3) . . ?
O8 C37 O7 124.8(3) . . ?
O8 C37 C38 119.4(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N51 C51 C52 179.3(8) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N61 C61 C62 179.1(5) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N71 C71 C72 178.8(5) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N41 C41 C42 179.0(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

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
Cu1 O1 C21 O2 7.2(4) . . . . ?
Cu1 O1 C21 C22 -172.4(2) . . . . ?
Cu1 O3 C23 O4 3.6(4) . . . . ?
Cu1 O3 C23 C24 -176.9(2) . . . . ?
Cu1 N1 C1 C2 -20.7(4) . . . . ?
Cu1 N1 C1 C10 159.0(2) . . . . ?
Cu1 N1 C16 N3 -52.1(3) . . . . ?
Cu1 N1 C16 N4 124.7(2) . . . . ?
Cu1 N2 C3 C2 -25.3(4) . . . . ?
Cu1 N2 C3 C4 157.3(2) . . . . ?
Cu1 N2 C11 N5 -58.2(3) . . . . ?
Cu1 N2 C11 N6 120.0(2) . . . . ?
Cu2 O5 C35 O6 -0.1(4) . . . . ?
Cu2 O5 C35 C36 179.8(2) . . . . ?
Cu2 O7 C37 O8 -8.0(4) . . . . ?
Cu2 O7 C37 C38 171.2(2) . . . . ?
Cu2 N7 C6 C5 156.0(2) . . . . ?
Cu2 N7 C6 C7 -25.9(4) . . . . ?
Cu2 N7 C25 N9 -56.7(4) . . . . ?
Cu2 N7 C25 N10 121.8(2) . . . . ?
Cu2 N8 C8 C7 -19.3(4) . . . . ?
Cu2 N8 C8 C9 162.2(2) . . . . ?
Cu2 N8 C30 N11 -66.0(3) . . . . ?
Cu2 N8 C30 N12 112.5(3) . . . . ?
N1 C1 C2 C3 12.4(4) . . . . ?
N1 C1 C2 C7 -169.4(2) . . . . ?
N1 C1 C10 C9 176.7(3) . . . . ?
N2 C3 C4 C5 175.3(2) . . . . ?
N7 C6 C7 C2 -167.6(2) . . . . ?
N7 C6 C7 C8 13.9(4) . . . . ?
N8 C8 C9 C10 176.6(3) . . . . ?
C1 N1 C16 N3 134.9(2) . . . . ?
C1 N1 C16 N4 -48.3(3) . . . . ?
C1 C2 C3 N2 10.8(4) . . . . ?
C1 C2 C3 C4 -171.9(2) . . . . ?
C1 C2 C7 C6 167.7(3) . . . . ?
C1 C2 C7 C8 -13.8(4) . . . . ?
C2 C1 C10 C9 -3.5(4) . . . . ?
C2 C3 C4 C5 -2.2(4) . . . . ?
C2 C7 C8 N8 -169.3(2) . . . . ?
C2 C7 C8 C9 9.2(4) . . . . ?
C3 N2 C11 N5 135.4(2) . . . . ?
C3 N2 C11 N6 -46.4(3) . . . . ?
C3 C2 C7 C6 -14.0(4) . . . . ?
C3 C2 C7 C8 164.5(2) . . . . ?
C3 C4 C5 C6 -1.5(4) . . . . ?
C4 C5 C6 N7 175.5(3) . . . . ?
C4 C5 C6 C7 -2.7(4) . . . . ?
C5 C6 C7 C2 10.5(4) . . . . ?
C5 C6 C7 C8 -168.0(3) . . . . ?
C6 N7 C25 N9 130.5(3) . . . . ?
C6 N7 C25 N10 -50.9(4) . . . . ?
C6 C7 C8 N8 9.2(4) . . . . ?
C6 C7 C8 C9 -172.3(3) . . . . ?
C7 C2 C3 N2 -167.5(2) . . . . ?
C7 C2 C3 C4 9.8(4) . . . . ?
C7 C8 C9 C10 -2.0(4) . . . . ?
C8 N8 C30 N11 127.6(3) . . . . ?
C8 N8 C30 N12 -53.9(4) . . . . ?
C8 C9 C10 C1 -1.0(4) . . . . ?
C10 C1 C2 C3 -167.3(2) . . . . ?
C10 C1 C2 C7 10.9(4) . . . . ?
C11 N2 C3 C2 139.6(3) . . . . ?
C11 N2 C3 C4 -37.7(3) . . . . ?
C12 N5 C11 N2 -18.8(4) . . . . ?
C12 N5 C11 N6 162.9(2) . . . . ?
C13 N5 C11 N2 149.9(3) . . . . ?
C13 N5 C11 N6 -28.4(4) . . . . ?
C14 N6 C11 N2 -22.6(4) . . . . ?
C14 N6 C11 N5 155.6(2) . . . . ?
C15 N6 C11 N2 134.1(3) . . . . ?
C15 N6 C11 N5 -47.7(4) . . . . ?
C16 N1 C1 C2 151.3(2) . . . . ?
C16 N1 C1 C10 -29.0(3) . . . . ?
C17 N3 C16 N1 148.4(3) . . . . ?
C17 N3 C16 N4 -28.6(4) . . . . ?
C18 N3 C16 N1 -18.4(4) . . . . ?
C18 N3 C16 N4 164.6(2) . . . . ?
C19 N4 C16 N1 135.5(3) . . . . ?
C19 N4 C16 N3 -47.6(3) . . . . ?
C20 N4 C16 N1 -20.5(4) . . . . ?
C20 N4 C16 N3 156.4(2) . . . . ?
C25 N7 C6 C5 -31.8(4) . . . . ?
C25 N7 C6 C7 146.3(3) . . . . ?
C26 N9 C25 N7 149.9(3) . . . . ?
C26 N9 C25 N10 -28.7(4) . . . . ?
C27 N9 C25 N7 -16.9(4) . . . . ?
C27 N9 C25 N10 164.5(3) . . . . ?
C28 N10 C25 N7 -23.9(4) . . . . ?
C28 N10 C25 N9 154.7(3) . . . . ?
C29 N10 C25 N7 138.5(3) . . . . ?
C29 N10 C25 N9 -42.9(4) . . . . ?
C30 N8 C8 C7 145.4(3) . . . . ?
C30 N8 C8 C9 -33.2(4) . . . . ?
C31 N11 C30 N8 -17.8(4) . . . . ?
C31 N11 C30 N12 163.6(3) . . . . ?
C32 N11 C30 N8 146.7(3) . . . . ?
C32 N11 C30 N12 -31.9(4) . . . . ?
C33 N12 C30 N8 -19.3(4) . . . . ?
C33 N12 C30 N11 159.3(3) . . . . ?
C34 N12 C30 N8 143.7(3) . . . . ?
C34 N12 C30 N11 -37.7(4) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3 8 -1 0.0295 2.9950 7.9945 -1.0026 0.0610 -0.3172 -0.9429
8 1 4 0.1182 8.0009 1.0001 3.9872 -0.1582 0.9854 -0.3717
-8 -1 -4 0.1036 -8.0009 -1.0001 -3.9872 0.1582 -0.9854 0.3717
0 1 13 0.0111 0.0120 1.0050 13.0022 -1.0127 -0.1078 -0.0083
0 -1 -13 0.0144 -0.0120 -1.0050 -13.0022 1.0127 0.1078 0.0083
-7 -7 -2 0.0544 -6.9970 -6.9958 -1.9906 0.0810 -0.3099 0.9669
-3 -8 1 0.0105 -2.9950 -7.9945 1.0026 -0.0610 0.3172 0.9429

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -1.0012 -0.0000 0.0007 0.0005 -1.0007 -0.0007 -0.6628 0.0349 1.0007
loop_
_twin_individual_mass_fraction_refined
0.5853(8)
0.4147(8)
_cell_oxdiff_length_a            12.3650(3)
_cell_oxdiff_length_b            12.5243(5)
_cell_oxdiff_length_c            20.2731(6)
_cell_oxdiff_angle_alpha         85.405(3)
_cell_oxdiff_angle_beta          78.567(2)
_cell_oxdiff_angle_gamma         63.473(3)
_cell_oxdiff_volume              2753.18(15)
_cell_oxdiff_measurement_reflns_used 26388
_cell_oxdiff_twin_number         2
_diffrn_measurement_specimen_support 'polyimid foil'



####################################################################### 
# 
# 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_az133a
_database_code_depnum_ccdc_archive 'CCDC 1414996'
_audit_update_record             
;
2015-07-24 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;                                                                             
 ?                                                                             
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H52 Cl2 F12 N12 P2'
_chemical_formula_weight         953.69

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   12.794(3)
_cell_length_b                   8.0020(16)
_cell_length_c                   21.272(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.49(3)
_cell_angle_gamma                90.00
_cell_volume                     2163.8(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      30.02

_exptl_crystal_description       'box shaped'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             988
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;                                                                               
 ?                                                                              
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11460
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         30.02
_reflns_number_total             6281
_reflns_number_gt                3726
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Bruker AXS, 1997-2009)'
_computing_cell_refinement       'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XPMA (Zsolnai, Huttner, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;                                                                               
 Refinement of F² against ALL reflections.  The weighted R-factor wR and      
 goodness of fit S are based on F², conventional R-factors R are based        
 on F, with F set to zero for negative F². The threshold expression of        
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is     
 not relevant to the choice of reflections for refinement.  R-factors based     
 on F² are statistically about twice as large as those based on F, and R-     
 factors based on ALL data will be even larger.                                 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0777P)²+0.6326P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6281
_refine_ls_number_parameters     288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1681
_refine_ls_wR_factor_gt          0.1418
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.51051(5) 0.17562(7) 0.78130(3) 0.03447(17) Uani 1 1 d . . .
F1 F 0.44238(12) 0.25742(19) 0.83182(8) 0.0490(4) Uani 1 1 d . . .
F2 F 0.57854(13) 0.09333(18) 0.73094(7) 0.0501(4) Uani 1 1 d . . .
F3 F 0.59403(15) 0.1131(3) 0.83654(9) 0.0792(6) Uani 1 1 d . . .
F4 F 0.42455(18) 0.2331(3) 0.72637(10) 0.0854(7) Uani 1 1 d . . .
F5 F 0.57209(18) 0.3450(2) 0.77703(11) 0.0945(9) Uani 1 1 d . . .
F6 F 0.44929(14) 0.00440(19) 0.78567(10) 0.0666(5) Uani 1 1 d . . .
N1 N 0.71841(14) 0.1287(2) 0.54795(9) 0.0293(4) Uani 1 1 d . . .
N2 N 0.76966(15) 0.2513(2) 0.64620(9) 0.0323(4) Uani 1 1 d . . .
N3 N 0.88393(14) 0.0739(2) 0.59987(9) 0.0313(4) Uani 1 1 d . . .
N4 N 0.61636(14) 0.3051(2) 0.45562(8) 0.0263(4) Uani 1 1 d . . .
N5 N 0.68197(14) 0.2782(2) 0.35678(8) 0.0269(4) Uani 1 1 d . . .
N6 N 0.66376(14) 0.5396(2) 0.40188(9) 0.0272(4) Uani 1 1 d . . .
C1 C 0.62882(16) 0.0479(3) 0.55082(10) 0.0243(4) Uani 1 1 d . . .
C2 C 0.54406(16) 0.0571(2) 0.50021(9) 0.0230(4) Uani 1 1 d . . .
C3 C 0.54712(16) 0.1770(3) 0.45124(10) 0.0239(4) Uani 1 1 d . . .
C4 C 0.46579(17) 0.1691(3) 0.39829(10) 0.0262(4) Uani 1 1 d . . .
H4 H 0.4702 0.2396 0.3639 0.031 Uiso 1 1 calc R . .
C5 C 0.38403(17) 0.0634(3) 0.39707(10) 0.0260(4) Uani 1 1 d . . .
H5 H 0.3342 0.0617 0.3617 0.031 Uiso 1 1 calc R . .
C6 C 0.79009(18) 0.1488(3) 0.59924(10) 0.0293(5) Uani 1 1 d . . .
C7 C 0.6858(2) 0.3758(3) 0.63619(12) 0.0399(6) Uani 1 1 d . . .
H7A H 0.6696 0.3963 0.5917 0.060 Uiso 1 1 calc R . .
H7B H 0.7086 0.4779 0.6572 0.060 Uiso 1 1 calc R . .
H7C H 0.6243 0.3351 0.6531 0.060 Uiso 1 1 calc R . .
C8 C 0.8180(2) 0.2314(3) 0.71169(11) 0.0368(5) Uani 1 1 d . . .
H8A H 0.8533 0.1255 0.7162 0.055 Uiso 1 1 calc R . .
H8B H 0.7644 0.2359 0.7398 0.055 Uiso 1 1 calc R . .
H8C H 0.8678 0.3196 0.7219 0.055 Uiso 1 1 calc R . .
C9 C 0.98211(19) 0.1488(3) 0.62915(12) 0.0409(6) Uani 1 1 d . . .
H9A H 0.9683 0.2596 0.6435 0.061 Uiso 1 1 calc R . .
H9B H 1.0319 0.1540 0.5987 0.061 Uiso 1 1 calc R . .
H9C H 1.0104 0.0818 0.6645 0.061 Uiso 1 1 calc R . .
C10 C 0.8942(2) -0.0644(3) 0.55600(12) 0.0425(6) Uani 1 1 d . . .
H10A H 0.8327 -0.1340 0.5541 0.064 Uiso 1 1 calc R . .
H10B H 0.9553 -0.1294 0.5705 0.064 Uiso 1 1 calc R . .
H10C H 0.9012 -0.0208 0.5147 0.064 Uiso 1 1 calc R . .
C11 C 0.65154(16) 0.3720(3) 0.40496(10) 0.0245(4) Uani 1 1 d . . .
C12 C 0.71045(19) 0.1023(3) 0.36638(12) 0.0330(5) Uani 1 1 d . . .
H12A H 0.7289 0.0816 0.4107 0.049 Uiso 1 1 calc R . .
H12B H 0.7694 0.0767 0.3438 0.049 Uiso 1 1 calc R . .
H12C H 0.6518 0.0333 0.3509 0.049 Uiso 1 1 calc R . .
C13 C 0.6727(2) 0.3368(3) 0.29144(11) 0.0356(5) Uani 1 1 d . . .
H13A H 0.6348 0.4406 0.2882 0.053 Uiso 1 1 calc R . .
H13B H 0.6355 0.2551 0.2644 0.053 Uiso 1 1 calc R . .
H13C H 0.7416 0.3532 0.2787 0.053 Uiso 1 1 calc R . .
C14 C 0.75308(19) 0.6175(3) 0.37589(12) 0.0357(5) Uani 1 1 d . . .
H14A H 0.7998 0.5323 0.3640 0.054 Uiso 1 1 calc R . .
H14B H 0.7900 0.6887 0.4073 0.054 Uiso 1 1 calc R . .
H14C H 0.7280 0.6827 0.3394 0.054 Uiso 1 1 calc R . .
C15 C 0.6093(2) 0.6476(3) 0.44271(12) 0.0375(6) Uani 1 1 d . . .
H15A H 0.5460 0.5938 0.4523 0.056 Uiso 1 1 calc R . .
H15B H 0.5921 0.7515 0.4215 0.056 Uiso 1 1 calc R . .
H15C H 0.6541 0.6686 0.4812 0.056 Uiso 1 1 calc R . .
C20 C 0.5033(6) 0.0321(10) 0.9677(4) 0.081(2) Uani 0.50 1 d P . .
Cl1 Cl 0.3922(2) 0.0449(4) 1.00834(15) 0.0840(9) Uani 0.50 1 d P . .
Cl2 Cl 0.5941(2) -0.1180(2) 1.00513(12) 0.0515(6) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 F5 1.5756(18) . ?
P1 F3 1.578(2) . ?
P1 F4 1.580(2) . ?
P1 F6 1.5862(17) . ?
P1 F2 1.5967(15) . ?
P1 F1 1.5983(15) . ?
N1 C1 1.323(3) . ?
N1 C6 1.353(3) . ?
N2 C6 1.341(3) . ?
N2 C7 1.462(3) . ?
N2 C8 1.468(3) . ?
N3 C6 1.340(3) . ?
N3 C10 1.463(3) . ?
N3 C9 1.466(3) . ?
N4 C11 1.327(3) . ?
N4 C3 1.351(3) . ?
N5 C11 1.362(3) . ?
N5 C13 1.459(3) . ?
N5 C12 1.462(3) . ?
N6 C11 1.352(3) . ?
N6 C15 1.457(3) . ?
N6 C14 1.464(3) . ?
C1 C2 1.441(3) . ?
C1 C5 1.446(3) 3_656 ?
C2 C3 1.420(3) . ?
C2 C2 1.451(4) 3_656 ?
C3 C4 1.446(3) . ?
C4 C5 1.343(3) . ?
C4 H4 0.9300 . ?
C5 C1 1.446(3) 3_656 ?
C5 H5 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C20 C20 1.480(15) 3_657 ?
C20 Cl1 1.508(8) 3_657 ?
C20 Cl2 1.588(8) 3_657 ?
C20 Cl1 1.749(8) . ?
C20 Cl2 1.794(7) . ?
Cl1 Cl2 0.683(3) 3_657 ?
Cl1 C20 1.508(8) 3_657 ?
Cl2 Cl1 0.683(3) 3_657 ?
Cl2 C20 1.588(8) 3_657 ?

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
F5 P1 F3 90.85(14) . . ?
F5 P1 F4 91.02(15) . . ?
F3 P1 F4 178.11(13) . . ?
F5 P1 F6 179.59(14) . . ?
F3 P1 F6 88.83(13) . . ?
F4 P1 F6 89.30(13) . . ?
F5 P1 F2 90.13(9) . . ?
F3 P1 F2 89.67(10) . . ?
F4 P1 F2 90.60(11) . . ?
F6 P1 F2 89.61(9) . . ?
F5 P1 F1 90.03(9) . . ?
F3 P1 F1 90.23(9) . . ?
F4 P1 F1 89.49(10) . . ?
F6 P1 F1 90.22(9) . . ?
F2 P1 F1 179.81(9) . . ?
C1 N1 C6 122.17(18) . . ?
C6 N2 C7 120.7(2) . . ?
C6 N2 C8 122.9(2) . . ?
C7 N2 C8 115.84(19) . . ?
C6 N3 C10 118.4(2) . . ?
C6 N3 C9 123.0(2) . . ?
C10 N3 C9 116.51(19) . . ?
C11 N4 C3 122.02(18) . . ?
C11 N5 C13 122.70(18) . . ?
C11 N5 C12 120.87(18) . . ?
C13 N5 C12 115.76(18) . . ?
C11 N6 C15 119.57(17) . . ?
C11 N6 C14 122.70(18) . . ?
C15 N6 C14 114.73(18) . . ?
N1 C1 C2 121.55(19) . . ?
N1 C1 C5 120.7(2) . 3_656 ?
C2 C1 C5 117.59(18) . 3_656 ?
C3 C2 C1 120.12(18) . . ?
C3 C2 C2 120.5(2) . 3_656 ?
C1 C2 C2 119.4(2) . 3_656 ?
N4 C3 C2 122.3(2) . . ?
N4 C3 C4 119.69(18) . . ?
C2 C3 C4 117.72(18) . . ?
C5 C4 C3 122.20(19) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C4 C5 C1 121.9(2) . 3_656 ?
C4 C5 H5 119.0 . . ?
C1 C5 H5 119.0 3_656 . ?
N3 C6 N2 121.0(2) . . ?
N3 C6 N1 118.7(2) . . ?
N2 C6 N1 120.1(2) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 N6 119.44(18) . . ?
N4 C11 N5 122.71(18) . . ?
N6 C11 N5 117.74(18) . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C20 C20 Cl1 71.6(6) 3_657 3_657 ?
C20 C20 Cl2 71.5(5) 3_657 3_657 ?
Cl1 C20 Cl2 139.1(6) 3_657 3_657 ?
C20 C20 Cl1 55.0(5) 3_657 . ?
Cl1 C20 Cl1 126.6(5) 3_657 . ?
Cl2 C20 Cl1 22.97(14) 3_657 . ?
C20 C20 Cl2 57.1(5) 3_657 . ?
Cl1 C20 Cl2 21.73(17) 3_657 . ?
Cl2 C20 Cl2 128.6(5) 3_657 . ?
Cl1 C20 Cl2 110.0(4) . . ?
Cl2 Cl1 C20 103.4(6) 3_657 3_657 ?
Cl2 Cl1 C20 65.2(5) 3_657 . ?
C20 Cl1 C20 53.4(5) 3_657 . ?
Cl1 Cl2 C20 91.8(5) 3_657 3_657 ?
Cl1 Cl2 C20 54.9(5) 3_657 . ?
C20 Cl2 C20 51.4(5) 3_657 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C1 C2 166.7(2) . . . . ?
C6 N1 C1 C5 -18.2(3) . . . 3_656 ?
N1 C1 C2 C3 -11.5(3) . . . . ?
C5 C1 C2 C3 173.22(18) 3_656 . . . ?
N1 C1 C2 C2 168.4(2) . . . 3_656 ?
C5 C1 C2 C2 -6.9(3) 3_656 . . 3_656 ?
C11 N4 C3 C2 150.8(2) . . . . ?
C11 N4 C3 C4 -35.8(3) . . . . ?
C1 C2 C3 N4 -12.8(3) . . . . ?
C2 C2 C3 N4 167.2(2) 3_656 . . . ?
C1 C2 C3 C4 173.62(18) . . . . ?
C2 C2 C3 C4 -6.3(3) 3_656 . . . ?
N4 C3 C4 C5 -167.72(19) . . . . ?
C2 C3 C4 C5 6.0(3) . . . . ?
C3 C4 C5 C1 1.0(3) . . . 3_656 ?
C10 N3 C6 N2 166.1(2) . . . . ?
C9 N3 C6 N2 -30.6(3) . . . . ?
C10 N3 C6 N1 -18.6(3) . . . . ?
C9 N3 C6 N1 144.6(2) . . . . ?
C7 N2 C6 N3 158.3(2) . . . . ?
C8 N2 C6 N3 -30.5(3) . . . . ?
C7 N2 C6 N1 -16.9(3) . . . . ?
C8 N2 C6 N1 154.3(2) . . . . ?
C1 N1 C6 N3 114.3(2) . . . . ?
C1 N1 C6 N2 -70.4(3) . . . . ?
C3 N4 C11 N6 140.1(2) . . . . ?
C3 N4 C11 N5 -43.7(3) . . . . ?
C15 N6 C11 N4 -19.0(3) . . . . ?
C14 N6 C11 N4 140.3(2) . . . . ?
C15 N6 C11 N5 164.6(2) . . . . ?
C14 N6 C11 N5 -36.0(3) . . . . ?
C13 N5 C11 N4 150.0(2) . . . . ?
C12 N5 C11 N4 -20.3(3) . . . . ?
C13 N5 C11 N6 -33.8(3) . . . . ?
C12 N5 C11 N6 156.0(2) . . . . ?
C20 C20 Cl1 Cl2 131.4(9) 3_657 . . 3_657 ?
Cl1 C20 Cl1 Cl2 131.4(9) 3_657 . . 3_657 ?
Cl2 C20 Cl1 Cl2 147.4(7) . . . 3_657 ?
Cl1 C20 Cl1 C20 0.002(2) 3_657 . . 3_657 ?
Cl2 C20 Cl1 C20 -131.4(9) 3_657 . . 3_657 ?
Cl2 C20 Cl1 C20 16.0(3) . . . 3_657 ?
C20 C20 Cl2 Cl1 -127.7(10) 3_657 . . 3_657 ?
Cl2 C20 Cl2 Cl1 -127.7(10) 3_657 . . 3_657 ?
Cl1 C20 Cl2 Cl1 -143.3(7) . . . 3_657 ?
Cl1 C20 Cl2 C20 127.7(10) 3_657 . . 3_657 ?
Cl2 C20 Cl2 C20 -0.002(2) 3_657 . . 3_657 ?
Cl1 C20 Cl2 C20 -15.6(3) . . . 3_657 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        30.02
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.065
