# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

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

data_CCDC_1511704
_database_code_depnum_ccdc_archive 'CCDC 1511704'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
_audit_creation_date             2017-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C23 H24 Cu N5 O4, H2 O, C8 H11 N2 O3'
_chemical_formula_sum            'C31 H37 Cu N7 O8'
_chemical_formula_weight         699.21
_chemical_melting_point          ?
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.1048(3)
_cell_length_b                   16.4602(7)
_cell_length_c                   24.4695(12)
_cell_angle_alpha                90
_cell_angle_beta                 95.214(4)
_cell_angle_gamma                90
_cell_volume                     3250.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5652
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.0630
_cell_measurement_theta_min      3.5710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.4948
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.0939
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15778
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.866
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -32.00   51.00   1.0000   68.6100
omega____ theta____ kappa____ phi______ frames
    -       17.2817  -19.0000   60.0000 83

#__ type_ start__ end____ width___ exp.time_
  2 omega  -18.00   18.00   1.0000   68.6100
omega____ theta____ kappa____ phi______ frames
    -      -19.3130  -99.0000   90.0000 36

#__ type_ start__ end____ width___ exp.time_
  3 omega  -49.00   37.00   1.0000   68.6100
omega____ theta____ kappa____ phi______ frames
    -       17.2817  -57.0000    0.0000 86

#__ type_ start__ end____ width___ exp.time_
  4 omega    8.00   63.00   1.0000   68.6100
omega____ theta____ kappa____ phi______ frames
    -       17.2817   77.0000  -90.0000 55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4591
_reflns_number_total             6629
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6629
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.028
_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)+(0.0443P)²+0.5148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1179
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O7W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Free rotating group:
 O7W(H7WA,H7WB)
3.b Rotating group:
 O8W(H8WA,H8WB)
3.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C25(H25A,H25B), C27(H27A,H27B)
3.d Aromatic/amide H refined with riding coordinates:
 N5(H5), C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12),
 C13(H13), C14(H14), C15(H15), N7(H7A)
3.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.69203(4) 0.65342(2) 0.40811(2) 0.02832(12) Uani 1 1 d . . . . .
O1 O 0.8304(3) 0.59002(13) 0.31420(9) 0.0433(6) Uani 1 1 d . . . . .
O2 O 0.6836(4) 0.31328(15) 0.31710(11) 0.0744(9) Uani 1 1 d . . . . .
O3 O 0.5068(3) 0.48988(13) 0.43745(9) 0.0401(6) Uani 1 1 d . . . . .
O7W O 0.7552(6) 0.7532(2) 0.28669(14) 0.1199(15) Uani 1 1 d . U . . .
H7WA H 0.683361 0.716738 0.277971 0.180 Uiso 1 1 d G . . . .
H7WB H 0.783887 0.775882 0.257843 0.180 Uiso 1 1 d G . . . .
O8W O 0.6519(3) 0.62769(15) 0.49546(9) 0.0510(7) Uani 1 1 d . . . . .
H8WA H 0.568620 0.594416 0.497612 0.076 Uiso 1 1 d GR . . . .
H8WB H 0.630200 0.672536 0.512552 0.076 Uiso 1 1 d GR . . . .
N1 N 0.4696(3) 0.69642(15) 0.37399(10) 0.0304(6) Uani 1 1 d . . . . .
N2 N 0.7338(3) 0.76978(15) 0.41161(10) 0.0320(6) Uani 1 1 d . . . . .
N3 N 0.9346(3) 0.65508(17) 0.43736(10) 0.0330(6) Uani 1 1 d . . . . .
N4 N 0.6787(3) 0.54148(14) 0.37820(10) 0.0261(5) Uani 1 1 d . . . . .
N5 N 0.5954(3) 0.40373(15) 0.37541(10) 0.0362(6) Uani 1 1 d . . . . .
H5 H 0.539212 0.365950 0.389420 0.043 Uiso 1 1 calc R . . . .
C1 C 1.0264(4) 0.5909(2) 0.45352(14) 0.0421(8) Uani 1 1 d . . . . .
H1 H 0.982001 0.539245 0.447509 0.051 Uiso 1 1 calc R . . . .
C2 C 1.1837(4) 0.5980(3) 0.47866(15) 0.0542(10) Uani 1 1 d . . . . .
H2 H 1.245423 0.552003 0.488994 0.065 Uiso 1 1 calc R . . . .
C3 C 1.2483(4) 0.6736(3) 0.48829(16) 0.0620(12) Uani 1 1 d . . . . .
H3 H 1.354455 0.679497 0.505730 0.074 Uiso 1 1 calc R . . . .
C4 C 1.1578(4) 0.7406(3) 0.47244(15) 0.0494(10) Uani 1 1 d . . . . .
H4 H 1.200983 0.792473 0.478588 0.059 Uiso 1 1 calc R . . . .
C5 C 0.9994(4) 0.7296(2) 0.44687(13) 0.0381(8) Uani 1 1 d . . . . .
C6 C 0.8850(4) 0.7957(2) 0.42869(13) 0.0390(8) Uani 1 1 d . . . . .
C7 C 0.9214(5) 0.8779(2) 0.42683(17) 0.0585(11) Uani 1 1 d . . . . .
H7 H 1.027283 0.896725 0.438115 0.070 Uiso 1 1 calc R . . . .
C8 C 0.8005(6) 0.9302(2) 0.40834(19) 0.0711(13) Uani 1 1 d . . . . .
H8 H 0.822876 0.985626 0.408078 0.085 Uiso 1 1 calc R . . . .
C9 C 0.6434(5) 0.9027(2) 0.38973(17) 0.0621(11) Uani 1 1 d . . . . .
H9 H 0.560621 0.938552 0.376325 0.074 Uiso 1 1 calc R . . . .
C10 C 0.6149(4) 0.8200(2) 0.39192(14) 0.0392(8) Uani 1 1 d . . . . .
C11 C 0.4606(4) 0.7777(2) 0.37084(13) 0.0375(8) Uani 1 1 d . . . . .
C12 C 0.3193(4) 0.8160(2) 0.34864(16) 0.0525(10) Uani 1 1 d . . . . .
H12 H 0.313864 0.872371 0.347337 0.063 Uiso 1 1 calc R . . . .
C13 C 0.1865(5) 0.7700(3) 0.32847(16) 0.0584(11) Uani 1 1 d . . . . .
H13 H 0.090542 0.795112 0.313024 0.070 Uiso 1 1 calc R . . . .
C14 C 0.1956(4) 0.6877(3) 0.33114(14) 0.0486(9) Uani 1 1 d . . . . .
H14 H 0.106902 0.655701 0.317278 0.058 Uiso 1 1 calc R . . . .
C15 C 0.3394(4) 0.6524(2) 0.35485(13) 0.0387(8) Uani 1 1 d . . . . .
H15 H 0.345330 0.596107 0.357506 0.046 Uiso 1 1 calc R . . . .
C16 C 1.0554(6) 0.4236(3) 0.3463(2) 0.1006(18) Uani 1 1 d . . . . .
H16A H 1.154851 0.395645 0.338841 0.151 Uiso 1 1 calc GR . . . .
H16B H 1.002223 0.394459 0.373861 0.151 Uiso 1 1 calc GR . . . .
H16C H 1.082631 0.477401 0.359306 0.151 Uiso 1 1 calc GR . . . .
C17 C 0.9415(5) 0.4286(3) 0.29525(19) 0.0679(13) Uani 1 1 d . . . . .
H17A H 0.942415 0.376554 0.276631 0.082 Uiso 1 1 calc R . . . .
H17B H 0.984614 0.468775 0.271296 0.082 Uiso 1 1 calc R . . . .
C18 C 0.7626(4) 0.45035(19) 0.30322(13) 0.0351(7) Uani 1 1 d . . . . .
C19 C 0.6641(5) 0.4604(2) 0.24644(14) 0.0615(12) Uani 1 1 d . . . . .
H19A H 0.712533 0.504391 0.226951 0.074 Uiso 1 1 calc R . . . .
H19B H 0.675245 0.411020 0.225405 0.074 Uiso 1 1 calc R . . . .
C20 C 0.4801(6) 0.4779(3) 0.2494(2) 0.0968(17) Uani 1 1 d . . . . .
H20A H 0.426788 0.483482 0.212875 0.145 Uiso 1 1 calc GR . . . .
H20B H 0.467581 0.527424 0.269328 0.145 Uiso 1 1 calc GR . . . .
H20C H 0.430221 0.433964 0.267694 0.145 Uiso 1 1 calc GR . . . .
C21 C 0.6807(4) 0.3827(2) 0.33240(13) 0.0402(8) Uani 1 1 d . . . . .
C22 C 0.5897(3) 0.47978(18) 0.39889(12) 0.0280(7) Uani 1 1 d . . . . .
C23 C 0.7583(3) 0.53172(18) 0.33287(12) 0.0293(7) Uani 1 1 d . . . . .
O4 O 0.3523(3) 0.29033(14) 0.39980(12) 0.0588(7) Uani 1 1 d . . . . .
O5 O 0.5904(4) 0.09760(17) 0.50935(11) 0.0769(9) Uani 1 1 d . . . . .
O6 O 0.2071(4) 0.01366(15) 0.37848(11) 0.0688(8) Uani 1 1 d . . . . .
N6 N 0.4720(4) 0.19777(18) 0.45662(12) 0.0485(8) Uani 1 1 d . . . . .
N7 N 0.3894(3) 0.06010(17) 0.44545(11) 0.0466(7) Uani 1 1 d . . . . .
H7A H 0.394081 0.012369 0.459794 0.056 Uiso 1 1 calc R . . . .
C24 C 0.0029(5) 0.1886(3) 0.4127(2) 0.0886(16) Uani 1 1 d . . . . .
H24A H -0.110771 0.201098 0.401341 0.133 Uiso 1 1 calc GR . . . .
H24B H 0.050439 0.231795 0.435357 0.133 Uiso 1 1 calc GR . . . .
H24C H 0.008547 0.138806 0.433211 0.133 Uiso 1 1 calc GR . . . .
C25 C 0.0975(5) 0.1795(2) 0.36300(17) 0.0613(11) Uani 1 1 d . . . . .
H25A H 0.092558 0.230588 0.343196 0.074 Uiso 1 1 calc R . . . .
H25B H 0.042445 0.138865 0.339093 0.074 Uiso 1 1 calc R . . . .
C26 C 0.2795(4) 0.1552(2) 0.37478(14) 0.0406(8) Uani 1 1 d . . . . .
C27 C 0.3612(5) 0.1525(2) 0.32068(16) 0.0599(11) Uani 1 1 d . . . . .
H27A H 0.297660 0.116169 0.295608 0.072 Uiso 1 1 calc R . . . .
H27B H 0.355459 0.206295 0.304479 0.072 Uiso 1 1 calc R . . . .
C28 C 0.5396(6) 0.1250(2) 0.32592(19) 0.0790(15) Uani 1 1 d . . . . .
H28A H 0.583397 0.128865 0.290858 0.119 Uiso 1 1 calc GR . . . .
H28B H 0.545785 0.069648 0.338345 0.119 Uiso 1 1 calc GR . . . .
H28C H 0.603080 0.158937 0.351891 0.119 Uiso 1 1 calc GR . . . .
C29 C 0.2867(4) 0.0709(2) 0.39941(14) 0.0438(9) Uani 1 1 d . . . . .
C30 C 0.4886(5) 0.1205(2) 0.47153(14) 0.0482(9) Uani 1 1 d . . . . .
C31 C 0.3726(4) 0.2179(2) 0.41283(15) 0.0420(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O8W 2.232(2) . ?
Cu1 N1 2.043(2) . ?
Cu1 N2 1.946(2) . ?
Cu1 N3 2.031(2) . ?
Cu1 N4 1.982(2) . ?
O1 C23 1.233(3) . ?
O2 C21 1.204(4) . ?
O3 C22 1.218(3) . ?
O7W H7WA 0.8503 . ?
O7W H7WB 0.8492 . ?
O8W H8WA 0.8745 . ?
O8W H8WB 0.8742 . ?
N1 C11 1.342(4) . ?
N1 C15 1.330(4) . ?
N2 C6 1.329(4) . ?
N2 C10 1.327(4) . ?
N3 C1 1.331(4) . ?
N3 C5 1.346(4) . ?
N4 C22 1.369(4) . ?
N4 C23 1.342(3) . ?
N5 H5 0.8600 . ?
N5 C21 1.356(4) . ?
N5 C22 1.380(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.369(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.362(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.361(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.388(4) . ?
C5 C6 1.472(5) . ?
C6 C7 1.387(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.352(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.383(5) . ?
C10 C11 1.482(5) . ?
C11 C12 1.375(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.370(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.359(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.382(4) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C17 1.487(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.523(5) . ?
C18 C19 1.547(5) . ?
C18 C21 1.509(4) . ?
C18 C23 1.525(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.527(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
O4 C31 1.242(4) . ?
O5 C30 1.241(4) . ?
O6 C29 1.227(4) . ?
N6 C30 1.327(4) . ?
N6 C31 1.323(4) . ?
N7 H7A 0.8600 . ?
N7 C29 1.350(4) . ?
N7 C30 1.395(4) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 C25 1.504(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.530(5) . ?
C26 C27 1.533(5) . ?
C26 C29 1.512(4) . ?
C26 C31 1.541(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.510(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 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
N1 Cu1 O8W 104.90(9) . . ?
N2 Cu1 O8W 100.64(10) . . ?
N2 Cu1 N1 79.65(10) . . ?
N2 Cu1 N3 79.18(11) . . ?
N2 Cu1 N4 159.22(10) . . ?
N3 Cu1 O8W 83.44(9) . . ?
N3 Cu1 N1 158.35(11) . . ?
N4 Cu1 O8W 99.76(9) . . ?
N4 Cu1 N1 98.91(10) . . ?
N4 Cu1 N3 99.27(10) . . ?
H7WA O7W H7WB 109.5 . . ?
Cu1 O8W H8WA 110.9 . . ?
Cu1 O8W H8WB 110.6 . . ?
H8WA O8W H8WB 108.1 . . ?
C11 N1 Cu1 114.2(2) . . ?
C15 N1 Cu1 126.7(2) . . ?
C15 N1 C11 119.1(3) . . ?
C6 N2 Cu1 118.8(2) . . ?
C10 N2 Cu1 118.7(2) . . ?
C10 N2 C6 122.2(3) . . ?
C1 N3 Cu1 126.2(2) . . ?
C1 N3 C5 118.2(3) . . ?
C5 N3 Cu1 115.0(2) . . ?
C22 N4 Cu1 124.46(19) . . ?
C23 N4 Cu1 113.73(18) . . ?
C23 N4 C22 121.7(2) . . ?
C21 N5 H5 116.8 . . ?
C21 N5 C22 126.4(3) . . ?
C22 N5 H5 116.8 . . ?
N3 C1 H1 118.7 . . ?
N3 C1 C2 122.5(4) . . ?
C2 C1 H1 118.7 . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.8 . . ?
C3 C4 C5 118.4(4) . . ?
C5 C4 H4 120.8 . . ?
N3 C5 C4 121.8(3) . . ?
N3 C5 C6 113.3(3) . . ?
C4 C5 C6 124.9(3) . . ?
N2 C6 C5 113.3(3) . . ?
N2 C6 C7 119.8(3) . . ?
C7 C6 C5 126.9(3) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.2(4) . . ?
C9 C8 H8 119.4 . . ?
C8 C9 H9 121.3 . . ?
C10 C9 C8 117.4(4) . . ?
C10 C9 H9 121.3 . . ?
N2 C10 C9 120.6(3) . . ?
N2 C10 C11 113.3(3) . . ?
C9 C10 C11 126.0(3) . . ?
N1 C11 C10 114.1(3) . . ?
N1 C11 C12 121.2(3) . . ?
C12 C11 C10 124.6(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 C11 119.2(4) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.7(3) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 120.7 . . ?
C13 C14 C15 118.6(4) . . ?
C15 C14 H14 120.7 . . ?
N1 C15 C14 122.1(3) . . ?
N1 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
C16 C17 H17A 108.4 . . ?
C16 C17 H17B 108.4 . . ?
C16 C17 C18 115.5(4) . . ?
H17A C17 H17B 107.5 . . ?
C18 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
C17 C18 C19 109.3(3) . . ?
C17 C18 C23 109.4(3) . . ?
C21 C18 C17 110.6(3) . . ?
C21 C18 C19 106.9(3) . . ?
C21 C18 C23 113.1(3) . . ?
C23 C18 C19 107.5(3) . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 C18 113.9(3) . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C21 N5 120.6(3) . . ?
O2 C21 C18 122.1(3) . . ?
N5 C21 C18 117.2(3) . . ?
O3 C22 N4 122.1(3) . . ?
O3 C22 N5 119.2(3) . . ?
N4 C22 N5 118.7(3) . . ?
O1 C23 N4 119.5(3) . . ?
O1 C23 C18 118.4(3) . . ?
N4 C23 C18 122.1(3) . . ?
C31 N6 C30 120.1(3) . . ?
C29 N7 H7A 117.5 . . ?
C29 N7 C30 125.0(3) . . ?
C30 N7 H7A 117.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
C24 C25 H25A 108.4 . . ?
C24 C25 H25B 108.4 . . ?
C24 C25 C26 115.3(3) . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
C25 C26 C27 109.2(3) . . ?
C25 C26 C31 110.5(3) . . ?
C27 C26 C31 108.4(3) . . ?
C29 C26 C25 108.5(3) . . ?
C29 C26 C27 108.3(3) . . ?
C29 C26 C31 112.0(3) . . ?
C26 C27 H27A 108.5 . . ?
C26 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C28 C27 C26 114.9(3) . . ?
C28 C27 H27A 108.5 . . ?
C28 C27 H27B 108.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O6 C29 N7 120.5(3) . . ?
O6 C29 C26 122.6(3) . . ?
N7 C29 C26 116.9(3) . . ?
O5 C30 N6 122.6(3) . . ?
O5 C30 N7 116.2(3) . . ?
N6 C30 N7 121.1(3) . . ?
O4 C31 N6 120.3(3) . . ?
O4 C31 C26 116.2(3) . . ?
N6 C31 C26 123.4(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7W H7WB O2 0.85 1.97 2.811(4) 168.1 2_655
O8W H8WA O3 0.87 2.29 2.871(3) 123.8 .
O8W H8WA O3 0.87 2.24 2.912(3) 133.9 3_666
O8W H8WB O4 0.87 2.22 2.899(4) 134.1 3_666
O8W H8WB N6 0.87 2.43 3.294(4) 167.9 3_666
N5 H5 O4 0.86 1.99 2.817(3) 159.6 .
C3 H3 N6 0.93 2.58 3.299(5) 134.1 3_766
N7 H7A O5 0.86 1.96 2.821(4) 178.1 3_656

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 N1 C11 C10 0.9(3) . . . . ?
Cu1 N1 C11 C12 179.7(2) . . . . ?
Cu1 N1 C15 C14 -178.2(2) . . . . ?
Cu1 N2 C6 C5 -4.3(3) . . . . ?
Cu1 N2 C6 C7 174.2(3) . . . . ?
Cu1 N2 C10 C9 -175.0(3) . . . . ?
Cu1 N2 C10 C11 1.6(4) . . . . ?
Cu1 N3 C1 C2 -172.2(3) . . . . ?
Cu1 N3 C5 C4 172.8(2) . . . . ?
Cu1 N3 C5 C6 -5.9(3) . . . . ?
Cu1 N4 C22 O3 1.8(4) . . . . ?
Cu1 N4 C22 N5 -177.8(2) . . . . ?
Cu1 N4 C23 O1 0.2(3) . . . . ?
Cu1 N4 C23 C18 -179.7(2) . . . . ?
N1 C11 C12 C13 -1.2(5) . . . . ?
N2 C6 C7 C8 1.0(5) . . . . ?
N2 C10 C11 N1 -1.7(4) . . . . ?
N2 C10 C11 C12 179.6(3) . . . . ?
N3 C1 C2 C3 1.0(5) . . . . ?
N3 C5 C6 N2 6.6(4) . . . . ?
N3 C5 C6 C7 -171.8(3) . . . . ?
C1 N3 C5 C4 0.4(5) . . . . ?
C1 N3 C5 C6 -178.3(3) . . . . ?
C1 C2 C3 C4 -0.8(6) . . . . ?
C2 C3 C4 C5 0.4(5) . . . . ?
C3 C4 C5 N3 -0.3(5) . . . . ?
C3 C4 C5 C6 178.3(3) . . . . ?
C4 C5 C6 N2 -172.1(3) . . . . ?
C4 C5 C6 C7 9.5(5) . . . . ?
C5 N3 C1 C2 -0.8(5) . . . . ?
C5 C6 C7 C8 179.4(3) . . . . ?
C6 N2 C10 C9 -1.7(5) . . . . ?
C6 N2 C10 C11 175.0(3) . . . . ?
C6 C7 C8 C9 -2.1(6) . . . . ?
C7 C8 C9 C10 1.3(6) . . . . ?
C8 C9 C10 N2 0.6(5) . . . . ?
C8 C9 C10 C11 -175.6(4) . . . . ?
C9 C10 C11 N1 174.8(3) . . . . ?
C9 C10 C11 C12 -3.9(5) . . . . ?
C10 N2 C6 C5 -177.7(3) . . . . ?
C10 N2 C6 C7 0.8(5) . . . . ?
C10 C11 C12 C13 177.4(3) . . . . ?
C11 N1 C15 C14 0.8(5) . . . . ?
C11 C12 C13 C14 0.6(6) . . . . ?
C12 C13 C14 C15 0.6(5) . . . . ?
C13 C14 C15 N1 -1.4(5) . . . . ?
C15 N1 C11 C10 -178.3(3) . . . . ?
C15 N1 C11 C12 0.5(5) . . . . ?
C16 C17 C18 C19 175.2(4) . . . . ?
C16 C17 C18 C21 -67.5(4) . . . . ?
C16 C17 C18 C23 57.7(5) . . . . ?
C17 C18 C19 C20 176.9(3) . . . . ?
C17 C18 C21 O2 -51.3(5) . . . . ?
C17 C18 C21 N5 132.0(3) . . . . ?
C17 C18 C23 O1 52.1(4) . . . . ?
C17 C18 C23 N4 -128.0(3) . . . . ?
C19 C18 C21 O2 67.6(4) . . . . ?
C19 C18 C21 N5 -109.1(3) . . . . ?
C19 C18 C23 O1 -66.4(4) . . . . ?
C19 C18 C23 N4 113.5(3) . . . . ?
C21 N5 C22 O3 179.7(3) . . . . ?
C21 N5 C22 N4 -0.7(5) . . . . ?
C21 C18 C19 C20 57.3(4) . . . . ?
C21 C18 C23 O1 175.8(3) . . . . ?
C21 C18 C23 N4 -4.3(4) . . . . ?
C22 N4 C23 O1 176.6(3) . . . . ?
C22 N4 C23 C18 -3.4(4) . . . . ?
C22 N5 C21 O2 176.1(3) . . . . ?
C22 N5 C21 C18 -7.2(5) . . . . ?
C23 N4 C22 O3 -174.2(3) . . . . ?
C23 N4 C22 N5 6.2(4) . . . . ?
C23 C18 C19 C20 -64.5(4) . . . . ?
C23 C18 C21 O2 -174.3(3) . . . . ?
C23 C18 C21 N5 9.0(4) . . . . ?
C24 C25 C26 C27 -177.2(3) . . . . ?
C24 C25 C26 C29 65.0(4) . . . . ?
C24 C25 C26 C31 -58.1(4) . . . . ?
C25 C26 C27 C28 -177.0(3) . . . . ?
C25 C26 C29 O6 50.4(5) . . . . ?
C25 C26 C29 N7 -131.4(3) . . . . ?
C25 C26 C31 O4 -48.5(4) . . . . ?
C25 C26 C31 N6 132.8(3) . . . . ?
C27 C26 C29 O6 -68.0(4) . . . . ?
C27 C26 C29 N7 110.2(4) . . . . ?
C27 C26 C31 O4 71.1(4) . . . . ?
C27 C26 C31 N6 -107.6(4) . . . . ?
C29 N7 C30 O5 -171.3(3) . . . . ?
C29 N7 C30 N6 9.4(6) . . . . ?
C29 C26 C27 C28 -59.1(4) . . . . ?
C29 C26 C31 O4 -169.5(3) . . . . ?
C29 C26 C31 N6 11.8(4) . . . . ?
C30 N6 C31 O4 177.5(3) . . . . ?
C30 N6 C31 C26 -3.8(5) . . . . ?
C30 N7 C29 O6 178.1(3) . . . . ?
C30 N7 C29 C26 -0.2(5) . . . . ?
C31 N6 C30 O5 173.7(4) . . . . ?
C31 N6 C30 N7 -7.1(5) . . . . ?
C31 C26 C27 C28 62.6(4) . . . . ?
C31 C26 C29 O6 172.6(3) . . . . ?
C31 C26 C29 N7 -9.2(4) . . . . ?

_olex2_date_sample_data_collection 2014-12-05
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CCDC_1511705
_database_code_depnum_ccdc_archive 'CCDC 1511705'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
# start Validation Reply Form

_vrf_PLAT414_I                   
;
PROBLEM: Short Intra D-H..H-X       H2B    ..  H6B    ..   1.57 Ang.
 Short Intra D-H..H-X       H2B    ..  H7B     ..       1.57 Ang.
RESPONSE: 
These errors are generated because there is a large amount of disorder 
in the molecule. The short non-bonding contacts are due to the disorder 
of the central N atom of bis(2-pyridylmethyl)amine within the 
molecule. Short interactions between disordered moieties are to be 
expected. The H atoms of the components of the disordered N atom were 
found from the electron density map and the DFIX restraint was applied to them.
;
# end Validation Reply Form 

_audit_creation_date             2017-02-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H35 Cu N7 O6, H2 O'
_chemical_formula_sum            'C28 H37 Cu N7 O7'
_chemical_formula_weight         647.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H34 Cu N7 O7'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.9550(3)
_cell_length_b                   13.1256(4)
_cell_length_c                   19.5245(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.522(3)
_cell_angle_gamma                90
_cell_volume                     3029.90(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5738
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.9880
_cell_measurement_theta_min      3.5130
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.4047
_exptl_crystal_size_min          0.2679
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.958
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    8.00   56.00   1.0000    8.9350
omega____ theta____ kappa____ phi______ frames
    -       17.4380   57.0000    0.0000 48

#__ type_ start__ end____ width___ exp.time_
  2 omega   -8.00   62.00   1.0000    8.9350
omega____ theta____ kappa____ phi______ frames
    -       17.4380   37.0000 -180.0000 70

#__ type_ start__ end____ width___ exp.time_
  3 omega   38.00   82.00   1.0000    8.9350
omega____ theta____ kappa____ phi______ frames
    -       17.4380   57.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  4 omega  -77.00    2.00   1.0000    8.9350
omega____ theta____ kappa____ phi______ frames
    -      -19.4692  -57.0000 -120.0000 79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0144263000
_diffrn_orient_matrix_UB_12      0.0429547000
_diffrn_orient_matrix_UB_13      -0.0215301000
_diffrn_orient_matrix_UB_21      -0.0581885000
_diffrn_orient_matrix_UB_22      -0.0118629000
_diffrn_orient_matrix_UB_23      -0.0013952000
_diffrn_orient_matrix_UB_31      -0.0022283000
_diffrn_orient_matrix_UB_32      0.0305559000
_diffrn_orient_matrix_UB_33      0.0297345000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5108
_reflns_number_total             6192
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6192
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0402
_refine_ls_restrained_S_all      1.051
_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)+(0.0473P)²+1.6338P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1049
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N2A-H2A
 0.86 with sigma of 0.02
 N2B-H2B
 0.86 with sigma of 0.02
3. Others
 Sof(N2B)=1-FVAR(1)
 Sof(N2A)=FVAR(1)
 Fixed Sof: H2A(0.475) H2B(0.525)
4.a Free rotating group:
 O7W(H7WA,H7WB)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B)
4.c Aromatic/amide H refined with riding coordinates:
 N7(H7), C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12)
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.44363(2) 0.82861(2) 0.20009(2) 0.02890(10) Uani 1 1 d . . . . .
O1 O 0.44212(14) 0.93666(13) 0.06106(8) 0.0367(4) Uani 1 1 d . . . . .
O2 O 0.63315(15) 0.66777(13) 0.16276(9) 0.0385(4) Uani 1 1 d . . . . .
O3 O 0.74324(16) 0.83356(14) -0.03128(9) 0.0436(5) Uani 1 1 d . . . . .
O4 O 0.31258(14) 0.78617(15) 0.31712(9) 0.0410(4) Uani 1 1 d . . . . .
O5 O 0.55602(18) 0.69694(18) 0.50367(9) 0.0575(6) Uani 1 1 d . . . . .
O6 O 0.68311(14) 0.80922(14) 0.29856(9) 0.0369(4) Uani 1 1 d . . . . .
N1 N 0.48254(17) 0.97822(15) 0.21092(9) 0.0313(4) Uani 1 1 d . . . . .
N2A N 0.2865(4) 0.8957(4) 0.1891(6) 0.028(2) Uani 0.475(18) 1 d D . P A 1
H2A H 0.269(5) 0.889(4) 0.2296(16) 0.034(16) Uiso 0.475 1 d D . P . .
N2B N 0.2913(3) 0.8850(4) 0.1496(5) 0.0302(18) Uani 0.525(18) 1 d D . P A 2
H2B H 0.305(4) 0.884(3) 0.1080(13) 0.021(12) Uiso 0.525 1 d D . P . .
N3 N 0.35153(18) 0.70026(16) 0.17771(10) 0.0356(5) Uani 1 1 d . . . . .
N4 N 0.54021(16) 0.80754(14) 0.11864(9) 0.0264(4) Uani 1 1 d . . . . .
N5 N 0.59623(17) 0.88455(16) 0.01850(10) 0.0314(5) Uani 1 1 d . . . . .
H5 H 0.587(2) 0.933(2) -0.0057(14) 0.038(8) Uiso 1 1 d . . . . .
N6 N 0.49701(15) 0.79036(15) 0.30249(9) 0.0268(4) Uani 1 1 d . . . . .
N7 N 0.43766(16) 0.73489(16) 0.40739(9) 0.0344(5) Uani 1 1 d . . . . .
H7 H 0.381869 0.715500 0.427409 0.041 Uiso 1 1 calc R . . . .
C1 C 0.5868(2) 1.0161(2) 0.22899(13) 0.0398(6) Uani 1 1 d . . . . .
H1 H 0.646174 0.971265 0.242631 0.048 Uiso 1 1 calc R . . . .
C2 C 0.6094(3) 1.1186(2) 0.22811(14) 0.0454(7) Uani 1 1 d . . . . .
H2 H 0.682379 1.142800 0.241718 0.054 Uiso 1 1 calc R . . . .
C3 C 0.5218(3) 1.1850(2) 0.20671(14) 0.0471(7) Uani 1 1 d . . . . .
H3 H 0.535120 1.254661 0.204812 0.057 Uiso 1 1 calc R . . . .
C4 C 0.4150(2) 1.1468(2) 0.18827(14) 0.0424(6) Uani 1 1 d . . . . .
H4 H 0.354776 1.190559 0.174101 0.051 Uiso 1 1 calc R . . . .
C5 C 0.3971(2) 1.04308(19) 0.19082(11) 0.0318(5) Uani 1 1 d . . . . .
C6 C 0.2828(2) 0.9964(2) 0.16952(14) 0.0386(6) Uani 1 1 d . . . . .
H6A H 0.243174 1.033834 0.130445 0.046 Uiso 1 1 calc R . . A 2
H6B H 0.239116 1.001798 0.207449 0.046 Uiso 1 1 calc R . . A 2
C7 C 0.2007(2) 0.8226(2) 0.15350(16) 0.0508(7) Uani 1 1 d . . . . .
H7A H 0.132837 0.826448 0.175116 0.061 Uiso 1 1 calc R . . A 1
H7B H 0.180823 0.843032 0.105504 0.061 Uiso 1 1 calc R . . A 1
C8 C 0.2411(2) 0.7149(2) 0.15586(12) 0.0390(6) Uani 1 1 d . . . . .
C9 C 0.1691(3) 0.6338(3) 0.13714(14) 0.0528(8) Uani 1 1 d . . . . .
H9 H 0.092583 0.645020 0.121997 0.063 Uiso 1 1 calc R . . . .
C10 C 0.2119(3) 0.5370(3) 0.14121(16) 0.0610(9) Uani 1 1 d . . . . .
H10 H 0.164544 0.481776 0.128556 0.073 Uiso 1 1 calc R . . . .
C11 C 0.3247(3) 0.5214(2) 0.16395(16) 0.0552(8) Uani 1 1 d . . . . .
H11 H 0.354871 0.455970 0.167095 0.066 Uiso 1 1 calc R . . . .
C12 C 0.3916(3) 0.6044(2) 0.18188(15) 0.0465(7) Uani 1 1 d . . . . .
H12 H 0.468117 0.594187 0.197621 0.056 Uiso 1 1 calc R . . . .
C13 C 0.5281(3) 0.6391(3) -0.02056(19) 0.0692(10) Uani 1 1 d . . . . .
H13A H 0.516711 0.698657 -0.049293 0.104 Uiso 1 1 calc GR . . . .
H13B H 0.479909 0.642321 0.014569 0.104 Uiso 1 1 calc GR . . . .
H13C H 0.510192 0.579384 -0.048414 0.104 Uiso 1 1 calc GR . . . .
C14 C 0.6507(2) 0.6343(2) 0.01336(14) 0.0444(6) Uani 1 1 d . . . . .
H14A H 0.698162 0.627796 -0.022631 0.053 Uiso 1 1 calc R . . . .
H14B H 0.661191 0.573395 0.041731 0.053 Uiso 1 1 calc R . . . .
C15 C 0.69147(19) 0.72717(17) 0.05894(11) 0.0273(5) Uani 1 1 d . . . . .
C16 C 0.8155(2) 0.7136(2) 0.09088(13) 0.0353(6) Uani 1 1 d . . . . .
H16A H 0.822392 0.652917 0.119565 0.042 Uiso 1 1 calc R . . . .
H16B H 0.860566 0.703259 0.054024 0.042 Uiso 1 1 calc R . . . .
C17 C 0.8625(3) 0.8034(2) 0.13428(16) 0.0536(8) Uani 1 1 d . . . . .
H17A H 0.863283 0.862367 0.105246 0.080 Uiso 1 1 calc GR . . . .
H17B H 0.938113 0.788403 0.155868 0.080 Uiso 1 1 calc GR . . . .
H17C H 0.815796 0.816594 0.169297 0.080 Uiso 1 1 calc GR . . . .
C18 C 0.61946(18) 0.73364(17) 0.11765(11) 0.0271(5) Uani 1 1 d . . . . .
C19 C 0.52238(19) 0.87665(17) 0.06676(11) 0.0270(5) Uani 1 1 d . . . . .
C20 C 0.68149(19) 0.81931(18) 0.01215(11) 0.0284(5) Uani 1 1 d . . . . .
C21 C 0.6899(4) 0.5784(3) 0.3841(3) 0.1015(16) Uani 1 1 d . . . . .
H21A H 0.659394 0.588876 0.336293 0.152 Uiso 1 1 calc GR . . . .
H21B H 0.632026 0.551639 0.408279 0.152 Uiso 1 1 calc GR . . . .
H21C H 0.751590 0.531038 0.387298 0.152 Uiso 1 1 calc GR . . . .
C22 C 0.7316(3) 0.6784(3) 0.41608(17) 0.0603(9) Uani 1 1 d . . . . .
H22A H 0.794666 0.701777 0.394219 0.072 Uiso 1 1 calc R . . . .
H22B H 0.759077 0.667714 0.464831 0.072 Uiso 1 1 calc R . . . .
C23 C 0.64046(19) 0.76125(19) 0.40899(11) 0.0318(5) Uani 1 1 d . . . . .
C24 C 0.6880(2) 0.8590(2) 0.44652(14) 0.0500(7) Uani 1 1 d . . . . .
H24A H 0.716149 0.842316 0.494381 0.060 Uiso 1 1 calc R . . . .
H24B H 0.751609 0.882721 0.425265 0.060 Uiso 1 1 calc R . . . .
C25 C 0.6034(3) 0.9442(2) 0.4452(2) 0.0701(10) Uani 1 1 d . . . . .
H25A H 0.579265 0.964987 0.398129 0.105 Uiso 1 1 calc GR . . . .
H25B H 0.637706 1.000950 0.471328 0.105 Uiso 1 1 calc GR . . . .
H25C H 0.539173 0.921131 0.465119 0.105 Uiso 1 1 calc GR . . . .
C26 C 0.5425(2) 0.7269(2) 0.44409(12) 0.0348(6) Uani 1 1 d . . . . .
C27 C 0.41221(19) 0.77173(17) 0.34017(11) 0.0282(5) Uani 1 1 d . . . . .
C28 C 0.60706(19) 0.78735(17) 0.33203(11) 0.0269(5) Uani 1 1 d . . . . .
O7W O 0.6196(2) 0.4449(2) 0.18678(17) 0.0780(7) Uani 1 1 d . . . . .
H7WA H 0.677327 0.406685 0.188151 0.117 Uiso 1 1 d G . . . .
H7WB H 0.636104 0.504730 0.175071 0.117 Uiso 1 1 d G . . . .


_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 N1 2.022(2) . ?
Cu1 N2A 2.057(5) . ?
Cu1 N2B 2.074(5) . ?
Cu1 N3 2.024(2) . ?
Cu1 N4 2.1171(17) . ?
Cu1 N6 2.0686(18) . ?
O1 C19 1.234(3) . ?
O2 C18 1.228(3) . ?
O3 C20 1.218(3) . ?
O4 C27 1.224(3) . ?
O5 C26 1.216(3) . ?
O6 C28 1.230(3) . ?
N1 C1 1.340(3) . ?
N1 C5 1.343(3) . ?
N2A H2A 0.85(2) . ?
N2A C6 1.375(5) . ?
N2A C7 1.498(7) . ?
N2B H2B 0.850(19) . ?
N2B C6 1.520(7) . ?
N2B C7 1.369(5) . ?
N3 C8 1.340(3) . ?
N3 C12 1.345(4) . ?
N4 C18 1.358(3) . ?
N4 C19 1.353(3) . ?
N5 H5 0.79(3) . ?
N5 C19 1.387(3) . ?
N5 C20 1.351(3) . ?
N6 C27 1.360(3) . ?
N6 C28 1.357(3) . ?
N7 H7 0.8600 . ?
N7 C26 1.352(3) . ?
N7 C27 1.389(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.372(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.378(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.370(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(4) . ?
C5 C6 1.499(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.492(4) . ?
C8 C9 1.383(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.369(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.371(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.367(4) . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13 C14 1.517(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.545(3) . ?
C15 C16 1.532(3) . ?
C15 C18 1.534(3) . ?
C15 C20 1.510(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.511(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 C22 1.506(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.531(4) . ?
C23 C24 1.543(4) . ?
C23 C26 1.511(3) . ?
C23 C28 1.535(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.506(5) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
O7W H7WA 0.8503 . ?
O7W H7WB 0.8496 . ?

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
N1 Cu1 N2A 77.75(14) . . ?
N1 Cu1 N2B 82.84(15) . . ?
N1 Cu1 N3 160.06(9) . . ?
N1 Cu1 N4 93.60(7) . . ?
N1 Cu1 N6 95.82(8) . . ?
N2A Cu1 N4 124.7(3) . . ?
N2A Cu1 N6 110.5(3) . . ?
N2B Cu1 N4 103.2(3) . . ?
N3 Cu1 N2A 82.78(16) . . ?
N3 Cu1 N2B 77.49(15) . . ?
N3 Cu1 N4 93.96(8) . . ?
N3 Cu1 N6 94.97(8) . . ?
N6 Cu1 N2B 132.0(3) . . ?
N6 Cu1 N4 124.74(7) . . ?
C1 N1 Cu1 125.36(17) . . ?
C1 N1 C5 118.7(2) . . ?
C5 N1 Cu1 115.57(17) . . ?
Cu1 N2A H2A 102(4) . . ?
C6 N2A Cu1 115.6(3) . . ?
C6 N2A H2A 111(4) . . ?
C6 N2A C7 119.7(5) . . ?
C7 N2A Cu1 109.0(4) . . ?
C7 N2A H2A 97(4) . . ?
Cu1 N2B H2B 100(3) . . ?
C6 N2B Cu1 108.0(4) . . ?
C6 N2B H2B 107(3) . . ?
C7 N2B Cu1 114.0(3) . . ?
C7 N2B H2B 108(3) . . ?
C7 N2B C6 118.5(5) . . ?
C8 N3 Cu1 115.34(18) . . ?
C8 N3 C12 118.6(2) . . ?
C12 N3 Cu1 126.00(19) . . ?
C18 N4 Cu1 124.29(14) . . ?
C19 N4 Cu1 115.59(14) . . ?
C19 N4 C18 120.06(18) . . ?
C19 N5 H5 115(2) . . ?
C20 N5 H5 119(2) . . ?
C20 N5 C19 125.4(2) . . ?
C27 N6 Cu1 114.74(15) . . ?
C28 N6 Cu1 123.97(14) . . ?
C28 N6 C27 121.24(18) . . ?
C26 N7 H7 117.2 . . ?
C26 N7 C27 125.70(19) . . ?
C27 N7 H7 117.2 . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.5(3) . . ?
C2 C1 H1 118.8 . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C3 118.8(3) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.0(3) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.7(3) . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.4(2) . . ?
N1 C5 C6 116.4(2) . . ?
C4 C5 C6 122.2(2) . . ?
N2A C6 C5 109.0(3) . . ?
N2B C6 H6A 109.3 . . ?
N2B C6 H6B 109.3 . . ?
C5 C6 N2B 111.8(2) . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N2A C7 H7A 108.9 . . ?
N2A C7 H7B 108.9 . . ?
N2B C7 C8 108.3(3) . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 N2A 113.4(3) . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
N3 C8 C7 116.4(2) . . ?
N3 C8 C9 121.3(3) . . ?
C9 C8 C7 122.3(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 119.9(3) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.8 . . ?
C12 C11 C10 118.3(3) . . ?
C12 C11 H11 120.8 . . ?
N3 C12 C11 122.7(3) . . ?
N3 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
C13 C14 H14A 108.6 . . ?
C13 C14 H14B 108.6 . . ?
C13 C14 C15 114.8(2) . . ?
H14A C14 H14B 107.5 . . ?
C15 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C16 C15 C14 110.27(19) . . ?
C16 C15 C18 108.59(18) . . ?
C18 C15 C14 108.1(2) . . ?
C20 C15 C14 107.1(2) . . ?
C20 C15 C16 108.94(19) . . ?
C20 C15 C18 113.89(18) . . ?
C15 C16 H16A 108.9 . . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C17 C16 C15 113.2(2) . . ?
C17 C16 H16A 108.9 . . ?
C17 C16 H16B 108.9 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 N4 120.8(2) . . ?
O2 C18 C15 117.85(19) . . ?
N4 C18 C15 121.33(19) . . ?
O1 C19 N4 122.00(19) . . ?
O1 C19 N5 117.1(2) . . ?
N4 C19 N5 120.88(19) . . ?
O3 C20 N5 120.6(2) . . ?
O3 C20 C15 122.9(2) . . ?
N5 C20 C15 116.43(19) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
C21 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
C21 C22 C23 113.2(3) . . ?
H22A C22 H22B 107.8 . . ?
C23 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C22 C23 C24 109.9(2) . . ?
C22 C23 C28 109.0(2) . . ?
C26 C23 C22 109.6(2) . . ?
C26 C23 C24 106.8(2) . . ?
C26 C23 C28 113.82(19) . . ?
C28 C23 C24 107.7(2) . . ?
C23 C24 H24A 108.7 . . ?
C23 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 C23 114.2(2) . . ?
C25 C24 H24A 108.7 . . ?
C25 C24 H24B 108.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O5 C26 N7 120.9(2) . . ?
O5 C26 C23 121.9(2) . . ?
N7 C26 C23 117.14(19) . . ?
O4 C27 N6 122.4(2) . . ?
O4 C27 N7 117.8(2) . . ?
N6 C27 N7 119.8(2) . . ?
O6 C28 N6 120.9(2) . . ?
O6 C28 C23 117.8(2) . . ?
N6 C28 C23 121.18(18) . . ?
H7WA O7W H7WB 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2A H2A O4 0.85(2) 2.18(4) 2.860(10) 137(5) .
N2B H2B O1 0.850(19) 2.11(3) 2.761(8) 133(4) .
N5 H5 O1 0.79(3) 2.03(3) 2.814(3) 175(3) 3_675
N7 H7 O3 0.86 2.05 2.910(2) 176.1 4_576
O7W H7WA O6 0.85 2.09 2.935(3) 174.4 2_645
O7W H7WB O2 0.85 2.15 2.971(3) 161.5 .

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 N1 C1 C2 172.67(19) . . . . ?
Cu1 N1 C5 C4 -172.74(18) . . . . ?
Cu1 N1 C5 C6 5.5(2) . . . . ?
Cu1 N2A C6 C5 -24.6(8) . . . . ?
Cu1 N2A C7 C8 18.3(7) . . . . ?
Cu1 N2B C6 C5 25.0(5) . . . . ?
Cu1 N2B C7 C8 -31.8(7) . . . . ?
Cu1 N3 C8 C7 -2.2(3) . . . . ?
Cu1 N3 C8 C9 178.33(19) . . . . ?
Cu1 N3 C12 C11 -178.0(2) . . . . ?
Cu1 N4 C18 O2 6.2(3) . . . . ?
Cu1 N4 C18 C15 -176.11(15) . . . . ?
Cu1 N4 C19 O1 -12.1(3) . . . . ?
Cu1 N4 C19 N5 166.13(17) . . . . ?
Cu1 N6 C27 O4 -6.8(3) . . . . ?
Cu1 N6 C27 N7 173.16(17) . . . . ?
Cu1 N6 C28 O6 1.0(3) . . . . ?
Cu1 N6 C28 C23 178.23(16) . . . . ?
N1 C1 C2 C3 -1.2(4) . . . . ?
N1 C5 C6 N2A 12.4(6) . . . . ?
N1 C5 C6 N2B -20.9(5) . . . . ?
N2A C7 C8 N3 -11.2(6) . . . . ?
N2A C7 C8 C9 168.3(5) . . . . ?
N2B C7 C8 N3 22.4(6) . . . . ?
N2B C7 C8 C9 -158.1(5) . . . . ?
N3 C8 C9 C10 0.1(4) . . . . ?
C1 N1 C5 C4 0.3(3) . . . . ?
C1 N1 C5 C6 178.5(2) . . . . ?
C1 C2 C3 C4 1.2(4) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C3 C4 C5 N1 -0.2(4) . . . . ?
C3 C4 C5 C6 -178.3(2) . . . . ?
C4 C5 C6 N2A -169.3(6) . . . . ?
C4 C5 C6 N2B 157.3(4) . . . . ?
C5 N1 C1 C2 0.4(4) . . . . ?
C6 N2A C7 C8 154.5(6) . . . . ?
C6 N2B C7 C8 -160.7(5) . . . . ?
C7 N2A C6 C5 -158.2(6) . . . . ?
C7 N2B C6 C5 156.5(5) . . . . ?
C7 C8 C9 C10 -179.4(3) . . . . ?
C8 N3 C12 C11 0.8(4) . . . . ?
C8 C9 C10 C11 0.3(4) . . . . ?
C9 C10 C11 C12 -0.2(4) . . . . ?
C10 C11 C12 N3 -0.4(4) . . . . ?
C12 N3 C8 C7 178.9(2) . . . . ?
C12 N3 C8 C9 -0.6(4) . . . . ?
C13 C14 C15 C16 179.5(3) . . . . ?
C13 C14 C15 C18 60.9(3) . . . . ?
C13 C14 C15 C20 -62.1(3) . . . . ?
C14 C15 C16 C17 178.0(2) . . . . ?
C14 C15 C18 O2 69.8(3) . . . . ?
C14 C15 C18 N4 -107.9(2) . . . . ?
C14 C15 C20 O3 -70.6(3) . . . . ?
C14 C15 C20 N5 106.6(2) . . . . ?
C16 C15 C18 O2 -49.8(3) . . . . ?
C16 C15 C18 N4 132.5(2) . . . . ?
C16 C15 C20 O3 48.7(3) . . . . ?
C16 C15 C20 N5 -134.2(2) . . . . ?
C18 N4 C19 O1 170.7(2) . . . . ?
C18 N4 C19 N5 -11.1(3) . . . . ?
C18 C15 C16 C17 -63.8(3) . . . . ?
C18 C15 C20 O3 170.0(2) . . . . ?
C18 C15 C20 N5 -12.8(3) . . . . ?
C19 N4 C18 O2 -176.8(2) . . . . ?
C19 N4 C18 C15 0.8(3) . . . . ?
C19 N5 C20 O3 -178.8(2) . . . . ?
C19 N5 C20 C15 4.0(4) . . . . ?
C20 N5 C19 O1 -172.8(2) . . . . ?
C20 N5 C19 N4 8.8(4) . . . . ?
C20 C15 C16 C17 60.8(3) . . . . ?
C20 C15 C18 O2 -171.4(2) . . . . ?
C20 C15 C18 N4 10.9(3) . . . . ?
C21 C22 C23 C24 176.8(3) . . . . ?
C21 C22 C23 C26 59.8(3) . . . . ?
C21 C22 C23 C28 -65.4(3) . . . . ?
C22 C23 C24 C25 -177.6(2) . . . . ?
C22 C23 C26 O5 52.6(3) . . . . ?
C22 C23 C26 N7 -130.2(3) . . . . ?
C22 C23 C28 O6 -52.4(3) . . . . ?
C22 C23 C28 N6 130.3(2) . . . . ?
C24 C23 C26 O5 -66.4(3) . . . . ?
C24 C23 C26 N7 110.8(3) . . . . ?
C24 C23 C28 O6 66.8(3) . . . . ?
C24 C23 C28 N6 -110.6(2) . . . . ?
C26 N7 C27 O4 -171.1(2) . . . . ?
C26 N7 C27 N6 9.0(4) . . . . ?
C26 C23 C24 C25 -58.8(3) . . . . ?
C26 C23 C28 O6 -175.1(2) . . . . ?
C26 C23 C28 N6 7.6(3) . . . . ?
C27 N6 C28 O6 -176.3(2) . . . . ?
C27 N6 C28 C23 0.9(3) . . . . ?
C27 N7 C26 O5 177.4(3) . . . . ?
C27 N7 C26 C23 0.2(4) . . . . ?
C28 N6 C27 O4 170.8(2) . . . . ?
C28 N6 C27 N7 -9.3(3) . . . . ?
C28 C23 C24 C25 63.8(3) . . . . ?
C28 C23 C26 O5 175.0(2) . . . . ?
C28 C23 C26 N7 -7.9(3) . . . . ?

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
-15 6 13 0.1813 -15.0004 5.9986 13.0229 0.1937 0.7835 0.6039
14 4 9 0.1619 14.0047 4.0107 8.9710 -0.2229 -0.8750 0.3581
-12 -6 -14 0.1873 -12.0055 -6.0119 -13.9729 0.2158 0.7894 -0.5724
4 -10 -23 0.2086 3.9958 -10.0083 -22.9991 0.0076 -0.0817 -0.9986
-3 -1 27 0.2370 -2.9863 -0.9891 26.9989 -0.5807 0.1478 0.7792
0 19 0 0.2233 -0.0127 18.9994 -0.0045 0.8164 -0.2246 0.5804
-1 -17 12 0.2029 -0.9828 -16.9944 12.0028 -0.9742 0.2420 -0.1602
10 14 3 0.1372 9.9942 14.0057 2.9775 0.3933 -0.7518 0.4942
-12 -12 6 0.1132 -11.9913 -12.0026 6.0234 -0.4723 0.8317 -0.1609
13 6 -18 0.2327 12.9895 5.9978 -18.0207 0.4582 -0.8018 -0.3815
-7 16 10 0.1987 -7.0070 16.0007 10.0066 0.5729 0.2040 0.8021
-9 16 -1 0.2287 -9.0130 15.9947 -0.9869 0.8383 0.3361 0.4795
-12 12 12 0.1670 -12.0043 11.9993 12.0162 0.4299 0.5394 0.7507
15 -8 2 0.1845 15.0094 -7.9916 1.9738 -0.6023 -0.7813 -0.2189
12 12 0 0.1157 11.9944 12.0053 -0.0249 0.3432 -0.8403 0.3394
-14 -10 8 0.1132 -13.9921 -10.0027 8.0261 -0.4006 0.9216 -0.0358
1 1 -27 0.2965 0.9859 0.9881 -26.9952 0.6094 -0.0314 -0.7747
-1 -1 27 0.2337 -0.9859 -0.9881 26.9952 -0.6094 0.0314 0.7747
-13 12 0 0.1974 -13.0106 11.9934 0.0211 0.7024 0.6148 0.3961
13 -12 2 0.1706 13.0116 -11.9925 1.9784 -0.7454 -0.6176 -0.3366
-11 -11 15 0.1490 -10.9873 -10.9980 15.0190 -0.6373 0.7488 0.1350
13 0 14 0.1799 13.0097 0.0126 13.9725 -0.4880 -0.7767 0.3869
1 -5 -26 0.2255 0.9904 -5.0112 -25.9940 0.3301 0.0381 -0.9282
12 -13 4 0.1653 12.0131 -12.9920 3.9800 -0.8171 -0.5505 -0.3054

_olex2_date_sample_data_collection 2015-01-22
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CCDC_1511703
_database_code_depnum_ccdc_archive 'CCDC 1511703'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
_audit_creation_date             2017-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H33 Cu N7 O6, H2 O'
_chemical_formula_sum            'C31 H35 Cu N7 O7'
_chemical_formula_weight         681.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         ' C31 H35 Cu N7 O7'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6201(7)
_cell_length_b                   12.9945(7)
_cell_length_c                   19.5366(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.576(5)
_cell_angle_gamma                90
_cell_volume                     3182.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5762
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.9330
_cell_measurement_theta_min      3.1850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 17 10 0.1357
-4 18 1 0.1322
4 -18 3 0.0614
-5 10 -20 0.1810
-17 -3 10 0.0756
-9 -7 -20 0.1318
-13 -13 5 0.0521
14 -12 1 0.0557
-10 13 14 0.1336
-10 2 -21 0.1364
8 0 23 0.1781
-1 -7 -25 0.1171
17 4 0 0.0809
12 6 17 0.1396
12 13 1 0.0719
-15 11 3 0.1067

_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.147
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9959 16.9899 9.9967 0.1897 0.7720 0.6031
-3.9975 17.9878 0.9999 0.2028 0.9448 0.2833
3.9987 -17.9873 2.9993 -0.2409 -0.9764 -0.1459
-5.0033 9.9903 -19.9937 0.1766 0.7634 -0.5870
-16.9867 -2.9980 10.0112 -0.9692 0.2498 0.0607
-9.0007 -6.9987 -19.9879 -0.3932 0.0782 -0.9285
-12.9905 -12.9917 5.0109 -0.9552 -0.2892 -0.2251
13.9920 -11.9908 0.9912 0.3869 -0.9557 0.0233
-9.9898 12.9925 14.0025 -0.3175 0.7740 0.5638
-10.0005 1.9951 -20.9884 -0.2300 0.5349 -0.8247
8.0023 0.0037 22.9892 0.1607 -0.4018 0.8998
-1.0070 -6.9987 -24.9929 0.0342 -0.1031 -0.9910
16.9897 3.9986 -0.0135 0.8963 -0.2818 0.2998
11.9980 5.9992 16.9865 0.5418 -0.1841 0.8495
11.9930 12.9924 0.9886 0.8506 0.2695 0.4177
-14.9902 10.9920 3.0089 -0.4948 0.9049 0.0836

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14785
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.135
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  72.00   1.00   75.19    --   17.28  77.00 -90.00   82
  2  ω     38.00  87.00   1.00   75.19    --   17.28 178.00-180.00   49
  3  ω    -73.00 -35.00   1.00   75.19    --  -19.31-178.00 -90.00   38
  4  ω    -40.00  37.00   1.00   75.19    --  -19.31  57.00-180.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0474866000
_diffrn_orient_matrix_UB_12      0.0223596000
_diffrn_orient_matrix_UB_13      -0.0095411000
_diffrn_orient_matrix_UB_21      -0.0276118000
_diffrn_orient_matrix_UB_22      0.0468286000
_diffrn_orient_matrix_UB_23      -0.0078756000
_diffrn_orient_matrix_UB_31      0.0137003000
_diffrn_orient_matrix_UB_32      0.0168854000
_diffrn_orient_matrix_UB_33      0.0343697000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5022
_reflns_number_total             6506
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0378
_refine_ls_restrained_S_all      1.011
_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)+(0.0409P)²+1.5852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0959
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O7W(H7WA,H7WB)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C25(H25A,H25B), C27(H27A,H27B)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N7(H7), C1(H1), C2(H2), C3(H3), C4(H4), C7(H7A), C8(H8), C9(H9),
 C12(H12), C13(H13), C14(H14), C15(H15)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.53404(2) 0.32405(2) 0.29660(2) 0.02881(9) Uani 1 1 d . . . . .
O1 O 0.67639(12) 0.27967(13) 0.18316(8) 0.0365(4) Uani 1 1 d . . . . .
O2 O 0.46172(16) 0.2439(2) -0.01234(9) 0.0726(7) Uani 1 1 d . . . . .
O3 O 0.32443(13) 0.31818(14) 0.19692(8) 0.0419(4) Uani 1 1 d . . . . .
O4 O 0.36611(14) 0.16838(13) 0.33660(9) 0.0437(4) Uani 1 1 d . . . . .
O5 O 0.54265(13) 0.44072(14) 0.43454(8) 0.0433(4) Uani 1 1 d . . . . .
O6 O 0.25949(15) 0.33219(15) 0.53319(9) 0.0529(5) Uani 1 1 d . . . . .
N1 N 0.62574(15) 0.19415(15) 0.31784(9) 0.0328(4) Uani 1 1 d . . . . .
N2 N 0.67932(14) 0.38480(14) 0.32277(9) 0.0280(4) Uani 1 1 d . . . . .
N3 N 0.50350(15) 0.48130(15) 0.28797(9) 0.0311(4) Uani 1 1 d . . . . .
N4 N 0.49998(14) 0.29341(14) 0.19443(9) 0.0279(4) Uani 1 1 d . . . . .
N5 N 0.56396(15) 0.24973(16) 0.08856(9) 0.0361(5) Uani 1 1 d . . . . .
H5 H 0.616439 0.225640 0.069066 0.043 Uiso 1 1 calc R . . . .
N6 N 0.45103(15) 0.30991(14) 0.37945(9) 0.0292(4) Uani 1 1 d . . . . .
N7 N 0.39988(15) 0.38493(15) 0.48181(9) 0.0349(5) Uani 1 1 d . . . . .
H7 H 0.410811 0.433241 0.511880 0.042 Uiso 1 1 calc R . . . .
C1 C 0.5919(2) 0.0968(2) 0.31326(13) 0.0440(6) Uani 1 1 d . . . . .
H1 H 0.520164 0.084248 0.299146 0.053 Uiso 1 1 calc R . . . .
C2 C 0.6584(3) 0.0146(2) 0.32848(15) 0.0553(8) Uani 1 1 d . . . . .
H2 H 0.632271 -0.052293 0.324956 0.066 Uiso 1 1 calc R . . . .
C3 C 0.7638(3) 0.0327(2) 0.34891(15) 0.0578(8) Uani 1 1 d . . . . .
H3 H 0.810269 -0.021993 0.359551 0.069 Uiso 1 1 calc R . . . .
C4 C 0.8011(2) 0.1322(2) 0.35372(13) 0.0482(7) Uani 1 1 d . . . . .
H4 H 0.872682 0.145446 0.367691 0.058 Uiso 1 1 calc R . . . .
C5 C 0.73051(19) 0.21210(19) 0.33748(11) 0.0335(5) Uani 1 1 d . . . . .
C6 C 0.76134(18) 0.32164(19) 0.33975(11) 0.0322(5) Uani 1 1 d . . . . .
C7 C 0.8623(2) 0.3613(2) 0.35776(13) 0.0465(7) Uani 1 1 d . . . . .
H7A H 0.920113 0.318003 0.369739 0.056 Uiso 1 1 calc R . . . .
C8 C 0.8751(2) 0.4658(2) 0.35753(15) 0.0537(7) Uani 1 1 d . . . . .
H8 H 0.942578 0.493797 0.369183 0.064 Uiso 1 1 calc R . . . .
C9 C 0.7896(2) 0.5302(2) 0.34031(13) 0.0435(6) Uani 1 1 d . . . . .
H9 H 0.798334 0.601238 0.340316 0.052 Uiso 1 1 calc R . . . .
C10 C 0.69072(18) 0.48632(18) 0.32306(11) 0.0304(5) Uani 1 1 d . . . . .
C11 C 0.58944(18) 0.54199(17) 0.30530(11) 0.0309(5) Uani 1 1 d . . . . .
C12 C 0.5798(2) 0.64765(19) 0.30859(13) 0.0421(6) Uani 1 1 d . . . . .
H12 H 0.639623 0.688600 0.320004 0.051 Uiso 1 1 calc R . . . .
C13 C 0.4801(2) 0.6918(2) 0.29471(15) 0.0511(7) Uani 1 1 d . . . . .
H13 H 0.472155 0.762804 0.296763 0.061 Uiso 1 1 calc R . . . .
C14 C 0.3931(2) 0.6302(2) 0.27792(14) 0.0475(7) Uani 1 1 d . . . . .
H14 H 0.325361 0.658675 0.268639 0.057 Uiso 1 1 calc R . . . .
C15 C 0.4077(2) 0.5251(2) 0.27499(13) 0.0404(6) Uani 1 1 d . . . . .
H15 H 0.348485 0.483302 0.263557 0.048 Uiso 1 1 calc R . . . .
C16 C 0.2968(4) 0.1165(3) 0.0831(3) 0.1092(16) Uani 1 1 d . . . . .
H16A H 0.351796 0.088472 0.058552 0.164 Uiso 1 1 calc GR . . . .
H16B H 0.231749 0.078970 0.071219 0.164 Uiso 1 1 calc GR . . . .
H16C H 0.317793 0.110875 0.131804 0.164 Uiso 1 1 calc GR . . . .
C17 C 0.2797(2) 0.2273(3) 0.06422(17) 0.0761(11) Uani 1 1 d . . . . .
H17A H 0.219706 0.253072 0.086068 0.091 Uiso 1 1 calc R . . . .
H17B H 0.261012 0.232226 0.014760 0.091 Uiso 1 1 calc R . . . .
C18 C 0.37609(19) 0.2957(2) 0.08492(12) 0.0414(6) Uani 1 1 d . . . . .
C19 C 0.3534(3) 0.4086(3) 0.05949(15) 0.0660(10) Uani 1 1 d . . . . .
H19A H 0.338808 0.408159 0.009651 0.079 Uiso 1 1 calc R . . . .
H19B H 0.289696 0.433094 0.077793 0.079 Uiso 1 1 calc R . . . .
C20 C 0.4430(3) 0.4833(2) 0.07990(18) 0.0756(10) Uani 1 1 d . . . . .
H20A H 0.425016 0.549403 0.059979 0.113 Uiso 1 1 calc GR . . . .
H20B H 0.507226 0.458580 0.063523 0.113 Uiso 1 1 calc GR . . . .
H20C H 0.453772 0.489271 0.129179 0.113 Uiso 1 1 calc GR . . . .
C21 C 0.58379(18) 0.27563(16) 0.15780(10) 0.0270(5) Uani 1 1 d . . . . .
C22 C 0.4694(2) 0.2592(2) 0.04931(12) 0.0442(6) Uani 1 1 d . . . . .
C23 C 0.39900(18) 0.30045(17) 0.16338(11) 0.0308(5) Uani 1 1 d . . . . .
C24 C 0.1639(3) 0.3279(4) 0.3594(2) 0.0923(14) Uani 1 1 d . . . . .
H24A H 0.212652 0.332513 0.325222 0.138 Uiso 1 1 calc GR . . . .
H24B H 0.171110 0.387725 0.388327 0.138 Uiso 1 1 calc GR . . . .
H24C H 0.092187 0.323807 0.337032 0.138 Uiso 1 1 calc GR . . . .
C25 C 0.1886(2) 0.2330(3) 0.40260(17) 0.0719(11) Uani 1 1 d . . . . .
H25A H 0.177090 0.172582 0.373499 0.086 Uiso 1 1 calc R . . . .
H25B H 0.139617 0.229227 0.437361 0.086 Uiso 1 1 calc R . . . .
C26 C 0.3036(2) 0.2316(2) 0.43828(12) 0.0418(6) Uani 1 1 d . . . . .
C27 C 0.3289(4) 0.1328(2) 0.48080(17) 0.0782(12) Uani 1 1 d . . . . .
H27A H 0.277932 0.126413 0.514179 0.094 Uiso 1 1 calc R . . . .
H27B H 0.319354 0.073897 0.450182 0.094 Uiso 1 1 calc R . . . .
C28 C 0.4399(4) 0.1295(3) 0.5184(2) 0.1061(16) Uani 1 1 d . . . . .
H28A H 0.491062 0.135318 0.485803 0.159 Uiso 1 1 calc GR . . . .
H28B H 0.450338 0.065586 0.542830 0.159 Uiso 1 1 calc GR . . . .
H28C H 0.449114 0.185660 0.550472 0.159 Uiso 1 1 calc GR . . . .
C29 C 0.31750(19) 0.32049(19) 0.48811(11) 0.0369(6) Uani 1 1 d . . . . .
C30 C 0.46860(18) 0.38013(18) 0.43104(11) 0.0310(5) Uani 1 1 d . . . . .
C31 C 0.37700(19) 0.23521(18) 0.38118(11) 0.0324(5) Uani 1 1 d . . . . .
O7W O 0.1285(2) 0.4423(2) 0.1821(2) 0.0994(9) Uani 1 1 d . . . . .
H7WA H 0.141320 0.505527 0.175326 0.149 Uiso 1 1 d G . . . .
H7WB H 0.186148 0.408144 0.183658 0.149 Uiso 1 1 d G . . . .


_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 N1 2.0618(19) . ?
Cu1 N2 2.0077(18) . ?
Cu1 N3 2.0826(19) . ?
Cu1 N4 2.0325(17) . ?
Cu1 N6 2.0344(17) . ?
O1 C21 1.217(3) . ?
O2 C22 1.213(3) . ?
O3 C23 1.228(3) . ?
O4 C31 1.226(3) . ?
O5 C30 1.218(3) . ?
O6 C29 1.218(3) . ?
N1 C1 1.335(3) . ?
N1 C5 1.354(3) . ?
N2 C6 1.333(3) . ?
N2 C10 1.327(3) . ?
N3 C11 1.352(3) . ?
N3 C15 1.335(3) . ?
N4 C21 1.363(3) . ?
N4 C23 1.350(3) . ?
N5 H5 0.8600 . ?
N5 C21 1.388(3) . ?
N5 C22 1.348(3) . ?
N6 C30 1.359(3) . ?
N6 C31 1.350(3) . ?
N7 H7 0.8600 . ?
N7 C29 1.351(3) . ?
N7 C30 1.392(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.370(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.364(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.375(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.381(3) . ?
C5 C6 1.475(3) . ?
C6 C7 1.382(3) . ?
C7 H7A 0.9300 . ?
C7 C8 1.368(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.376(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.378(3) . ?
C10 C11 1.475(3) . ?
C11 C12 1.381(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.381(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.367(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.380(4) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C17 1.496(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.524(4) . ?
C18 C19 1.565(4) . ?
C18 C22 1.511(3) . ?
C18 C23 1.528(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.508(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 C25 1.507(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.537(4) . ?
C26 C27 1.543(4) . ?
C26 C29 1.508(3) . ?
C26 C31 1.530(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.507(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O7W H7WA 0.8508 . ?
O7W H7WB 0.8493 . ?

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
N1 Cu1 N3 156.06(8) . . ?
N2 Cu1 N1 78.20(8) . . ?
N2 Cu1 N3 77.88(7) . . ?
N2 Cu1 N4 114.29(7) . . ?
N2 Cu1 N6 111.80(7) . . ?
N4 Cu1 N1 95.05(7) . . ?
N4 Cu1 N3 95.53(7) . . ?
N4 Cu1 N6 133.89(7) . . ?
N6 Cu1 N1 95.41(7) . . ?
N6 Cu1 N3 92.62(7) . . ?
C1 N1 Cu1 126.47(18) . . ?
C1 N1 C5 118.5(2) . . ?
C5 N1 Cu1 115.04(15) . . ?
C6 N2 Cu1 118.81(15) . . ?
C10 N2 Cu1 119.17(15) . . ?
C10 N2 C6 122.0(2) . . ?
C11 N3 Cu1 114.60(15) . . ?
C15 N3 Cu1 126.11(17) . . ?
C15 N3 C11 118.8(2) . . ?
C21 N4 Cu1 117.35(14) . . ?
C23 N4 Cu1 120.69(14) . . ?
C23 N4 C21 121.66(18) . . ?
C21 N5 H5 117.2 . . ?
C22 N5 H5 117.2 . . ?
C22 N5 C21 125.53(19) . . ?
C30 N6 Cu1 118.32(14) . . ?
C31 N6 Cu1 120.37(14) . . ?
C31 N6 C30 121.24(18) . . ?
C29 N7 H7 117.1 . . ?
C29 N7 C30 125.85(19) . . ?
C30 N7 H7 117.1 . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.7(3) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.8(3) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.8(3) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 121.2(2) . . ?
N1 C5 C6 114.9(2) . . ?
C4 C5 C6 123.9(2) . . ?
N2 C6 C5 113.1(2) . . ?
N2 C6 C7 120.0(2) . . ?
C7 C6 C5 126.9(2) . . ?
C6 C7 H7A 120.8 . . ?
C8 C7 C6 118.4(3) . . ?
C8 C7 H7A 120.8 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C8 C9 H9 120.9 . . ?
C8 C9 C10 118.1(3) . . ?
C10 C9 H9 120.9 . . ?
N2 C10 C9 120.4(2) . . ?
N2 C10 C11 113.3(2) . . ?
C9 C10 C11 126.2(2) . . ?
N3 C11 C10 114.9(2) . . ?
N3 C11 C12 121.3(2) . . ?
C12 C11 C10 123.8(2) . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.1(3) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.5(2) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.8(3) . . ?
C15 C14 H14 120.6 . . ?
N3 C15 C14 122.4(2) . . ?
N3 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
C16 C17 H17A 108.7 . . ?
C16 C17 H17B 108.7 . . ?
C16 C17 C18 114.0(3) . . ?
H17A C17 H17B 107.6 . . ?
C18 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
C17 C18 C19 110.5(3) . . ?
C17 C18 C23 110.1(2) . . ?
C22 C18 C17 109.6(2) . . ?
C22 C18 C19 105.8(2) . . ?
C22 C18 C23 114.00(19) . . ?
C23 C18 C19 106.7(2) . . ?
C18 C19 H19A 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 C18 114.5(2) . . ?
C20 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C21 N4 123.06(19) . . ?
O1 C21 N5 117.69(19) . . ?
N4 C21 N5 119.24(19) . . ?
O2 C22 N5 121.0(2) . . ?
O2 C22 C18 122.1(2) . . ?
N5 C22 C18 116.9(2) . . ?
O3 C23 N4 121.0(2) . . ?
O3 C23 C18 118.3(2) . . ?
N4 C23 C18 120.55(19) . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
C24 C25 H25A 109.0 . . ?
C24 C25 H25B 109.0 . . ?
C24 C25 C26 112.8(3) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
C25 C26 C27 112.3(3) . . ?
C29 C26 C25 108.5(2) . . ?
C29 C26 C27 106.8(2) . . ?
C29 C26 C31 114.33(19) . . ?
C31 C26 C25 106.8(2) . . ?
C31 C26 C27 108.3(2) . . ?
C26 C27 H27A 108.7 . . ?
C26 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C28 C27 C26 114.1(3) . . ?
C28 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O6 C29 N7 121.4(2) . . ?
O6 C29 C26 121.9(2) . . ?
N7 C29 C26 116.72(19) . . ?
O5 C30 N6 122.31(19) . . ?
O5 C30 N7 117.9(2) . . ?
N6 C30 N7 119.79(19) . . ?
O4 C31 N6 120.8(2) . . ?
O4 C31 C26 117.9(2) . . ?
N6 C31 C26 121.24(19) . . ?
H7WA O7W H7WB 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5 O6 0.86 2.15 3.001(2) 172.5 4_665
N7 H7 O5 0.86 2.00 2.839(2) 166.4 3_666
O7W H7WA O4 0.85 2.13 2.962(3) 165.9 2
O7W H7WB O3 0.85 2.09 2.938(3) 174.3 .

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 N1 C1 C2 -179.92(19) . . . . ?
Cu1 N1 C5 C4 179.58(17) . . . . ?
Cu1 N1 C5 C6 -0.5(2) . . . . ?
Cu1 N2 C6 C5 -0.9(2) . . . . ?
Cu1 N2 C6 C7 179.78(17) . . . . ?
Cu1 N2 C10 C9 -179.52(16) . . . . ?
Cu1 N2 C10 C11 1.9(2) . . . . ?
Cu1 N3 C11 C10 3.6(2) . . . . ?
Cu1 N3 C11 C12 -173.69(17) . . . . ?
Cu1 N3 C15 C14 172.33(19) . . . . ?
Cu1 N4 C21 O1 -1.7(3) . . . . ?
Cu1 N4 C21 N5 177.06(15) . . . . ?
Cu1 N4 C23 O3 -5.3(3) . . . . ?
Cu1 N4 C23 C18 169.42(17) . . . . ?
Cu1 N6 C30 O5 -11.5(3) . . . . ?
Cu1 N6 C30 N7 167.87(17) . . . . ?
Cu1 N6 C31 O4 7.6(3) . . . . ?
Cu1 N6 C31 C26 -171.96(18) . . . . ?
N1 C1 C2 C3 -0.3(4) . . . . ?
N1 C5 C6 N2 0.9(3) . . . . ?
N1 C5 C6 C7 -179.8(2) . . . . ?
N2 C6 C7 C8 -0.1(4) . . . . ?
N2 C10 C11 N3 -3.6(3) . . . . ?
N2 C10 C11 C12 173.6(2) . . . . ?
N3 C11 C12 C13 0.8(4) . . . . ?
C1 N1 C5 C4 -1.2(3) . . . . ?
C1 N1 C5 C6 178.76(19) . . . . ?
C1 C2 C3 C4 -0.1(4) . . . . ?
C2 C3 C4 C5 -0.1(4) . . . . ?
C3 C4 C5 N1 0.8(4) . . . . ?
C3 C4 C5 C6 -179.1(2) . . . . ?
C4 C5 C6 N2 -179.2(2) . . . . ?
C4 C5 C6 C7 0.1(4) . . . . ?
C5 N1 C1 C2 0.9(4) . . . . ?
C5 C6 C7 C8 -179.3(2) . . . . ?
C6 N2 C10 C9 0.9(3) . . . . ?
C6 N2 C10 C11 -177.73(18) . . . . ?
C6 C7 C8 C9 0.5(4) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C8 C9 C10 N2 -0.5(3) . . . . ?
C8 C9 C10 C11 178.0(2) . . . . ?
C9 C10 C11 N3 177.9(2) . . . . ?
C9 C10 C11 C12 -4.9(3) . . . . ?
C10 N2 C6 C5 178.69(18) . . . . ?
C10 N2 C6 C7 -0.6(3) . . . . ?
C10 C11 C12 C13 -176.3(2) . . . . ?
C11 N3 C15 C14 0.7(3) . . . . ?
C11 C12 C13 C14 -0.1(4) . . . . ?
C12 C13 C14 C15 -0.3(4) . . . . ?
C13 C14 C15 N3 0.0(4) . . . . ?
C15 N3 C11 C10 176.22(19) . . . . ?
C15 N3 C11 C12 -1.1(3) . . . . ?
C16 C17 C18 C19 176.8(3) . . . . ?
C16 C17 C18 C22 60.5(4) . . . . ?
C16 C17 C18 C23 -65.6(4) . . . . ?
C17 C18 C19 C20 177.8(3) . . . . ?
C17 C18 C22 O2 50.6(4) . . . . ?
C17 C18 C22 N5 -133.1(3) . . . . ?
C17 C18 C23 O3 -48.4(3) . . . . ?
C17 C18 C23 N4 136.8(2) . . . . ?
C19 C18 C22 O2 -68.6(4) . . . . ?
C19 C18 C22 N5 107.7(3) . . . . ?
C19 C18 C23 O3 71.6(3) . . . . ?
C19 C18 C23 N4 -103.3(3) . . . . ?
C21 N4 C23 O3 -178.8(2) . . . . ?
C21 N4 C23 C18 -4.1(3) . . . . ?
C21 N5 C22 O2 172.9(3) . . . . ?
C21 N5 C22 C18 -3.5(4) . . . . ?
C22 N5 C21 O1 -167.6(2) . . . . ?
C22 N5 C21 N4 13.6(4) . . . . ?
C22 C18 C19 C20 -63.6(3) . . . . ?
C22 C18 C23 O3 -172.0(2) . . . . ?
C22 C18 C23 N4 13.1(3) . . . . ?
C23 N4 C21 O1 172.0(2) . . . . ?
C23 N4 C21 N5 -9.3(3) . . . . ?
C23 C18 C19 C20 58.1(3) . . . . ?
C23 C18 C22 O2 174.5(3) . . . . ?
C23 C18 C22 N5 -9.2(4) . . . . ?
C24 C25 C26 C27 -178.5(3) . . . . ?
C24 C25 C26 C29 63.7(3) . . . . ?
C24 C25 C26 C31 -60.0(3) . . . . ?
C25 C26 C27 C28 -178.3(3) . . . . ?
C25 C26 C29 O6 55.5(3) . . . . ?
C25 C26 C29 N7 -126.6(3) . . . . ?
C25 C26 C31 O4 -56.1(3) . . . . ?
C25 C26 C31 N6 123.4(3) . . . . ?
C27 C26 C29 O6 -65.8(3) . . . . ?
C27 C26 C29 N7 112.1(3) . . . . ?
C27 C26 C31 O4 65.0(3) . . . . ?
C27 C26 C31 N6 -115.4(3) . . . . ?
C29 N7 C30 O5 -176.2(2) . . . . ?
C29 N7 C30 N6 4.4(4) . . . . ?
C29 C26 C27 C28 -59.5(3) . . . . ?
C29 C26 C31 O4 -176.1(2) . . . . ?
C29 C26 C31 N6 3.4(4) . . . . ?
C30 N6 C31 O4 -175.5(2) . . . . ?
C30 N6 C31 C26 5.0(3) . . . . ?
C30 N7 C29 O6 -177.9(2) . . . . ?
C30 N7 C29 C26 4.2(4) . . . . ?
C31 N6 C30 O5 171.5(2) . . . . ?
C31 N6 C30 N7 -9.1(3) . . . . ?
C31 C26 C27 C28 64.1(3) . . . . ?
C31 C26 C29 O6 174.5(2) . . . . ?
C31 C26 C29 N7 -7.6(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.850
####################################################################### 
# 
# 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_CCDC_1511707
_database_code_depnum_ccdc_archive 'CCDC 1511707'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;


# start Validation Reply Form

_vrf_PLAT771_III                 
;
PROBLEM: 
Suspect N-H Bond in CIF:   N2A    --  H2B     ..       1.51 Ang.  
Suspect N-H Bond in CIF:   N2B    --  H2A     ..       1.51 Ang. 
RESPONSE: 
These errors are generated because there is a large amount of disorder 
in the molecule. The short non-bonding contacts are due to the disorder 
of the central N atom of bis(2-pyridylmethyl)amine within the 
molecule. Short interactions between disordered moieties are to be 
expected. The H atoms of the components of the disordered N atom were 
found from the electron density map and the DFIX restraint was applied to them
with 0.5 occupancies each one.
;
# end Validation Reply Form 

_audit_creation_date             2017-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H35 N7 O6 Zn, H2 O'
_chemical_formula_sum            'C28 H37 N7 O7 Zn'
_chemical_formula_weight         649.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H37 N7 O7 Zn'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.0293(5)
_cell_length_b                   13.1743(6)
_cell_length_c                   19.3947(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.840(4)
_cell_angle_gamma                90
_cell_volume                     3044.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4082
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9730
_cell_measurement_theta_min      3.3970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
13 -12 1 0.0205
-14 11 3 0.0685
-11 -1 23 0.1096
9 4 -25 0.1383
8 16 4 0.0757
-8 -16 -3 0.0856
-1 -12 21 0.0956
16 6 3 0.0574
-16 -6 -4 0.1001
-13 -11 11 0.0846
14 1 12 0.0653
0 -19 -1 0.0596
0 -17 11 0.0641
0 4 -27 0.1634
4 -18 -2 0.0478
16 -5 1 0.0322
12 -9 12 0.0429
-16 -2 12 0.0850
13 12 4 0.0631
4 14 16 0.1018

_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.11
loop_
_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
12.9263 -11.9761 1.0256 0.1997 0.8646 0.4823
-13.9251 10.9764 2.9489 -0.2155 -0.9308 -0.3376
-10.9641 -1.0081 22.8409 -0.1758 -0.7311 0.6520
8.9774 4.0024 -24.8339 0.1334 0.5941 -0.8171
7.9443 15.9204 4.0245 -0.9272 0.1961 -0.3151
-7.9455 -15.9217 -3.0297 0.9072 -0.2023 0.3453
-1.0169 -11.9794 20.8731 0.1074 -0.0248 0.9934
15.9016 5.9472 3.0458 -0.6622 0.7735 0.0128
-15.9003 -5.9459 -4.0405 0.6821 -0.7672 -0.0429
-12.9350 -10.9509 10.8856 0.5274 -0.6303 0.5821
13.9034 0.9581 11.9862 -0.5878 0.6752 0.4238
0.0063 -18.9256 -1.0163 0.8183 0.2620 0.5500
-0.0091 -16.9488 10.9232 0.4950 0.1598 0.8510
0.0323 4.0195 -26.8542 0.3703 0.1156 -0.9368
3.9839 -17.9346 -1.9962 0.7086 0.4731 0.5156
15.9069 -5.0079 1.0438 -0.1601 0.9341 0.2883
11.9177 -9.0002 11.9681 -0.1238 0.7007 0.7160
-15.9212 -1.9820 11.8803 0.1950 -0.9214 0.3177
12.9162 11.9277 4.0371 -0.8686 0.5227 -0.1600
3.9533 13.9190 15.9458 -0.9949 -0.0706 0.0817

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13518
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.970
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  79.00   1.00   40.38    --   17.28   0.00 150.00  129
  2  ω     59.00  89.00   1.00   40.38    --   17.28 178.00 -90.00   30
  3  ω    -19.00   7.00   1.00   40.38    --  -19.31 -99.00-150.00   26
  4  ω    -56.00  -4.00   1.00   40.38    --  -19.31 -77.00  90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0220192000
_diffrn_orient_matrix_UB_12      -0.0421633000
_diffrn_orient_matrix_UB_13      -0.0201277000
_diffrn_orient_matrix_UB_21      0.0548866000
_diffrn_orient_matrix_UB_22      -0.0134915000
_diffrn_orient_matrix_UB_23      -0.0062565000
_diffrn_orient_matrix_UB_31      0.0064756000
_diffrn_orient_matrix_UB_32      -0.0306838000
_diffrn_orient_matrix_UB_33      0.0303003000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4517
_reflns_number_total             6222
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6222
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0445
_refine_ls_restrained_S_all      1.034
_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)+(0.0387P)²+1.0245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1043
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N2A-H2A
 0.86 with sigma of 0.04
 N2B-H2B
 0.86 with sigma of 0.04
3. Others
 Sof(N2B)=1-FVAR(1)
 Sof(N2A)=FVAR(1)
 Fixed Sof: H2A(0.5) H2B(0.5)
4.a Free rotating group:
 O7W(H7WA,H7WB)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B)
4.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N7(H7), C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11),
 C12(H12)
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.54260(3) 0.32657(3) 0.29836(2) 0.02927(11) Uani 1 1 d . . . . .
O1 O 0.55094(16) 0.43955(16) 0.43548(10) 0.0407(5) Uani 1 1 d . . . . .
O2 O 0.25458(17) 0.33396(16) 0.53178(10) 0.0447(6) Uani 1 1 d . . . . .
O3 O 0.36456(16) 0.17145(15) 0.33525(10) 0.0380(5) Uani 1 1 d . . . . .
O4 O 0.67978(16) 0.28288(18) 0.18253(10) 0.0460(6) Uani 1 1 d . . . . .
O5 O 0.43849(19) 0.1953(2) -0.00378(10) 0.0570(7) Uani 1 1 d . . . . .
O6 O 0.31459(15) 0.31610(15) 0.20217(10) 0.0374(5) Uani 1 1 d . . . . .
N1 N 0.51475(19) 0.48988(18) 0.28476(11) 0.0333(6) Uani 1 1 d . . . . .
N2A N 0.7053(6) 0.3943(7) 0.3097(13) 0.034(3) Uani 0.51(4) 1 d D . P A 1
H2A H 0.720(4) 0.383(4) 0.268(2) 0.022(15) Uiso 0.5 1 d D . P . .
N2B N 0.7018(5) 0.3844(7) 0.3433(14) 0.030(4) Uani 0.49(4) 1 d D . P A 2
H2B H 0.691(5) 0.384(5) 0.386(2) 0.04(2) Uiso 0.5 1 d D . P . .
N3 N 0.6509(2) 0.19332(19) 0.32695(12) 0.0379(6) Uani 1 1 d . . . . .
N4 N 0.45250(18) 0.31177(16) 0.37895(10) 0.0269(5) Uani 1 1 d . . . . .
N5 N 0.40053(19) 0.38554(18) 0.48122(11) 0.0336(6) Uani 1 1 d . . . . .
H5 H 0.410890 0.434484 0.510741 0.040 Uiso 1 1 calc R . . . .
N6 N 0.49697(18) 0.28934(18) 0.19747(10) 0.0285(5) Uani 1 1 d . . . . .
N7 N 0.55595(19) 0.23338(19) 0.09220(11) 0.0360(6) Uani 1 1 d . . . . .
H7 H 0.611276 0.213670 0.071746 0.043 Uiso 1 1 calc R . . . .
C1 C 0.4150(3) 0.5345(2) 0.26703(15) 0.0404(7) Uani 1 1 d . . . . .
H1 H 0.353743 0.493830 0.251056 0.048 Uiso 1 1 calc R . . . .
C2 C 0.3987(3) 0.6368(3) 0.27117(16) 0.0459(8) Uani 1 1 d . . . . .
H2 H 0.328090 0.665159 0.258271 0.055 Uiso 1 1 calc R . . . .
C3 C 0.4892(3) 0.6965(3) 0.29491(16) 0.0484(8) Uani 1 1 d . . . . .
H3 H 0.480722 0.766338 0.299017 0.058 Uiso 1 1 calc R . . . .
C4 C 0.5922(3) 0.6525(2) 0.31248(15) 0.0438(8) Uani 1 1 d . . . . .
H4 H 0.654580 0.692193 0.327908 0.053 Uiso 1 1 calc R . . . .
C5 C 0.6027(2) 0.5483(2) 0.30709(13) 0.0334(7) Uani 1 1 d . . . . .
C6 C 0.7127(2) 0.4958(2) 0.32754(16) 0.0422(8) Uani 1 1 d . . . . .
H6A H 0.752059 0.529158 0.368326 0.051 Uiso 1 1 calc R . . A 2
H6B H 0.758000 0.503164 0.290117 0.051 Uiso 1 1 calc R . . A 2
C7 C 0.7919(3) 0.3239(3) 0.34476(19) 0.0539(9) Uani 1 1 d . . . . .
H7A H 0.811502 0.345923 0.392589 0.065 Uiso 1 1 calc R . . A 1
H7B H 0.858678 0.329832 0.322145 0.065 Uiso 1 1 calc R . . A 1
C8 C 0.7591(2) 0.2142(3) 0.34509(14) 0.0386(7) Uani 1 1 d . . . . .
C9 C 0.8369(3) 0.1391(3) 0.36273(17) 0.0534(9) Uani 1 1 d . . . . .
H9 H 0.912235 0.155257 0.375324 0.064 Uiso 1 1 calc R . . . .
C10 C 0.8020(3) 0.0399(3) 0.36152(17) 0.0587(10) Uani 1 1 d . . . . .
H10 H 0.853706 -0.011943 0.373136 0.070 Uiso 1 1 calc R . . . .
C11 C 0.6913(3) 0.0177(3) 0.34321(18) 0.0562(9) Uani 1 1 d . . . . .
H11 H 0.666206 -0.049126 0.342374 0.067 Uiso 1 1 calc R . . . .
C12 C 0.6179(3) 0.0960(3) 0.32606(17) 0.0506(9) Uani 1 1 d . . . . .
H12 H 0.542342 0.081210 0.313307 0.061 Uiso 1 1 calc R . . . .
C13 C 0.3045(4) 0.0821(3) 0.1198(3) 0.1002(17) Uani 1 1 d . . . . .
H13A H 0.363792 0.054651 0.096987 0.150 Uiso 1 1 calc GR . . . .
H13B H 0.243305 0.034759 0.116293 0.150 Uiso 1 1 calc GR . . . .
H13C H 0.331811 0.094072 0.167972 0.150 Uiso 1 1 calc GR . . . .
C14 C 0.2649(3) 0.1798(3) 0.08586(18) 0.0584(10) Uani 1 1 d . . . . .
H14A H 0.201482 0.204420 0.106999 0.070 Uiso 1 1 calc R . . . .
H14B H 0.239087 0.167224 0.037022 0.070 Uiso 1 1 calc R . . . .
C15 C 0.3551(2) 0.2622(2) 0.09166(14) 0.0334(7) Uani 1 1 d . . . . .
C16 C 0.3083(3) 0.3588(3) 0.05262(16) 0.0481(9) Uani 1 1 d . . . . .
H16A H 0.281702 0.340983 0.004664 0.058 Uiso 1 1 calc R . . . .
H16B H 0.244323 0.382827 0.073492 0.058 Uiso 1 1 calc R . . . .
C17 C 0.3920(3) 0.4438(3) 0.0533(2) 0.0659(11) Uani 1 1 d . . . . .
H17A H 0.358686 0.499300 0.025847 0.099 Uiso 1 1 calc GR . . . .
H17B H 0.456898 0.420132 0.034250 0.099 Uiso 1 1 calc GR . . . .
H17C H 0.413924 0.466119 0.100332 0.099 Uiso 1 1 calc GR . . . .
C18 C 0.3883(2) 0.2898(2) 0.16802(13) 0.0286(6) Uani 1 1 d . . . . .
C19 C 0.5809(2) 0.2694(2) 0.15934(14) 0.0316(6) Uani 1 1 d . . . . .
C20 C 0.4518(2) 0.2264(2) 0.05572(14) 0.0354(7) Uani 1 1 d . . . . .
C21 C 0.1354(3) 0.3079(3) 0.36768(18) 0.0527(9) Uani 1 1 d . . . . .
H21A H 0.182028 0.323016 0.332570 0.079 Uiso 1 1 calc GR . . . .
H21B H 0.133990 0.365316 0.398052 0.079 Uiso 1 1 calc GR . . . .
H21C H 0.060595 0.293304 0.345940 0.079 Uiso 1 1 calc GR . . . .
C22 C 0.1820(2) 0.2171(2) 0.40927(15) 0.0367(7) Uani 1 1 d . . . . .
H22A H 0.174899 0.157689 0.379427 0.044 Uiso 1 1 calc R . . . .
H22B H 0.137704 0.205329 0.446707 0.044 Uiso 1 1 calc R . . . .
C23 C 0.3053(2) 0.2299(2) 0.44026(13) 0.0288(6) Uani 1 1 d . . . . .
C24 C 0.3456(3) 0.1365(2) 0.48487(16) 0.0447(8) Uani 1 1 d . . . . .
H24A H 0.298808 0.129365 0.521535 0.054 Uiso 1 1 calc R . . . .
H24B H 0.334949 0.076419 0.455850 0.054 Uiso 1 1 calc R . . . .
C25 C 0.4678(3) 0.1409(3) 0.5179(2) 0.0672(11) Uani 1 1 d . . . . .
H25A H 0.515427 0.143691 0.482049 0.101 Uiso 1 1 calc GR . . . .
H25B H 0.485476 0.081464 0.545909 0.101 Uiso 1 1 calc GR . . . .
H25C H 0.479683 0.200330 0.546633 0.101 Uiso 1 1 calc GR . . . .
C26 C 0.3758(2) 0.2368(2) 0.38037(13) 0.0278(6) Uani 1 1 d . . . . .
C27 C 0.4722(2) 0.3800(2) 0.43123(13) 0.0293(6) Uani 1 1 d . . . . .
C28 C 0.3156(2) 0.3204(2) 0.48750(13) 0.0307(6) Uani 1 1 d . . . . .
O7W O 0.1187(2) 0.4483(2) 0.1837(2) 0.0871(9) Uani 1 1 d . . . . .
H7WA H 0.176544 0.410639 0.186138 0.131 Uiso 1 1 d G . . . .
H7WB H 0.138426 0.510207 0.183089 0.131 Uiso 1 1 d G . . . .


_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
Zn1 N1 2.188(2) . ?
Zn1 N2A 2.135(9) . ?
Zn1 N2B 2.133(9) . ?
Zn1 N3 2.211(2) . ?
Zn1 N4 2.029(2) . ?
Zn1 N6 2.019(2) . ?
O1 C27 1.224(3) . ?
O2 C28 1.217(3) . ?
O3 C26 1.221(3) . ?
O4 C19 1.226(3) . ?
O5 C20 1.214(3) . ?
O6 C18 1.227(3) . ?
N1 C1 1.338(4) . ?
N1 C5 1.332(3) . ?
N2A H2A 0.86(3) . ?
N2A H2B 1.51(4) . ?
N2A C6 1.381(8) . ?
N2A C7 1.488(12) . ?
N2B H2A 1.51(4) . ?
N2B H2B 0.85(4) . ?
N2B C6 1.508(13) . ?
N2B C7 1.342(7) . ?
N3 C8 1.330(4) . ?
N3 C12 1.341(4) . ?
N4 C26 1.355(3) . ?
N4 C27 1.351(3) . ?
N5 H5 0.8600 . ?
N5 C27 1.384(3) . ?
N5 C28 1.352(3) . ?
N6 C18 1.354(3) . ?
N6 C19 1.356(3) . ?
N7 H7 0.8600 . ?
N7 C19 1.380(3) . ?
N7 C20 1.355(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.366(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.371(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.368(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.383(4) . ?
C5 C6 1.498(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.499(5) . ?
C8 C9 1.373(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.372(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.362(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.370(5) . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13 C14 1.494(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.527(4) . ?
C15 C16 1.547(4) . ?
C15 C18 1.524(4) . ?
C15 C20 1.511(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.505(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 C22 1.508(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.531(4) . ?
C23 C24 1.544(4) . ?
C23 C26 1.532(3) . ?
C23 C28 1.499(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.523(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
O7W H7WA 0.8504 . ?
O7W H7WB 0.8504 . ?

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
N1 Zn1 N3 152.41(9) . . ?
N2A Zn1 N1 74.0(2) . . ?
N2A Zn1 N3 78.8(3) . . ?
N2B Zn1 N1 79.2(3) . . ?
N2B Zn1 N3 73.5(3) . . ?
N4 Zn1 N1 95.64(8) . . ?
N4 Zn1 N2A 122.6(7) . . ?
N4 Zn1 N2B 105.3(7) . . ?
N4 Zn1 N3 95.09(9) . . ?
N6 Zn1 N1 96.03(9) . . ?
N6 Zn1 N2A 109.0(7) . . ?
N6 Zn1 N2B 126.3(7) . . ?
N6 Zn1 N3 97.07(9) . . ?
N6 Zn1 N4 128.31(9) . . ?
C1 N1 Zn1 125.5(2) . . ?
C5 N1 Zn1 115.32(19) . . ?
C5 N1 C1 118.3(3) . . ?
Zn1 N2A H2A 98(3) . . ?
Zn1 N2A H2B 81(2) . . ?
H2A N2A H2B 164(4) . . ?
C6 N2A Zn1 117.2(6) . . ?
C6 N2A H2A 113(4) . . ?
C6 N2A H2B 82(3) . . ?
C6 N2A C7 118.2(8) . . ?
C7 N2A Zn1 111.2(8) . . ?
C7 N2A H2A 96(4) . . ?
C7 N2A H2B 70(2) . . ?
Zn1 N2B H2A 81(2) . . ?
Zn1 N2B H2B 98(4) . . ?
H2A N2B H2B 179(5) . . ?
C6 N2B Zn1 111.3(9) . . ?
C6 N2B H2A 78(2) . . ?
C6 N2B H2B 104(4) . . ?
C7 N2B Zn1 118.3(6) . . ?
C7 N2B H2A 78(2) . . ?
C7 N2B H2B 102(4) . . ?
C7 N2B C6 119.3(8) . . ?
C8 N3 Zn1 115.1(2) . . ?
C8 N3 C12 118.5(3) . . ?
C12 N3 Zn1 126.4(2) . . ?
C26 N4 Zn1 121.49(17) . . ?
C27 N4 Zn1 117.17(17) . . ?
C27 N4 C26 121.3(2) . . ?
C27 N5 H5 117.3 . . ?
C28 N5 H5 117.3 . . ?
C28 N5 C27 125.4(2) . . ?
C18 N6 Zn1 121.81(17) . . ?
C18 N6 C19 121.2(2) . . ?
C19 N6 Zn1 116.84(17) . . ?
C19 N7 H7 117.2 . . ?
C20 N7 H7 117.2 . . ?
C20 N7 C19 125.6(2) . . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.4(3) . . ?
C2 C1 H1 118.3 . . ?
C1 C2 H2 120.9 . . ?
C1 C2 C3 118.1(3) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C6 116.9(3) . . ?
C4 C5 C6 121.6(3) . . ?
N2A C6 C5 110.9(4) . . ?
N2B C6 H6A 108.8 . . ?
N2B C6 H6B 108.8 . . ?
C5 C6 N2B 113.9(3) . . ?
C5 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
N2A C7 H7A 108.3 . . ?
N2A C7 H7B 108.3 . . ?
N2A C7 C8 115.8(4) . . ?
N2B C7 C8 111.2(5) . . ?
H7A C7 H7B 107.4 . . ?
C8 C7 H7A 108.3 . . ?
C8 C7 H7B 108.3 . . ?
N3 C8 C7 116.5(3) . . ?
N3 C8 C9 121.8(3) . . ?
C9 C8 C7 121.7(3) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 119.0(3) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 120.8 . . ?
C10 C11 C12 118.4(4) . . ?
C12 C11 H11 120.8 . . ?
N3 C12 C11 122.5(3) . . ?
N3 C12 H12 118.7 . . ?
C11 C12 H12 118.7 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
C13 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
C13 C14 C15 113.5(3) . . ?
H14A C14 H14B 107.7 . . ?
C15 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C14 C15 C16 109.9(3) . . ?
C18 C15 C14 109.3(2) . . ?
C18 C15 C16 108.0(2) . . ?
C20 C15 C14 109.1(3) . . ?
C20 C15 C16 106.4(2) . . ?
C20 C15 C18 114.0(2) . . ?
C15 C16 H16A 108.7 . . ?
C15 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 C15 114.1(3) . . ?
C17 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C18 N6 120.1(2) . . ?
O6 C18 C15 118.6(2) . . ?
N6 C18 C15 121.3(2) . . ?
O4 C19 N6 121.9(2) . . ?
O4 C19 N7 118.1(2) . . ?
N6 C19 N7 120.0(2) . . ?
O5 C20 N7 120.8(3) . . ?
O5 C20 C15 122.2(3) . . ?
N7 C20 C15 116.9(2) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
C21 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
C21 C22 C23 113.1(2) . . ?
H22A C22 H22B 107.8 . . ?
C23 C22 H22A 109.0 . . ?
C23 C22 H22B 109.0 . . ?
C22 C23 C24 110.2(2) . . ?
C22 C23 C26 108.4(2) . . ?
C26 C23 C24 107.9(2) . . ?
C28 C23 C22 108.9(2) . . ?
C28 C23 C24 107.3(2) . . ?
C28 C23 C26 114.1(2) . . ?
C23 C24 H24A 108.6 . . ?
C23 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 C23 114.7(3) . . ?
C25 C24 H24A 108.6 . . ?
C25 C24 H24B 108.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O3 C26 N4 120.6(2) . . ?
O3 C26 C23 118.9(2) . . ?
N4 C26 C23 120.5(2) . . ?
O1 C27 N4 122.1(2) . . ?
O1 C27 N5 118.0(2) . . ?
N4 C27 N5 119.9(2) . . ?
O2 C28 N5 120.5(3) . . ?
O2 C28 C23 122.7(2) . . ?
N5 C28 C23 116.8(2) . . ?
H7WA O7W H7WB 109.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2A H2A O4 0.86(3) 2.12(4) 2.850(19) 141(5) .
N2B H2B O1 0.85(4) 2.18(5) 2.811(19) 131(5) .
N5 H5 O1 0.86 1.98 2.829(3) 168.8 3_666
N7 H7 O2 0.86 2.08 2.938(3) 174.4 4_665
O7W H7WA O6 0.85 2.07 2.913(3) 174.3 .
O7W H7WB O3 0.85 2.15 2.973(4) 161.9 2

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 N1 C1 C2 167.8(2) . . . . ?
Zn1 N1 C5 C4 -169.1(2) . . . . ?
Zn1 N1 C5 C6 9.6(3) . . . . ?
Zn1 N2A C6 C5 -23.6(17) . . . . ?
Zn1 N2A C7 C8 18.1(15) . . . . ?
Zn1 N2B C6 C5 19.9(15) . . . . ?
Zn1 N2B C7 C8 -26.4(19) . . . . ?
Zn1 N3 C8 C7 1.0(3) . . . . ?
Zn1 N3 C8 C9 -178.6(2) . . . . ?
Zn1 N3 C12 C11 178.5(2) . . . . ?
Zn1 N4 C26 O3 5.2(4) . . . . ?
Zn1 N4 C26 C23 -177.37(18) . . . . ?
Zn1 N4 C27 O1 -10.0(4) . . . . ?
Zn1 N4 C27 N5 168.5(2) . . . . ?
Zn1 N6 C18 O6 2.1(4) . . . . ?
Zn1 N6 C18 C15 179.59(19) . . . . ?
Zn1 N6 C19 O4 -7.0(4) . . . . ?
Zn1 N6 C19 N7 173.3(2) . . . . ?
N1 C1 C2 C3 -0.1(5) . . . . ?
N1 C5 C6 N2A 8.6(12) . . . . ?
N1 C5 C6 N2B -19.8(11) . . . . ?
N2A C7 C8 N3 -12.9(11) . . . . ?
N2A C7 C8 C9 166.7(11) . . . . ?
N2B C7 C8 N3 15.9(13) . . . . ?
N2B C7 C8 C9 -164.5(13) . . . . ?
N3 C8 C9 C10 0.1(5) . . . . ?
C1 N1 C5 C4 0.4(4) . . . . ?
C1 N1 C5 C6 179.1(2) . . . . ?
C1 C2 C3 C4 1.0(5) . . . . ?
C2 C3 C4 C5 -1.1(5) . . . . ?
C3 C4 C5 N1 0.4(4) . . . . ?
C3 C4 C5 C6 -178.2(3) . . . . ?
C4 C5 C6 N2A -172.7(12) . . . . ?
C4 C5 C6 N2B 158.9(11) . . . . ?
C5 N1 C1 C2 -0.5(4) . . . . ?
C6 N2A C7 C8 157.9(12) . . . . ?
C6 N2B C7 C8 -167.2(13) . . . . ?
C7 N2A C6 C5 -160.9(12) . . . . ?
C7 N2B C6 C5 163.2(14) . . . . ?
C7 C8 C9 C10 -179.5(3) . . . . ?
C8 N3 C12 C11 0.1(5) . . . . ?
C8 C9 C10 C11 -0.3(5) . . . . ?
C9 C10 C11 C12 0.4(5) . . . . ?
C10 C11 C12 N3 -0.3(5) . . . . ?
C12 N3 C8 C7 179.5(3) . . . . ?
C12 N3 C8 C9 0.0(4) . . . . ?
C13 C14 C15 C16 177.7(3) . . . . ?
C13 C14 C15 C18 -63.9(4) . . . . ?
C13 C14 C15 C20 61.3(4) . . . . ?
C14 C15 C16 C17 -178.2(3) . . . . ?
C14 C15 C18 O6 -54.9(4) . . . . ?
C14 C15 C18 N6 127.6(3) . . . . ?
C14 C15 C20 O5 52.7(4) . . . . ?
C14 C15 C20 N7 -129.4(3) . . . . ?
C16 C15 C18 O6 64.6(3) . . . . ?
C16 C15 C18 N6 -112.9(3) . . . . ?
C16 C15 C20 O5 -65.9(4) . . . . ?
C16 C15 C20 N7 112.0(3) . . . . ?
C18 N6 C19 O4 169.3(3) . . . . ?
C18 N6 C19 N7 -10.3(4) . . . . ?
C18 C15 C16 C17 62.6(3) . . . . ?
C18 C15 C20 O5 175.2(3) . . . . ?
C18 C15 C20 N7 -6.9(4) . . . . ?
C19 N6 C18 O6 -174.0(3) . . . . ?
C19 N6 C18 C15 3.4(4) . . . . ?
C19 N7 C20 O5 178.6(3) . . . . ?
C19 N7 C20 C15 0.7(4) . . . . ?
C20 N7 C19 O4 -171.2(3) . . . . ?
C20 N7 C19 N6 8.4(5) . . . . ?
C20 C15 C16 C17 -60.1(3) . . . . ?
C20 C15 C18 O6 -177.3(3) . . . . ?
C20 C15 C18 N6 5.2(4) . . . . ?
C21 C22 C23 C24 177.3(2) . . . . ?
C21 C22 C23 C26 -64.8(3) . . . . ?
C21 C22 C23 C28 59.8(3) . . . . ?
C22 C23 C24 C25 179.6(3) . . . . ?
C22 C23 C26 O3 -51.4(3) . . . . ?
C22 C23 C26 N4 131.1(3) . . . . ?
C22 C23 C28 O2 48.6(4) . . . . ?
C22 C23 C28 N5 -134.5(3) . . . . ?
C24 C23 C26 O3 67.9(3) . . . . ?
C24 C23 C26 N4 -109.5(3) . . . . ?
C24 C23 C28 O2 -70.7(3) . . . . ?
C24 C23 C28 N5 106.2(3) . . . . ?
C26 N4 C27 O1 170.1(3) . . . . ?
C26 N4 C27 N5 -11.5(4) . . . . ?
C26 C23 C24 C25 61.4(3) . . . . ?
C26 C23 C28 O2 169.8(3) . . . . ?
C26 C23 C28 N5 -13.3(3) . . . . ?
C27 N4 C26 O3 -174.8(3) . . . . ?
C27 N4 C26 C23 2.6(4) . . . . ?
C27 N5 C28 O2 -177.3(3) . . . . ?
C27 N5 C28 C23 5.7(4) . . . . ?
C28 N5 C27 O1 -174.2(3) . . . . ?
C28 N5 C27 N4 7.3(4) . . . . ?
C28 C23 C24 C25 -62.0(3) . . . . ?
C28 C23 C26 O3 -172.9(2) . . . . ?
C28 C23 C26 N4 9.7(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.124
_oxdiff_exptl_absorpt_empirical_full_min 0.906
####################################################################### 
# 
# 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_CCDC_1511701
_database_code_depnum_ccdc_archive 'CCDC 1511701'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
_audit_creation_date             2017-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H33 N7 Ni O6, H2 O'
_chemical_formula_sum            'C31 H35 N7 Ni O7'
_chemical_formula_weight         676.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H35 N7 Ni O7'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.5914(7)
_cell_length_b                   13.0083(7)
_cell_length_c                   19.7972(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.786(5)
_cell_angle_gamma                90
_cell_volume                     3212.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3694
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.6610
_cell_measurement_theta_min      3.4700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 18 -1 0.0997
14 11 -5 0.0860
4 -3 26 0.1521
-13 -12 -1 0.0586
10 15 -2 0.0958
-11 -14 -2 0.0644
10 -12 -16 0.1545
-13 13 -1 0.0831
11 0 19 0.1365
-16 -1 -9 0.0939
15 3 -16 0.1646
18 2 -2 0.0985
-17 -2 -1 0.0865
5 -9 21 0.1547
-5 7 -23 0.2079
12 -13 -2 0.0946
2 -18 -3 0.1049
-11 -11 -13 0.1092

_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.17
loop_
_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
-3.0033 17.9872 -0.9876 0.2472 0.9528 0.1577
13.9882 10.9910 -5.0038 -0.7124 0.6833 -0.1050
3.9980 -2.9959 25.9784 0.0301 -0.1105 -1.0029
-12.9884 -11.9909 -0.9938 0.5963 -0.7365 0.2882
9.9895 14.9886 -2.0002 -0.4532 0.8760 -0.1075
-10.9891 -13.9896 -1.9959 0.4716 -0.8324 0.2720
9.9974 -11.9932 -16.0048 -0.7424 -0.5982 0.2956
-12.9956 12.9912 -0.9812 0.7372 0.6159 0.3657
10.9929 0.0010 18.9781 -0.3842 0.0915 -0.9066
-15.9896 -0.9993 -8.9805 0.7355 -0.1692 0.6675
14.9900 2.9958 -16.0017 -0.9169 0.2465 0.2304
17.9882 1.9975 -2.0138 -0.9411 0.2259 -0.3266
-16.9888 -1.9978 -0.9852 0.8599 -0.2222 0.4086
4.9992 -8.9921 20.9777 -0.1044 -0.4333 -0.8699
-4.9986 6.9933 -22.9774 0.0736 0.3232 0.9333
11.9963 -12.9914 -2.0160 -0.7147 -0.6254 -0.2390
2.0040 -17.9874 -3.0089 -0.2345 -0.9633 0.0038
-10.9898 -10.9927 -12.9874 0.3809 -0.6808 0.6639

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11461
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.680
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         3.218
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  46.00   1.00   22.86    --   17.28 -77.00 -60.00   99
  2  ω    -13.00  86.00   1.00   22.86    --   17.28  77.00 150.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0518462000
_diffrn_orient_matrix_UB_12      0.0056225000
_diffrn_orient_matrix_UB_13      0.0097873000
_diffrn_orient_matrix_UB_21      0.0066554000
_diffrn_orient_matrix_UB_22      0.0541366000
_diffrn_orient_matrix_UB_23      0.0009638000
_diffrn_orient_matrix_UB_31      -0.0223996000
_diffrn_orient_matrix_UB_32      0.0031139000
_diffrn_orient_matrix_UB_33      -0.0347970000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4415
_reflns_number_total             6051
_reflns_odcompleteness_completeness 99.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6051
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.010
_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)+(0.0414P)²+0.8343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0984
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O7W(H7WA,H7WB)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C25(H25A,H25B), C27(H27A,H27B)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N7(H7), C1(H1), C2(H2), C3(H3), C4(H4), C7(H7A), C8(H8), C9(H9),
 C12(H12), C13(H13), C14(H14), C15(H15)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.51905(3) 0.31064(2) 0.29395(2) 0.02667(11) Uani 1 1 d . . . . .
O1 O 0.68683(14) 0.26682(15) 0.18383(9) 0.0375(4) Uani 1 1 d . . . . .
O2 O 0.46860(17) 0.2475(2) -0.01362(9) 0.0706(8) Uani 1 1 d . . . . .
O3 O 0.33413(15) 0.30888(16) 0.19448(9) 0.0448(5) Uani 1 1 d . . . . .
O4 O 0.36710(16) 0.16931(16) 0.33734(10) 0.0482(5) Uani 1 1 d . . . . .
O5 O 0.26507(17) 0.33038(17) 0.53303(10) 0.0573(6) Uani 1 1 d . . . . .
O6 O 0.54638(16) 0.44031(16) 0.43624(9) 0.0474(5) Uani 1 1 d . . . . .
N1 N 0.61438(18) 0.17687(16) 0.31600(10) 0.0332(5) Uani 1 1 d . . . . .
N2 N 0.66244(16) 0.37141(16) 0.32013(9) 0.0267(5) Uani 1 1 d . . . . .
N3 N 0.48546(17) 0.47307(17) 0.28522(10) 0.0311(5) Uani 1 1 d . . . . .
N4 N 0.50947(17) 0.28748(16) 0.19196(10) 0.0286(5) Uani 1 1 d . . . . .
N5 N 0.57246(17) 0.24672(18) 0.08743(10) 0.0362(6) Uani 1 1 d . . . . .
H5 H 0.624794 0.223785 0.068009 0.043 Uiso 1 1 calc R . . . .
N6 N 0.45583(17) 0.30685(16) 0.38275(10) 0.0319(5) Uani 1 1 d . . . . .
N7 N 0.40446(18) 0.38336(17) 0.48260(10) 0.0376(6) Uani 1 1 d . . . . .
H7 H 0.415294 0.432116 0.512060 0.045 Uiso 1 1 calc R . . . .
C1 C 0.5843(3) 0.0780(2) 0.31103(14) 0.0447(8) Uani 1 1 d . . . . .
H1 H 0.512443 0.062893 0.297107 0.054 Uiso 1 1 calc R . . . .
C2 C 0.6547(3) -0.0019(2) 0.32559(16) 0.0579(9) Uani 1 1 d . . . . .
H2 H 0.631153 -0.069678 0.321297 0.070 Uiso 1 1 calc R . . . .
C3 C 0.7601(3) 0.0199(3) 0.34649(17) 0.0650(10) Uani 1 1 d . . . . .
H3 H 0.809030 -0.033082 0.357129 0.078 Uiso 1 1 calc R . . . .
C4 C 0.7937(3) 0.1212(3) 0.35180(15) 0.0528(9) Uani 1 1 d . . . . .
H4 H 0.865326 0.137117 0.365858 0.063 Uiso 1 1 calc R . . . .
C5 C 0.7188(2) 0.1984(2) 0.33577(12) 0.0340(6) Uani 1 1 d . . . . .
C6 C 0.7463(2) 0.3089(2) 0.33824(12) 0.0317(6) Uani 1 1 d . . . . .
C7 C 0.8477(2) 0.3496(3) 0.35741(14) 0.0461(7) Uani 1 1 d . . . . .
H7A H 0.905936 0.306450 0.369969 0.055 Uiso 1 1 calc R . . . .
C8 C 0.8608(2) 0.4535(3) 0.35760(16) 0.0518(8) Uani 1 1 d . . . . .
H8 H 0.928602 0.481603 0.370010 0.062 Uiso 1 1 calc R . . . .
C9 C 0.7744(2) 0.5172(2) 0.33952(14) 0.0429(7) Uani 1 1 d . . . . .
H9 H 0.782891 0.588228 0.339826 0.051 Uiso 1 1 calc R . . . .
C10 C 0.6746(2) 0.4736(2) 0.32090(11) 0.0286(6) Uani 1 1 d . . . . .
C11 C 0.5731(2) 0.5315(2) 0.30285(12) 0.0309(6) Uani 1 1 d . . . . .
C12 C 0.5671(3) 0.6376(2) 0.30693(14) 0.0449(7) Uani 1 1 d . . . . .
H12 H 0.628810 0.676716 0.318342 0.054 Uiso 1 1 calc R . . . .
C13 C 0.4688(3) 0.6840(2) 0.29385(17) 0.0547(8) Uani 1 1 d . . . . .
H13 H 0.463160 0.755173 0.296520 0.066 Uiso 1 1 calc R . . . .
C14 C 0.3782(3) 0.6250(3) 0.27674(15) 0.0521(8) Uani 1 1 d . . . . .
H14 H 0.310830 0.655271 0.268169 0.063 Uiso 1 1 calc R . . . .
C15 C 0.3902(2) 0.5197(2) 0.27266(14) 0.0406(7) Uani 1 1 d . . . . .
H15 H 0.329478 0.479553 0.260677 0.049 Uiso 1 1 calc R . . . .
C16 C 0.1612(3) 0.3229(4) 0.3620(2) 0.0971(16) Uani 1 1 d . . . . .
H16A H 0.207568 0.328736 0.327449 0.146 Uiso 1 1 calc GR . . . .
H16B H 0.168886 0.382801 0.390557 0.146 Uiso 1 1 calc GR . . . .
H16C H 0.088234 0.317249 0.340802 0.146 Uiso 1 1 calc GR . . . .
C17 C 0.1910(3) 0.2288(3) 0.40451(19) 0.0733(13) Uani 1 1 d . . . . .
H17A H 0.179413 0.168466 0.375625 0.088 Uiso 1 1 calc R . . . .
H17B H 0.143748 0.223604 0.439192 0.088 Uiso 1 1 calc R . . . .
C18 C 0.3080(2) 0.2285(2) 0.43953(14) 0.0442(8) Uani 1 1 d . . . . .
C19 C 0.3369(4) 0.1302(3) 0.48207(18) 0.0801(14) Uani 1 1 d . . . . .
H19A H 0.286331 0.122494 0.514611 0.096 Uiso 1 1 calc R . . . .
H19B H 0.328400 0.071213 0.451805 0.096 Uiso 1 1 calc R . . . .
C20 C 0.4493(5) 0.1290(4) 0.5204(2) 0.1060(17) Uani 1 1 d . . . . .
H20A H 0.500152 0.137047 0.488781 0.159 Uiso 1 1 calc GR . . . .
H20B H 0.461764 0.064831 0.544071 0.159 Uiso 1 1 calc GR . . . .
H20C H 0.457292 0.184487 0.552685 0.159 Uiso 1 1 calc GR . . . .
C21 C 0.3221(2) 0.3184(2) 0.48851(13) 0.0391(7) Uani 1 1 d . . . . .
C22 C 0.4732(2) 0.3784(2) 0.43315(12) 0.0331(6) Uani 1 1 d . . . . .
C23 C 0.3795(2) 0.2337(2) 0.38350(13) 0.0344(6) Uani 1 1 d . . . . .
C24 C 0.4467(3) 0.4819(3) 0.08035(19) 0.0750(12) Uani 1 1 d . . . . .
H24A H 0.426746 0.548244 0.061581 0.112 Uiso 1 1 calc GR . . . .
H24B H 0.510964 0.459131 0.063798 0.112 Uiso 1 1 calc GR . . . .
H24C H 0.459069 0.486361 0.129191 0.112 Uiso 1 1 calc GR . . . .
C25 C 0.3574(3) 0.4061(3) 0.05909(17) 0.0650(11) Uani 1 1 d . . . . .
H25A H 0.341179 0.407167 0.009784 0.078 Uiso 1 1 calc R . . . .
H25B H 0.293802 0.428697 0.077512 0.078 Uiso 1 1 calc R . . . .
C26 C 0.3824(2) 0.2929(2) 0.08242(13) 0.0403(7) Uani 1 1 d . . . . .
C27 C 0.2861(3) 0.2233(4) 0.06023(18) 0.0762(13) Uani 1 1 d . . . . .
H27A H 0.225596 0.247556 0.081387 0.091 Uiso 1 1 calc R . . . .
H27B H 0.266897 0.229055 0.011246 0.091 Uiso 1 1 calc R . . . .
C28 C 0.3052(4) 0.1117(4) 0.0782(3) 0.1095(17) Uani 1 1 d . . . . .
H28A H 0.361428 0.085471 0.054815 0.164 Uiso 1 1 calc GR . . . .
H28B H 0.240678 0.073332 0.064833 0.164 Uiso 1 1 calc GR . . . .
H28C H 0.325742 0.105236 0.126548 0.164 Uiso 1 1 calc GR . . . .
C29 C 0.4770(2) 0.2591(2) 0.04768(13) 0.0415(7) Uani 1 1 d . . . . .
C30 C 0.5936(2) 0.26786(19) 0.15722(12) 0.0283(6) Uani 1 1 d . . . . .
C31 C 0.4082(2) 0.29485(19) 0.16018(13) 0.0314(6) Uani 1 1 d . . . . .
O7W O 0.1360(2) 0.4349(3) 0.1773(2) 0.1158(11) Uani 1 1 d . . . . .
H7WA H 0.151126 0.497410 0.170626 0.174 Uiso 1 1 d G . . . .
H7WB H 0.193029 0.399126 0.181042 0.174 Uiso 1 1 d G . . . .


_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
Ni1 N1 2.125(2) . ?
Ni1 N2 1.975(2) . ?
Ni1 N3 2.157(2) . ?
Ni1 N4 2.0289(19) . ?
Ni1 N6 2.0263(19) . ?
O1 C30 1.220(3) . ?
O2 C29 1.213(3) . ?
O3 C31 1.239(3) . ?
O4 C23 1.234(3) . ?
O5 C21 1.220(3) . ?
O6 C22 1.219(3) . ?
N1 C1 1.341(3) . ?
N1 C5 1.349(3) . ?
N2 C6 1.342(3) . ?
N2 C10 1.337(3) . ?
N3 C11 1.346(3) . ?
N3 C15 1.337(3) . ?
N4 C30 1.363(3) . ?
N4 C31 1.347(3) . ?
N5 H5 0.8600 . ?
N5 C29 1.354(3) . ?
N5 C30 1.399(3) . ?
N6 C22 1.360(3) . ?
N6 C23 1.353(3) . ?
N7 H7 0.8600 . ?
N7 C21 1.355(3) . ?
N7 C22 1.393(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.371(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.365(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.383(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.385(4) . ?
C5 C6 1.478(4) . ?
C6 C7 1.387(4) . ?
C7 H7A 0.9300 . ?
C7 C8 1.362(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.376(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.382(4) . ?
C10 C11 1.484(4) . ?
C11 C12 1.386(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.370(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.378(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.382(4) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C17 1.505(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.540(5) . ?
C18 C19 1.548(5) . ?
C18 C21 1.514(4) . ?
C18 C23 1.522(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.513(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 C25 1.511(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.562(4) . ?
C26 C27 1.530(4) . ?
C26 C29 1.520(4) . ?
C26 C31 1.530(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.506(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O7W H7WA 0.8498 . ?
O7W H7WB 0.8500 . ?

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
N1 Ni1 N3 156.57(9) . . ?
N2 Ni1 N1 78.64(8) . . ?
N2 Ni1 N3 77.95(8) . . ?
N2 Ni1 N4 104.46(8) . . ?
N2 Ni1 N6 103.57(8) . . ?
N4 Ni1 N1 92.21(8) . . ?
N4 Ni1 N3 94.65(8) . . ?
N6 Ni1 N1 94.54(8) . . ?
N6 Ni1 N3 89.85(8) . . ?
N6 Ni1 N4 151.94(9) . . ?
C1 N1 Ni1 128.6(2) . . ?
C1 N1 C5 118.3(3) . . ?
C5 N1 Ni1 113.00(17) . . ?
C6 N2 Ni1 119.05(18) . . ?
C10 N2 Ni1 119.99(18) . . ?
C10 N2 C6 120.9(2) . . ?
C11 N3 Ni1 112.76(17) . . ?
C15 N3 Ni1 128.36(19) . . ?
C15 N3 C11 118.4(2) . . ?
C30 N4 Ni1 125.76(17) . . ?
C31 N4 Ni1 112.28(15) . . ?
C31 N4 C30 122.0(2) . . ?
C29 N5 H5 117.1 . . ?
C29 N5 C30 125.9(2) . . ?
C30 N5 H5 117.1 . . ?
C22 N6 Ni1 125.23(17) . . ?
C23 N6 Ni1 112.92(16) . . ?
C23 N6 C22 121.1(2) . . ?
C21 N7 H7 117.0 . . ?
C21 N7 C22 126.0(2) . . ?
C22 N7 H7 117.0 . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 122.9(3) . . ?
C2 C1 H1 118.5 . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.7(3) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.8(3) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.7(3) . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.5(3) . . ?
N1 C5 C6 115.2(2) . . ?
C4 C5 C6 123.3(3) . . ?
N2 C6 C5 114.1(2) . . ?
N2 C6 C7 120.3(3) . . ?
C7 C6 C5 125.6(3) . . ?
C6 C7 H7A 120.5 . . ?
C8 C7 C6 119.1(3) . . ?
C8 C7 H7A 120.5 . . ?
C7 C8 H8 119.8 . . ?
C7 C8 C9 120.3(3) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 120.6 . . ?
C8 C9 C10 118.7(3) . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 120.6(3) . . ?
N2 C10 C11 114.1(2) . . ?
C9 C10 C11 125.3(2) . . ?
N3 C11 C10 115.1(2) . . ?
N3 C11 C12 121.9(3) . . ?
C12 C11 C10 122.9(3) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 H12 120.6 . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.8(3) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 120.9 . . ?
C13 C14 C15 118.2(3) . . ?
C15 C14 H14 120.9 . . ?
N3 C15 C14 122.8(3) . . ?
N3 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
C16 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
C16 C17 C18 113.8(3) . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
C17 C18 C19 112.7(3) . . ?
C21 C18 C17 108.0(3) . . ?
C21 C18 C19 106.9(2) . . ?
C21 C18 C23 113.7(2) . . ?
C23 C18 C17 107.2(2) . . ?
C23 C18 C19 108.3(3) . . ?
C18 C19 H19A 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 C18 114.6(3) . . ?
C20 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O5 C21 N7 121.0(2) . . ?
O5 C21 C18 122.1(2) . . ?
N7 C21 C18 116.8(2) . . ?
O6 C22 N6 122.3(2) . . ?
O6 C22 N7 118.1(2) . . ?
N6 C22 N7 119.6(2) . . ?
O4 C23 N6 119.2(2) . . ?
O4 C23 C18 118.8(2) . . ?
N6 C23 C18 122.0(2) . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
C24 C25 H25A 108.6 . . ?
C24 C25 H25B 108.6 . . ?
C24 C25 C26 114.9(3) . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 H25A 108.6 . . ?
C26 C25 H25B 108.6 . . ?
C27 C26 C25 110.7(3) . . ?
C27 C26 C31 110.5(2) . . ?
C29 C26 C25 106.1(2) . . ?
C29 C26 C27 109.8(2) . . ?
C29 C26 C31 112.8(2) . . ?
C31 C26 C25 106.8(2) . . ?
C26 C27 H27A 108.7 . . ?
C26 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C28 C27 C26 114.0(3) . . ?
C28 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O2 C29 N5 121.1(3) . . ?
O2 C29 C26 121.4(3) . . ?
N5 C29 C26 117.4(2) . . ?
O1 C30 N4 123.5(2) . . ?
O1 C30 N5 117.9(2) . . ?
N4 C30 N5 118.6(2) . . ?
O3 C31 N4 119.3(2) . . ?
O3 C31 C26 118.7(2) . . ?
N4 C31 C26 121.8(2) . . ?
H7WA O7W H7WB 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5 O5 0.86 2.10 2.959(3) 172.5 4_665
N7 H7 O6 0.86 1.98 2.821(3) 167.5 3_666
C7 H7A O2 0.93 2.44 3.062(4) 124.7 4_666
O7W H7WA O4 0.85 2.25 3.063(4) 159.9 2
O7W H7WB O3 0.85 2.12 2.965(4) 177.7 .

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
Ni1 N1 C1 C2 178.6(2) . . . . ?
Ni1 N1 C5 C4 -179.4(2) . . . . ?
Ni1 N1 C5 C6 0.0(3) . . . . ?
Ni1 N2 C6 C5 0.2(3) . . . . ?
Ni1 N2 C6 C7 -179.45(18) . . . . ?
Ni1 N2 C10 C9 179.60(18) . . . . ?
Ni1 N2 C10 C11 1.6(3) . . . . ?
Ni1 N3 C11 C10 3.1(2) . . . . ?
Ni1 N3 C11 C12 -173.88(19) . . . . ?
Ni1 N3 C15 C14 171.6(2) . . . . ?
Ni1 N4 C30 O1 -3.7(4) . . . . ?
Ni1 N4 C30 N5 175.68(17) . . . . ?
Ni1 N4 C31 O3 -3.5(3) . . . . ?
Ni1 N4 C31 C26 172.7(2) . . . . ?
Ni1 N6 C22 O6 -16.1(4) . . . . ?
Ni1 N6 C22 N7 162.68(19) . . . . ?
Ni1 N6 C23 O4 10.4(3) . . . . ?
Ni1 N6 C23 C18 -169.4(2) . . . . ?
N1 C1 C2 C3 0.4(5) . . . . ?
N1 C5 C6 N2 -0.1(3) . . . . ?
N1 C5 C6 C7 179.5(2) . . . . ?
N2 C6 C7 C8 0.0(4) . . . . ?
N2 C10 C11 N3 -3.2(3) . . . . ?
N2 C10 C11 C12 173.8(2) . . . . ?
N3 C11 C12 C13 1.2(4) . . . . ?
C1 N1 C5 C4 -1.0(4) . . . . ?
C1 N1 C5 C6 178.4(2) . . . . ?
C1 C2 C3 C4 -0.7(5) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C3 C4 C5 N1 0.7(4) . . . . ?
C3 C4 C5 C6 -178.7(3) . . . . ?
C4 C5 C6 N2 179.3(2) . . . . ?
C4 C5 C6 C7 -1.1(4) . . . . ?
C5 N1 C1 C2 0.4(4) . . . . ?
C5 C6 C7 C8 -179.6(3) . . . . ?
C6 N2 C10 C9 0.9(3) . . . . ?
C6 N2 C10 C11 -177.06(19) . . . . ?
C6 C7 C8 C9 0.5(4) . . . . ?
C7 C8 C9 C10 -0.4(4) . . . . ?
C8 C9 C10 N2 -0.3(4) . . . . ?
C8 C9 C10 C11 177.4(2) . . . . ?
C9 C10 C11 N3 179.0(2) . . . . ?
C9 C10 C11 C12 -4.1(4) . . . . ?
C10 N2 C6 C5 178.94(19) . . . . ?
C10 N2 C6 C7 -0.7(3) . . . . ?
C10 C11 C12 C13 -175.5(2) . . . . ?
C11 N3 C15 C14 0.3(4) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
C12 C13 C14 C15 -0.7(5) . . . . ?
C13 C14 C15 N3 0.7(4) . . . . ?
C15 N3 C11 C10 175.7(2) . . . . ?
C15 N3 C11 C12 -1.3(3) . . . . ?
C16 C17 C18 C19 -179.2(3) . . . . ?
C16 C17 C18 C21 62.9(3) . . . . ?
C16 C17 C18 C23 -60.0(4) . . . . ?
C17 C18 C19 C20 -176.9(3) . . . . ?
C17 C18 C21 O5 55.2(4) . . . . ?
C17 C18 C21 N7 -127.5(3) . . . . ?
C17 C18 C23 O4 -54.0(4) . . . . ?
C17 C18 C23 N6 125.8(3) . . . . ?
C19 C18 C21 O5 -66.4(4) . . . . ?
C19 C18 C21 N7 110.9(3) . . . . ?
C19 C18 C23 O4 67.9(4) . . . . ?
C19 C18 C23 N6 -112.3(3) . . . . ?
C21 N7 C22 O6 -177.1(3) . . . . ?
C21 N7 C22 N6 4.0(4) . . . . ?
C21 C18 C19 C20 -58.4(4) . . . . ?
C21 C18 C23 O4 -173.3(3) . . . . ?
C21 C18 C23 N6 6.4(4) . . . . ?
C22 N6 C23 O4 -179.1(3) . . . . ?
C22 N6 C23 C18 1.2(4) . . . . ?
C22 N7 C21 O5 -178.6(3) . . . . ?
C22 N7 C21 C18 4.0(4) . . . . ?
C23 N6 C22 O6 174.6(3) . . . . ?
C23 N6 C22 N7 -6.7(4) . . . . ?
C23 C18 C19 C20 64.6(4) . . . . ?
C23 C18 C21 O5 174.1(3) . . . . ?
C23 C18 C21 N7 -8.6(4) . . . . ?
C24 C25 C26 C27 178.3(3) . . . . ?
C24 C25 C26 C29 -62.6(3) . . . . ?
C24 C25 C26 C31 58.0(3) . . . . ?
C25 C26 C27 C28 177.6(3) . . . . ?
C25 C26 C29 O2 -67.8(4) . . . . ?
C25 C26 C29 N5 109.4(3) . . . . ?
C25 C26 C31 O3 72.6(3) . . . . ?
C25 C26 C31 N4 -103.7(3) . . . . ?
C27 C26 C29 O2 51.9(4) . . . . ?
C27 C26 C29 N5 -130.9(3) . . . . ?
C27 C26 C31 O3 -47.9(4) . . . . ?
C27 C26 C31 N4 135.8(3) . . . . ?
C29 N5 C30 O1 -169.7(3) . . . . ?
C29 N5 C30 N4 10.9(4) . . . . ?
C29 C26 C27 C28 60.7(4) . . . . ?
C29 C26 C31 O3 -171.3(3) . . . . ?
C29 C26 C31 N4 12.5(4) . . . . ?
C30 N4 C31 O3 177.2(2) . . . . ?
C30 N4 C31 C26 -6.5(4) . . . . ?
C30 N5 C29 O2 173.3(3) . . . . ?
C30 N5 C29 C26 -3.9(4) . . . . ?
C31 N4 C30 O1 175.4(2) . . . . ?
C31 N4 C30 N5 -5.2(4) . . . . ?
C31 C26 C27 C28 -64.3(4) . . . . ?
C31 C26 C29 O2 175.7(3) . . . . ?
C31 C26 C29 N5 -7.2(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.200
_oxdiff_exptl_absorpt_empirical_full_min 0.844
####################################################################### 
# 
# 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_CCDC_1511702
_database_code_depnum_ccdc_archive 'CCDC 1511702'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
_audit_creation_date             2017-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H33 N7 O6 Zn, H2 O'
_chemical_formula_sum            'C31 H35 N7 O7 Zn'
_chemical_formula_weight         683.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H35 N7 O7 Zn'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6345(5)
_cell_length_b                   13.0965(6)
_cell_length_c                   19.4378(10)
_cell_angle_alpha                90
_cell_angle_beta                 95.957(4)
_cell_angle_gamma                90
_cell_volume                     3199.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5019
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9740
_cell_measurement_theta_min      3.4110
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 0 27 0.2695
3 0 -27 0.2695
-16 -9 0 0.0815
15 9 2 0.0585
8 -16 1 0.0705
-14 11 -2 0.0675
14 -11 1 0.0594
9 16 1 0.0649
-9 -16 0 0.0871
-10 15 0 0.0641

_exptl_crystal_size_max          0.545
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.135
loop_
_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
-3.0136 0.0027 27.0034 -0.0545 -0.1973 0.9657
3.0136 -0.0027 -27.0034 0.0545 0.1973 -0.9657
-15.9674 -8.9869 -0.0206 0.2337 0.9604 0.2706
14.9678 8.9873 2.0204 -0.2087 -0.9440 -0.1881
7.9902 -15.9863 0.9834 -0.9481 0.2424 0.0004
-13.9767 10.9927 -1.9934 0.9765 0.1877 0.0749
13.9774 -10.9928 0.9933 -0.9704 -0.1760 -0.1091
8.9771 15.9819 1.0262 0.3026 -0.9438 -0.1722
-8.9778 -15.9819 -0.0260 -0.3088 0.9321 0.2064
-9.9869 14.9878 0.0144 0.9762 -0.1386 0.0670

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.963
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     41.00  78.00   1.00   25.36    --   17.28 178.00-180.00   37
  2  ω    -13.00  60.00   1.00   25.36    --   17.28  77.00   0.00   73
  3  ω    -25.00  15.00   1.00   25.36    --   17.28 -99.00  90.00   40
  4  ω    -39.00  23.00   1.00   25.36    --  -19.31  57.00 -90.00   62
  5  ω    -16.00  50.00   1.00   25.36    --  -19.31  77.00 150.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0373008000
_diffrn_orient_matrix_UB_12      0.0402861000
_diffrn_orient_matrix_UB_13      -0.0061858000
_diffrn_orient_matrix_UB_21      -0.0399534000
_diffrn_orient_matrix_UB_22      -0.0358564000
_diffrn_orient_matrix_UB_23      -0.0117629000
_diffrn_orient_matrix_UB_31      -0.0141706000
_diffrn_orient_matrix_UB_32      -0.0050081000
_diffrn_orient_matrix_UB_33      0.0341818000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5152
_reflns_number_total             6535
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6535
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      1.031
_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)+(0.0349P)²+1.2688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0872
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 C26, C25, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Free rotating group:
 O7W(H7WA,H7WB)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C25(H25A,H25B), C27(H27A,H27B)
3.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N7(H7), C1(H1), C2(H2), C3(H3), C4(H4), C7(H7A), C8(H8), C9(H9),
 C12(H12), C13(H13), C14(H14), C15(H15)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.53087(2) 0.32446(2) 0.29594(2) 0.02933(8) Uani 1 1 d . . . . .
O1 O 0.53733(13) 0.44435(13) 0.43241(8) 0.0477(4) Uani 1 1 d . . . . .
O2 O 0.25773(14) 0.32920(14) 0.53360(9) 0.0542(5) Uani 1 1 d . . . . .
O3 O 0.36980(13) 0.17021(12) 0.33551(8) 0.0452(4) Uani 1 1 d . . . . .
O4 O 0.67102(11) 0.28126(13) 0.18229(8) 0.0402(4) Uani 1 1 d . . . . .
O5 O 0.45358(16) 0.2293(2) -0.01002(10) 0.0897(8) Uani 1 1 d . . . . .
O6 O 0.32147(12) 0.32174(13) 0.19990(8) 0.0443(4) Uani 1 1 d . . . . .
N1 N 0.63583(15) 0.19107(14) 0.32250(10) 0.0375(4) Uani 1 1 d . . . . .
N2 N 0.67871(13) 0.38777(13) 0.32177(8) 0.0287(4) Uani 1 1 d . . . . .
N3 N 0.50478(14) 0.49352(14) 0.28459(9) 0.0343(4) Uani 1 1 d . . . . .
N4 N 0.44780(14) 0.31323(13) 0.37788(9) 0.0308(4) Uani 1 1 d . . . . .
N5 N 0.39704(14) 0.38462(14) 0.48160(9) 0.0373(5) Uani 1 1 d . . . . .
H5 H 0.407281 0.431963 0.512228 0.045 Uiso 1 1 calc R . . . .
N6 N 0.49545(13) 0.29270(13) 0.19529(9) 0.0292(4) Uani 1 1 d . . . . .
N7 N 0.55794(14) 0.24636(15) 0.08879(9) 0.0388(5) Uani 1 1 d . . . . .
H7 H 0.610897 0.224713 0.068432 0.047 Uiso 1 1 calc R . . . .
C1 C 0.41177(19) 0.54170(19) 0.27154(13) 0.0436(6) Uani 1 1 d . . . . .
H1 H 0.351424 0.503218 0.257718 0.052 Uiso 1 1 calc R . . . .
C2 C 0.4012(2) 0.6456(2) 0.27763(14) 0.0506(7) Uani 1 1 d . . . . .
H2 H 0.335165 0.676874 0.268491 0.061 Uiso 1 1 calc R . . . .
C3 C 0.4909(2) 0.70237(19) 0.29757(14) 0.0538(7) Uani 1 1 d . . . . .
H3 H 0.486152 0.772899 0.301944 0.065 Uiso 1 1 calc R . . . .
C4 C 0.5876(2) 0.65396(18) 0.31102(13) 0.0449(6) Uani 1 1 d . . . . .
H4 H 0.649082 0.691210 0.324104 0.054 Uiso 1 1 calc R . . . .
C5 C 0.59152(17) 0.54861(16) 0.30467(11) 0.0329(5) Uani 1 1 d . . . . .
C6 C 0.69049(16) 0.48894(17) 0.32148(11) 0.0319(5) Uani 1 1 d . . . . .
C7 C 0.78966(19) 0.5330(2) 0.33695(13) 0.0467(6) Uani 1 1 d . . . . .
H7A H 0.797937 0.603499 0.336335 0.056 Uiso 1 1 calc R . . . .
C8 C 0.8757(2) 0.4700(2) 0.35325(15) 0.0583(7) Uani 1 1 d . . . . .
H8 H 0.943257 0.497867 0.363321 0.070 Uiso 1 1 calc R . . . .
C9 C 0.86232(19) 0.3666(2) 0.35469(14) 0.0507(7) Uani 1 1 d . . . . .
H9 H 0.920041 0.323795 0.366695 0.061 Uiso 1 1 calc R . . . .
C10 C 0.76234(17) 0.32654(18) 0.33814(11) 0.0338(5) Uani 1 1 d . . . . .
C11 C 0.73810(18) 0.21575(18) 0.33880(11) 0.0356(5) Uani 1 1 d . . . . .
C12 C 0.8146(2) 0.1417(2) 0.35497(13) 0.0530(7) Uani 1 1 d . . . . .
H12 H 0.885357 0.159785 0.366675 0.064 Uiso 1 1 calc R . . . .
C13 C 0.7844(3) 0.0407(2) 0.35347(14) 0.0635(8) Uani 1 1 d . . . . .
H13 H 0.834953 -0.010200 0.363667 0.076 Uiso 1 1 calc R . . . .
C14 C 0.6803(3) 0.0154(2) 0.33703(15) 0.0599(8) Uani 1 1 d . . . . .
H14 H 0.658713 -0.052515 0.336200 0.072 Uiso 1 1 calc R . . . .
C15 C 0.6083(2) 0.09217(18) 0.32176(14) 0.0499(7) Uani 1 1 d . . . . .
H15 H 0.537180 0.075039 0.310372 0.060 Uiso 1 1 calc R . . . .
C16 C 0.4470(4) 0.1327(3) 0.5167(2) 0.1014(13) Uani 1 1 d . . . . .
H16A H 0.496440 0.140788 0.482766 0.152 Uiso 1 1 calc GR . . . .
H16B H 0.460328 0.069101 0.540551 0.152 Uiso 1 1 calc GR . . . .
H16C H 0.455517 0.187962 0.549247 0.152 Uiso 1 1 calc GR . . . .
C17 C 0.3350(3) 0.1332(2) 0.48131(16) 0.0713(10) Uani 1 1 d . . . . .
H17A H 0.285827 0.125939 0.516162 0.086 Uiso 1 1 calc R . . . .
H17B H 0.325903 0.074299 0.451013 0.086 Uiso 1 1 calc R . . . .
C18 C 0.30540(19) 0.22961(17) 0.43870(12) 0.0401(6) Uani 1 1 d . . . . .
C19 C 0.1904(2) 0.2265(3) 0.40463(15) 0.0660(9) Uani 1 1 d . . . . .
H19A H 0.181350 0.167063 0.374827 0.079 Uiso 1 1 calc R . . . .
H19B H 0.142557 0.219356 0.440286 0.079 Uiso 1 1 calc R . . . .
C20 C 0.1604(2) 0.3210(3) 0.3625(2) 0.0898(12) Uani 1 1 d . . . . .
H20A H 0.210667 0.331437 0.329386 0.135 Uiso 1 1 calc GR . . . .
H20B H 0.160900 0.379147 0.392633 0.135 Uiso 1 1 calc GR . . . .
H20C H 0.090454 0.312585 0.338696 0.135 Uiso 1 1 calc GR . . . .
C21 C 0.37743(17) 0.23637(16) 0.38031(11) 0.0331(5) Uani 1 1 d . . . . .
C22 C 0.46496(17) 0.38264(17) 0.42990(11) 0.0331(5) Uani 1 1 d . . . . .
C23 C 0.31621(18) 0.31884(17) 0.48817(11) 0.0373(5) Uani 1 1 d . . . . .
C24 C 0.2998(4) 0.1049(3) 0.0974(3) 0.141(2) Uani 1 1 d . U . . .
H24A H 0.353691 0.075918 0.071979 0.212 Uiso 1 1 calc GR . . . .
H24B H 0.236384 0.064284 0.090369 0.212 Uiso 1 1 calc GR . . . .
H24C H 0.324750 0.106114 0.145793 0.212 Uiso 1 1 calc GR . . . .
C25 C 0.2763(3) 0.2102(4) 0.07303(19) 0.0968(13) Uani 1 1 d . U . . .
H25A H 0.215877 0.235473 0.094954 0.116 Uiso 1 1 calc R . . . .
H25B H 0.255682 0.208323 0.023562 0.116 Uiso 1 1 calc R . . . .
C26 C 0.36854(19) 0.2852(2) 0.08749(13) 0.0491(6) Uani 1 1 d . U . . .
C27 C 0.3365(3) 0.3912(3) 0.05671(16) 0.0889(13) Uani 1 1 d . . . . .
H27A H 0.318631 0.384233 0.007184 0.107 Uiso 1 1 calc R . . . .
H27B H 0.273235 0.414552 0.076360 0.107 Uiso 1 1 calc R . . . .
C28 C 0.4229(4) 0.4710(3) 0.0700(2) 0.1209(19) Uani 1 1 d . . . . .
H28A H 0.400218 0.533387 0.047129 0.181 Uiso 1 1 calc GR . . . .
H28B H 0.486769 0.447182 0.052539 0.181 Uiso 1 1 calc GR . . . .
H28C H 0.436405 0.482972 0.118877 0.181 Uiso 1 1 calc GR . . . .
C29 C 0.4623(2) 0.2497(2) 0.05086(13) 0.0520(7) Uani 1 1 d . . . . .
C30 C 0.57860(17) 0.27466(15) 0.15763(11) 0.0293(5) Uani 1 1 d . . . . .
C31 C 0.39398(17) 0.29916(16) 0.16511(11) 0.0339(5) Uani 1 1 d . . . . .
O7W O 0.12612(18) 0.44665(19) 0.1841(2) 0.1066(9) Uani 1 1 d . . . . .
H7WA H 0.139002 0.509569 0.178133 0.160 Uiso 1 1 d G . . . .
H7WB H 0.184325 0.414277 0.192036 0.160 Uiso 1 1 d G . . . .


_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
Zn1 N1 2.2215(18) . ?
Zn1 N2 2.0577(17) . ?
Zn1 N3 2.2460(18) . ?
Zn1 N4 2.0017(17) . ?
Zn1 N6 2.0048(17) . ?
O1 C22 1.217(2) . ?
O2 C23 1.216(3) . ?
O3 C21 1.225(2) . ?
O4 C30 1.218(2) . ?
O5 C29 1.207(3) . ?
O6 C31 1.230(3) . ?
N1 C11 1.338(3) . ?
N1 C15 1.341(3) . ?
N2 C6 1.333(3) . ?
N2 C10 1.338(3) . ?
N3 C1 1.335(3) . ?
N3 C5 1.336(3) . ?
N4 C21 1.347(3) . ?
N4 C22 1.360(3) . ?
N5 H5 0.8600 . ?
N5 C22 1.388(3) . ?
N5 C23 1.352(3) . ?
N6 C30 1.362(3) . ?
N6 C31 1.356(3) . ?
N7 H7 0.8600 . ?
N7 C29 1.349(3) . ?
N7 C30 1.387(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.374(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.376(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.378(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(3) . ?
C5 C6 1.482(3) . ?
C6 C7 1.384(3) . ?
C7 H7A 0.9300 . ?
C7 C8 1.376(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.365(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.375(3) . ?
C10 C11 1.483(3) . ?
C11 C12 1.383(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.376(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.361(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.368(4) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C17 1.508(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.535(4) . ?
C18 C19 1.534(4) . ?
C18 C21 1.529(3) . ?
C18 C23 1.510(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.511(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 C25 1.478(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.529(4) . ?
C26 C27 1.549(4) . ?
C26 C29 1.517(3) . ?
C26 C31 1.521(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.514(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O7W H7WA 0.8501 . ?
O7W H7WB 0.8491 . ?

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
N1 Zn1 N3 151.17(7) . . ?
N2 Zn1 N1 75.83(7) . . ?
N2 Zn1 N3 75.35(7) . . ?
N4 Zn1 N1 96.14(7) . . ?
N4 Zn1 N2 111.91(7) . . ?
N4 Zn1 N3 93.84(7) . . ?
N4 Zn1 N6 132.76(7) . . ?
N6 Zn1 N1 97.53(7) . . ?
N6 Zn1 N2 115.26(7) . . ?
N6 Zn1 N3 95.34(7) . . ?
C11 N1 Zn1 113.81(15) . . ?
C11 N1 C15 118.6(2) . . ?
C15 N1 Zn1 127.52(17) . . ?
C6 N2 Zn1 119.88(14) . . ?
C6 N2 C10 120.72(19) . . ?
C10 N2 Zn1 119.40(14) . . ?
C1 N3 Zn1 127.01(15) . . ?
C1 N3 C5 118.7(2) . . ?
C5 N3 Zn1 113.33(14) . . ?
C21 N4 Zn1 119.03(14) . . ?
C21 N4 C22 121.89(17) . . ?
C22 N4 Zn1 119.08(13) . . ?
C22 N5 H5 117.1 . . ?
C23 N5 H5 117.1 . . ?
C23 N5 C22 125.89(18) . . ?
C30 N6 Zn1 117.00(14) . . ?
C31 N6 Zn1 120.96(14) . . ?
C31 N6 C30 121.71(18) . . ?
C29 N7 H7 117.0 . . ?
C29 N7 C30 125.93(19) . . ?
C30 N7 H7 117.0 . . ?
N3 C1 H1 118.5 . . ?
N3 C1 C2 122.9(2) . . ?
C2 C1 H1 118.5 . . ?
C1 C2 H2 120.8 . . ?
C1 C2 C3 118.4(2) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.5(2) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.7(2) . . ?
C5 C4 H4 120.7 . . ?
N3 C5 C4 121.8(2) . . ?
N3 C5 C6 115.30(18) . . ?
C4 C5 C6 122.8(2) . . ?
N2 C6 C5 115.66(18) . . ?
N2 C6 C7 120.8(2) . . ?
C7 C6 C5 123.5(2) . . ?
C6 C7 H7A 120.8 . . ?
C8 C7 C6 118.5(2) . . ?
C8 C7 H7A 120.8 . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.2(2) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.1(2) . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 120.7(2) . . ?
N2 C10 C11 115.44(19) . . ?
C9 C10 C11 123.8(2) . . ?
N1 C11 C10 115.44(19) . . ?
N1 C11 C12 121.3(2) . . ?
C12 C11 C10 123.3(2) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.5(3) . . ?
C15 C14 H14 120.8 . . ?
N1 C15 C14 122.8(3) . . ?
N1 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
C16 C17 H17A 108.6 . . ?
C16 C17 H17B 108.6 . . ?
C16 C17 C18 114.5(2) . . ?
H17A C17 H17B 107.6 . . ?
C18 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
C19 C18 C17 112.2(2) . . ?
C21 C18 C17 108.5(2) . . ?
C21 C18 C19 106.93(19) . . ?
C23 C18 C17 107.0(2) . . ?
C23 C18 C19 108.3(2) . . ?
C23 C18 C21 113.97(18) . . ?
C18 C19 H19A 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 C18 112.7(2) . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 N4 120.48(19) . . ?
O3 C21 C18 118.53(19) . . ?
N4 C21 C18 120.99(18) . . ?
O1 C22 N4 122.31(18) . . ?
O1 C22 N5 118.48(19) . . ?
N4 C22 N5 119.20(18) . . ?
O2 C23 N5 121.3(2) . . ?
O2 C23 C18 121.8(2) . . ?
N5 C23 C18 116.88(18) . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
C24 C25 H25A 108.6 . . ?
C24 C25 H25B 108.6 . . ?
C24 C25 C26 114.6(3) . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 H25A 108.6 . . ?
C26 C25 H25B 108.6 . . ?
C25 C26 C27 109.9(3) . . ?
C29 C26 C25 109.5(2) . . ?
C29 C26 C27 106.2(2) . . ?
C29 C26 C31 114.0(2) . . ?
C31 C26 C25 109.8(2) . . ?
C31 C26 C27 107.2(2) . . ?
C26 C27 H27A 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 C26 113.4(3) . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O5 C29 N7 120.9(2) . . ?
O5 C29 C26 122.1(2) . . ?
N7 C29 C26 116.9(2) . . ?
O4 C30 N6 122.51(19) . . ?
O4 C30 N7 118.38(18) . . ?
N6 C30 N7 119.11(19) . . ?
O6 C31 N6 120.1(2) . . ?
O6 C31 C26 118.8(2) . . ?
N6 C31 C26 120.98(19) . . ?
H7WA O7W H7WB 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5 O1 0.86 2.03 2.865(2) 164.1 3_666
N7 H7 O2 0.86 2.16 3.011(2) 170.8 4_665
O7W H7WA O3 0.85 2.12 2.954(3) 165.9 2
O7W H7WB O6 0.85 2.11 2.950(3) 172.1 .

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
Zn1 N1 C11 C10 1.6(2) . . . . ?
Zn1 N1 C11 C12 -178.37(17) . . . . ?
Zn1 N1 C15 C14 177.85(19) . . . . ?
Zn1 N2 C6 C5 2.4(2) . . . . ?
Zn1 N2 C6 C7 -178.32(16) . . . . ?
Zn1 N2 C10 C9 179.10(17) . . . . ?
Zn1 N2 C10 C11 -2.5(2) . . . . ?
Zn1 N3 C1 C2 167.97(19) . . . . ?
Zn1 N3 C5 C4 -170.55(17) . . . . ?
Zn1 N3 C5 C6 7.7(2) . . . . ?
Zn1 N4 C21 O3 5.1(3) . . . . ?
Zn1 N4 C21 C18 -174.81(16) . . . . ?
Zn1 N4 C22 O1 -8.6(3) . . . . ?
Zn1 N4 C22 N5 170.47(16) . . . . ?
Zn1 N6 C30 O4 -3.0(3) . . . . ?
Zn1 N6 C30 N7 176.16(15) . . . . ?
Zn1 N6 C31 O6 -2.2(3) . . . . ?
Zn1 N6 C31 C26 173.99(17) . . . . ?
N1 C11 C12 C13 0.7(4) . . . . ?
N2 C6 C7 C8 -0.6(3) . . . . ?
N2 C10 C11 N1 0.4(3) . . . . ?
N2 C10 C11 C12 -179.6(2) . . . . ?
N3 C1 C2 C3 0.5(4) . . . . ?
N3 C5 C6 N2 -7.0(3) . . . . ?
N3 C5 C6 C7 173.8(2) . . . . ?
C1 N3 C5 C4 -1.2(3) . . . . ?
C1 N3 C5 C6 177.07(19) . . . . ?
C1 C2 C3 C4 -0.3(4) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
C3 C4 C5 N3 1.4(4) . . . . ?
C3 C4 C5 C6 -176.7(2) . . . . ?
C4 C5 C6 N2 171.3(2) . . . . ?
C4 C5 C6 C7 -8.0(3) . . . . ?
C5 N3 C1 C2 0.2(3) . . . . ?
C5 C6 C7 C8 178.6(2) . . . . ?
C6 N2 C10 C9 -0.3(3) . . . . ?
C6 N2 C10 C11 178.06(18) . . . . ?
C6 C7 C8 C9 -0.7(4) . . . . ?
C7 C8 C9 C10 1.5(4) . . . . ?
C8 C9 C10 N2 -1.0(4) . . . . ?
C8 C9 C10 C11 -179.2(2) . . . . ?
C9 C10 C11 N1 178.8(2) . . . . ?
C9 C10 C11 C12 -1.3(3) . . . . ?
C10 N2 C6 C5 -178.15(17) . . . . ?
C10 N2 C6 C7 1.1(3) . . . . ?
C10 C11 C12 C13 -179.3(2) . . . . ?
C11 N1 C15 C14 0.1(4) . . . . ?
C11 C12 C13 C14 -0.8(4) . . . . ?
C12 C13 C14 C15 0.5(4) . . . . ?
C13 C14 C15 N1 -0.2(4) . . . . ?
C15 N1 C11 C10 179.7(2) . . . . ?
C15 N1 C11 C12 -0.3(3) . . . . ?
C16 C17 C18 C19 -179.3(3) . . . . ?
C16 C17 C18 C21 62.7(3) . . . . ?
C16 C17 C18 C23 -60.7(3) . . . . ?
C17 C18 C19 C20 -180.0(2) . . . . ?
C17 C18 C21 O3 64.9(3) . . . . ?
C17 C18 C21 N4 -115.1(2) . . . . ?
C17 C18 C23 O2 -66.7(3) . . . . ?
C17 C18 C23 N5 110.5(3) . . . . ?
C19 C18 C21 O3 -56.3(3) . . . . ?
C19 C18 C21 N4 123.6(2) . . . . ?
C19 C18 C23 O2 54.5(3) . . . . ?
C19 C18 C23 N5 -128.3(2) . . . . ?
C21 N4 C22 O1 170.6(2) . . . . ?
C21 N4 C22 N5 -10.4(3) . . . . ?
C21 C18 C19 C20 -61.1(3) . . . . ?
C21 C18 C23 O2 173.3(2) . . . . ?
C21 C18 C23 N5 -9.4(3) . . . . ?
C22 N4 C21 O3 -174.0(2) . . . . ?
C22 N4 C21 C18 6.0(3) . . . . ?
C22 N5 C23 O2 -176.7(2) . . . . ?
C22 N5 C23 C18 6.0(3) . . . . ?
C23 N5 C22 O1 -176.8(2) . . . . ?
C23 N5 C22 N4 4.1(4) . . . . ?
C23 C18 C19 C20 62.2(3) . . . . ?
C23 C18 C21 O3 -176.0(2) . . . . ?
C23 C18 C21 N4 3.9(3) . . . . ?
C24 C25 C26 C27 177.3(3) . . . . ?
C24 C25 C26 C29 61.0(4) . . . . ?
C24 C25 C26 C31 -65.0(4) . . . . ?
C25 C26 C27 C28 178.8(3) . . . . ?
C25 C26 C29 O5 52.1(4) . . . . ?
C25 C26 C29 N7 -131.0(3) . . . . ?
C25 C26 C31 O6 -52.3(3) . . . . ?
C25 C26 C31 N6 131.5(3) . . . . ?
C27 C26 C29 O5 -66.6(4) . . . . ?
C27 C26 C29 N7 110.3(3) . . . . ?
C27 C26 C31 O6 67.1(3) . . . . ?
C27 C26 C31 N6 -109.1(3) . . . . ?
C29 N7 C30 O4 -169.8(2) . . . . ?
C29 N7 C30 N6 11.1(4) . . . . ?
C29 C26 C27 C28 -62.8(3) . . . . ?
C29 C26 C31 O6 -175.6(2) . . . . ?
C29 C26 C31 N6 8.1(3) . . . . ?
C30 N6 C31 O6 -175.5(2) . . . . ?
C30 N6 C31 C26 0.7(3) . . . . ?
C30 N7 C29 O5 175.4(3) . . . . ?
C30 N7 C29 C26 -1.6(4) . . . . ?
C31 N6 C30 O4 170.6(2) . . . . ?
C31 N6 C30 N7 -10.3(3) . . . . ?
C31 C26 C27 C28 59.5(3) . . . . ?
C31 C26 C29 O5 175.5(3) . . . . ?
C31 C26 C29 N7 -7.5(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.857
####################################################################### 
# 
# 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_CCDC_1511706
_database_code_depnum_ccdc_archive 'CCDC 1511706'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
# start Validation Reply Form

_vrf_PLAT230_I                   
;
PROBLEM:  Hirshfeld Test Diff for    C30    --  C31     ..       25.5 s.u.    
RESPONSE: 
These errors were probably caused  by disorder of the ethyl groups of 
one uncoordinated 5,5-diethylbarbiturate ligand in the crystal 
structure. One of the ethyl groups has an abnormal orientation.
;
# end Validation Reply Form 


_audit_creation_date             2017-02-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H37 N7 Ni O7, H2 O, 2(C8 H12 N2 O3)'
_chemical_formula_sum            'C44 H63 N11 Ni O14'
_chemical_formula_weight         1028.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H63 N11 Ni O14'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6756(3)
_cell_length_b                   12.8419(4)
_cell_length_c                   19.8099(7)
_cell_angle_alpha                101.496(3)
_cell_angle_beta                 96.128(3)
_cell_angle_gamma                101.120(3)
_cell_volume                     2581.44(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8121
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.2520
_cell_measurement_theta_min      3.4880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 18 -4 0.1330
1 -18 3 0.0858
0 -5 -24 0.1787
-13 -5 9 0.1698
13 6 -6 0.1973
12 8 -9 0.1889
-12 -6 11 0.1526
8 -8 -20 0.2406
-2 17 -15 0.0968
0 12 15 0.1639
-1 9 -26 0.1592
3 -2 26 0.1738
3 -17 15 0.1132
15 -5 1 0.2102
-6 -7 -17 0.1393

_exptl_crystal_size_max          0.476
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.217
loop_
_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
0.0020 17.9991 -3.9951 0.1963 0.8516 0.5199
0.9978 -17.9993 2.9957 -0.1894 -0.8808 -0.4536
0.0012 -4.9929 -24.0095 0.7901 -0.6012 -0.0202
-12.9980 -4.9978 8.9930 0.0276 0.0689 -0.9805
12.9983 5.9977 -5.9943 -0.1250 0.0252 0.9935
11.9986 7.9978 -8.9927 0.0095 0.0974 1.0026
-11.9982 -5.9979 10.9921 -0.0698 0.0328 -0.9568
7.9966 -8.0006 -19.9907 0.4310 -0.8122 0.3669
-1.9984 16.9996 -14.9904 0.6161 0.6707 0.4236
0.0024 11.9992 14.9950 -0.4629 0.8243 0.2595
-1.0002 9.0000 -25.9864 0.9316 0.0920 0.3169
3.0008 -2.0006 25.9879 -0.9610 0.2324 0.0003
2.9983 -16.9998 14.9905 -0.6428 -0.6854 -0.3623
14.9970 -5.0021 1.0009 -0.4515 -0.4585 0.7760
-5.9988 -6.9948 -17.0113 0.7082 -0.5126 -0.4784

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20865
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         2.975
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  44.00   1.00   29.43    --   20.07 -57.00 150.00   94
  2  ω     -3.00  89.00   1.00   29.43    --   20.07  57.00 -60.00   92
  3  ω    -53.00  40.00   1.00   29.43    --   20.07 -37.00  30.00   93
  4  ω     50.00  98.00   1.00   29.43    --   20.07 178.00  90.00   48
  5  ω    -33.00   4.00   1.00   29.43    --  -22.02  37.00  60.00   37
  6  ω    -31.00  -5.00   1.00   29.43    --  -22.02  57.00  90.00   26
  7  ω    -25.00  19.00   1.00   29.43    --  -22.02 -99.00  90.00   44
  8  ω    -17.00   8.00   1.00   29.43    --  -22.02 -99.00 -60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0267126000
_diffrn_orient_matrix_UB_12      0.0034478000
_diffrn_orient_matrix_UB_13      -0.0336271000
_diffrn_orient_matrix_UB_21      -0.0146861000
_diffrn_orient_matrix_UB_22      0.0505415000
_diffrn_orient_matrix_UB_23      0.0145285000
_diffrn_orient_matrix_UB_31      0.0613411000
_diffrn_orient_matrix_UB_32      0.0277813000
_diffrn_orient_matrix_UB_33      -0.0049331000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8408
_reflns_number_total             10555
_reflns_odcompleteness_completeness 96.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.415
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         10555
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0581
_refine_ls_restrained_S_all      1.022
_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)+(0.0816P)²+2.3890P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1650
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O14W-H14C
 0.86 with sigma of 0.02
 O14W-H14D
 0.86 with sigma of 0.02
 C31-C32
 1.54 with sigma of 0.04
 C30-C31
 1.54 with sigma of 0.04
 H13A-O13W
 0.86 with sigma of 0.02
 O13W-H13B
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C29) = Uanis(C30) = Uanis(C32) = Uanis(C33)
4.a Ternary CH refined with riding coordinates:
 N2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C38(H38A,H38B), C40(H40A,H40B), C30(H30A,H30B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N7(H7), C1(H1), C2(H2A), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11),
 C12(H12), N8(H8), N9(H9A), N10(H10A), N11(H11A)
4.d Idealised Me refined as rotating group:
 C13(H13C,H13D,H13E), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C29(H29A,H29B,H29C), C33(H33A,
 H33B,H33C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.53924(3) 0.79179(3) 0.71418(2) 0.03564(12) Uani 1 1 d . . . . .
O1 O 0.6228(2) 0.66624(18) 0.82664(13) 0.0517(6) Uani 1 1 d . . . . .
O2 O 1.0410(2) 0.7951(2) 0.91049(14) 0.0636(7) Uani 1 1 d . . . . .
O3 O 0.8294(2) 0.94772(19) 0.74710(13) 0.0572(6) Uani 1 1 d . . . . .
O4 O 0.8324(2) 0.6511(2) 0.46699(12) 0.0562(6) Uani 1 1 d . . . . .
O5 O 0.6912(2) 0.60665(17) 0.66506(11) 0.0457(5) Uani 1 1 d . . . . .
O6 O 0.5869(2) 0.88325(17) 0.57733(12) 0.0482(5) Uani 1 1 d . . . . .
O13W O 0.5917(2) 0.95749(17) 0.71233(13) 0.0480(5) Uani 1 1 d D . . . .
N1 N 0.3666(2) 0.7768(2) 0.64509(14) 0.0452(6) Uani 1 1 d . . . . .
N2 N 0.4381(2) 0.6342(2) 0.71077(14) 0.0446(6) Uani 1 1 d . . . . .
H2 H 0.499352 0.589490 0.720803 0.053 Uiso 1 1 calc R . . . .
N3 N 0.4509(2) 0.8265(2) 0.80130(13) 0.0419(6) Uani 1 1 d . . . . .
N4 N 0.7180(2) 0.80604(18) 0.78278(12) 0.0349(5) Uani 1 1 d . . . . .
N5 N 0.8337(2) 0.7302(2) 0.86327(14) 0.0467(6) Uani 1 1 d . . . . .
H5 H 0.830955 0.678511 0.885136 0.056 Uiso 1 1 calc R . . . .
N6 N 0.6323(2) 0.74623(19) 0.62471(12) 0.0350(5) Uani 1 1 d . . . . .
N7 N 0.7663(3) 0.6393(2) 0.56869(13) 0.0449(6) Uani 1 1 d . . . . .
H7 H 0.811477 0.591329 0.571879 0.054 Uiso 1 1 calc R . . . .
C1 C 0.3208(3) 0.8562(3) 0.6251(2) 0.0563(8) Uani 1 1 d . . . . .
H1 H 0.361570 0.927851 0.646210 0.068 Uiso 1 1 calc R . . . .
C2 C 0.2159(4) 0.8373(4) 0.5748(2) 0.0701(11) Uani 1 1 d . . . . .
H2A H 0.186674 0.895040 0.561573 0.084 Uiso 1 1 calc R . . . .
C3 C 0.1544(4) 0.7319(4) 0.5442(2) 0.0731(12) Uani 1 1 d . . . . .
H3 H 0.082700 0.717232 0.509977 0.088 Uiso 1 1 calc R . . . .
C4 C 0.1994(3) 0.6481(3) 0.56444(19) 0.0589(9) Uani 1 1 d . . . . .
H4 H 0.158625 0.575989 0.544629 0.071 Uiso 1 1 calc R . . . .
C5 C 0.3069(3) 0.6738(3) 0.61503(17) 0.0480(7) Uani 1 1 d . . . . .
C6 C 0.3683(3) 0.5901(3) 0.64006(19) 0.0530(8) Uani 1 1 d . . . . .
H6A H 0.302235 0.526263 0.639463 0.064 Uiso 1 1 calc R . . . .
H6B H 0.427603 0.568112 0.609048 0.064 Uiso 1 1 calc R . . . .
C7 C 0.3483(3) 0.6366(3) 0.76305(19) 0.0515(8) Uani 1 1 d . . . . .
H7A H 0.352790 0.577366 0.786282 0.062 Uiso 1 1 calc R . . . .
H7B H 0.260861 0.624046 0.739038 0.062 Uiso 1 1 calc R . . . .
C8 C 0.3763(3) 0.7417(3) 0.81711(17) 0.0446(7) Uani 1 1 d . . . . .
C9 C 0.3240(3) 0.7515(3) 0.87860(19) 0.0568(9) Uani 1 1 d . . . . .
H9 H 0.272301 0.691305 0.888792 0.068 Uiso 1 1 calc R . . . .
C10 C 0.3495(4) 0.8507(4) 0.92395(19) 0.0626(10) Uani 1 1 d . . . . .
H10 H 0.315651 0.859060 0.965554 0.075 Uiso 1 1 calc R . . . .
C11 C 0.4260(4) 0.9379(3) 0.90716(19) 0.0592(9) Uani 1 1 d . . . . .
H11 H 0.443924 1.006530 0.936958 0.071 Uiso 1 1 calc R . . . .
C12 C 0.4752(3) 0.9223(3) 0.84613(17) 0.0497(7) Uani 1 1 d . . . . .
H12 H 0.528143 0.981446 0.835411 0.060 Uiso 1 1 calc R . . . .
C13 C 1.0369(5) 0.7628(5) 0.7329(3) 0.0958(16) Uani 1 1 d . . . . .
H13C H 0.955890 0.749568 0.702944 0.144 Uiso 1 1 calc GR . . . .
H13D H 1.034610 0.707433 0.759219 0.144 Uiso 1 1 calc GR . . . .
H13E H 1.105271 0.761229 0.705197 0.144 Uiso 1 1 calc GR . . . .
C14 C 1.0599(3) 0.8721(4) 0.7817(2) 0.0725(13) Uani 1 1 d . . . . .
H14A H 1.065943 0.927389 0.754525 0.087 Uiso 1 1 calc R . . . .
H14B H 1.142428 0.884708 0.811191 0.087 Uiso 1 1 calc R . . . .
C15 C 0.9546(3) 0.8861(3) 0.82887(17) 0.0462(7) Uani 1 1 d . . . . .
C16 C 0.9899(5) 0.9987(3) 0.8796(3) 0.0878(16) Uani 1 1 d . . . . .
H16A H 1.069002 1.003589 0.910303 0.105 Uiso 1 1 calc R . . . .
H16B H 1.006976 1.054234 0.852996 0.105 Uiso 1 1 calc R . . . .
C17 C 0.8880(7) 1.0228(5) 0.9234(3) 0.128(3) Uani 1 1 d . . . . .
H17A H 0.809999 1.020794 0.893700 0.191 Uiso 1 1 calc GR . . . .
H17B H 0.917366 1.093798 0.953748 0.191 Uiso 1 1 calc GR . . . .
H17C H 0.871460 0.969219 0.950824 0.191 Uiso 1 1 calc GR . . . .
C18 C 0.9483(3) 0.8012(3) 0.87123(16) 0.0443(7) Uani 1 1 d . . . . .
C19 C 0.7200(3) 0.7328(2) 0.82310(15) 0.0391(6) Uani 1 1 d . . . . .
C20 C 0.8273(3) 0.8795(2) 0.78327(16) 0.0399(6) Uani 1 1 d . . . . .
C21 C 0.9022(4) 0.9202(4) 0.5681(3) 0.0875(15) Uani 1 1 d . . . . .
H21A H 0.961540 0.982307 0.561279 0.131 Uiso 1 1 calc GR . . . .
H21B H 0.948048 0.864943 0.575150 0.131 Uiso 1 1 calc GR . . . .
H21C H 0.862024 0.941466 0.608193 0.131 Uiso 1 1 calc GR . . . .
C22 C 0.8011(4) 0.8765(3) 0.5053(2) 0.0681(11) Uani 1 1 d . . . . .
H22A H 0.843028 0.858498 0.464719 0.082 Uiso 1 1 calc R . . . .
H22B H 0.755736 0.933016 0.498460 0.082 Uiso 1 1 calc R . . . .
C23 C 0.7011(3) 0.7739(3) 0.51001(16) 0.0435(7) Uani 1 1 d . . . . .
C24 C 0.5976(4) 0.7387(4) 0.44485(19) 0.0709(11) Uani 1 1 d . . . . .
H24A H 0.562666 0.801019 0.438530 0.085 Uiso 1 1 calc R . . . .
H24B H 0.638238 0.716298 0.404478 0.085 Uiso 1 1 calc R . . . .
C25 C 0.4875(5) 0.6466(4) 0.4478(3) 0.0914(15) Uani 1 1 d . . . . .
H25A H 0.436015 0.619611 0.402580 0.137 Uiso 1 1 calc GR . . . .
H25B H 0.434936 0.672847 0.480879 0.137 Uiso 1 1 calc GR . . . .
H25C H 0.521641 0.588968 0.461736 0.137 Uiso 1 1 calc GR . . . .
C26 C 0.7722(3) 0.6839(2) 0.51235(15) 0.0409(6) Uani 1 1 d . . . . .
C27 C 0.6943(3) 0.6636(2) 0.62193(15) 0.0363(6) Uani 1 1 d . . . . .
C28 C 0.6370(3) 0.8037(2) 0.57387(15) 0.0375(6) Uani 1 1 d . . . . .
O14W O 1.0650(3) 0.6529(3) 0.9998(2) 0.0920(11) Uani 1 1 d D . . . .
O7 O 0.9383(2) 0.5001(2) 0.59462(13) 0.0597(6) Uani 1 1 d . . . . .
O8 O 0.7523(3) 0.3995(2) 0.77092(16) 0.0762(8) Uani 1 1 d . . . . .
O9 O 1.0924(4) 0.2507(3) 0.6871(2) 0.0995(12) Uani 1 1 d . . . . .
N8 N 1.0170(3) 0.3776(2) 0.64403(14) 0.0483(6) Uani 1 1 d . . . . .
H8 H 1.074841 0.378021 0.616941 0.058 Uiso 1 1 calc R . . . .
N9 N 0.8506(3) 0.4518(2) 0.68560(14) 0.0456(6) Uani 1 1 d . . . . .
H9A H 0.804482 0.499743 0.685305 0.055 Uiso 1 1 calc R . . . .
C37 C 0.7516(7) 0.1711(4) 0.6364(4) 0.113(2) Uani 1 1 d . . . . .
H37A H 0.690520 0.216884 0.635089 0.169 Uiso 1 1 calc GR . . . .
H37B H 0.706951 0.096101 0.621399 0.169 Uiso 1 1 calc GR . . . .
H37C H 0.813300 0.187388 0.606069 0.169 Uiso 1 1 calc GR . . . .
C38 C 0.8204(5) 0.1913(3) 0.7096(3) 0.0836(14) Uani 1 1 d . . . . .
H38A H 0.869082 0.135469 0.712284 0.100 Uiso 1 1 calc R . . . .
H38B H 0.756474 0.184347 0.740731 0.100 Uiso 1 1 calc R . . . .
C39 C 0.9130(4) 0.3038(3) 0.7354(2) 0.0579(9) Uani 1 1 d . . . . .
C40 C 0.9787(5) 0.3184(5) 0.8111(2) 0.0911(17) Uani 1 1 d . . . . .
H40A H 0.912430 0.308319 0.840548 0.109 Uiso 1 1 calc R . . . .
H40B H 1.027362 0.262255 0.812700 0.109 Uiso 1 1 calc R . . . .
C41 C 1.0693(6) 0.4296(6) 0.8404(3) 0.117(2) Uani 1 1 d . . . . .
H41A H 1.113352 0.430969 0.885563 0.175 Uiso 1 1 calc GR . . . .
H41B H 1.020159 0.485193 0.844470 0.175 Uiso 1 1 calc GR . . . .
H41C H 1.131413 0.442669 0.809722 0.175 Uiso 1 1 calc GR . . . .
C42 C 0.8323(3) 0.3882(3) 0.73327(18) 0.0509(8) Uani 1 1 d . . . . .
C43 C 0.9351(3) 0.4463(2) 0.63858(16) 0.0423(7) Uani 1 1 d . . . . .
C44 C 1.0161(4) 0.3080(3) 0.6885(2) 0.0610(10) Uani 1 1 d . . . . .
O10 O 0.8022(2) 0.5401(2) 0.93320(14) 0.0624(7) Uani 1 1 d . . . . .
O11 O 0.6105(3) 0.1895(2) 0.91286(17) 0.0784(8) Uani 1 1 d . . . . .
O12 O 0.3957(3) 0.4260(3) 0.8220(3) 0.1213(16) Uani 1 1 d . . . . .
N10 N 0.7008(3) 0.3664(2) 0.92859(15) 0.0518(7) Uani 1 1 d . . . . .
H10A H 0.767303 0.357489 0.953457 0.062 Uiso 1 1 calc R . . . .
N11 N 0.5955(3) 0.4825(2) 0.88111(15) 0.0503(7) Uani 1 1 d . . . . .
H11A H 0.596128 0.546793 0.874537 0.060 Uiso 1 1 calc R . . . .
C29 C 0.4507(8) 0.1984(6) 0.7605(4) 0.1380(13) Uani 1 1 d . . . . .
H29A H 0.388686 0.155991 0.721269 0.207 Uiso 1 1 calc GR . . . .
H29B H 0.519616 0.161579 0.767439 0.207 Uiso 1 1 calc GR . . . .
H29C H 0.484925 0.268534 0.751957 0.207 Uiso 1 1 calc GR . . . .
C30 C 0.3862(8) 0.2125(6) 0.8247(4) 0.1380(13) Uani 1 1 d D . . . .
H30A H 0.303782 0.231733 0.814672 0.166 Uiso 1 1 calc R . . . .
H30B H 0.371589 0.145594 0.841251 0.166 Uiso 1 1 calc R . . . .
C31 C 0.4728(4) 0.2986(3) 0.8759(3) 0.0758(13) Uani 1 1 d D . . . .
C32 C 0.3909(8) 0.3241(6) 0.9481(4) 0.1380(13) Uani 1 1 d D . . . .
H32A H 0.446855 0.382048 0.983924 0.166 Uiso 1 1 calc R . . . .
H32B H 0.315112 0.350186 0.933882 0.166 Uiso 1 1 calc R . . . .
C33 C 0.3540(8) 0.2395(6) 0.9758(4) 0.1380(13) Uani 1 1 d . . . . .
H33A H 0.311323 0.177342 0.939573 0.207 Uiso 1 1 calc GR . . . .
H33B H 0.295638 0.256249 1.007976 0.207 Uiso 1 1 calc GR . . . .
H33C H 0.428274 0.223482 1.000051 0.207 Uiso 1 1 calc GR . . . .
C34 C 0.5993(4) 0.2778(3) 0.90575(19) 0.0560(8) Uani 1 1 d . . . . .
C35 C 0.7055(3) 0.4674(3) 0.91537(17) 0.0475(7) Uani 1 1 d . . . . .
C36 C 0.4838(4) 0.4054(3) 0.8561(2) 0.0659(10) Uani 1 1 d . . . . .
H14C H 1.058(6) 0.685(4) 0.967(2) 0.112(19) Uiso 1 1 d D . . . .
H14D H 0.996(4) 0.605(4) 0.984(3) 0.13(2) Uiso 1 1 d D . . . .
H13A H 0.581(5) 0.942(4) 0.6673(10) 0.106(19) Uiso 1 1 d D . . . .
H13B H 0.673(3) 0.967(5) 0.730(3) 0.15(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O13W 2.102(2) . ?
Ni1 N1 2.127(3) . ?
Ni1 N2 2.086(2) . ?
Ni1 N3 2.066(2) . ?
Ni1 N4 2.176(2) . ?
Ni1 N6 2.158(2) . ?
O1 C19 1.229(3) . ?
O2 C18 1.217(4) . ?
O3 C20 1.236(3) . ?
O4 C26 1.214(4) . ?
O5 C27 1.230(3) . ?
O6 C28 1.235(3) . ?
O13W H13A 0.865(19) . ?
O13W H13B 0.88(2) . ?
N1 C1 1.321(4) . ?
N1 C5 1.339(4) . ?
N2 H2 0.9800 . ?
N2 C6 1.462(4) . ?
N2 C7 1.484(4) . ?
N3 C8 1.332(4) . ?
N3 C12 1.328(4) . ?
N4 C19 1.351(3) . ?
N4 C20 1.350(4) . ?
N5 H5 0.8600 . ?
N5 C18 1.350(4) . ?
N5 C19 1.389(4) . ?
N6 C27 1.350(3) . ?
N6 C28 1.362(4) . ?
N7 H7 0.8600 . ?
N7 C26 1.354(4) . ?
N7 C27 1.391(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.366(5) . ?
C2 H2A 0.9300 . ?
C2 C3 1.370(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.370(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.381(5) . ?
C5 C6 1.498(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.503(5) . ?
C8 C9 1.387(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.364(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.373(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.363(5) . ?
C12 H12 0.9300 . ?
C13 H13C 0.9600 . ?
C13 H13D 0.9600 . ?
C13 H13E 0.9600 . ?
C13 C14 1.497(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.551(5) . ?
C15 C16 1.540(5) . ?
C15 C18 1.499(4) . ?
C15 C20 1.527(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.502(9) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 C22 1.493(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.553(5) . ?
C23 C24 1.537(5) . ?
C23 C26 1.505(4) . ?
C23 C28 1.520(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.513(7) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
O14W H14C 0.84(2) . ?
O14W H14D 0.85(2) . ?
O7 C43 1.214(4) . ?
O8 C42 1.203(4) . ?
O9 C44 1.198(4) . ?
N8 H8 0.8600 . ?
N8 C43 1.367(4) . ?
N8 C44 1.374(4) . ?
N9 H9A 0.8600 . ?
N9 C42 1.372(4) . ?
N9 C43 1.365(4) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C37 C38 1.503(8) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.540(6) . ?
C39 C40 1.546(6) . ?
C39 C42 1.513(5) . ?
C39 C44 1.514(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.526(8) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
O10 C35 1.217(4) . ?
O11 C34 1.196(4) . ?
O12 C36 1.201(5) . ?
N10 H10A 0.8600 . ?
N10 C34 1.374(4) . ?
N10 C35 1.366(4) . ?
N11 H11A 0.8600 . ?
N11 C35 1.359(4) . ?
N11 C36 1.367(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C29 C30 1.505(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.437(8) . ?
C31 C32 1.763(8) . ?
C31 C34 1.509(6) . ?
C31 C36 1.487(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.325(8) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 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
O13W Ni1 N1 89.47(10) . . ?
O13W Ni1 N4 90.55(9) . . ?
O13W Ni1 N6 91.41(9) . . ?
N1 Ni1 N4 178.68(9) . . ?
N1 Ni1 N6 88.68(9) . . ?
N2 Ni1 O13W 164.82(10) . . ?
N2 Ni1 N1 77.16(10) . . ?
N2 Ni1 N4 102.98(9) . . ?
N2 Ni1 N6 95.40(9) . . ?
N3 Ni1 O13W 91.83(10) . . ?
N3 Ni1 N1 92.57(10) . . ?
N3 Ni1 N2 81.75(10) . . ?
N3 Ni1 N4 88.75(9) . . ?
N3 Ni1 N6 176.54(9) . . ?
N6 Ni1 N4 90.00(9) . . ?
Ni1 O13W H13A 91(3) . . ?
Ni1 O13W H13B 96(4) . . ?
H13A O13W H13B 112(6) . . ?
C1 N1 Ni1 127.4(2) . . ?
C1 N1 C5 118.4(3) . . ?
C5 N1 Ni1 114.0(2) . . ?
Ni1 N2 H2 109.4 . . ?
C6 N2 Ni1 107.13(19) . . ?
C6 N2 H2 109.4 . . ?
C6 N2 C7 111.4(3) . . ?
C7 N2 Ni1 110.16(19) . . ?
C7 N2 H2 109.4 . . ?
C8 N3 Ni1 115.9(2) . . ?
C12 N3 Ni1 125.1(2) . . ?
C12 N3 C8 118.5(3) . . ?
C19 N4 Ni1 117.55(18) . . ?
C20 N4 Ni1 122.96(18) . . ?
C20 N4 C19 119.3(2) . . ?
C18 N5 H5 116.9 . . ?
C18 N5 C19 126.2(2) . . ?
C19 N5 H5 116.9 . . ?
C27 N6 Ni1 118.82(17) . . ?
C27 N6 C28 119.7(2) . . ?
C28 N6 Ni1 121.30(18) . . ?
C26 N7 H7 116.8 . . ?
C26 N7 C27 126.3(2) . . ?
C27 N7 H7 116.8 . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.8(4) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2A 120.6 . . ?
C1 C2 C3 118.8(4) . . ?
C3 C2 H2A 120.6 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.5(3) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.9 . . ?
C3 C4 C5 118.2(4) . . ?
C5 C4 H4 120.9 . . ?
N1 C5 C4 122.3(3) . . ?
N1 C5 C6 114.2(3) . . ?
C4 C5 C6 123.5(3) . . ?
N2 C6 C5 110.4(3) . . ?
N2 C6 H6A 109.6 . . ?
N2 C6 H6B 109.6 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
N2 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
N2 C7 C8 113.9(3) . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
N3 C8 C7 115.9(3) . . ?
N3 C8 C9 121.7(3) . . ?
C9 C8 C7 122.4(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 120.5 . . ?
C9 C10 C11 118.9(3) . . ?
C11 C10 H10 120.5 . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 118.9(4) . . ?
C12 C11 H11 120.5 . . ?
N3 C12 C11 122.9(3) . . ?
N3 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
H13C C13 H13D 109.5 . . ?
H13C C13 H13E 109.5 . . ?
H13D C13 H13E 109.5 . . ?
C14 C13 H13C 109.5 . . ?
C14 C13 H13D 109.5 . . ?
C14 C13 H13E 109.5 . . ?
C13 C14 H14A 108.6 . . ?
C13 C14 H14B 108.6 . . ?
C13 C14 C15 114.7(3) . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C16 C15 C14 111.0(3) . . ?
C18 C15 C14 107.8(3) . . ?
C18 C15 C16 107.9(3) . . ?
C18 C15 C20 113.9(2) . . ?
C20 C15 C14 109.0(3) . . ?
C20 C15 C16 107.3(3) . . ?
C15 C16 H16A 108.6 . . ?
C15 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 C15 114.5(4) . . ?
C17 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 N5 121.1(3) . . ?
O2 C18 C15 122.4(3) . . ?
N5 C18 C15 116.5(3) . . ?
O1 C19 N4 122.4(3) . . ?
O1 C19 N5 116.7(3) . . ?
N4 C19 N5 120.9(2) . . ?
O3 C20 N4 121.3(3) . . ?
O3 C20 C15 115.6(3) . . ?
N4 C20 C15 123.1(2) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
C21 C22 H22A 108.8 . . ?
C21 C22 H22B 108.8 . . ?
C21 C22 C23 113.8(3) . . ?
H22A C22 H22B 107.7 . . ?
C23 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
C24 C23 C22 109.9(3) . . ?
C26 C23 C22 107.5(3) . . ?
C26 C23 C24 108.7(3) . . ?
C26 C23 C28 113.8(2) . . ?
C28 C23 C22 107.9(3) . . ?
C28 C23 C24 109.0(3) . . ?
C23 C24 H24A 108.7 . . ?
C23 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 C23 114.1(3) . . ?
C25 C24 H24A 108.7 . . ?
C25 C24 H24B 108.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O4 C26 N7 120.2(3) . . ?
O4 C26 C23 123.3(3) . . ?
N7 C26 C23 116.4(2) . . ?
O5 C27 N6 123.1(3) . . ?
O5 C27 N7 116.6(2) . . ?
N6 C27 N7 120.3(2) . . ?
O6 C28 N6 120.8(3) . . ?
O6 C28 C23 116.4(2) . . ?
N6 C28 C23 122.8(2) . . ?
H14C O14W H14D 94(5) . . ?
C43 N8 H8 116.8 . . ?
C43 N8 C44 126.4(3) . . ?
C44 N8 H8 116.8 . . ?
C42 N9 H9A 116.9 . . ?
C43 N9 H9A 116.9 . . ?
C43 N9 C42 126.3(3) . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
C37 C38 H38A 108.7 . . ?
C37 C38 H38B 108.7 . . ?
C37 C38 C39 114.2(3) . . ?
H38A C38 H38B 107.6 . . ?
C39 C38 H38A 108.7 . . ?
C39 C38 H38B 108.7 . . ?
C38 C39 C40 110.9(4) . . ?
C42 C39 C38 106.9(3) . . ?
C42 C39 C40 109.0(3) . . ?
C42 C39 C44 114.6(3) . . ?
C44 C39 C38 106.9(3) . . ?
C44 C39 C40 108.6(3) . . ?
C39 C40 H40A 108.9 . . ?
C39 C40 H40B 108.9 . . ?
H40A C40 H40B 107.7 . . ?
C41 C40 C39 113.6(4) . . ?
C41 C40 H40A 108.9 . . ?
C41 C40 H40B 108.9 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O8 C42 N9 119.8(3) . . ?
O8 C42 C39 122.2(3) . . ?
N9 C42 C39 118.0(3) . . ?
O7 C43 N8 121.6(3) . . ?
O7 C43 N9 122.0(3) . . ?
N9 C43 N8 116.4(3) . . ?
O9 C44 N8 119.6(3) . . ?
O9 C44 C39 122.7(3) . . ?
N8 C44 C39 117.7(3) . . ?
C34 N10 H10A 117.1 . . ?
C35 N10 H10A 117.1 . . ?
C35 N10 C34 125.9(3) . . ?
C35 N11 H11A 116.8 . . ?
C35 N11 C36 126.3(3) . . ?
C36 N11 H11A 116.8 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
C29 C30 H30A 110.5 . . ?
C29 C30 H30B 110.5 . . ?
H30A C30 H30B 108.7 . . ?
C31 C30 C29 106.1(6) . . ?
C31 C30 H30A 110.5 . . ?
C31 C30 H30B 110.5 . . ?
C30 C31 C32 106.2(5) . . ?
C30 C31 C34 118.4(5) . . ?
C30 C31 C36 111.8(4) . . ?
C34 C31 C32 104.5(4) . . ?
C36 C31 C32 99.1(4) . . ?
C36 C31 C34 114.3(3) . . ?
C31 C32 H32A 108.4 . . ?
C31 C32 H32B 108.4 . . ?
H32A C32 H32B 107.5 . . ?
C33 C32 C31 115.4(6) . . ?
C33 C32 H32A 108.4 . . ?
C33 C32 H32B 108.4 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O11 C34 N10 120.6(4) . . ?
O11 C34 C31 122.2(3) . . ?
N10 C34 C31 117.0(3) . . ?
O10 C35 N10 122.3(3) . . ?
O10 C35 N11 121.6(3) . . ?
N11 C35 N10 116.1(3) . . ?
O12 C36 N11 120.4(4) . . ?
O12 C36 C31 121.6(4) . . ?
N11 C36 C31 117.9(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5 O10 0.86 2.16 3.021(3) 173.4 .
N7 H7 O7 0.86 2.03 2.875(3) 169.2 .
N8 H8 O4 0.86 2.03 2.866(3) 163.1 2_766
N9 H9A O5 0.86 2.06 2.915(3) 169.5 .
N10 H10A O14W 0.86 1.97 2.820(4) 171.1 2_767
N11 H11A O1 0.86 1.95 2.763(3) 157.1 .
O14W H14C O2 0.84(2) 1.99(3) 2.811(4) 164(6) .
O14W H14D O10 0.85(2) 2.13(3) 2.931(4) 157(6) .

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
Ni1 N1 C1 C2 172.9(3) . . . . ?
Ni1 N1 C5 C4 -174.6(2) . . . . ?
Ni1 N1 C5 C6 4.2(3) . . . . ?
Ni1 N2 C6 C5 -43.5(3) . . . . ?
Ni1 N2 C7 C8 -15.7(3) . . . . ?
Ni1 N3 C8 C7 -10.3(3) . . . . ?
Ni1 N3 C8 C9 172.1(2) . . . . ?
Ni1 N3 C12 C11 -171.9(3) . . . . ?
Ni1 N4 C19 O1 -6.6(4) . . . . ?
Ni1 N4 C19 N5 173.9(2) . . . . ?
Ni1 N4 C20 O3 4.4(4) . . . . ?
Ni1 N4 C20 C15 -177.0(2) . . . . ?
Ni1 N6 C27 O5 6.4(4) . . . . ?
Ni1 N6 C27 N7 -173.4(2) . . . . ?
Ni1 N6 C28 O6 -0.6(4) . . . . ?
Ni1 N6 C28 C23 -179.8(2) . . . . ?
N1 C1 C2 C3 0.8(6) . . . . ?
N1 C5 C6 N2 26.3(4) . . . . ?
N2 C7 C8 N3 17.6(4) . . . . ?
N2 C7 C8 C9 -164.9(3) . . . . ?
N3 C8 C9 C10 0.1(5) . . . . ?
C1 N1 C5 C4 -0.2(5) . . . . ?
C1 N1 C5 C6 178.6(3) . . . . ?
C1 C2 C3 C4 -0.2(6) . . . . ?
C2 C3 C4 C5 -0.6(6) . . . . ?
C3 C4 C5 N1 0.8(5) . . . . ?
C3 C4 C5 C6 -177.9(3) . . . . ?
C4 C5 C6 N2 -154.9(3) . . . . ?
C5 N1 C1 C2 -0.6(5) . . . . ?
C6 N2 C7 C8 -134.5(3) . . . . ?
C7 N2 C6 C5 77.1(3) . . . . ?
C7 C8 C9 C10 -177.3(3) . . . . ?
C8 N3 C12 C11 -0.8(5) . . . . ?
C8 C9 C10 C11 0.2(5) . . . . ?
C9 C10 C11 C12 -0.8(6) . . . . ?
C10 C11 C12 N3 1.1(5) . . . . ?
C12 N3 C8 C7 177.7(3) . . . . ?
C12 N3 C8 C9 0.2(4) . . . . ?
C13 C14 C15 C16 177.2(4) . . . . ?
C13 C14 C15 C18 59.2(4) . . . . ?
C13 C14 C15 C20 -64.8(4) . . . . ?
C14 C15 C16 C17 175.3(4) . . . . ?
C14 C15 C18 O2 59.1(4) . . . . ?
C14 C15 C18 N5 -120.3(3) . . . . ?
C14 C15 C20 O3 -58.9(4) . . . . ?
C14 C15 C20 N4 122.4(3) . . . . ?
C16 C15 C18 O2 -60.8(5) . . . . ?
C16 C15 C18 N5 119.8(4) . . . . ?
C16 C15 C20 O3 61.3(4) . . . . ?
C16 C15 C20 N4 -117.4(4) . . . . ?
C18 N5 C19 O1 -174.4(3) . . . . ?
C18 N5 C19 N4 5.2(5) . . . . ?
C18 C15 C16 C17 -66.8(5) . . . . ?
C18 C15 C20 O3 -179.3(3) . . . . ?
C18 C15 C20 N4 2.0(4) . . . . ?
C19 N4 C20 O3 180.0(3) . . . . ?
C19 N4 C20 C15 -1.4(4) . . . . ?
C19 N5 C18 O2 176.3(3) . . . . ?
C19 N5 C18 C15 -4.3(5) . . . . ?
C20 N4 C19 O1 177.6(3) . . . . ?
C20 N4 C19 N5 -1.9(4) . . . . ?
C20 C15 C16 C17 56.3(5) . . . . ?
C20 C15 C18 O2 -179.8(3) . . . . ?
C20 C15 C18 N5 0.8(4) . . . . ?
C21 C22 C23 C24 177.1(3) . . . . ?
C21 C22 C23 C26 -64.8(4) . . . . ?
C21 C22 C23 C28 58.4(4) . . . . ?
C22 C23 C24 C25 -173.8(3) . . . . ?
C22 C23 C26 O4 -58.4(4) . . . . ?
C22 C23 C26 N7 121.7(3) . . . . ?
C22 C23 C28 O6 54.7(4) . . . . ?
C22 C23 C28 N6 -126.1(3) . . . . ?
C24 C23 C26 O4 60.5(4) . . . . ?
C24 C23 C26 N7 -119.4(3) . . . . ?
C24 C23 C28 O6 -64.6(4) . . . . ?
C24 C23 C28 N6 114.6(3) . . . . ?
C26 N7 C27 O5 172.9(3) . . . . ?
C26 N7 C27 N6 -7.3(5) . . . . ?
C26 C23 C24 C25 68.9(4) . . . . ?
C26 C23 C28 O6 174.0(3) . . . . ?
C26 C23 C28 N6 -6.9(4) . . . . ?
C27 N6 C28 O6 -176.1(3) . . . . ?
C27 N6 C28 C23 4.8(4) . . . . ?
C27 N7 C26 O4 -175.4(3) . . . . ?
C27 N7 C26 C23 4.5(5) . . . . ?
C28 N6 C27 O5 -178.0(3) . . . . ?
C28 N6 C27 N7 2.1(4) . . . . ?
C28 C23 C24 C25 -55.7(4) . . . . ?
C28 C23 C26 O4 -177.9(3) . . . . ?
C28 C23 C26 N7 2.2(4) . . . . ?
C37 C38 C39 C40 179.5(4) . . . . ?
C37 C38 C39 C42 60.8(5) . . . . ?
C37 C38 C39 C44 -62.3(5) . . . . ?
C38 C39 C40 C41 -178.5(4) . . . . ?
C38 C39 C42 O8 66.7(5) . . . . ?
C38 C39 C42 N9 -112.1(4) . . . . ?
C38 C39 C44 O9 -65.9(6) . . . . ?
C38 C39 C44 N8 111.2(4) . . . . ?
C40 C39 C42 O8 -53.3(5) . . . . ?
C40 C39 C42 N9 128.0(4) . . . . ?
C40 C39 C44 O9 53.8(6) . . . . ?
C40 C39 C44 N8 -129.1(4) . . . . ?
C42 N9 C43 O7 174.3(3) . . . . ?
C42 N9 C43 N8 -6.3(5) . . . . ?
C42 C39 C40 C41 -61.0(5) . . . . ?
C42 C39 C44 O9 175.8(4) . . . . ?
C42 C39 C44 N8 -7.0(6) . . . . ?
C43 N8 C44 O9 178.8(4) . . . . ?
C43 N8 C44 C39 1.5(6) . . . . ?
C43 N9 C42 O8 -178.3(4) . . . . ?
C43 N9 C42 C39 0.5(5) . . . . ?
C44 N8 C43 O7 -175.4(4) . . . . ?
C44 N8 C43 N9 5.2(5) . . . . ?
C44 C39 C40 C41 64.4(5) . . . . ?
C44 C39 C42 O8 -175.1(4) . . . . ?
C44 C39 C42 N9 6.1(5) . . . . ?
C29 C30 C31 C32 174.5(5) . . . . ?
C29 C30 C31 C34 -68.5(7) . . . . ?
C29 C30 C31 C36 67.5(7) . . . . ?
C30 C31 C32 C33 58.2(9) . . . . ?
C30 C31 C34 O11 -31.8(7) . . . . ?
C30 C31 C34 N10 152.0(5) . . . . ?
C30 C31 C36 O12 30.3(8) . . . . ?
C30 C31 C36 N11 -153.3(5) . . . . ?
C32 C31 C34 O11 86.1(5) . . . . ?
C32 C31 C34 N10 -90.1(4) . . . . ?
C32 C31 C36 O12 -81.2(6) . . . . ?
C32 C31 C36 N11 95.1(5) . . . . ?
C34 N10 C35 O10 -174.7(3) . . . . ?
C34 N10 C35 N11 5.4(5) . . . . ?
C34 C31 C32 C33 -67.8(8) . . . . ?
C34 C31 C36 O12 168.2(5) . . . . ?
C34 C31 C36 N11 -15.4(6) . . . . ?
C35 N10 C34 O11 170.8(4) . . . . ?
C35 N10 C34 C31 -12.9(5) . . . . ?
C35 N11 C36 O12 -174.4(4) . . . . ?
C35 N11 C36 C31 9.1(6) . . . . ?
C36 N11 C35 O10 176.9(4) . . . . ?
C36 N11 C35 N10 -3.3(5) . . . . ?
C36 C31 C32 C33 174.1(7) . . . . ?
C36 C31 C34 O11 -166.7(4) . . . . ?
C36 C31 C34 N10 17.1(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.127
_oxdiff_exptl_absorpt_empirical_full_min 0.931
