# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_zn100last_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2046660'
loop_
_audit_author_name
_audit_author_address
'Claire Deville'
;Technical University of Denmark (current)
Denmark
;
_audit_update_record             
;
2020-11-26 deposited with the CCDC.	2021-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Zn N4 O5, 3( C3 H7 N O), H2 O'
_chemical_formula_sum            'C33 H41 N7 O9 Zn'
_chemical_formula_weight         745.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3242 0.9375 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_H-M_alt        'P 41'
_space_group_name_Hall           'P 4w'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'

_cell_length_a                   13.6127(13)
_cell_length_b                   13.6127(13)
_cell_length_c                   19.6051(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3632.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9757
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      20.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   0.6272
_exptl_transmission_factor_max   0.7445
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.395
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6272
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71252
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.180
_diffrn_reflns_theta_max         20.587
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7439
_reflns_number_gt                6545
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.999

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0914P)²+1.6752P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2800 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.067(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7439
_refine_ls_number_parameters     433
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1500
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT987_zn100last_a_sq      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Refinement gives BASF = 0.080(30). Deviation from zero is likely 
a consquence of Ag radiation.  
;
_vrf_PLAT094_zn100last_a_sq      
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       3.43 Report
RESPONSE: The one "peak" > 0.5 eA-3 is in an electron density ring around 
the Zn atom.
;
_vrf_FORMU01_zn100last_a_sq      
;
PROBLEM: There is a discrepancy between the atom counts in the
 _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C33 H41 N7 O9 Zn1
            Atom count from the _atom_site data:  C30 H34 N6 O8 Zn1
RESPONSE: _chemical_formula_sum includes one additional DMF from SQUEEZE.
;
# end Validation Reply Form

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 0.52722(5) 0.17082(5) 0.47048(3) 0.0371(2) Uani 1 1 d . . . . .
N1 N 0.4087(4) 0.2533(4) 0.4547(2) 0.0399(12) Uani 1 1 d . . . . .
C1 C 0.3142(5) 0.2157(5) 0.4510(3) 0.0478(16) Uani 1 1 d . . . . .
O2 O 0.4966(4) 0.0813(3) 0.5466(2) 0.0444(10) Uani 1 1 d . . . . .
N2 N 0.3123(4) 0.3712(4) 0.4195(3) 0.0422(12) Uani 1 1 d D . . . .
H2N H 0.297(6) 0.432(3) 0.406(4) 0.063 Uiso 1 1 d D U . . .
C2 C 0.2778(6) 0.1232(6) 0.4647(4) 0.0581(18) Uani 1 1 d . . . . .
H2 H 0.318744 0.072394 0.481892 0.070 Uiso 1 1 calc R U . . .
O3 O 0.4773(3) 0.2173(3) 0.6067(2) 0.0408(10) Uani 1 1 d . . . . .
N3 N 0.6396(4) 0.2602(4) 0.4847(2) 0.0391(11) Uani 1 1 d . . . . .
C3 C 0.1806(8) 0.1080(8) 0.4523(5) 0.077(3) Uani 1 1 d . . . . .
H3 H 0.152817 0.045161 0.460896 0.092 Uiso 1 1 calc R U . . .
N4 N 0.7268(4) 0.3867(4) 0.5210(2) 0.0404(12) Uani 1 1 d D . . . .
H4N H 0.738(6) 0.447(3) 0.536(4) 0.061 Uiso 1 1 d D U . . .
O4 O 0.4430(4) -0.0751(3) 0.89836(19) 0.0404(10) Uani 1 1 d . . . . .
C4 C 0.1203(7) 0.1844(8) 0.4269(5) 0.075(2) Uani 1 1 d . . . . .
H4 H 0.052601 0.171668 0.418969 0.090 Uiso 1 1 calc R U . . .
O5 O 0.4463(3) -0.2087(3) 0.83281(19) 0.0362(9) Uani 1 1 d . . . . .
C5 C 0.1558(6) 0.2736(7) 0.4138(5) 0.065(2) Uani 1 1 d . . . . .
H5 H 0.114900 0.324059 0.396052 0.078 Uiso 1 1 calc R U . . .
C6 C 0.2533(6) 0.2903(6) 0.4266(4) 0.0541(17) Uani 1 1 d . . . . .
N6 N 0.6465(6) 0.8360(5) 0.5404(4) 0.0688(19) Uani 1 1 d . . . . .
C7 C 0.4037(5) 0.3434(5) 0.4365(3) 0.0370(13) Uani 1 1 d . . . . .
O7 O 0.5737(7) 0.8067(5) 0.4371(4) 0.094(2) Uani 1 1 d D . . . .
O8 O 0.6176(6) 0.6163(5) 0.3965(4) 0.0829(19) Uani 1 1 d D . . . .
H8WA H 0.669(5) 0.612(8) 0.372(4) 0.124 Uiso 1 1 d D U . . .
H8WB H 0.597(8) 0.675(3) 0.399(5) 0.124 Uiso 1 1 d D U . . .
C8A C 0.4886(5) 0.4133(4) 0.4320(3) 0.0354(13) Uani 0.599(15) 1 d . . P A 1
H8A H 0.533379 0.390815 0.394678 0.043 Uiso 0.599(15) 1 calc R U P A 1
C9A C 0.5487(5) 0.4186(4) 0.4998(3) 0.0358(12) Uani 0.599(15) 1 d . . P A 1
H9AA H 0.569888 0.487311 0.507278 0.043 Uiso 0.599(15) 1 calc R U P A 1
H9AB H 0.505193 0.399998 0.538169 0.043 Uiso 0.599(15) 1 calc R U P A 1
O1A O 0.4549(6) 0.5083(5) 0.4161(4) 0.042(2) Uani 0.599(15) 1 d . . P A 1
H1A H 0.502864 0.547013 0.413910 0.063 Uiso 0.599(15) 1 calc R U P A 1
C8B C 0.4886(5) 0.4133(4) 0.4320(3) 0.0354(13) Uani 0.401(15) 1 d . . P A 2
H8BA H 0.463676 0.479666 0.420750 0.043 Uiso 0.401(15) 1 calc R U P A 2
H8BB H 0.532699 0.392300 0.394565 0.043 Uiso 0.401(15) 1 calc R U P A 2
C9B C 0.5487(5) 0.4186(4) 0.4998(3) 0.0358(12) Uani 0.401(15) 1 d . . P A 2
H9B H 0.504378 0.396435 0.537476 0.043 Uiso 0.401(15) 1 calc R U P A 2
O1B O 0.5702(10) 0.5194(9) 0.5112(7) 0.055(4) Uani 0.401(15) 1 d . . P A 2
H1B H 0.564677 0.550516 0.474430 0.083 Uiso 0.401(15) 1 calc R U P A 2
C11 C 0.7912(5) 0.3080(5) 0.5174(3) 0.0447(15) Uani 1 1 d . . . . .
C10 C 0.6366(4) 0.3541(4) 0.5007(3) 0.0322(12) Uani 1 1 d . . . . .
C12 C 0.8905(6) 0.3002(6) 0.5353(4) 0.0591(18) Uani 1 1 d . . . . .
H12 H 0.927868 0.354528 0.551200 0.071 Uiso 1 1 calc R U . . .
C14 C 0.8770(6) 0.1272(6) 0.5007(5) 0.066(2) Uani 1 1 d . . . . .
H14 H 0.908606 0.065620 0.494407 0.079 Uiso 1 1 calc R U . . .
C13 C 0.9298(6) 0.2072(7) 0.5279(5) 0.070(2) Uani 1 1 d . . . . .
H13 H 0.995794 0.196699 0.541902 0.084 Uiso 1 1 calc R U . . .
C15 C 0.7804(6) 0.1382(6) 0.4834(4) 0.0590(19) Uani 1 1 d . . . . .
H15 H 0.744252 0.085001 0.464571 0.071 Uiso 1 1 calc R U . . .
C16 C 0.7360(5) 0.2295(5) 0.4939(3) 0.0440(15) Uani 1 1 d . . . . .
C17 C 0.4771(4) 0.1274(4) 0.6019(3) 0.0358(12) Uani 1 1 d . . . . .
C18 C 0.4572(4) 0.0635(4) 0.6628(3) 0.0326(12) Uani 1 1 d . . . . .
C19 C 0.4464(5) -0.0375(4) 0.6567(3) 0.0336(12) Uani 1 1 d . . . . .
H19 H 0.445715 -0.066704 0.612686 0.040 Uiso 1 1 calc R U . . .
C20 C 0.4368(4) -0.0957(4) 0.7135(3) 0.0338(12) Uani 1 1 d . . . . .
H20 H 0.428504 -0.164688 0.708684 0.041 Uiso 1 1 calc R U . . .
C21 C 0.4393(4) -0.0528(4) 0.7789(3) 0.0326(12) Uani 1 1 d . . . . .
C22 C 0.4416(5) -0.1184(5) 0.8398(3) 0.0369(13) Uani 1 1 d . . . . .
C23 C 0.4539(5) 0.1063(4) 0.7274(3) 0.0398(13) Uani 1 1 d . . . . .
H23 H 0.457632 0.175681 0.732017 0.048 Uiso 1 1 calc R U . . .
C24 C 0.4451(5) 0.0480(4) 0.7848(3) 0.0375(13) Uani 1 1 d . . . . .
H24 H 0.443062 0.077551 0.828686 0.045 Uiso 1 1 calc R U . . .
C25 C 0.7201(8) 0.6392(9) 0.2348(5) 0.088(3) Uani 1 1 d . . . . .
H25 H 0.651054 0.634993 0.228346 0.105 Uiso 1 1 calc R U . . .
C26 C 0.8832(10) 0.6553(15) 0.1874(8) 0.140(6) Uani 1 1 d . . . . .
H26A H 0.906745 0.587441 0.184032 0.211 Uiso 1 1 calc R U . . .
H26B H 0.900521 0.682156 0.232194 0.211 Uiso 1 1 calc R U . . .
H26C H 0.913896 0.695085 0.151594 0.211 Uiso 1 1 calc R U . . .
C27 C 0.7387(13) 0.6549(13) 0.1154(7) 0.141(7) Uani 1 1 d . . . . .
H27A H 0.769543 0.601341 0.089825 0.211 Uiso 1 1 calc R U . . .
H27B H 0.752246 0.717552 0.092650 0.211 Uiso 1 1 calc R U . . .
H27C H 0.667562 0.644235 0.117433 0.211 Uiso 1 1 calc R U . . .
N5 N 0.7753(8) 0.6572(8) 0.1789(5) 0.099(3) Uani 1 1 d . . . . .
O6 O 0.7513(7) 0.6275(10) 0.2942(5) 0.136(4) Uani 1 1 d D . . . .
C28 C 0.6052(7) 0.8635(6) 0.4830(4) 0.064(2) Uani 1 1 d . . . . .
H28 H 0.598433 0.932075 0.475355 0.076 Uiso 1 1 calc R U . . .
C29 C 0.6422(19) 0.7409(9) 0.5631(8) 0.188(11) Uani 1 1 d . . . . .
H29A H 0.667466 0.696853 0.527618 0.283 Uiso 1 1 calc R U . . .
H29B H 0.573918 0.723683 0.573412 0.283 Uiso 1 1 calc R U . . .
H29C H 0.682202 0.734117 0.604358 0.283 Uiso 1 1 calc R U . . .
C30 C 0.6898(7) 0.9086(7) 0.5874(5) 0.074(2) Uani 1 1 d . . . . .
H30A H 0.755171 0.886418 0.601509 0.111 Uiso 1 1 calc R U . . .
H30B H 0.647646 0.915399 0.627667 0.111 Uiso 1 1 calc R U . . .
H30C H 0.695236 0.972178 0.564287 0.111 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.965(4) 2_654 ?
Zn1 O2 1.970(4) . ?
Zn1 N3 1.974(5) . ?
Zn1 N1 1.990(5) . ?
N1 C7 1.280(8) . ?
N1 C1 1.386(9) . ?
C1 C2 1.379(10) . ?
C1 C6 1.396(11) . ?
O2 C17 1.280(7) . ?
N2 C7 1.343(8) . ?
N2 C6 1.370(10) . ?
N2 H2N 0.90(3) . ?
C2 C3 1.361(13) . ?
C2 H2 0.9500 . ?
O3 C17 1.227(7) . ?
N3 C10 1.316(8) . ?
N3 C16 1.389(9) . ?
C3 C4 1.416(15) . ?
C3 H3 0.9500 . ?
N4 C10 1.365(8) . ?
N4 C11 1.386(9) . ?
N4 H4N 0.89(3) . ?
O4 C22 1.291(7) . ?
C4 C5 1.333(13) . ?
C4 H4 0.9500 . ?
O5 C22 1.239(7) . ?
C5 C6 1.369(11) . ?
C5 H5 0.9500 . ?
N6 C28 1.312(10) . ?
N6 C29 1.370(14) . ?
N6 C30 1.474(11) . ?
C7 C8B 1.500(9) . ?
C7 C8A 1.500(9) . ?
O7 C28 1.262(10) . ?
O8 H8WA 0.85(3) . ?
O8 H8WB 0.85(3) . ?
C8A O1A 1.408(9) . ?
C8A C9A 1.562(7) . ?
C8A H8A 1.0000 . ?
C9A C10 1.485(9) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
O1A H1A 0.8400 . ?
C8B C9B 1.562(7) . ?
C8B H8BA 0.9900 . ?
C8B H8BB 0.9900 . ?
C9B O1B 1.421(14) . ?
C9B C10 1.485(9) . ?
C9B H9B 1.0000 . ?
O1B H1B 0.8400 . ?
C11 C16 1.385(10) . ?
C11 C12 1.401(10) . ?
C12 C13 1.382(12) . ?
C12 H12 0.9500 . ?
C14 C15 1.367(11) . ?
C14 C13 1.410(13) . ?
C14 H14 0.9500 . ?
C13 H13 0.9500 . ?
C15 C16 1.397(10) . ?
C15 H15 0.9500 . ?
C17 C18 1.503(8) . ?
C18 C19 1.388(8) . ?
C18 C23 1.396(8) . ?
C19 C20 1.373(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.410(8) . ?
C20 H20 0.9500 . ?
C21 C24 1.379(8) . ?
C21 C22 1.491(8) . ?
C23 C24 1.382(8) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 O6 1.250(14) . ?
C25 N5 1.351(14) . ?
C25 H25 0.9500 . ?
C26 N5 1.479(17) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 N5 1.341(17) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zn1 O2 100.27(17) 2_654 . ?
O4 Zn1 N3 110.5(2) 2_654 . ?
O2 Zn1 N3 115.96(19) . . ?
O4 Zn1 N1 115.44(19) 2_654 . ?
O2 Zn1 N1 107.1(2) . . ?
N3 Zn1 N1 107.6(2) . . ?
C7 N1 C1 106.9(5) . . ?
C7 N1 Zn1 128.8(5) . . ?
C1 N1 Zn1 123.5(5) . . ?
C2 C1 N1 131.3(7) . . ?
C2 C1 C6 121.2(7) . . ?
N1 C1 C6 107.5(6) . . ?
C17 O2 Zn1 112.4(4) . . ?
C7 N2 C6 106.9(6) . . ?
C7 N2 H2N 124(5) . . ?
C6 N2 H2N 129(5) . . ?
C3 C2 C1 117.0(8) . . ?
C3 C2 H2 121.5 . . ?
C1 C2 H2 121.5 . . ?
C10 N3 C16 106.9(5) . . ?
C10 N3 Zn1 127.5(4) . . ?
C16 N3 Zn1 124.4(4) . . ?
C2 C3 C4 121.0(9) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C10 N4 C11 107.6(5) . . ?
C10 N4 H4N 124(5) . . ?
C11 N4 H4N 129(5) . . ?
C22 O4 Zn1 109.9(4) . 2_655 ?
C5 C4 C3 121.8(9) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 117.9(9) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C5 C6 N2 133.0(8) . . ?
C5 C6 C1 121.2(8) . . ?
N2 C6 C1 105.8(6) . . ?
C28 N6 C29 122.0(9) . . ?
C28 N6 C30 121.1(7) . . ?
C29 N6 C30 116.6(8) . . ?
N1 C7 N2 112.9(6) . . ?
N1 C7 C8B 125.7(5) . . ?
N2 C7 C8B 121.4(5) . . ?
N1 C7 C8A 125.7(5) . . ?
N2 C7 C8A 121.4(5) . . ?
H8WA O8 H8WB 111(7) . . ?
O1A C8A C7 110.1(6) . . ?
O1A C8A C9A 108.5(5) . . ?
C7 C8A C9A 112.5(5) . . ?
O1A C8A H8A 108.5 . . ?
C7 C8A H8A 108.5 . . ?
C9A C8A H8A 108.5 . . ?
C10 C9A C8A 113.9(5) . . ?
C10 C9A H9AA 108.8 . . ?
C8A C9A H9AA 108.8 . . ?
C10 C9A H9AB 108.8 . . ?
C8A C9A H9AB 108.8 . . ?
H9AA C9A H9AB 107.7 . . ?
C8A O1A H1A 109.5 . . ?
C7 C8B C9B 112.5(5) . . ?
C7 C8B H8BA 109.1 . . ?
C9B C8B H8BA 109.1 . . ?
C7 C8B H8BB 109.1 . . ?
C9B C8B H8BB 109.1 . . ?
H8BA C8B H8BB 107.8 . . ?
O1B C9B C10 113.8(7) . . ?
O1B C9B C8B 106.6(7) . . ?
C10 C9B C8B 113.9(5) . . ?
O1B C9B H9B 107.4 . . ?
C10 C9B H9B 107.4 . . ?
C8B C9B H9B 107.4 . . ?
C9B O1B H1B 109.5 . . ?
C16 C11 N4 105.7(6) . . ?
C16 C11 C12 123.2(7) . . ?
N4 C11 C12 131.0(7) . . ?
N3 C10 N4 111.0(5) . . ?
N3 C10 C9B 126.6(5) . . ?
N4 C10 C9B 122.4(5) . . ?
N3 C10 C9A 126.6(5) . . ?
N4 C10 C9A 122.4(5) . . ?
C13 C12 C11 114.7(8) . . ?
C13 C12 H12 122.7 . . ?
C11 C12 H12 122.7 . . ?
C15 C14 C13 120.0(8) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C12 C13 C14 123.4(8) . . ?
C12 C13 H13 118.3 . . ?
C14 C13 H13 118.3 . . ?
C14 C15 C16 118.5(7) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C11 C16 N3 108.9(6) . . ?
C11 C16 C15 120.0(7) . . ?
N3 C16 C15 131.1(7) . . ?
O3 C17 O2 123.6(5) . . ?
O3 C17 C18 121.1(5) . . ?
O2 C17 C18 115.3(5) . . ?
C19 C18 C23 119.3(5) . . ?
C19 C18 C17 121.6(5) . . ?
C23 C18 C17 119.1(5) . . ?
C20 C19 C18 120.8(5) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 119.7(5) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C24 C21 C20 119.4(5) . . ?
C24 C21 C22 121.8(5) . . ?
C20 C21 C22 118.7(5) . . ?
O5 C22 O4 123.4(5) . . ?
O5 C22 C21 120.5(5) . . ?
O4 C22 C21 116.0(5) . . ?
C24 C23 C18 120.1(5) . . ?
C24 C23 H23 119.9 . . ?
C18 C23 H23 119.9 . . ?
C21 C24 C23 120.5(5) . . ?
C21 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
O6 C25 N5 126.2(11) . . ?
O6 C25 H25 116.9 . . ?
N5 C25 H25 116.9 . . ?
N5 C26 H26A 109.5 . . ?
N5 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N5 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N5 C27 H27A 109.5 . . ?
N5 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N5 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C27 N5 C25 122.8(12) . . ?
C27 N5 C26 118.2(12) . . ?
C25 N5 C26 117.3(11) . . ?
O7 C28 N6 125.7(7) . . ?
O7 C28 H28 117.2 . . ?
N6 C28 H28 117.2 . . ?
N6 C29 H29A 109.5 . . ?
N6 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N6 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N6 C30 H30A 109.5 . . ?
N6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
N2 H2N O3 0.90(3) 1.90(5) 2.728(7) 152(8) 4_564
N4 H4N O5 0.89(3) 1.86(4) 2.721(7) 162(8) 4_664
O8 H8WA O6 0.85(3) 1.90(3) 2.711(11) 159(8) .
O8 H8WB O7 0.85(3) 1.97(3) 2.776(10) 159(9) .
O1A H1A O8 0.84 1.86 2.687(10) 169.1 .
O1B H1B O8 0.84 1.91 2.687(16) 152.7 .

_refine_diff_density_max         1.061
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.074



####################################################################### 
# 
# 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_zn150re_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2046661'
loop_
_audit_author_name
_audit_author_address
'Claire Deville'
;Technical University of Denmark (current)
Denmark
;
_audit_update_record             
;
2020-11-26 deposited with the CCDC.	2021-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Zn N4 O5, 2( C3 H7 N O), H2 O'
_chemical_formula_sum            'C33 H41 N7 O9 Zn'
_chemical_formula_weight         745.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3242 0.9375 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_H-M_alt        'P 41'
_space_group_name_Hall           'P 4w'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'

_cell_length_a                   13.6439(7)
_cell_length_b                   13.6439(7)
_cell_length_c                   19.6066(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3649.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9893
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      19.91

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   0.7054
_exptl_transmission_factor_max   0.7445
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.393
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7054
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63305
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.178
_diffrn_reflns_theta_max         20.562
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7482
_reflns_number_gt                6612
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+0.8146P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2871 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.048(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7482
_refine_ls_number_parameters     433
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1474
_refine_ls_wR_factor_gt          0.1417
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT987_zn150re_a_sq        
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Refinement gives BASF = 0.069(28). Deviation from zero is likely 
a consquence of Ag radiation.  
;
_vrf_PLAT094_zn150re_a_sq        
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.18 Report
RESPONSE: The one "peak" >0.5eA-3 is an electron density ring around the Zn Atom.
;
_vrf_FORMU01_zn150re_a_sq        
;
PROBLEM: There is a discrepancy between the atom counts in the
 _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C33 H41 N7 O9 Zn1
            Atom count from the _atom_site data:  C30 H34 N6 O8 Zn1
RESPONSE: _chemical_formula_sum includes one additional DMF from SQUEEZE.
;
# end Validation Reply Form

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 0.47506(5) 0.17080(4) 0.53559(3) 0.04011(19) Uani 1 1 d . . . . .
N1 N 0.5932(4) 0.2524(4) 0.5511(2) 0.0435(11) Uani 1 1 d . . . . .
C1 C 0.6863(5) 0.2163(5) 0.5549(3) 0.0522(15) Uani 1 1 d . . . . .
O2 O 0.5056(4) 0.0816(3) 0.45938(19) 0.0485(10) Uani 1 1 d . . . . .
N2 N 0.6885(4) 0.3711(4) 0.5860(2) 0.0459(11) Uani 1 1 d D . . . .
H2N H 0.705(6) 0.429(3) 0.605(4) 0.069 Uiso 1 1 d D U . . .
C2 C 0.7249(6) 0.1245(5) 0.5410(4) 0.0633(17) Uani 1 1 d . . . . .
H2A H 0.685156 0.073571 0.522904 0.076 Uiso 1 1 calc R U . . .
O3 O 0.5234(3) 0.2169(3) 0.39871(19) 0.0453(9) Uani 1 1 d . . . . .
N3 N 0.3629(4) 0.2591(4) 0.5215(2) 0.0428(11) Uani 1 1 d . . . . .
C3 C 0.8209(8) 0.1101(7) 0.5539(5) 0.084(3) Uani 1 1 d . . . . .
H3 H 0.849210 0.047593 0.545833 0.101 Uiso 1 1 calc R U . . .
N4 N 0.2748(4) 0.3857(4) 0.4855(2) 0.0438(11) Uani 1 1 d D . . . .
H4N H 0.256(6) 0.444(3) 0.469(4) 0.066 Uiso 1 1 d D U . . .
O4 O 0.5538(3) -0.0752(3) 0.10789(18) 0.0452(9) Uani 1 1 d . . . . .
C4 C 0.8789(7) 0.1860(8) 0.5791(5) 0.084(3) Uani 1 1 d . . . . .
H4A H 0.946336 0.173158 0.587367 0.101 Uiso 1 1 calc R U . . .
N5 N 0.2251(7) 0.6553(8) 0.8264(5) 0.104(3) Uani 1 1 d . . . . .
O5 O 0.5510(3) -0.2088(3) 0.17335(19) 0.0411(8) Uani 1 1 d . . . . .
C5 C 0.8456(6) 0.2737(7) 0.5920(5) 0.072(2) Uani 1 1 d . . . . .
H5 H 0.887142 0.323518 0.609625 0.086 Uiso 1 1 calc R U . . .
C6 C 0.7468(5) 0.2914(6) 0.5790(3) 0.0571(16) Uani 1 1 d . . . . .
O6 O 0.2492(8) 0.6235(11) 0.7119(5) 0.163(5) Uani 1 1 d D . . . .
N6 N 0.3527(6) 0.8349(5) 0.4667(4) 0.078(2) Uani 1 1 d . . . . .
C7 C 0.5977(4) 0.3438(4) 0.5697(2) 0.0393(12) Uani 1 1 d . . . . .
O7 O 0.4240(7) 0.8056(5) 0.5691(4) 0.105(2) Uani 1 1 d D . . . .
O8 O 0.3819(7) 0.6136(6) 0.6107(4) 0.108(2) Uani 1 1 d D . . . .
H8W1 H 0.326(5) 0.606(8) 0.630(4) 0.162 Uiso 1 1 d D U . . .
H8W2 H 0.390(10) 0.675(3) 0.608(6) 0.162 Uiso 1 1 d D U . . .
C8A C 0.5131(4) 0.4127(4) 0.5739(2) 0.0402(12) Uani 0.595(15) 1 d . . P A 1
H8A H 0.468631 0.390410 0.611347 0.048 Uiso 0.595(15) 1 calc R U P A 1
C9A C 0.4531(4) 0.4179(4) 0.5063(3) 0.0397(12) Uani 0.595(15) 1 d . . P A 1
H9AA H 0.431499 0.486391 0.498982 0.048 Uiso 0.595(15) 1 calc R U P A 1
H9AB H 0.496468 0.399780 0.467841 0.048 Uiso 0.595(15) 1 calc R U P A 1
O1A O 0.5458(5) 0.5072(5) 0.5891(4) 0.047(2) Uani 0.595(15) 1 d . . P A 1
H1A H 0.497586 0.545436 0.591169 0.071 Uiso 0.595(15) 1 calc R U P A 1
C8B C 0.5131(4) 0.4127(4) 0.5739(2) 0.0402(12) Uani 0.405(15) 1 d . . P A 2
H8BA H 0.537748 0.479060 0.585154 0.048 Uiso 0.405(15) 1 calc R U P A 2
H8BB H 0.469261 0.391651 0.611364 0.048 Uiso 0.405(15) 1 calc R U P A 2
C9B C 0.4531(4) 0.4179(4) 0.5063(3) 0.0397(12) Uani 0.405(15) 1 d . . P A 2
H9B H 0.497290 0.396352 0.468483 0.048 Uiso 0.405(15) 1 calc R U P A 2
O1B O 0.4294(9) 0.5181(9) 0.4946(7) 0.061(4) Uani 0.405(15) 1 d . . P A 2
H1B H 0.426654 0.547845 0.532031 0.092 Uiso 0.405(15) 1 calc R U P A 2
C10 C 0.3650(4) 0.3525(4) 0.5054(2) 0.0349(10) Uani 1 1 d . . . . .
C12 C 0.1133(6) 0.2969(6) 0.4716(4) 0.0669(19) Uani 1 1 d . . . . .
H12 H 0.075692 0.351027 0.455953 0.080 Uiso 1 1 calc R U . . .
C11 C 0.2115(5) 0.3076(5) 0.4890(3) 0.0489(14) Uani 1 1 d . . . . .
C13 C 0.0733(6) 0.2067(7) 0.4779(5) 0.074(2) Uani 1 1 d . . . . .
H13 H 0.007603 0.196481 0.463570 0.089 Uiso 1 1 calc R U . . .
C15 C 0.2242(6) 0.1366(5) 0.5225(4) 0.0651(19) Uani 1 1 d . . . . .
H15 H 0.260663 0.083111 0.540380 0.078 Uiso 1 1 calc R U . . .
C14 C 0.1266(6) 0.1277(6) 0.5051(5) 0.075(2) Uani 1 1 d . . . . .
H14 H 0.094543 0.066597 0.511634 0.090 Uiso 1 1 calc R U . . .
C16 C 0.2661(5) 0.2288(5) 0.5123(3) 0.0492(14) Uani 1 1 d . . . . .
C17 C 0.5234(4) 0.1272(4) 0.4040(3) 0.0387(11) Uani 1 1 d . . . . .
C18 C 0.5424(4) 0.0633(4) 0.3433(3) 0.0374(11) Uani 1 1 d . . . . .
C19 C 0.5450(5) 0.1063(4) 0.2785(3) 0.0436(12) Uani 1 1 d . . . . .
H19 H 0.541073 0.175515 0.273861 0.052 Uiso 1 1 calc R U . . .
C20 C 0.5533(4) 0.0473(4) 0.2211(3) 0.0412(12) Uani 1 1 d . . . . .
H20 H 0.555158 0.076418 0.177167 0.049 Uiso 1 1 calc R U . . .
C21 C 0.5588(4) -0.0528(4) 0.2273(3) 0.0362(11) Uani 1 1 d . . . . .
C22 C 0.5560(4) -0.1184(4) 0.1659(3) 0.0418(12) Uani 1 1 d . . . . .
C23 C 0.5515(4) -0.0372(4) 0.3494(3) 0.0380(12) Uani 1 1 d . . . . .
H23 H 0.551116 -0.066474 0.393384 0.046 Uiso 1 1 calc R U . . .
C24 C 0.5611(4) -0.0956(4) 0.2922(3) 0.0411(12) Uani 1 1 d . . . . .
H24 H 0.569166 -0.164480 0.296843 0.049 Uiso 1 1 calc R U . . .
C25 C 0.2804(9) 0.6380(10) 0.7715(6) 0.100(3) Uani 1 1 d . . . . .
H25 H 0.349351 0.636391 0.778057 0.120 Uiso 1 1 calc R U . . .
C26 C 0.2659(16) 0.6537(15) 0.8897(8) 0.168(8) Uani 1 1 d . . . . .
H26A H 0.327434 0.690712 0.889252 0.252 Uiso 1 1 calc R U . . .
H26B H 0.279076 0.585703 0.903033 0.252 Uiso 1 1 calc R U . . .
H26C H 0.220575 0.683432 0.922521 0.252 Uiso 1 1 calc R U . . .
C27 C 0.1173(10) 0.6596(15) 0.8180(9) 0.160(7) Uani 1 1 d . . . . .
H27A H 0.091558 0.593098 0.812024 0.240 Uiso 1 1 calc R U . . .
H27B H 0.101303 0.699116 0.777771 0.240 Uiso 1 1 calc R U . . .
H27C H 0.087849 0.689377 0.858571 0.240 Uiso 1 1 calc R U . . .
C28 C 0.3952(7) 0.8619(6) 0.5223(4) 0.074(2) Uani 1 1 d . . . . .
H28 H 0.405623 0.930173 0.528598 0.088 Uiso 1 1 calc R U . . .
C29 C 0.3110(8) 0.9072(7) 0.4198(5) 0.089(3) Uani 1 1 d . . . . .
H29A H 0.351967 0.911572 0.378871 0.134 Uiso 1 1 calc R U . . .
H29B H 0.308579 0.971323 0.442288 0.134 Uiso 1 1 calc R U . . .
H29C H 0.244564 0.887179 0.406944 0.134 Uiso 1 1 calc R U . . .
C30 C 0.3558(18) 0.7408(9) 0.4427(8) 0.193(11) Uani 1 1 d . . . . .
H30A H 0.344366 0.695090 0.480395 0.290 Uiso 1 1 calc R U . . .
H30B H 0.420351 0.728026 0.422594 0.290 Uiso 1 1 calc R U . . .
H30C H 0.305042 0.731935 0.407897 0.290 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.966(4) 2_655 ?
Zn1 N3 1.967(5) . ?
Zn1 O2 1.972(4) . ?
Zn1 N1 1.983(5) . ?
N1 C7 1.300(8) . ?
N1 C1 1.364(9) . ?
C1 C2 1.385(9) . ?
C1 C6 1.398(10) . ?
O2 C17 1.275(7) . ?
N2 C7 1.332(8) . ?
N2 C6 1.355(9) . ?
N2 H2N 0.90(3) . ?
C2 C3 1.348(13) . ?
C2 H2A 0.9500 . ?
O3 C17 1.228(7) . ?
N3 C10 1.314(7) . ?
N3 C16 1.396(8) . ?
C3 C4 1.394(15) . ?
C3 H3 0.9500 . ?
N4 C10 1.368(7) . ?
N4 C11 1.374(8) . ?
N4 H4N 0.90(3) . ?
O4 C22 1.281(7) . ?
C4 C5 1.304(13) . ?
C4 H4A 0.9500 . ?
N5 C25 1.335(14) . ?
N5 C26 1.361(18) . ?
N5 C27 1.480(17) . ?
O5 C22 1.244(7) . ?
C5 C6 1.393(11) . ?
C5 H5 0.9500 . ?
O6 C25 1.259(15) . ?
N6 C28 1.290(11) . ?
N6 C30 1.367(14) . ?
N6 C29 1.463(12) . ?
C7 C8B 1.492(8) . ?
C7 C8A 1.492(8) . ?
O7 C28 1.259(11) . ?
O8 H8W1 0.86(3) . ?
O8 H8W2 0.85(3) . ?
C8A O1A 1.396(9) . ?
C8A C9A 1.560(7) . ?
C8A H8A 1.0000 . ?
C9A C10 1.496(8) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
O1A H1A 0.8400 . ?
C8B C9B 1.560(7) . ?
C8B H8BA 0.9900 . ?
C8B H8BB 0.9900 . ?
C9B O1B 1.423(13) . ?
C9B C10 1.496(8) . ?
C9B H9B 1.0000 . ?
O1B H1B 0.8400 . ?
C12 C13 1.352(12) . ?
C12 C11 1.389(10) . ?
C12 H12 0.9500 . ?
C11 C16 1.386(9) . ?
C13 C14 1.405(13) . ?
C13 H13 0.9500 . ?
C15 C14 1.380(11) . ?
C15 C16 1.397(10) . ?
C15 H15 0.9500 . ?
C14 H14 0.9500 . ?
C17 C18 1.498(7) . ?
C18 C23 1.383(8) . ?
C18 C19 1.399(8) . ?
C19 C20 1.389(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.373(8) . ?
C20 H20 0.9500 . ?
C21 C24 1.400(8) . ?
C21 C22 1.501(7) . ?
C23 C24 1.383(7) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zn1 N3 110.59(19) 2_655 . ?
O4 Zn1 O2 100.31(15) 2_655 . ?
N3 Zn1 O2 115.87(18) . . ?
O4 Zn1 N1 115.12(18) 2_655 . ?
N3 Zn1 N1 108.1(2) . . ?
O2 Zn1 N1 106.9(2) . . ?
C7 N1 C1 106.7(5) . . ?
C7 N1 Zn1 128.3(4) . . ?
C1 N1 Zn1 124.2(4) . . ?
N1 C1 C2 132.0(7) . . ?
N1 C1 C6 107.7(6) . . ?
C2 C1 C6 120.3(7) . . ?
C17 O2 Zn1 112.6(3) . . ?
C7 N2 C6 107.3(5) . . ?
C7 N2 H2N 126(5) . . ?
C6 N2 H2N 127(5) . . ?
C3 C2 C1 117.6(8) . . ?
C3 C2 H2A 121.2 . . ?
C1 C2 H2A 121.2 . . ?
C10 N3 C16 106.1(5) . . ?
C10 N3 Zn1 127.6(4) . . ?
C16 N3 Zn1 124.9(4) . . ?
C2 C3 C4 120.7(8) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C10 N4 C11 107.2(5) . . ?
C10 N4 H4N 131(5) . . ?
C11 N4 H4N 121(5) . . ?
C22 O4 Zn1 109.8(4) . 2_654 ?
C5 C4 C3 123.5(8) . . ?
C5 C4 H4A 118.3 . . ?
C3 C4 H4A 118.3 . . ?
C25 N5 C26 120.1(13) . . ?
C25 N5 C27 118.6(12) . . ?
C26 N5 C27 120.6(13) . . ?
C4 C5 C6 117.4(9) . . ?
C4 C5 H5 121.3 . . ?
C6 C5 H5 121.3 . . ?
N2 C6 C5 133.5(7) . . ?
N2 C6 C1 106.0(6) . . ?
C5 C6 C1 120.4(7) . . ?
C28 N6 C30 123.1(9) . . ?
C28 N6 C29 120.8(7) . . ?
C30 N6 C29 115.4(9) . . ?
N1 C7 N2 112.3(5) . . ?
N1 C7 C8B 125.7(5) . . ?
N2 C7 C8B 122.0(5) . . ?
N1 C7 C8A 125.7(5) . . ?
N2 C7 C8A 122.0(5) . . ?
H8W1 O8 H8W2 105(5) . . ?
O1A C8A C7 110.3(5) . . ?
O1A C8A C9A 107.9(5) . . ?
C7 C8A C9A 112.8(4) . . ?
O1A C8A H8A 108.6 . . ?
C7 C8A H8A 108.6 . . ?
C9A C8A H8A 108.6 . . ?
C10 C9A C8A 113.9(4) . . ?
C10 C9A H9AA 108.8 . . ?
C8A C9A H9AA 108.8 . . ?
C10 C9A H9AB 108.8 . . ?
C8A C9A H9AB 108.8 . . ?
H9AA C9A H9AB 107.7 . . ?
C8A O1A H1A 109.5 . . ?
C7 C8B C9B 112.8(4) . . ?
C7 C8B H8BA 109.0 . . ?
C9B C8B H8BA 109.0 . . ?
C7 C8B H8BB 109.0 . . ?
C9B C8B H8BB 109.0 . . ?
H8BA C8B H8BB 107.8 . . ?
O1B C9B C10 112.8(7) . . ?
O1B C9B C8B 107.5(7) . . ?
C10 C9B C8B 113.9(4) . . ?
O1B C9B H9B 107.5 . . ?
C10 C9B H9B 107.5 . . ?
C8B C9B H9B 107.5 . . ?
C9B O1B H1B 109.5 . . ?
N3 C10 N4 111.7(5) . . ?
N3 C10 C9B 126.4(5) . . ?
N4 C10 C9B 121.9(5) . . ?
N3 C10 C9A 126.4(5) . . ?
N4 C10 C9A 121.9(5) . . ?
C13 C12 C11 117.5(8) . . ?
C13 C12 H12 121.2 . . ?
C11 C12 H12 121.2 . . ?
N4 C11 C16 106.3(5) . . ?
N4 C11 C12 132.5(7) . . ?
C16 C11 C12 121.2(7) . . ?
C12 C13 C14 121.6(7) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C14 C15 C16 116.0(7) . . ?
C14 C15 H15 122.0 . . ?
C16 C15 H15 122.0 . . ?
C15 C14 C13 121.7(7) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C11 C16 N3 108.7(5) . . ?
C11 C16 C15 121.7(6) . . ?
N3 C16 C15 129.5(6) . . ?
O3 C17 O2 124.0(5) . . ?
O3 C17 C18 120.8(5) . . ?
O2 C17 C18 115.2(5) . . ?
C23 C18 C19 119.5(5) . . ?
C23 C18 C17 121.6(5) . . ?
C19 C18 C17 118.8(5) . . ?
C20 C19 C18 119.6(5) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C21 C20 C19 120.7(5) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C24 119.8(5) . . ?
C20 C21 C22 121.4(5) . . ?
C24 C21 C22 118.7(5) . . ?
O5 C22 O4 124.1(5) . . ?
O5 C22 C21 119.9(5) . . ?
O4 C22 C21 116.0(5) . . ?
C24 C23 C18 120.7(5) . . ?
C24 C23 H23 119.7 . . ?
C18 C23 H23 119.7 . . ?
C23 C24 C21 119.6(5) . . ?
C23 C24 H24 120.2 . . ?
C21 C24 H24 120.2 . . ?
O6 C25 N5 125.8(12) . . ?
O6 C25 H25 117.1 . . ?
N5 C25 H25 117.1 . . ?
N5 C26 H26A 109.5 . . ?
N5 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N5 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N5 C27 H27A 109.5 . . ?
N5 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N5 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O7 C28 N6 125.6(8) . . ?
O7 C28 H28 117.2 . . ?
N6 C28 H28 117.2 . . ?
N6 C29 H29A 109.5 . . ?
N6 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N6 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N6 C30 H30A 109.5 . . ?
N6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
N2 H2N O3 0.90(3) 1.88(4) 2.738(6) 159(8) 3_655
N4 H4N O5 0.90(3) 1.83(3) 2.717(6) 171(8) 3
O8 H8W1 O6 0.86(3) 1.93(3) 2.691(12) 147(6) .
O8 H8W2 O7 0.85(3) 1.99(3) 2.803(11) 160(10) .
O1A H1A O8 0.84 1.87 2.699(10) 168.1 .
O1B H1B O8 0.84 1.89 2.702(16) 163.6 .

_refine_diff_density_max         0.866
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.070



####################################################################### 
# 
# 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_ZnDimer
_database_code_depnum_ccdc_archive 'CCDC 2046662'
loop_
_audit_author_name
_audit_author_address
'Claire Deville'
;Technical University of Denmark (current)
Denmark
;
_audit_update_record             
;
2020-11-26 deposited with the CCDC.	2021-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H32 Cl2 N8 O6 Zn2, 4( C3 H7 N O)'
_chemical_formula_sum            'C52 H60 Cl2 N12 O10 Zn2'
_chemical_formula_weight         1214.76

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   8.8946(8)
_cell_length_b                   11.6045(8)
_cell_length_c                   13.7282(9)
_cell_angle_alpha                93.542(6)
_cell_angle_beta                 100.835(7)
_cell_angle_gamma                95.115(7)
_cell_volume                     1381.71(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    100.01(14)
_cell_measurement_reflns_used    4258
_cell_measurement_theta_min      2.7880
_cell_measurement_theta_max      23.0310

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             630
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.033
_shelx_estimated_absorpt_T_min   0.820
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87675
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_reflns_number            29231
_diffrn_reflns_av_unetI/netI     0.1624
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.234
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.025
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9746
_reflns_number_gt                5471
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    0.991

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0303P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1614 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         9746
_refine_ls_number_parameters     704
_refine_ls_number_restraints     813
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0673
_refine_ls_wR_factor_ref         0.1392
_refine_ls_wR_factor_gt          0.1122
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      0.977
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
# start Validation Reply Form
_vrf_PLAT341_ZnDimer             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02861 Ang.  
RESPONSE: Weak diffraction of a small crystal, coupled with significant disorder
 limited the data quality and resolution of the structure.
;
# end Validation Reply Form

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 0.24656(16) 0.20937(14) 0.73607(11) 0.0331(7) Uani 1 1 d D . . . .
Cl1 Cl 0.3466(6) 0.0428(5) 0.7582(4) 0.0453(17) Uani 1 1 d D . . . .
N1 N 0.2926(18) 0.3150(14) 0.8635(11) 0.034(4) Uani 1 1 d D . . . .
N2 N 0.251(2) 0.4416(16) 0.9796(12) 0.043(4) Uani 1 1 d D . . . .
H2N H 0.207705 0.495067 1.009364 0.051 Uiso 1 1 calc R U . . .
N3 N 0.0133(17) 0.1854(15) 0.7068(12) 0.038(4) Uani 1 1 d D . . . .
N4 N -0.2351(19) 0.1967(17) 0.7072(13) 0.059(5) Uani 1 1 d D . . . .
H4N H -0.319259 0.224527 0.719112 0.071 Uiso 1 1 calc R U . . .
C1 C 0.406(2) 0.3122(18) 0.9457(13) 0.031(5) Uani 1 1 d D . . . .
C2 C 0.536(2) 0.250(2) 0.9614(17) 0.050(6) Uani 1 1 d D . . . .
H2 H 0.555423 0.196122 0.911594 0.060 Uiso 1 1 calc R U . . .
C3 C 0.635(3) 0.272(2) 1.0515(17) 0.062(7) Uani 1 1 d D . . . .
H3 H 0.726695 0.234816 1.064220 0.074 Uiso 1 1 calc R U . . .
C4 C 0.599(3) 0.351(2) 1.1268(16) 0.060(7) Uani 1 1 d D . . . .
H4 H 0.665965 0.359421 1.190142 0.072 Uiso 1 1 calc R U . . .
C5 C 0.478(3) 0.413(2) 1.1134(14) 0.047(6) Uani 1 1 d D . . . .
H5 H 0.459274 0.467588 1.163544 0.056 Uiso 1 1 calc R U . . .
C6 C 0.382(2) 0.3927(18) 1.0212(14) 0.032(4) Uani 1 1 d D . . . .
C7 C 0.202(2) 0.393(2) 0.8847(16) 0.052(6) Uani 1 1 d D . . . .
C8 C 0.0834(15) 0.4370(12) 0.8096(10) 0.051(4) Uani 1 1 d D . . . .
H8A H 0.116156 0.433907 0.744570 0.062 Uiso 1 1 calc R U . . .
H8AB H 0.073283 0.519127 0.829198 0.062 Uiso 1 1 calc R U . . .
C9 C -0.0743(16) 0.3650(13) 0.7991(10) 0.054(4) Uani 1 1 d D . . . .
H9 H -0.149811 0.412150 0.760474 0.065 Uiso 1 1 calc R U . . .
O1 O -0.1140(17) 0.3629(15) 0.8929(9) 0.059(4) Uani 1 1 d D . . . .
H1O H -0.101789 0.293391 0.911593 0.088 Uiso 1 1 d R U . . .
C10 C -0.090(2) 0.249(2) 0.7363(17) 0.053(5) Uani 1 1 d D . . . .
C11 C -0.077(2) 0.0837(19) 0.6536(16) 0.037(5) Uani 1 1 d D . . . .
C12 C -0.028(2) -0.0075(19) 0.6053(16) 0.043(5) Uani 1 1 d D . . . .
H12 H 0.076906 -0.012031 0.602887 0.051 Uiso 1 1 calc R U . . .
C13 C -0.145(2) -0.095(2) 0.5592(17) 0.050(6) Uani 1 1 d D . . . .
H13 H -0.114765 -0.161039 0.526837 0.060 Uiso 1 1 calc R U . . .
C14 C -0.295(2) -0.090(2) 0.5581(17) 0.053(6) Uani 1 1 d D . . . .
H14 H -0.368819 -0.149875 0.523538 0.064 Uiso 1 1 calc R U . . .
C15 C -0.342(2) 0.005(2) 0.6090(17) 0.051(6) Uani 1 1 d D . . . .
H15 H -0.446899 0.010025 0.611489 0.061 Uiso 1 1 calc R U . . .
C16 C -0.228(2) 0.093(2) 0.6559(17) 0.045(6) Uani 1 1 d D . . . .
Zn2 Zn 0.76769(16) 0.76768(14) 0.24043(11) 0.0349(7) Uani 1 1 d D . . . .
Cl2 Cl 0.6714(7) 0.9379(5) 0.2178(5) 0.0526(19) Uani 1 1 d D . . . .
N5 N 1.0015(16) 0.7971(15) 0.2812(14) 0.046(5) Uani 1 1 d D . . . .
N6 N 1.2425(19) 0.7655(17) 0.2824(14) 0.059(5) Uani 1 1 d D . . . .
H6N H 1.322246 0.730269 0.271955 0.070 Uiso 1 1 calc R U . . .
N7 N 0.7361(17) 0.6673(16) 0.1132(11) 0.038(4) Uani 1 1 d D . . . .
N8 N 0.768(2) 0.5512(17) -0.0140(12) 0.054(5) Uani 1 1 d D . . . .
H8 H 0.810467 0.501944 -0.048979 0.065 Uiso 1 1 calc R U . . .
C17 C 1.0928(19) 0.8958(17) 0.3236(16) 0.031(5) Uani 1 1 d D . . . .
C18 C 1.054(2) 1.0005(18) 0.3671(16) 0.037(5) Uani 1 1 d D . . . .
H18 H 0.950360 1.015462 0.364470 0.044 Uiso 1 1 calc R U . . .
C19 C 1.175(2) 1.079(2) 0.4131(18) 0.056(7) Uani 1 1 d D . . . .
H19 H 1.156368 1.147680 0.448310 0.067 Uiso 1 1 calc R U . . .
C20 C 1.330(2) 1.057(2) 0.4078(17) 0.054(6) Uani 1 1 d D . . . .
H20 H 1.409611 1.116798 0.434019 0.065 Uiso 1 1 calc R U . . .
C21 C 1.371(2) 0.958(2) 0.3689(18) 0.054(6) Uani 1 1 d D . . . .
H21 H 1.475646 0.943635 0.371556 0.065 Uiso 1 1 calc R U . . .
C22 C 1.248(2) 0.8785(19) 0.3245(15) 0.033(4) Uani 1 1 d D . . . .
C23 C 1.095(2) 0.7192(19) 0.2603(19) 0.062(6) Uani 1 1 d D . . . .
C24 C 1.0392(17) 0.5953(11) 0.2358(10) 0.055(4) Uani 1 1 d D . . . .
H24A H 0.952316 0.576065 0.269660 0.066 Uiso 1 1 calc R U . A 1
H24B H 1.122733 0.548007 0.262269 0.066 Uiso 1 1 calc R U . A 1
C25 C 0.9875(15) 0.5628(14) 0.1268(10) 0.048(4) Uani 0.75 1 d D . P B 1
H25 H 0.981440 0.476153 0.119740 0.058 Uiso 0.75 1 calc R U P B 1
O2 O 1.103(2) 0.601(2) 0.0739(14) 0.057(5) Uani 0.75 1 d D . P B 1
H2O H 1.054548 0.665805 0.055497 0.085 Uiso 0.75 1 d R U P B 1
C26 C 0.824(2) 0.592(2) 0.0808(16) 0.045(5) Uani 1 1 d D . . . .
C27 C 0.610(2) 0.6695(19) 0.0295(14) 0.032(5) Uani 1 1 d D . . . .
C28 C 0.483(2) 0.728(2) 0.0225(17) 0.049(7) Uani 1 1 d D . . . .
H28 H 0.464117 0.775767 0.076905 0.059 Uiso 1 1 calc R U . . .
C29 C 0.382(3) 0.715(3) -0.0705(18) 0.073(9) Uani 1 1 d D . . . .
H29 H 0.296597 0.758921 -0.080352 0.087 Uiso 1 1 calc R U . . .
C30 C 0.403(3) 0.641(2) -0.1467(17) 0.065(7) Uani 1 1 d D . . . .
H30 H 0.327223 0.631304 -0.206473 0.078 Uiso 1 1 calc R U . . .
C31 C 0.531(2) 0.581(2) -0.1388(15) 0.045(5) Uani 1 1 d D . . . .
H31 H 0.547328 0.530692 -0.192206 0.054 Uiso 1 1 calc R U . . .
C32 C 0.635(2) 0.598(2) -0.0473(15) 0.041(5) Uani 1 1 d D . . . .
O3 O 0.2834(14) 0.2950(13) 0.6227(9) 0.037(4) Uani 1 1 d D . . . .
O4 O 0.5222(15) 0.3269(13) 0.7111(9) 0.032(4) Uani 1 1 d D . . . .
C33 C 0.4233(17) 0.3402(17) 0.6349(12) 0.034(5) Uani 1 1 d D . . . .
C34 C 0.4674(18) 0.4170(17) 0.5584(11) 0.033(5) Uani 1 1 d D . . . .
C35 C 0.3771(18) 0.4079(16) 0.4631(10) 0.027(4) Uani 1 1 d D . . . .
H35 H 0.289036 0.352689 0.445863 0.032 Uiso 1 1 calc R U . . .
C36 C 0.418(2) 0.4815(17) 0.3931(12) 0.037(5) Uani 1 1 d D . . . .
H36 H 0.355225 0.477477 0.328732 0.044 Uiso 1 1 calc R U . . .
C37 C 0.5475(19) 0.5588(16) 0.4156(11) 0.032(5) Uani 1 1 d D . . . .
C38 C 0.637(2) 0.5679(19) 0.5117(12) 0.045(6) Uani 1 1 d D . . . .
H38 H 0.726501 0.621992 0.528306 0.054 Uiso 1 1 calc R U . . .
C39 C 0.5953(19) 0.4977(16) 0.5831(12) 0.033(5) Uani 1 1 d D . . . .
H39 H 0.654754 0.505364 0.648804 0.039 Uiso 1 1 calc R U . . .
C40 C 0.5904(18) 0.6335(16) 0.3378(12) 0.032(4) Uani 1 1 d D . . . .
O6 O 0.4911(16) 0.6521(14) 0.2663(10) 0.040(4) Uani 1 1 d D . . . .
O5 O 0.7320(14) 0.6765(14) 0.3533(10) 0.042(4) Uani 1 1 d D . . . .
O7 O 0.9775(18) 0.6519(17) 0.6834(13) 0.075(6) Uani 1 1 d D . . . .
C41 C 1.092(2) 0.717(2) 0.6768(15) 0.067(7) Uani 1 1 d D . . . .
H41 H 1.130907 0.776411 0.728275 0.081 Uiso 1 1 calc R U . . .
N9 N 1.1628(19) 0.7062(16) 0.6000(13) 0.050(5) Uani 1 1 d D . . . .
C42 C 1.101(3) 0.624(3) 0.5161(19) 0.087(10) Uani 1 1 d D . . . .
H42A H 1.101235 0.661711 0.454296 0.131 Uiso 1 1 calc R U . . .
H42B H 0.995886 0.594206 0.519403 0.131 Uiso 1 1 calc R U . . .
H42C H 1.165304 0.559027 0.517527 0.131 Uiso 1 1 calc R U . . .
C43 C 1.302(2) 0.780(2) 0.5935(19) 0.068(8) Uani 1 1 d D . . . .
H43A H 1.372584 0.733185 0.565648 0.102 Uiso 1 1 calc R U . . .
H43B H 1.352013 0.813754 0.660164 0.102 Uiso 1 1 calc R U . . .
H43C H 1.274696 0.842151 0.550485 0.102 Uiso 1 1 calc R U . . .
O8 O 0.029(3) 0.213(2) 1.0078(18) 0.067(9) Uiso 0.5 1 d D U P C 1
C44 C 0.104(3) 0.134(3) 0.9813(17) 0.121(11) Uiso 0.5 1 d D U P C 1
H44 H 0.094637 0.111725 0.912432 0.145 Uiso 0.5 1 calc R U P C 1
N10 N 0.195(5) 0.079(4) 1.048(2) 0.088(16) Uiso 0.5 1 d D U P C 1
C45 C 0.231(6) 0.111(5) 1.153(2) 0.13(2) Uiso 0.5 1 d D U P C 1
H45A H 0.184672 0.182412 1.166678 0.193 Uiso 0.5 1 calc R U P C 1
H45B H 0.342782 0.124480 1.174791 0.193 Uiso 0.5 1 calc R U P C 1
H45C H 0.189592 0.048571 1.187780 0.193 Uiso 0.5 1 calc R U P C 1
C46 C 0.303(5) 0.005(4) 1.012(3) 0.12(2) Uiso 0.5 1 d D U P C 1
H46A H 0.268981 -0.014445 0.940775 0.185 Uiso 0.5 1 calc R U P C 1
H46B H 0.304696 -0.065847 1.047271 0.185 Uiso 0.5 1 calc R U P C 1
H46C H 0.406148 0.047137 1.025528 0.185 Uiso 0.5 1 calc R U P C 1
O8' O -0.007(2) 0.185(2) 0.9592(19) 0.048(7) Uiso 0.5 1 d D U P D 2
C44' C 0.104(3) 0.134(3) 0.9813(17) 0.121(11) Uiso 0.5 1 d D U P D 2
H44' H 0.134700 0.102687 0.923333 0.145 Uiso 0.5 1 calc R U P D 2
N10' N 0.196(4) 0.108(3) 1.0622(18) 0.050(11) Uiso 0.5 1 d D U P D 2
C45' C 0.172(5) 0.152(4) 1.157(2) 0.082(15) Uiso 0.5 1 d D U P D 2
H45D H 0.096058 0.208873 1.147958 0.122 Uiso 0.5 1 calc R U P D 2
H45E H 0.269416 0.190112 1.196547 0.122 Uiso 0.5 1 calc R U P D 2
H45F H 0.134104 0.088353 1.192749 0.122 Uiso 0.5 1 calc R U P D 2
C46' C 0.329(4) 0.040(4) 1.070(3) 0.074(13) Uiso 0.5 1 d D U P D 2
H46D H 0.293651 -0.042684 1.058836 0.111 Uiso 0.5 1 calc R U P D 2
H46E H 0.393432 0.056263 1.136804 0.111 Uiso 0.5 1 calc R U P D 2
H46F H 0.389706 0.062369 1.020246 0.111 Uiso 0.5 1 calc R U P D 2
O9 O 1.027(2) 0.332(2) 0.2889(18) 0.116(8) Uani 1 1 d D . . . .
C47 C 0.915(3) 0.269(2) 0.3009(16) 0.060(7) Uani 1 1 d D . . . .
H47 H 0.866232 0.216886 0.245770 0.072 Uiso 1 1 calc R U . . .
N11 N 0.854(2) 0.2659(16) 0.3816(13) 0.050(5) Uani 1 1 d D . . . .
C48 C 0.919(3) 0.345(3) 0.4676(19) 0.097(11) Uani 1 1 d D . . . .
H48A H 0.968878 0.415192 0.446246 0.145 Uiso 1 1 calc R U . . .
H48B H 0.995151 0.307546 0.512740 0.145 Uiso 1 1 calc R U . . .
H48C H 0.837139 0.365957 0.502139 0.145 Uiso 1 1 calc R U . . .
C49 C 0.715(3) 0.194(2) 0.3865(18) 0.067(8) Uani 1 1 d D . . . .
H49A H 0.691926 0.134667 0.330193 0.100 Uiso 1 1 calc R U . . .
H49B H 0.629375 0.241861 0.383722 0.100 Uiso 1 1 calc R U . . .
H49C H 0.729596 0.155873 0.448949 0.100 Uiso 1 1 calc R U . . .
O10 O 1.054(2) 0.8327(18) 0.0490(15) 0.050(6) Uiso 0.5 1 d D U P E 1
C50 C 0.935(3) 0.887(2) 0.0340(17) 0.034(7) Uiso 0.5 1 d D U P E 1
H50 H 0.905680 0.926634 0.089003 0.041 Uiso 0.5 1 calc R U P E 1
N12 N 0.847(3) 0.889(3) -0.0579(16) 0.043(8) Uiso 0.5 1 d D U P E 1
C51 C 0.887(4) 0.834(3) -0.146(2) 0.063(10) Uiso 0.5 1 d D U P E 1
H51A H 0.937478 0.892969 -0.180353 0.095 Uiso 0.5 1 calc R U P E 1
H51B H 0.793382 0.797197 -0.189667 0.095 Uiso 0.5 1 calc R U P E 1
H51C H 0.957138 0.775570 -0.126060 0.095 Uiso 0.5 1 calc R U P E 1
C52 C 0.716(6) 0.959(6) -0.072(3) 0.046(6) Uiso 0.5 1 d D U P E 1
H52A H 0.724094 1.010743 -0.124493 0.069 Uiso 0.5 1 calc R U P E 1
H52B H 0.715180 1.004775 -0.009539 0.069 Uiso 0.5 1 calc R U P E 1
H52C H 0.619612 0.907080 -0.090527 0.069 Uiso 0.5 1 calc R U P E 1
O10' O 1.013(3) 0.791(3) -0.012(2) 0.061(8) Uiso 0.5 1 d D U P F 2
C50' C 0.913(3) 0.858(3) -0.0033(19) 0.024(8) Uiso 0.5 1 d D U P F 2
H50' H 0.910097 0.891930 0.060963 0.029 Uiso 0.5 1 calc R U P F 2
N12' N 0.810(3) 0.884(3) -0.0813(18) 0.035(9) Uiso 0.5 1 d D U P F 2
C51' C 0.797(4) 0.828(3) -0.1779(19) 0.048(9) Uiso 0.5 1 d D U P F 2
H51D H 0.688466 0.804009 -0.206588 0.072 Uiso 0.5 1 calc R U P F 2
H51E H 0.854243 0.759431 -0.173554 0.072 Uiso 0.5 1 calc R U P F 2
H51F H 0.839720 0.881846 -0.220318 0.072 Uiso 0.5 1 calc R U P F 2
C52' C 0.715(6) 0.978(5) -0.067(3) 0.046(6) Uiso 0.5 1 d D U P F 2
H52D H 0.746990 1.044796 -0.101320 0.069 Uiso 0.5 1 calc R U P F 2
H52E H 0.728376 1.001357 0.004575 0.069 Uiso 0.5 1 calc R U P F 2
H52F H 0.606522 0.951840 -0.093456 0.069 Uiso 0.5 1 calc R U P F 2
C25' C 0.9875(15) 0.5628(14) 0.1268(10) 0.048(4) Uani 0.25 1 d D . P B 2
H25' H 1.058445 0.612306 0.094279 0.058 Uiso 0.25 1 calc R U P B 2
O2' O 1.037(4) 0.453(3) 0.121(3) 0.072(12) Uiso 0.25 1 d D . P B 2
H2' H 0.959920 0.402939 0.109371 0.108 Uiso 0.25 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 1.961(14) . ?
Zn1 N1 2.027(13) . ?
Zn1 N3 2.029(15) . ?
Zn1 Cl1 2.213(6) . ?
N1 C7 1.32(2) . ?
N1 C1 1.37(2) . ?
N2 C7 1.36(2) . ?
N2 C6 1.38(2) . ?
N2 H2N 0.8800 . ?
N3 C10 1.33(2) . ?
N3 C11 1.44(2) . ?
N4 C10 1.35(2) . ?
N4 C16 1.37(2) . ?
N4 H4N 0.8800 . ?
C1 C2 1.40(2) . ?
C1 C6 1.41(2) . ?
C2 C3 1.37(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.44(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.35(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.38(2) . ?
C5 H5 0.9500 . ?
C7 C8 1.48(2) . ?
C8 C9 1.545(16) . ?
C8 H8A 0.9900 . ?
C8 H8AB 0.9900 . ?
C9 O1 1.399(15) . ?
C9 C10 1.53(2) . ?
C9 H9 1.0000 . ?
O1 H1O 0.8710 . ?
C11 C12 1.36(2) . ?
C11 C16 1.36(2) . ?
C12 C13 1.41(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.34(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.40(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.40(2) . ?
C15 H15 0.9500 . ?
Zn2 O5 1.987(15) . ?
Zn2 N7 1.998(14) . ?
Zn2 N5 2.042(14) . ?
Zn2 Cl2 2.238(6) . ?
N5 C23 1.33(2) . ?
N5 C17 1.37(2) . ?
N6 C23 1.34(2) . ?
N6 C22 1.39(2) . ?
N6 H6N 0.8800 . ?
N7 C26 1.33(2) . ?
N7 C27 1.45(2) . ?
N8 C26 1.34(2) . ?
N8 C32 1.36(2) . ?
N8 H8 0.8800 . ?
C17 C22 1.41(2) . ?
C17 C18 1.42(2) . ?
C18 C19 1.37(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.44(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.35(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.38(2) . ?
C21 H21 0.9500 . ?
C23 C24 1.48(2) . ?
C24 C25' 1.495(15) . ?
C24 C25 1.495(15) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 O2 1.418(17) . ?
C25 C26 1.55(2) . ?
C25 H25 1.0000 . ?
O2 H2O 0.9242 . ?
C26 C25' 1.55(2) . ?
C27 C32 1.36(2) . ?
C27 C28 1.36(2) . ?
C28 C29 1.41(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.36(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.38(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.41(2) . ?
C31 H31 0.9500 . ?
O3 C33 1.283(13) . ?
O4 C33 1.261(13) . ?
C33 C34 1.503(15) . ?
C34 C39 1.383(15) . ?
C34 C35 1.393(14) . ?
C35 C36 1.402(15) . ?
C35 H35 0.9500 . ?
C36 C37 1.368(14) . ?
C36 H36 0.9500 . ?
C37 C38 1.400(14) . ?
C37 C40 1.499(15) . ?
C38 C39 1.395(15) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 O6 1.235(14) . ?
C40 O5 1.286(14) . ?
O7 C41 1.232(15) . ?
C41 N9 1.331(16) . ?
C41 H41 0.9500 . ?
N9 C42 1.441(15) . ?
N9 C43 1.461(14) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
O8 C44 1.258(19) . ?
C44 N10 1.34(2) . ?
C44 H44 0.9500 . ?
N10 C45 1.42(2) . ?
N10 C46 1.47(2) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
O8' C44' 1.199(18) . ?
C44' N10' 1.319(19) . ?
C44' H44' 0.9500 . ?
N10' C45' 1.44(2) . ?
N10' C46' 1.47(2) . ?
C45' H45D 0.9800 . ?
C45' H45E 0.9800 . ?
C45' H45F 0.9800 . ?
C46' H46D 0.9800 . ?
C46' H46E 0.9800 . ?
C46' H46F 0.9800 . ?
O9 C47 1.220(16) . ?
C47 N11 1.326(15) . ?
C47 H47 0.9500 . ?
N11 C49 1.441(15) . ?
N11 C48 1.445(15) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
O10 C50 1.270(18) . ?
C50 N12 1.355(19) . ?
C50 H50 0.9500 . ?
N12 C51 1.442(19) . ?
N12 C52 1.474(19) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
O10' C50' 1.247(18) . ?
C50' N12' 1.342(19) . ?
C50' H50' 0.9500 . ?
N12' C51' 1.419(19) . ?
N12' C52' 1.469(19) . ?
C51' H51D 0.9800 . ?
C51' H51E 0.9800 . ?
C51' H51F 0.9800 . ?
C52' H52D 0.9800 . ?
C52' H52E 0.9800 . ?
C52' H52F 0.9800 . ?
C25' O2' 1.39(2) . ?
C25' H25' 1.0000 . ?
O2' H2' 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 N1 111.0(7) . . ?
O3 Zn1 N3 100.5(6) . . ?
N1 Zn1 N3 102.4(6) . . ?
O3 Zn1 Cl1 118.7(5) . . ?
N1 Zn1 Cl1 111.3(5) . . ?
N3 Zn1 Cl1 111.2(5) . . ?
C7 N1 C1 107.7(15) . . ?
C7 N1 Zn1 123.2(13) . . ?
C1 N1 Zn1 128.7(12) . . ?
C7 N2 C6 108.5(16) . . ?
C7 N2 H2N 125.7 . . ?
C6 N2 H2N 125.7 . . ?
C10 N3 C11 104.2(15) . . ?
C10 N3 Zn1 130.8(13) . . ?
C11 N3 Zn1 124.7(13) . . ?
C10 N4 C16 108.1(17) . . ?
C10 N4 H4N 125.9 . . ?
C16 N4 H4N 125.9 . . ?
N1 C1 C2 131.2(17) . . ?
N1 C1 C6 108.6(16) . . ?
C2 C1 C6 120.1(18) . . ?
C3 C2 C1 117.1(19) . . ?
C3 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C2 C3 C4 120(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 124(2) . . ?
C5 C4 H4 117.9 . . ?
C3 C4 H4 117.9 . . ?
C4 C5 C6 114.9(19) . . ?
C4 C5 H5 122.6 . . ?
C6 C5 H5 122.6 . . ?
N2 C6 C5 131.6(17) . . ?
N2 C6 C1 104.9(15) . . ?
C5 C6 C1 123.5(18) . . ?
N1 C7 N2 110.3(17) . . ?
N1 C7 C8 123.7(17) . . ?
N2 C7 C8 124.9(17) . . ?
C7 C8 C9 111.5(15) . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8AB 109.3 . . ?
C9 C8 H8AB 109.3 . . ?
H8A C8 H8AB 108.0 . . ?
O1 C9 C10 117.4(15) . . ?
O1 C9 C8 108.8(12) . . ?
C10 C9 C8 114.5(13) . . ?
O1 C9 H9 104.9 . . ?
C10 C9 H9 104.9 . . ?
C8 C9 H9 104.9 . . ?
C9 O1 H1O 106.2 . . ?
N3 C10 N4 112.0(17) . . ?
N3 C10 C9 132.3(17) . . ?
N4 C10 C9 115.7(17) . . ?
C12 C11 C16 123.0(19) . . ?
C12 C11 N3 128.4(18) . . ?
C16 C11 N3 108.5(17) . . ?
C11 C12 C13 115.4(19) . . ?
C11 C12 H12 122.3 . . ?
C13 C12 H12 122.3 . . ?
C14 C13 C12 124(2) . . ?
C14 C13 H13 117.9 . . ?
C12 C13 H13 117.9 . . ?
C13 C14 C15 119(2) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 117.9(19) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C11 C16 N4 107.1(18) . . ?
C11 C16 C15 120.4(19) . . ?
N4 C16 C15 132.5(19) . . ?
O5 Zn2 N7 111.7(7) . . ?
O5 Zn2 N5 97.3(7) . . ?
N7 Zn2 N5 103.4(6) . . ?
O5 Zn2 Cl2 121.2(5) . . ?
N7 Zn2 Cl2 111.8(5) . . ?
N5 Zn2 Cl2 108.8(5) . . ?
C23 N5 C17 107.2(15) . . ?
C23 N5 Zn2 122.5(13) . . ?
C17 N5 Zn2 130.0(13) . . ?
C23 N6 C22 108.8(17) . . ?
C23 N6 H6N 125.6 . . ?
C22 N6 H6N 125.6 . . ?
C26 N7 C27 103.7(14) . . ?
C26 N7 Zn2 130.9(13) . . ?
C27 N7 Zn2 125.2(12) . . ?
C26 N8 C32 109.1(17) . . ?
C26 N8 H8 125.5 . . ?
C32 N8 H8 125.5 . . ?
N5 C17 C22 108.8(16) . . ?
N5 C17 C18 130.7(16) . . ?
C22 C17 C18 120.4(17) . . ?
C19 C18 C17 116.5(18) . . ?
C19 C18 H18 121.8 . . ?
C17 C18 H18 121.8 . . ?
C18 C19 C20 120(2) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C21 C20 C19 125.4(19) . . ?
C21 C20 H20 117.3 . . ?
C19 C20 H20 117.3 . . ?
C20 C21 C22 113.9(19) . . ?
C20 C21 H21 123.1 . . ?
C22 C21 H21 123.1 . . ?
C21 C22 N6 131.4(18) . . ?
C21 C22 C17 123.9(19) . . ?
N6 C22 C17 104.4(16) . . ?
N5 C23 N6 110.7(18) . . ?
N5 C23 C24 121.5(17) . . ?
N6 C23 C24 126.7(18) . . ?
C23 C24 C25' 113.7(15) . . ?
C23 C24 C25 113.7(15) . . ?
C23 C24 H24A 108.8 . . ?
C25 C24 H24A 108.8 . . ?
C23 C24 H24B 108.8 . . ?
C25 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
O2 C25 C24 110.8(14) . . ?
O2 C25 C26 114.2(15) . . ?
C24 C25 C26 115.7(13) . . ?
O2 C25 H25 105.0 . . ?
C24 C25 H25 105.0 . . ?
C26 C25 H25 105.0 . . ?
C25 O2 H2O 92.5 . . ?
N7 C26 N8 111.9(17) . . ?
N7 C26 C25' 130.5(16) . . ?
N8 C26 C25' 116.6(16) . . ?
N7 C26 C25 130.5(16) . . ?
N8 C26 C25 116.6(16) . . ?
C32 C27 C28 122.1(18) . . ?
C32 C27 N7 108.7(16) . . ?
C28 C27 N7 129.2(17) . . ?
C27 C28 C29 115.7(19) . . ?
C27 C28 H28 122.1 . . ?
C29 C28 H28 122.1 . . ?
C30 C29 C28 123(2) . . ?
C30 C29 H29 118.6 . . ?
C28 C29 H29 118.6 . . ?
C29 C30 C31 121(2) . . ?
C29 C30 H30 119.5 . . ?
C31 C30 H30 119.5 . . ?
C30 C31 C32 116.2(19) . . ?
C30 C31 H31 121.9 . . ?
C32 C31 H31 121.9 . . ?
N8 C32 C27 106.6(16) . . ?
N8 C32 C31 131.4(18) . . ?
C27 C32 C31 121.9(18) . . ?
C33 O3 Zn1 111.8(11) . . ?
O4 C33 O3 122.1(14) . . ?
O4 C33 C34 119.3(13) . . ?
O3 C33 C34 118.5(13) . . ?
C39 C34 C35 120.2(12) . . ?
C39 C34 C33 120.1(12) . . ?
C35 C34 C33 119.6(12) . . ?
C34 C35 C36 118.9(13) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C37 C36 C35 121.4(13) . . ?
C37 C36 H36 119.3 . . ?
C35 C36 H36 119.3 . . ?
C36 C37 C38 119.3(13) . . ?
C36 C37 C40 119.8(11) . . ?
C38 C37 C40 120.9(12) . . ?
C39 C38 C37 120.1(13) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C34 C39 C38 120.0(13) . . ?
C34 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
O6 C40 O5 124.7(15) . . ?
O6 C40 C37 119.8(13) . . ?
O5 C40 C37 115.5(13) . . ?
C40 O5 Zn2 109.5(11) . . ?
O7 C41 N9 122(2) . . ?
O7 C41 H41 118.9 . . ?
N9 C41 H41 118.9 . . ?
C41 N9 C42 121.2(16) . . ?
C41 N9 C43 122.5(16) . . ?
C42 N9 C43 116.2(16) . . ?
N9 C42 H42A 109.5 . . ?
N9 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N9 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 H43A 109.5 . . ?
N9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O8 C44 N10 121(2) . . ?
O8 C44 H44 119.4 . . ?
N10 C44 H44 119.4 . . ?
C44 N10 C45 125(3) . . ?
C44 N10 C46 118(3) . . ?
C45 N10 C46 114(2) . . ?
N10 C45 H45A 109.5 . . ?
N10 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N10 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N10 C46 H46A 109.5 . . ?
N10 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N10 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O8' C44' N10' 139(3) . . ?
O8' C44' H44' 110.6 . . ?
N10' C44' H44' 110.6 . . ?
C44' N10' C45' 119(2) . . ?
C44' N10' C46' 129(2) . . ?
C45' N10' C46' 113(2) . . ?
N10' C45' H45D 109.5 . . ?
N10' C45' H45E 109.5 . . ?
H45D C45' H45E 109.5 . . ?
N10' C45' H45F 109.5 . . ?
H45D C45' H45F 109.5 . . ?
H45E C45' H45F 109.5 . . ?
N10' C46' H46D 109.5 . . ?
N10' C46' H46E 109.5 . . ?
H46D C46' H46E 109.5 . . ?
N10' C46' H46F 109.5 . . ?
H46D C46' H46F 109.5 . . ?
H46E C46' H46F 109.5 . . ?
O9 C47 N11 128(2) . . ?
O9 C47 H47 116.1 . . ?
N11 C47 H47 116.1 . . ?
C47 N11 C49 123.6(16) . . ?
C47 N11 C48 119.4(17) . . ?
C49 N11 C48 116.7(16) . . ?
N11 C48 H48A 109.5 . . ?
N11 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N11 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N11 C49 H49A 109.5 . . ?
N11 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
N11 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O10 C50 N12 122(2) . . ?
O10 C50 H50 119.0 . . ?
N12 C50 H50 119.0 . . ?
C50 N12 C51 122(2) . . ?
C50 N12 C52 120(2) . . ?
C51 N12 C52 118(2) . . ?
N12 C51 H51A 109.5 . . ?
N12 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N12 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N12 C52 H52A 109.5 . . ?
N12 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N12 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O10' C50' N12' 123(2) . . ?
O10' C50' H50' 118.7 . . ?
N12' C50' H50' 118.7 . . ?
C50' N12' C51' 122(2) . . ?
C50' N12' C52' 118(2) . . ?
C51' N12' C52' 120(2) . . ?
N12' C51' H51D 109.5 . . ?
N12' C51' H51E 109.5 . . ?
H51D C51' H51E 109.5 . . ?
N12' C51' H51F 109.5 . . ?
H51D C51' H51F 109.5 . . ?
H51E C51' H51F 109.5 . . ?
N12' C52' H52D 109.5 . . ?
N12' C52' H52E 109.5 . . ?
H52D C52' H52E 109.5 . . ?
N12' C52' H52F 109.5 . . ?
H52D C52' H52F 109.5 . . ?
H52E C52' H52F 109.5 . . ?
O2' C25' C24 99.8(19) . . ?
O2' C25' C26 124(2) . . ?
C24 C25' C26 115.7(13) . . ?
O2' C25' H25' 105.0 . . ?
C24 C25' H25' 105.0 . . ?
C26 C25' H25' 105.0 . . ?
C25' O2' H2' 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
_geom_hbond_publ_flag
O1 H1O O8^a 0.87 1.93 2.66(3) 140.8 . yes
O2^a H2O^a O10^a 0.92 1.94 2.79(3) 151.8 . yes
N2 H2N O2^a 0.88 1.88 2.76(3) 175.8 1_456 yes
N4 H4N O4 0.88 1.92 2.75(2) 157.7 1_455 yes
N6 H6N O6 0.88 1.83 2.71(2) 172.9 1_655 yes
N8 H8 O1 0.88 1.98 2.84(2) 165.8 1_654 yes
O2'^b H2'^b O9 0.84 2.63 2.78(4) 91.8 . yes

_refine_diff_density_max         0.476
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.082

####################################################################### 
# 
# 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_zn200re_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2046663'
loop_
_audit_author_name
_audit_author_address
'Claire Deville'
;Technical University of Denmark (current)
Denmark
;
_audit_update_record             
;
2020-11-26 deposited with the CCDC.	2021-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Zn N4 O5, 3( C3 H7 N O), H2 O'
_chemical_formula_sum            'C33 H41 N7 O9 Zn'
_chemical_formula_weight         745.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3242 0.9375 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_H-M_alt        'P 41'
_space_group_name_Hall           'P 4w'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'

_cell_length_a                   13.7346(12)
_cell_length_b                   13.7346(12)
_cell_length_c                   19.6084(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3698.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      19.12

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   0.6653
_exptl_transmission_factor_max   0.7445
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.388
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70999
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.170
_diffrn_reflns_theta_max         20.566
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7604
_reflns_number_gt                6731
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0737P)²+0.8816P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2933 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7604
_refine_ls_number_parameters     433
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1226
_refine_ls_wR_factor_gt          0.1174
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001

# start Validation Reply Form
_vrf_PLAT987_zn200re_a_sq        
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Refinement gives BASF = 0.045(25). Deviation from zero is likely 
a consquence of Ag radiation.  
;
_vrf_FORMU01_zn200re_a_sq        
;
PROBLEM: There is a discrepancy between the atom counts in the
 _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C33 H41 N7 O9 Zn1
            Atom count from the _atom_site data:  C30 H34 N6 O8 Zn1
RESPONSE: _chemical_formula_sum includes one additional DMF from SQUEEZE.
;
# end Validation Reply Form

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 0.82857(4) 0.52574(4) 0.46176(3) 0.03815(16) Uani 1 1 d . . . . .
N1 N 0.7475(3) 0.4082(3) 0.44659(18) 0.0406(9) Uani 1 1 d . . . . .
C1 C 0.7835(4) 0.3142(4) 0.4428(2) 0.0480(12) Uani 1 1 d . . . . .
O2 O 0.9173(3) 0.4966(3) 0.53792(17) 0.0481(9) Uani 1 1 d . . . . .
N2 N 0.6301(3) 0.3124(3) 0.4122(2) 0.0446(10) Uani 1 1 d D . . . .
H2N H 0.573(3) 0.293(5) 0.397(3) 0.067 Uiso 1 1 d D U . . .
C2 C 0.8752(4) 0.2777(5) 0.4568(3) 0.0616(14) Uani 1 1 d . . . . .
H2A H 0.925601 0.318081 0.474066 0.074 Uiso 1 1 calc R U . . .
O3 O 0.7835(2) 0.4789(3) 0.59949(17) 0.0462(8) Uani 1 1 d . . . . .
N3 N 0.7402(3) 0.6373(3) 0.47534(18) 0.0405(9) Uani 1 1 d . . . . .
C3 C 0.8898(6) 0.1806(6) 0.4446(4) 0.078(2) Uani 1 1 d . . . . .
H3 H 0.951998 0.152897 0.453167 0.094 Uiso 1 1 calc R U . . .
N4 N 0.6146(3) 0.7240(3) 0.5116(2) 0.0434(9) Uani 1 1 d D . . . .
H4N H 0.555(3) 0.736(5) 0.529(3) 0.065 Uiso 1 1 d D U . . .
O4 O 1.0767(2) 0.4462(3) 0.88941(16) 0.0460(8) Uani 1 1 d . . . . .
C4 C 0.8157(6) 0.1223(5) 0.4202(4) 0.078(2) Uani 1 1 d . . . . .
H4A H 0.828530 0.055226 0.412644 0.094 Uiso 1 1 calc R U . . .
N5 N 0.3445(8) 0.7747(7) 0.1709(5) 0.118(3) Uani 1 1 d . . . . .
C5 C 0.7270(6) 0.1564(5) 0.4068(4) 0.0703(18) Uani 1 1 d . . . . .
H5 H 0.677423 0.114972 0.389477 0.084 Uiso 1 1 calc R U . . .
O5 O 1.2080(2) 0.4497(3) 0.82351(17) 0.0413(7) Uani 1 1 d . . . . .
C6 C 0.7094(5) 0.2541(4) 0.4190(3) 0.0517(13) Uani 1 1 d . . . . .
O6 O 0.3773(10) 0.7526(8) 0.2852(5) 0.186(5) Uani 1 1 d D . . . .
N6 N 0.1650(5) 0.6512(6) 0.5299(3) 0.089(2) Uani 1 1 d . . . . .
C7 C 0.6564(4) 0.4037(4) 0.4283(2) 0.0383(10) Uani 1 1 d . . . . .
O7 O 0.1956(5) 0.5795(7) 0.4275(4) 0.128(3) Uani 1 1 d D . . . .
O8 O 0.3859(5) 0.6147(6) 0.3859(4) 0.124(3) Uani 1 1 d D . . . .
H8WA H 0.396(7) 0.668(5) 0.365(4) 0.185 Uiso 1 1 d D U . . .
H8WB H 0.324(2) 0.610(9) 0.386(5) 0.185 Uiso 1 1 d D U . . .
O1A O 0.4937(5) 0.4541(5) 0.4087(3) 0.046(2) Uani 0.565(12) 1 d . . P A 1
H1A H 0.455341 0.501603 0.406406 0.069 Uiso 0.565(12) 1 calc R U P A 1
C8A C 0.5880(4) 0.4878(4) 0.4236(2) 0.0398(10) Uani 0.565(12) 1 d . . P A 1
H8A H 0.609946 0.531655 0.385959 0.048 Uiso 0.565(12) 1 calc R U P A 1
C9A C 0.5825(4) 0.5478(4) 0.4911(2) 0.0407(11) Uani 0.565(12) 1 d . . P A 1
H9AA H 0.514343 0.568799 0.498417 0.049 Uiso 0.565(12) 1 calc R U P A 1
H9AB H 0.600897 0.505068 0.529688 0.049 Uiso 0.565(12) 1 calc R U P A 1
O1B O 0.4832(7) 0.5713(8) 0.5019(6) 0.066(3) Uani 0.435(12) 1 d D . P A 2
H1B H 0.456417 0.582718 0.464255 0.100 Uiso 0.435(12) 1 calc DR U P A 2
C8B C 0.5880(4) 0.4878(4) 0.4236(2) 0.0398(10) Uani 0.435(12) 1 d . . P A 2
H8BA H 0.522178 0.463285 0.412260 0.048 Uiso 0.435(12) 1 calc R U P A 2
H8BB H 0.609222 0.531122 0.386140 0.048 Uiso 0.435(12) 1 calc R U P A 2
C9B C 0.5825(4) 0.5478(4) 0.4911(2) 0.0407(11) Uani 0.435(12) 1 d . . P A 2
H9B H 0.603710 0.504331 0.529244 0.049 Uiso 0.435(12) 1 calc R U P A 2
C11 C 0.6927(4) 0.7876(4) 0.5084(3) 0.0477(12) Uani 1 1 d . . . . .
C10 C 0.6465(3) 0.6352(3) 0.4916(2) 0.0353(9) Uani 1 1 d . . . . .
C12 C 0.7017(5) 0.8856(4) 0.5255(3) 0.0635(16) Uani 1 1 d . . . . .
H12 H 0.647751 0.922870 0.540937 0.076 Uiso 1 1 calc R U . . .
C13 C 0.7925(6) 0.9254(5) 0.5187(4) 0.0753(19) Uani 1 1 d . . . . .
H13 H 0.802752 0.990914 0.532403 0.090 Uiso 1 1 calc R U . . .
C14 C 0.8717(5) 0.8718(5) 0.4918(4) 0.0713(18) Uani 1 1 d . . . . .
H14 H 0.932881 0.902830 0.485488 0.086 Uiso 1 1 calc R U . . .
C15 C 0.8613(5) 0.7755(5) 0.4747(4) 0.0623(16) Uani 1 1 d . . . . .
H15 H 0.914089 0.739066 0.456671 0.075 Uiso 1 1 calc R U . . .
C16 C 0.7702(4) 0.7333(4) 0.4848(3) 0.0455(12) Uani 1 1 d . . . . .
C17 C 0.8724(4) 0.4789(4) 0.5936(2) 0.0388(10) Uani 1 1 d . . . . .
C18 C 0.9359(3) 0.4599(4) 0.6543(2) 0.0376(10) Uani 1 1 d . . . . .
C19 C 0.8949(3) 0.4567(4) 0.7191(3) 0.0461(11) Uani 1 1 d . . . . .
H19 H 0.826295 0.460909 0.724331 0.055 Uiso 1 1 calc R U . . .
C20 C 0.9538(4) 0.4475(4) 0.7761(2) 0.0430(11) Uani 1 1 d . . . . .
H20 H 0.924884 0.444746 0.820116 0.052 Uiso 1 1 calc R U . . .
C21 C 1.0536(3) 0.4424(4) 0.7699(2) 0.0367(10) Uani 1 1 d . . . . .
C22 C 1.1181(4) 0.4449(4) 0.8309(2) 0.0398(10) Uani 1 1 d . . . . .
C23 C 1.0364(4) 0.4503(4) 0.6479(2) 0.0396(11) Uani 1 1 d . . . . .
H23 H 1.065218 0.450312 0.603829 0.048 Uiso 1 1 calc R U . . .
C24 C 1.0946(3) 0.4408(4) 0.7048(3) 0.0429(11) Uani 1 1 d . . . . .
H24 H 1.162906 0.433081 0.699606 0.051 Uiso 1 1 calc R U . . .
C25 C 0.3614(10) 0.7191(9) 0.2261(6) 0.121(4) Uani 1 1 d . . . . .
H25 H 0.361469 0.650430 0.220382 0.145 Uiso 1 1 calc R U . . .
C26 C 0.3441(14) 0.7386(13) 0.1054(7) 0.181(7) Uani 1 1 d . . . . .
H26A H 0.289454 0.766808 0.080028 0.271 Uiso 1 1 calc R U . . .
H26B H 0.337239 0.667599 0.106707 0.271 Uiso 1 1 calc R U . . .
H26C H 0.405377 0.755686 0.082703 0.271 Uiso 1 1 calc R U . . .
C27 C 0.3434(14) 0.8795(9) 0.1778(8) 0.183(7) Uani 1 1 d . . . . .
H27A H 0.343220 0.909521 0.132483 0.274 Uiso 1 1 calc R U . . .
H27B H 0.401299 0.900694 0.202965 0.274 Uiso 1 1 calc R U . . .
H27C H 0.284787 0.899461 0.202740 0.274 Uiso 1 1 calc R U . . .
C28 C 0.1384(6) 0.6071(7) 0.4744(4) 0.085(2) Uani 1 1 d . . . . .
H28 H 0.070927 0.594557 0.468450 0.102 Uiso 1 1 calc R U . . .
C29 C 0.0915(7) 0.6890(7) 0.5773(5) 0.099(3) Uani 1 1 d . . . . .
H29A H 0.111645 0.753270 0.593805 0.149 Uiso 1 1 calc R U . . .
H29B H 0.084788 0.644408 0.616003 0.149 Uiso 1 1 calc R U . . .
H29C H 0.028817 0.694670 0.553677 0.149 Uiso 1 1 calc R U . . .
C30 C 0.2599(8) 0.6541(16) 0.5517(7) 0.213(11) Uani 1 1 d . . . . .
H30A H 0.302925 0.664476 0.512479 0.319 Uiso 1 1 calc R U . . .
H30B H 0.276432 0.592313 0.573812 0.319 Uiso 1 1 calc R U . . .
H30C H 0.267996 0.707566 0.584252 0.319 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.963(3) 2_764 ?
Zn1 O2 1.969(3) . ?
Zn1 N3 1.973(4) . ?
Zn1 N1 1.983(4) . ?
N1 C7 1.304(7) . ?
N1 C1 1.385(7) . ?
C1 C2 1.382(8) . ?
C1 C6 1.391(8) . ?
O2 C17 1.277(6) . ?
N2 C7 1.343(7) . ?
N2 C6 1.359(8) . ?
N2 H2N 0.89(3) . ?
C2 C3 1.369(10) . ?
C2 H2A 0.9500 . ?
O3 C17 1.227(6) . ?
N3 C10 1.326(6) . ?
N3 C16 1.394(7) . ?
C3 C4 1.381(12) . ?
C3 H3 0.9500 . ?
N4 C10 1.353(6) . ?
N4 C11 1.385(7) . ?
N4 H4N 0.91(3) . ?
O4 C22 1.280(6) . ?
C4 C5 1.331(11) . ?
C4 H4A 0.9500 . ?
N5 C25 1.345(14) . ?
N5 C26 1.378(15) . ?
N5 C27 1.446(15) . ?
C5 C6 1.385(9) . ?
C5 H5 0.9500 . ?
O5 C22 1.245(6) . ?
O6 C25 1.265(14) . ?
N6 C28 1.298(10) . ?
N6 C30 1.371(12) . ?
N6 C29 1.468(10) . ?
C7 C8B 1.491(7) . ?
C7 C8A 1.491(7) . ?
O7 C28 1.267(10) . ?
O8 H8WA 0.85(3) . ?
O8 H8WB 0.85(3) . ?
O1A C8A 1.406(8) . ?
O1A H1A 0.8400 . ?
C8A C9A 1.561(6) . ?
C8A H8A 1.0000 . ?
C9A C10 1.489(7) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
O1B C9B 1.417(11) . ?
O1B H1B 0.8400 . ?
C8B C9B 1.561(6) . ?
C8B H8BA 0.9900 . ?
C8B H8BB 0.9900 . ?
C9B C10 1.489(7) . ?
C9B H9B 1.0000 . ?
C11 C16 1.380(8) . ?
C11 C12 1.393(8) . ?
C12 C13 1.368(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.415(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.371(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.393(8) . ?
C15 H15 0.9500 . ?
C17 C18 1.498(7) . ?
C18 C19 1.390(7) . ?
C18 C23 1.393(7) . ?
C19 C20 1.385(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(7) . ?
C20 H20 0.9500 . ?
C21 C24 1.397(7) . ?
C21 C22 1.489(6) . ?
C23 C24 1.378(7) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zn1 O2 100.23(14) 2_764 . ?
O4 Zn1 N3 110.65(16) 2_764 . ?
O2 Zn1 N3 115.90(16) . . ?
O4 Zn1 N1 115.06(16) 2_764 . ?
O2 Zn1 N1 107.19(17) . . ?
N3 Zn1 N1 107.88(17) . . ?
C7 N1 C1 106.5(4) . . ?
C7 N1 Zn1 128.2(3) . . ?
C1 N1 Zn1 124.5(4) . . ?
C2 C1 N1 130.7(6) . . ?
C2 C1 C6 121.2(6) . . ?
N1 C1 C6 108.1(5) . . ?
C17 O2 Zn1 112.8(3) . . ?
C7 N2 C6 108.2(4) . . ?
C7 N2 H2N 127(4) . . ?
C6 N2 H2N 125(4) . . ?
C3 C2 C1 116.9(7) . . ?
C3 C2 H2A 121.6 . . ?
C1 C2 H2A 121.6 . . ?
C10 N3 C16 105.9(4) . . ?
C10 N3 Zn1 127.8(3) . . ?
C16 N3 Zn1 124.8(4) . . ?
C2 C3 C4 121.1(7) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C10 N4 C11 107.7(4) . . ?
C10 N4 H4N 125(4) . . ?
C11 N4 H4N 127(4) . . ?
C22 O4 Zn1 110.8(3) . 2_765 ?
C5 C4 C3 122.7(7) . . ?
C5 C4 H4A 118.7 . . ?
C3 C4 H4A 118.7 . . ?
C25 N5 C26 123.2(12) . . ?
C25 N5 C27 119.5(11) . . ?
C26 N5 C27 116.5(12) . . ?
C4 C5 C6 117.8(7) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
N2 C6 C5 134.0(6) . . ?
N2 C6 C1 105.7(5) . . ?
C5 C6 C1 120.3(6) . . ?
C28 N6 C30 122.8(9) . . ?
C28 N6 C29 120.1(7) . . ?
C30 N6 C29 116.5(8) . . ?
N1 C7 N2 111.5(4) . . ?
N1 C7 C8B 125.8(4) . . ?
N2 C7 C8B 122.6(4) . . ?
N1 C7 C8A 125.8(4) . . ?
N2 C7 C8A 122.6(4) . . ?
H8WA O8 H8WB 103(4) . . ?
C8A O1A H1A 109.5 . . ?
O1A C8A C7 109.8(5) . . ?
O1A C8A C9A 107.8(4) . . ?
C7 C8A C9A 112.8(4) . . ?
O1A C8A H8A 108.8 . . ?
C7 C8A H8A 108.8 . . ?
C9A C8A H8A 108.8 . . ?
C10 C9A C8A 113.8(4) . . ?
C10 C9A H9AA 108.8 . . ?
C8A C9A H9AA 108.8 . . ?
C10 C9A H9AB 108.8 . . ?
C8A C9A H9AB 108.8 . . ?
H9AA C9A H9AB 107.7 . . ?
C9B O1B H1B 109.5 . . ?
C7 C8B C9B 112.8(4) . . ?
C7 C8B H8BA 109.0 . . ?
C9B C8B H8BA 109.0 . . ?
C7 C8B H8BB 109.0 . . ?
C9B C8B H8BB 109.0 . . ?
H8BA C8B H8BB 107.8 . . ?
O1B C9B C10 112.6(6) . . ?
O1B C9B C8B 107.1(6) . . ?
C10 C9B C8B 113.8(4) . . ?
O1B C9B H9B 107.7 . . ?
C10 C9B H9B 107.7 . . ?
C8B C9B H9B 107.7 . . ?
C16 C11 N4 105.8(5) . . ?
C16 C11 C12 122.3(6) . . ?
N4 C11 C12 131.9(6) . . ?
N3 C10 N4 111.4(4) . . ?
N3 C10 C9B 126.0(4) . . ?
N4 C10 C9B 122.5(4) . . ?
N3 C10 C9A 126.0(4) . . ?
N4 C10 C9A 122.5(4) . . ?
C13 C12 C11 116.3(7) . . ?
C13 C12 H12 121.8 . . ?
C11 C12 H12 121.8 . . ?
C12 C13 C14 122.0(6) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C15 C14 C13 120.8(6) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 117.5(6) . . ?
C14 C15 H15 121.3 . . ?
C16 C15 H15 121.3 . . ?
C11 C16 C15 121.0(5) . . ?
C11 C16 N3 109.1(5) . . ?
C15 C16 N3 129.8(5) . . ?
O3 C17 O2 124.2(4) . . ?
O3 C17 C18 120.2(4) . . ?
O2 C17 C18 115.6(4) . . ?
C19 C18 C23 118.7(4) . . ?
C19 C18 C17 119.8(4) . . ?
C23 C18 C17 121.4(4) . . ?
C20 C19 C18 120.3(4) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C21 C20 C19 120.9(4) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C24 118.8(4) . . ?
C20 C21 C22 121.4(4) . . ?
C24 C21 C22 119.7(4) . . ?
O5 C22 O4 123.0(4) . . ?
O5 C22 C21 119.9(4) . . ?
O4 C22 C21 117.1(4) . . ?
C24 C23 C18 120.7(4) . . ?
C24 C23 H23 119.7 . . ?
C18 C23 H23 119.7 . . ?
C23 C24 C21 120.4(4) . . ?
C23 C24 H24 119.8 . . ?
C21 C24 H24 119.8 . . ?
O6 C25 N5 124.1(12) . . ?
O6 C25 H25 118.0 . . ?
N5 C25 H25 118.0 . . ?
N5 C26 H26A 109.5 . . ?
N5 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N5 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N5 C27 H27A 109.5 . . ?
N5 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N5 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O7 C28 N6 125.0(7) . . ?
O7 C28 H28 117.5 . . ?
N6 C28 H28 117.5 . . ?
N6 C29 H29A 109.5 . . ?
N6 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N6 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N6 C30 H30A 109.5 . . ?
N6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
N2 H2N O3 0.89(3) 1.90(4) 2.750(6) 159(6) 4_564
N4 H4N O5 0.91(3) 1.85(3) 2.734(5) 164(6) 4_574
O1B H1B O8 0.84 1.87 2.705(13) 173.8 .
O8 H8WA O6 0.85(3) 1.96(3) 2.738(12) 150(7) .
O8 H8WB O7 0.85(3) 1.99(3) 2.780(10) 154(8) .
O1A H1A O8 0.84 1.87 2.694(9) 168.2 .

_refine_diff_density_max         0.560
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.057



####################################################################### 
# 
# 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_zn250re_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2046664'
loop_
_audit_author_name
_audit_author_address
'Claire Deville'
;Technical University of Denmark (current)
Denmark
;
_audit_update_record             
;
2020-11-26 deposited with the CCDC.	2021-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Zn N4 O5, 3( C3 H7 N O), H2 O'
_chemical_formula_sum            'C33 H41 N7 O9 Zn'
_chemical_formula_weight         745.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3242 0.9375 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_H-M_alt        'P 41'
_space_group_name_Hall           'P 4w'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'

_cell_length_a                   13.7729(8)
_cell_length_b                   13.7729(8)
_cell_length_c                   19.5804(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3714.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    9247
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      19.68

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   0.6839
_exptl_transmission_factor_max   0.7445
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.386
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6839
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50711
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.167
_diffrn_reflns_theta_max         20.558
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7637
_reflns_number_gt                6778
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.998

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0677P)²+0.1484P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2958 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7637
_refine_ls_number_parameters     432
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.1054
_refine_ls_wR_factor_gt          0.1013
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT987_zn250re_a_sq        
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Refinement gives BASF = 0.036(21). Deviation from zero is likely 
a consquence of Ag radiation.  
;

_vrf_FORMU01_zn250re_a_sq        
;
PROBLEM: There is a discrepancy between the atom counts in the
 _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C33 H41 N7 O9 Zn1
            Atom count from the _atom_site data:  C30 H34 N6 O8 Zn1
RESPONSE: _chemical_formula_sum includes one additional DMF from SQUEEZE.
;
# end Validation Reply Form

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 0.82841(3) 0.47553(3) 0.34223(2) 0.03992(14) Uani 1 1 d . . . . .
N1 N 0.7471(3) 0.5926(3) 0.35745(15) 0.0428(8) Uani 1 1 d . . . . .
C1 C 0.7827(3) 0.6867(3) 0.3612(2) 0.0490(10) Uani 1 1 d . . . . .
O2 O 1.0831(2) 0.4963(3) 0.76629(14) 0.0516(7) Uani 1 1 d . . . . .
N2 N 0.6299(3) 0.6878(3) 0.39166(18) 0.0465(8) Uani 1 1 d D . . . .
H2N H 0.571(2) 0.708(4) 0.402(3) 0.070 Uiso 1 1 d D U . . .
C2 C 0.8744(4) 0.7219(4) 0.3470(3) 0.0650(12) Uani 1 1 d . . . . .
H2 H 0.924092 0.681766 0.330161 0.078 Uiso 1 1 calc R U . . .
N3 N 0.7402(3) 0.3641(3) 0.32844(15) 0.0431(8) Uani 1 1 d . . . . .
O3 O 1.2160(2) 0.4791(2) 0.70416(15) 0.0512(7) Uani 1 1 d . . . . .
C3 C 0.8887(5) 0.8200(5) 0.3590(3) 0.0856(19) Uani 1 1 d . . . . .
H3 H 0.949949 0.847597 0.350431 0.103 Uiso 1 1 calc R U . . .
N4 N 0.6149(3) 0.2780(3) 0.29279(17) 0.0476(8) Uani 1 1 d D . . . .
O4 O 0.9225(2) 0.4475(3) 0.41481(13) 0.0499(7) Uani 1 1 d . . . . .
H4N H 0.556(3) 0.263(4) 0.275(3) 0.075 Uiso 1 1 d D U . . .
C4 C 0.8149(6) 0.8778(4) 0.3832(4) 0.0820(18) Uani 1 1 d . . . . .
H4 H 0.827505 0.943964 0.390966 0.098 Uiso 1 1 calc R U . . .
N5 N 0.3450(7) 0.2257(6) 0.6343(5) 0.131(3) Uani 1 1 d . . . . .
O5 O 0.7922(2) 0.4509(2) 0.48105(14) 0.0453(6) Uani 1 1 d . . . . .
C5 C 0.7269(5) 0.8438(4) 0.3960(3) 0.0733(15) Uani 1 1 d . . . . .
H5 H 0.677662 0.884779 0.412698 0.088 Uiso 1 1 calc R U . . .
C6 C 0.7092(4) 0.7462(3) 0.3842(2) 0.0525(11) Uani 1 1 d . . . . .
N6 N 0.1677(4) 0.3447(6) 0.2755(3) 0.107(2) Uani 1 1 d . . . . .
C7 C 0.6561(3) 0.5970(3) 0.37567(18) 0.0400(8) Uani 1 1 d . . . . .
O6 O 0.3812(10) 0.2461(8) 0.5187(5) 0.219(5) Uani 1 1 d D . . . .
O7 O 0.1965(5) 0.4158(7) 0.3783(4) 0.161(3) Uani 1 1 d D . . . .
O8 O 0.3883(5) 0.3877(6) 0.4207(4) 0.148(3) Uani 1 1 d D . . . .
H8WA H 0.395(8) 0.335(6) 0.444(4) 0.222 Uiso 1 1 d D U . . .
H8WB H 0.326(2) 0.394(10) 0.420(5) 0.222 Uiso 1 1 d D U . . .
C8A C 0.5886(3) 0.5130(3) 0.3802(2) 0.0426(9) Uani 0.574(10) 1 d . . P A 1
H8A H 0.610240 0.469718 0.417630 0.051 Uiso 0.574(10) 1 calc R U P A 1
C9A C 0.5829(3) 0.4533(3) 0.3129(2) 0.0437(9) Uani 0.574(10) 1 d . . P A 1
H9AA H 0.515564 0.432605 0.305804 0.052 Uiso 0.574(10) 1 calc R U P A 1
H9AB H 0.600909 0.495492 0.274655 0.052 Uiso 0.574(10) 1 calc R U P A 1
O1A O 0.4945(4) 0.5468(4) 0.3950(3) 0.0506(18) Uani 0.574(10) 1 d . . P A 1
H1A H 0.456618 0.500018 0.397448 0.076 Uiso 0.574(10) 1 calc R U P A 1
C8B C 0.5886(3) 0.5130(3) 0.3802(2) 0.0426(9) Uani 0.426(10) 1 d . . P A 2
H8BA H 0.523540 0.536757 0.391721 0.051 Uiso 0.426(10) 1 calc R U P A 2
H8BB H 0.609916 0.470174 0.417293 0.051 Uiso 0.426(10) 1 calc R U P A 2
C9B C 0.5829(3) 0.4533(3) 0.3129(2) 0.0437(9) Uani 0.426(10) 1 d . . P A 2
H9B H 0.603930 0.496248 0.275166 0.052 Uiso 0.426(10) 1 calc R U P A 2
O1B O 0.4838(6) 0.4295(6) 0.3016(5) 0.065(3) Uani 0.426(10) 1 d . . P A 2
H1B H 0.475935 0.416213 0.338558 0.097 Uiso 0.426(10) 1 d R U P A 2
C10 C 0.6468(3) 0.3660(3) 0.31226(18) 0.0373(8) Uani 1 1 d . . . . .
C11 C 0.6927(4) 0.2150(3) 0.2956(2) 0.0507(10) Uani 1 1 d . . . . .
C12 C 0.7022(5) 0.1169(4) 0.2791(3) 0.0687(14) Uani 1 1 d . . . . .
H12 H 0.648860 0.080009 0.264212 0.082 Uiso 1 1 calc R U . . .
C13 C 0.7918(5) 0.0770(4) 0.2854(3) 0.0803(17) Uani 1 1 d . . . . .
H13 H 0.801774 0.012337 0.271734 0.096 Uiso 1 1 calc R U . . .
C14 C 0.8710(5) 0.1310(4) 0.3124(3) 0.0768(16) Uani 1 1 d . . . . .
H14 H 0.931237 0.100289 0.318738 0.092 Uiso 1 1 calc R U . . .
C15 C 0.8609(4) 0.2269(4) 0.3292(3) 0.0655(13) Uani 1 1 d . . . . .
H15 H 0.913186 0.262983 0.346833 0.079 Uiso 1 1 calc R U . . .
C16 C 0.7705(3) 0.2686(3) 0.3192(2) 0.0476(10) Uani 1 1 d . . . . .
C17 C 1.1271(3) 0.4788(3) 0.7103(2) 0.0410(9) Uani 1 1 d . . . . .
C18 C 1.0636(3) 0.4605(3) 0.64956(19) 0.0409(9) Uani 1 1 d . . . . .
C20 C 1.0454(3) 0.4483(4) 0.5279(2) 0.0475(10) Uani 1 1 d . . . . .
H20 H 1.073601 0.445486 0.484249 0.057 Uiso 1 1 calc R U . . .
C19 C 1.1042(3) 0.4572(3) 0.5847(2) 0.0498(10) Uani 1 1 d . . . . .
H19 H 1.171942 0.461074 0.579476 0.060 Uiso 1 1 calc R U . . .
C23 C 0.9055(3) 0.4426(3) 0.5993(2) 0.0466(9) Uani 1 1 d . . . . .
H23 H 0.838021 0.435804 0.604555 0.056 Uiso 1 1 calc R U . . .
C22 C 0.8810(3) 0.4459(3) 0.47339(19) 0.0408(9) Uani 1 1 d . . . . .
C21 C 0.9458(3) 0.4433(3) 0.53456(19) 0.0406(9) Uani 1 1 d . . . . .
C24 C 0.9641(3) 0.4518(3) 0.6564(2) 0.0443(9) Uani 1 1 d . . . . .
H24 H 0.935991 0.452078 0.700194 0.053 Uiso 1 1 calc R U . . .
C25 C 0.3622(9) 0.2826(9) 0.5794(6) 0.142(4) Uani 1 1 d . . . . .
H25 H 0.360526 0.350396 0.584642 0.171 Uiso 1 1 calc R U . . .
C26 C 0.3449(13) 0.2621(12) 0.7009(6) 0.213(8) Uani 1 1 d . . . . .
H26A H 0.333679 0.331617 0.699799 0.320 Uiso 1 1 calc R U . . .
H26B H 0.407161 0.249077 0.722204 0.320 Uiso 1 1 calc R U . . .
H26C H 0.293800 0.230916 0.727005 0.320 Uiso 1 1 calc R U . . .
C28 C 0.1389(6) 0.3905(7) 0.3304(4) 0.110(3) Uani 1 1 d . . . . .
H28 H 0.072634 0.405387 0.334884 0.132 Uiso 1 1 calc R U . . .
C27 C 0.3444(14) 0.1198(8) 0.6289(9) 0.222(8) Uani 1 1 d . . . . .
H27A H 0.290905 0.099607 0.600046 0.332 Uiso 1 1 calc R U . . .
H27B H 0.336848 0.091678 0.673998 0.332 Uiso 1 1 calc R U . . .
H27C H 0.405183 0.098022 0.609083 0.332 Uiso 1 1 calc R U . . .
C29 C 0.0927(6) 0.3126(7) 0.2280(5) 0.118(3) Uani 1 1 d . . . . .
H29A H 0.078089 0.364627 0.196163 0.177 Uiso 1 1 calc R U . . .
H29B H 0.034482 0.295641 0.253161 0.177 Uiso 1 1 calc R U . . .
H29C H 0.115657 0.256357 0.202955 0.177 Uiso 1 1 calc R U . . .
C30 C 0.2615(7) 0.3468(15) 0.2529(7) 0.271(13) Uani 1 1 d . . . . .
H30A H 0.305083 0.334329 0.290753 0.407 Uiso 1 1 calc R U . . .
H30B H 0.275455 0.410245 0.233669 0.407 Uiso 1 1 calc R U . . .
H30C H 0.270441 0.297500 0.218092 0.407 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O2 1.962(3) 2_764 ?
Zn1 O4 1.962(3) . ?
Zn1 N3 1.976(4) . ?
Zn1 N1 1.985(4) . ?
N1 C7 1.305(5) . ?
N1 C1 1.388(6) . ?
C1 C6 1.378(7) . ?
C1 C2 1.380(7) . ?
O2 C17 1.275(5) . ?
N2 C7 1.338(5) . ?
N2 C6 1.365(6) . ?
N2 H2N 0.88(3) . ?
C2 C3 1.386(9) . ?
C2 H2 0.9400 . ?
N3 C10 1.326(5) . ?
N3 C16 1.392(6) . ?
O3 C17 1.231(5) . ?
C3 C4 1.375(10) . ?
C3 H3 0.9400 . ?
N4 C10 1.344(5) . ?
N4 C11 1.380(6) . ?
N4 H4N 0.91(3) . ?
O4 C22 1.282(5) . ?
C4 C5 1.324(9) . ?
C4 H4 0.9400 . ?
N5 C25 1.352(13) . ?
N5 C26 1.397(14) . ?
N5 C27 1.462(14) . ?
O5 C22 1.234(5) . ?
C5 C6 1.386(7) . ?
C5 H5 0.9400 . ?
N6 C28 1.308(10) . ?
N6 C30 1.366(12) . ?
N6 C29 1.459(10) . ?
C7 C8B 1.487(6) . ?
C7 C8A 1.487(6) . ?
O6 C25 1.317(14) . ?
O7 C28 1.276(10) . ?
O8 H8WA 0.86(3) . ?
O8 H8WB 0.86(3) . ?
C8A O1A 1.407(6) . ?
C8A C9A 1.555(5) . ?
C8A H8A 0.9900 . ?
C9A C10 1.490(6) . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
O1A H1A 0.8300 . ?
C8B C9B 1.555(5) . ?
C8B H8BA 0.9800 . ?
C8B H8BB 0.9800 . ?
C9B O1B 1.421(9) . ?
C9B C10 1.490(6) . ?
C9B H9B 0.9900 . ?
O1B H1B 0.7540 . ?
C11 C16 1.381(7) . ?
C11 C12 1.395(7) . ?
C12 C13 1.356(8) . ?
C12 H12 0.9400 . ?
C13 C14 1.421(10) . ?
C13 H13 0.9400 . ?
C14 C15 1.369(8) . ?
C14 H14 0.9400 . ?
C15 C16 1.386(7) . ?
C15 H15 0.9400 . ?
C17 C18 1.498(5) . ?
C18 C24 1.382(6) . ?
C18 C19 1.388(6) . ?
C20 C21 1.380(6) . ?
C20 C19 1.381(6) . ?
C20 H20 0.9400 . ?
C19 H19 0.9400 . ?
C23 C21 1.384(6) . ?
C23 C24 1.385(6) . ?
C23 H23 0.9400 . ?
C22 C21 1.494(5) . ?
C24 H24 0.9400 . ?
C25 H25 0.9400 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C28 H28 0.9400 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 H30C 0.9700 . ?

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
O2 Zn1 O4 100.22(11) 2_764 . ?
O2 Zn1 N3 115.60(14) 2_764 . ?
O4 Zn1 N3 110.63(14) . . ?
O2 Zn1 N1 107.69(14) 2_764 . ?
O4 Zn1 N1 115.07(13) . . ?
N3 Zn1 N1 107.71(14) . . ?
C7 N1 C1 106.4(3) . . ?
C7 N1 Zn1 128.4(3) . . ?
C1 N1 Zn1 124.5(3) . . ?
C6 C1 C2 121.9(5) . . ?
C6 C1 N1 108.2(4) . . ?
C2 C1 N1 129.9(5) . . ?
C17 O2 Zn1 113.1(3) . 2_765 ?
C7 N2 C6 108.0(4) . . ?
C7 N2 H2N 127(4) . . ?
C6 N2 H2N 125(4) . . ?
C1 C2 C3 116.0(6) . . ?
C1 C2 H2 122.0 . . ?
C3 C2 H2 122.0 . . ?
C10 N3 C16 106.1(3) . . ?
C10 N3 Zn1 127.9(3) . . ?
C16 N3 Zn1 124.6(3) . . ?
C4 C3 C2 121.2(6) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C10 N4 C11 107.6(4) . . ?
C10 N4 H4N 128(4) . . ?
C11 N4 H4N 124(4) . . ?
C22 O4 Zn1 110.9(3) . . ?
C5 C4 C3 122.6(6) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C25 N5 C26 122.4(11) . . ?
C25 N5 C27 121.4(11) . . ?
C26 N5 C27 115.2(11) . . ?
C4 C5 C6 118.1(6) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
N2 C6 C1 105.9(4) . . ?
N2 C6 C5 134.0(5) . . ?
C1 C6 C5 120.2(5) . . ?
C28 N6 C30 122.9(8) . . ?
C28 N6 C29 117.2(7) . . ?
C30 N6 C29 117.9(8) . . ?
N1 C7 N2 111.5(4) . . ?
N1 C7 C8B 125.5(4) . . ?
N2 C7 C8B 123.0(4) . . ?
N1 C7 C8A 125.5(4) . . ?
N2 C7 C8A 123.0(4) . . ?
H8WA O8 H8WB 101(4) . . ?
O1A C8A C7 109.3(4) . . ?
O1A C8A C9A 107.6(4) . . ?
C7 C8A C9A 113.1(3) . . ?
O1A C8A H8A 108.9 . . ?
C7 C8A H8A 108.9 . . ?
C9A C8A H8A 108.9 . . ?
C10 C9A C8A 113.8(3) . . ?
C10 C9A H9AA 108.8 . . ?
C8A C9A H9AA 108.8 . . ?
C10 C9A H9AB 108.8 . . ?
C8A C9A H9AB 108.8 . . ?
H9AA C9A H9AB 107.7 . . ?
C8A O1A H1A 109.5 . . ?
C7 C8B C9B 113.1(3) . . ?
C7 C8B H8BA 109.0 . . ?
C9B C8B H8BA 109.0 . . ?
C7 C8B H8BB 109.0 . . ?
C9B C8B H8BB 109.0 . . ?
H8BA C8B H8BB 107.8 . . ?
O1B C9B C10 112.3(5) . . ?
O1B C9B C8B 107.6(5) . . ?
C10 C9B C8B 113.8(3) . . ?
O1B C9B H9B 107.6 . . ?
C10 C9B H9B 107.6 . . ?
C8B C9B H9B 107.6 . . ?
C9B O1B H1B 92.6 . . ?
N3 C10 N4 111.5(4) . . ?
N3 C10 C9B 125.9(4) . . ?
N4 C10 C9B 122.5(4) . . ?
N3 C10 C9A 125.9(4) . . ?
N4 C10 C9A 122.5(4) . . ?
N4 C11 C16 106.2(4) . . ?
N4 C11 C12 132.3(5) . . ?
C16 C11 C12 121.5(5) . . ?
C13 C12 C11 117.2(6) . . ?
C13 C12 H12 121.4 . . ?
C11 C12 H12 121.4 . . ?
C12 C13 C14 121.3(5) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 121.2(5) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 117.2(5) . . ?
C14 C15 H15 121.4 . . ?
C16 C15 H15 121.4 . . ?
C11 C16 C15 121.6(4) . . ?
C11 C16 N3 108.5(4) . . ?
C15 C16 N3 130.0(4) . . ?
O3 C17 O2 123.8(4) . . ?
O3 C17 C18 120.2(4) . . ?
O2 C17 C18 115.9(4) . . ?
C24 C18 C19 119.1(4) . . ?
C24 C18 C17 121.1(3) . . ?
C19 C18 C17 119.8(4) . . ?
C21 C20 C19 120.8(4) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C19 C18 120.2(4) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C21 C23 C24 120.4(4) . . ?
C21 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
O5 C22 O4 123.4(4) . . ?
O5 C22 C21 119.7(3) . . ?
O4 C22 C21 116.8(4) . . ?
C20 C21 C23 119.0(4) . . ?
C20 C21 C22 121.2(4) . . ?
C23 C21 C22 119.7(4) . . ?
C18 C24 C23 120.4(4) . . ?
C18 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
O6 C25 N5 122.2(11) . . ?
O6 C25 H25 118.9 . . ?
N5 C25 H25 118.9 . . ?
N5 C26 H26A 109.5 . . ?
N5 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N5 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O7 C28 N6 123.2(7) . . ?
O7 C28 H28 118.4 . . ?
N6 C28 H28 118.4 . . ?
N5 C27 H27A 109.5 . . ?
N5 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N5 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N6 C29 H29A 109.5 . . ?
N6 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N6 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N6 C30 H30A 109.5 . . ?
N6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
N2 H2N O3 0.88(3) 1.93(4) 2.750(5) 154(5) 4_574
N4 H4N O5 0.91(3) 1.85(3) 2.738(5) 167(6) 4_564
O8 H8WA O6 0.86(3) 1.91(3) 2.737(11) 159(8) .
O8 H8WB O7 0.86(3) 1.99(3) 2.797(11) 157(8) .
O1A H1A O8 0.83 1.87 2.681(8) 166.7 .
O1B H1B O8 0.75 2.05 2.739(12) 152.2 .

_refine_diff_density_max         0.279
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.048



