# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2023

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2282116'
loop_
_audit_author_name
_audit_author_address
'Constantina Papatriantafyllopoulou' 'University of Galway'
_audit_update_record             
;
2023-09-17 deposited with the CCDC.	2023-10-04 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         ?
_chemical_formula_sum            'C29 H37 N9 O11 Zn'
_chemical_formula_weight         753.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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'
'-x, -y, -z'

_cell_length_a                   9.3796(7)
_cell_length_b                   12.5378(8)
_cell_length_c                   15.3451(10)
_cell_angle_alpha                87.967(5)
_cell_angle_beta                 73.076(6)
_cell_angle_gamma                84.839(6)
_cell_volume                     1719.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3120
_cell_measurement_theta_min      4.5880
_cell_measurement_theta_max      73.5940

_exptl_crystal_description       Blocks
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.608
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.53663
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11682
_diffrn_reflns_av_unetI/netI     0.0919
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.627
_diffrn_reflns_theta_max         73.880
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6767
_reflns_number_gt                4974
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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)+(0.0629P)²+4.1742P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6767
_refine_ls_number_parameters     483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.2009
_refine_ls_wR_factor_gt          0.1816
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6694(6) 0.5599(5) 0.0400(4) 0.0332(12) Uani 1 1 d . . . . .
H1 H 0.599262 0.613326 0.031301 0.040 Uiso 1 1 calc R U . . .
C2 C 0.7153(7) 0.4767(5) -0.0213(4) 0.0433(15) Uani 1 1 d . . . . .
H2 H 0.676370 0.474218 -0.070426 0.052 Uiso 1 1 calc R U . . .
C3 C 0.8192(8) 0.3978(5) -0.0087(4) 0.0471(16) Uani 1 1 d . . . . .
H3 H 0.851087 0.340907 -0.048965 0.056 Uiso 1 1 calc R U . . .
C4 C 0.8761(7) 0.4038(5) 0.0648(4) 0.0384(13) Uani 1 1 d . . . . .
H4 H 0.945462 0.350803 0.075270 0.046 Uiso 1 1 calc R U . . .
C5 C 0.8272(5) 0.4904(4) 0.1220(3) 0.0261(10) Uani 1 1 d . . . . .
C6 C 0.8841(5) 0.5072(4) 0.2011(3) 0.0236(9) Uani 1 1 d . . . . .
C7 C 0.5255(6) 0.5030(4) 0.3662(3) 0.0293(11) Uani 1 1 d . . . . .
H7 H 0.625226 0.487622 0.364208 0.035 Uiso 1 1 calc R U . . .
C8 C 0.4173(6) 0.4467(5) 0.4275(4) 0.0345(12) Uani 1 1 d . . . . .
H8 H 0.444762 0.394135 0.465214 0.041 Uiso 1 1 calc R U . . .
C9 C 0.2704(6) 0.4695(5) 0.4316(4) 0.0339(12) Uani 1 1 d . . . . .
H9 H 0.196162 0.434685 0.473651 0.041 Uiso 1 1 calc R U . . .
C10 C 0.2331(6) 0.5461(4) 0.3714(3) 0.0295(11) Uani 1 1 d . . . . .
H10 H 0.134092 0.561642 0.371760 0.035 Uiso 1 1 calc R U . . .
C11 C 0.3457(5) 0.5979(4) 0.3117(3) 0.0211(9) Uani 1 1 d . . . . .
C12 C 0.3192(5) 0.6797(4) 0.2449(3) 0.0201(9) Uani 1 1 d . . . . .
C13 C 0.7467(5) 0.8789(4) 0.0867(3) 0.0244(10) Uani 1 1 d . . . . .
C14 C 0.8782(5) 0.9412(4) 0.0422(3) 0.0218(9) Uani 1 1 d . . . . .
C15 C 0.8622(5) 1.0282(4) -0.0148(3) 0.0237(9) Uani 1 1 d . . . . .
C16 C 1.0188(5) 0.9134(4) 0.0565(3) 0.0234(9) Uani 1 1 d . . . . .
C17 C 0.6406(5) 0.8126(4) 0.3930(3) 0.0248(10) Uani 1 1 d . . . . .
C18 C 0.5668(5) 0.9098(4) 0.4474(3) 0.0254(10) Uani 1 1 d . . . . .
C19 C 0.5872(6) 0.9224(4) 0.5328(3) 0.0287(11) Uani 1 1 d . . . . .
C20 C 0.4785(6) 0.9892(4) 0.4141(3) 0.0283(10) Uani 1 1 d . . . . .
C21 C 0.4193(9) 0.8127(7) 0.7857(5) 0.063(2) Uani 1 1 d . . . . .
H21 H 0.374956 0.880536 0.804757 0.075 Uiso 1 1 calc R U . . .
C22 C 0.5868(11) 0.6633(7) 0.8025(6) 0.074(3) Uani 1 1 d . . . . .
H22A H 0.650845 0.643702 0.840169 0.111 Uiso 1 1 calc R U . . .
H22B H 0.513432 0.612174 0.811012 0.111 Uiso 1 1 calc R U . . .
H22C H 0.645450 0.664001 0.739739 0.111 Uiso 1 1 calc R U . . .
C23 C 0.5337(8) 0.8168(6) 0.9075(5) 0.0524(17) Uani 1 1 d . . . . .
H23A H 0.606377 0.772714 0.928524 0.079 Uiso 1 1 calc R U . . .
H23B H 0.568154 0.886703 0.891766 0.079 Uiso 1 1 calc R U . . .
H23C H 0.440388 0.822815 0.954876 0.079 Uiso 1 1 calc R U . . .
C24 C 0.9977(8) 0.2817(6) 0.4513(5) 0.0555(18) Uani 1 1 d . . . . .
H24 H 1.076757 0.261297 0.475043 0.067 Uiso 1 1 calc R U . . .
C25 C 0.7488(9) 0.2550(7) 0.4505(7) 0.071(2) Uani 1 1 d . . . . .
H25A H 0.674737 0.206300 0.478081 0.106 Uiso 1 1 calc R U . . .
H25B H 0.709809 0.326792 0.468796 0.106 Uiso 1 1 calc R U . . .
H25C H 0.773911 0.250187 0.385384 0.106 Uiso 1 1 calc R U . . .
C26 C 0.8707(12) 0.1444(7) 0.5475(6) 0.075(3) Uani 1 1 d . . . . .
H26A H 0.776665 0.113643 0.559447 0.112 Uiso 1 1 calc R U . . .
H26B H 0.950888 0.089895 0.525930 0.112 Uiso 1 1 calc R U . . .
H26C H 0.878322 0.174314 0.602515 0.112 Uiso 1 1 calc R U . . .
C27 C 0.9884(8) 0.1569(6) 0.1972(5) 0.0512(17) Uani 1 1 d . . . . .
H27 H 0.892999 0.168640 0.190212 0.061 Uiso 1 1 calc R U . . .
C28 C 1.1557(10) 0.0493(9) 0.2610(8) 0.097(4) Uani 1 1 d . . . . .
H28A H 1.153814 -0.012672 0.299793 0.146 Uiso 1 1 calc R U . . .
H28B H 1.227869 0.035038 0.202997 0.146 Uiso 1 1 calc R U . . .
H28C H 1.182578 0.108993 0.288632 0.146 Uiso 1 1 calc R U . . .
C29 C 0.8939(9) 0.0040(7) 0.2930(6) 0.064(2) Uani 1 1 d . . . . .
H29A H 0.933322 -0.050936 0.326852 0.096 Uiso 1 1 calc R U . . .
H29B H 0.811714 0.045228 0.333692 0.096 Uiso 1 1 calc R U . . .
H29C H 0.859761 -0.028309 0.247757 0.096 Uiso 1 1 calc R U . . .
N1 N 0.7230(5) 0.5660(3) 0.1115(3) 0.0239(8) Uani 1 1 d . . . . .
N2 N 0.8320(4) 0.5951(3) 0.2459(3) 0.0217(8) Uani 1 1 d . . . . .
N3 N 0.9837(6) 0.4342(4) 0.2223(4) 0.0363(11) Uani 1 1 d . . . . .
N4 N 0.4912(4) 0.5781(3) 0.3102(3) 0.0232(8) Uani 1 1 d . . . . .
N5 N 0.4333(4) 0.7283(3) 0.1991(3) 0.0219(8) Uani 1 1 d . . . . .
N6 N 0.1818(5) 0.7014(4) 0.2349(3) 0.0302(10) Uani 1 1 d . . . . .
N7 N 0.5126(6) 0.7682(4) 0.8273(3) 0.0407(12) Uani 1 1 d . . . . .
N8 N 0.8798(6) 0.2278(4) 0.4790(4) 0.0412(12) Uani 1 1 d . . . . .
N9 N 1.0107(6) 0.0740(4) 0.2486(4) 0.0437(12) Uani 1 1 d . . . . .
O1 O 0.8895(4) 0.6026(3) 0.3200(2) 0.0259(7) Uani 1 1 d . . . . .
O2 O 0.3957(4) 0.8030(3) 0.1378(3) 0.0307(8) Uani 1 1 d . . . . .
O3 O 0.7719(4) 0.7946(3) 0.1296(3) 0.0290(8) Uani 1 1 d . . . . .
O4 O 0.6210(4) 0.9131(3) 0.0801(3) 0.0395(10) Uani 1 1 d . . . . .
O5 O 0.6069(4) 0.8000(3) 0.3199(2) 0.0331(8) Uani 1 1 d . . . . .
O6 O 0.7275(5) 0.7504(3) 0.4218(3) 0.0407(10) Uani 1 1 d . . . . .
O7 O 1.0391(4) 0.8295(3) 0.1128(3) 0.0303(8) Uani 1 1 d . . . . .
O8 O 0.4525(5) 0.9818(4) 0.3321(3) 0.0436(11) Uani 1 1 d . . . . .
O9 O 0.3845(8) 0.7726(6) 0.7229(5) 0.092(2) Uani 1 1 d . . . . .
O10 O 1.0141(7) 0.3573(5) 0.3963(4) 0.0722(18) Uani 1 1 d . . . . .
O11 O 1.0785(5) 0.2199(4) 0.1579(4) 0.0505(11) Uani 1 1 d . . . . .
Zn01 Zn 0.64580(7) 0.68553(5) 0.21879(4) 0.01989(18) Uani 1 1 d . . . . .
H1N6 H 0.112(7) 0.672(5) 0.264(4) 0.033(17) Uiso 1 1 d . . . . .
H2O H 0.490(9) 0.834(6) 0.113(6) 0.06(2) Uiso 1 1 d . . . . .
H2N3 H 0.995(8) 0.438(6) 0.273(5) 0.05(2) Uiso 1 1 d . . . . .
H2N6 H 0.171(8) 0.751(6) 0.195(5) 0.044(19) Uiso 1 1 d . . . . .
H1N3 H 0.996(10) 0.373(7) 0.194(6) 0.07(3) Uiso 1 1 d . . . . .
H1O H 0.831(9) 0.661(7) 0.357(6) 0.07(3) Uiso 1 1 d . . . . .
H7O H 0.940(7) 0.790(5) 0.128(4) 0.034(16) Uiso 1 1 d . . . . .
H8O H 0.511(13) 0.924(9) 0.300(8) 0.13(5) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.341(6) . ?
C1 C2 1.382(8) . ?
C2 C3 1.376(9) . ?
C3 C4 1.388(8) . ?
C4 C5 1.380(8) . ?
C5 N1 1.339(6) . ?
C5 C6 1.490(7) . ?
C6 N2 1.298(6) . ?
C6 N3 1.348(6) . ?
C7 N4 1.333(6) . ?
C7 C8 1.392(8) . ?
C8 C9 1.366(7) . ?
C9 C10 1.400(7) . ?
C10 C11 1.377(7) . ?
C11 N4 1.358(6) . ?
C11 C12 1.481(6) . ?
C12 N5 1.288(6) . ?
C12 N6 1.344(6) . ?
C13 O4 1.250(6) . ?
C13 O3 1.266(6) . ?
C13 C14 1.498(7) . ?
C14 C15 1.399(6) . ?
C14 C16 1.410(6) . ?
C15 C16 1.375(7) 2_775 ?
C16 O7 1.372(5) . ?
C17 O6 1.240(6) . ?
C17 O5 1.269(6) . ?
C17 C18 1.499(7) . ?
C18 C19 1.395(7) . ?
C18 C20 1.414(7) . ?
C19 C20 1.386(7) 2_676 ?
C20 O8 1.356(6) . ?
C21 O9 1.239(10) . ?
C21 N7 1.303(9) . ?
C22 N7 1.441(9) . ?
C23 N7 1.464(8) . ?
C24 O10 1.237(8) . ?
C24 N8 1.303(9) . ?
C25 N8 1.430(8) . ?
C26 N8 1.446(8) . ?
C27 O11 1.221(8) . ?
C27 N9 1.320(8) . ?
C28 N9 1.433(9) . ?
C29 N9 1.460(9) . ?
N1 Zn01 2.183(4) . ?
N2 O1 1.403(5) . ?
N2 Zn01 2.131(4) . ?
N4 Zn01 2.218(4) . ?
N5 O2 1.400(5) . ?
N5 Zn01 2.121(3) . ?
O3 Zn01 2.087(3) . ?
O5 Zn01 2.082(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.1(5) . . ?
C3 C2 C1 119.0(5) . . ?
C2 C3 C4 119.3(6) . . ?
C5 C4 C3 118.3(5) . . ?
N1 C5 C4 122.7(5) . . ?
N1 C5 C6 114.3(4) . . ?
C4 C5 C6 123.0(4) . . ?
N2 C6 N3 123.9(5) . . ?
N2 C6 C5 115.6(4) . . ?
N3 C6 C5 120.4(5) . . ?
N4 C7 C8 122.3(4) . . ?
C9 C8 C7 119.2(4) . . ?
C8 C9 C10 119.0(5) . . ?
C11 C10 C9 118.8(5) . . ?
N4 C11 C10 122.1(4) . . ?
N4 C11 C12 114.6(4) . . ?
C10 C11 C12 123.3(4) . . ?
N5 C12 N6 123.1(4) . . ?
N5 C12 C11 116.4(4) . . ?
N6 C12 C11 120.5(4) . . ?
O4 C13 O3 124.6(5) . . ?
O4 C13 C14 118.7(4) . . ?
O3 C13 C14 116.7(4) . . ?
C15 C14 C16 119.2(4) . . ?
C15 C14 C13 119.8(4) . . ?
C16 C14 C13 121.0(4) . . ?
C16 C15 C14 120.9(4) 2_775 . ?
O7 C16 C15 118.9(4) . 2_775 ?
O7 C16 C14 121.2(4) . . ?
C15 C16 C14 119.9(4) 2_775 . ?
O6 C17 O5 124.8(5) . . ?
O6 C17 C18 119.1(4) . . ?
O5 C17 C18 116.1(4) . . ?
C19 C18 C20 119.4(5) . . ?
C19 C18 C17 118.9(4) . . ?
C20 C18 C17 121.8(4) . . ?
C20 C19 C18 121.2(4) 2_676 . ?
O8 C20 C19 117.9(4) . 2_676 ?
O8 C20 C18 122.7(5) . . ?
C19 C20 C18 119.4(4) 2_676 . ?
O9 C21 N7 125.7(8) . . ?
O10 C24 N8 126.0(6) . . ?
O11 C27 N9 127.5(6) . . ?
C5 N1 C1 118.6(4) . . ?
C5 N1 Zn01 116.0(3) . . ?
C1 N1 Zn01 125.3(3) . . ?
C6 N2 O1 111.4(4) . . ?
C6 N2 Zn01 118.3(3) . . ?
O1 N2 Zn01 128.7(3) . . ?
C7 N4 C11 118.5(4) . . ?
C7 N4 Zn01 126.8(3) . . ?
C11 N4 Zn01 114.6(3) . . ?
C12 N5 O2 111.5(3) . . ?
C12 N5 Zn01 119.8(3) . . ?
O2 N5 Zn01 128.6(3) . . ?
C21 N7 C22 121.2(6) . . ?
C21 N7 C23 121.5(6) . . ?
C22 N7 C23 116.9(5) . . ?
C24 N8 C25 122.0(6) . . ?
C24 N8 C26 120.9(6) . . ?
C25 N8 C26 116.9(7) . . ?
C27 N9 C28 119.5(6) . . ?
C27 N9 C29 122.9(6) . . ?
C28 N9 C29 117.6(6) . . ?
C13 O3 Zn01 137.0(3) . . ?
C17 O5 Zn01 138.4(3) . . ?
O5 Zn01 O3 87.34(16) . . ?
O5 Zn01 N5 91.30(15) . . ?
O3 Zn01 N5 99.76(14) . . ?
O5 Zn01 N2 98.47(15) . . ?
O3 Zn01 N2 95.63(14) . . ?
N5 Zn01 N2 162.13(16) . . ?
O5 Zn01 N1 171.16(15) . . ?
O3 Zn01 N1 88.43(15) . . ?
N5 Zn01 N1 97.06(15) . . ?
N2 Zn01 N1 74.23(15) . . ?
O5 Zn01 N4 92.21(16) . . ?
O3 Zn01 N4 174.06(14) . . ?
N5 Zn01 N4 74.33(15) . . ?
N2 Zn01 N4 90.30(15) . . ?
N1 Zn01 N4 92.80(16) . . ?

_refine_diff_density_max         0.919
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.100

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

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2282120'
loop_
_audit_author_name
_audit_author_address
'Constantina Papatriantafyllopoulou' 'University of Galway'
_audit_update_record             
;
2023-09-17 deposited with the CCDC.	2023-10-04 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         'C20 H16 N2 O7 Zn [+ solvent]'
_chemical_formula_sum            'C20 H16 N2 O7 Zn [+ solvent]'
_chemical_formula_weight         461.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

_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+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   9.4920(2)
_cell_length_b                   10.0245(3)
_cell_length_c                   13.4633(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.449(2)
_cell_angle_gamma                90
_cell_volume                     1278.75(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296.59(10)
_cell_measurement_reflns_used    5478
_cell_measurement_theta_min      4.3780
_cell_measurement_theta_max      70.9950

_exptl_crystal_description       block
_exptl_crystal_colour            yellowish
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_F_000             472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.654
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.362
_oxdiff_exptl_absorpt_empirical_full_max 4.884
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296.59(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.4223
_diffrn_reflns_number            8300
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.411
_diffrn_reflns_theta_max         70.887
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2437
_reflns_number_gt                2202
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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)+(0.0711P)²+0.1797P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2437
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1199
_refine_ls_wR_factor_gt          0.1167
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4094(2) 0.2448(2) 0.59079(18) 0.0713(5) Uani 1 1 d . . . . .
C2 C 0.4548(2) 0.1169(2) 0.54475(17) 0.0680(5) Uani 1 1 d . . . . .
C3 C 0.4073(3) -0.0069(2) 0.57613(18) 0.0761(6) Uani 1 1 d . . . . .
C4 C 0.5483(3) 0.1223(2) 0.46834(19) 0.0745(6) Uani 1 1 d . . . . .
H4 H 0.580778 0.204524 0.447309 0.089 Uiso 1 1 calc R U . . .
C5 C 0.4838(3) 0.3248(3) 0.9114(2) 0.0924(8) Uani 1 1 d . . . . .
H5 H 0.427127 0.253739 0.928694 0.111 Uiso 1 1 calc R U . . .
C6 C 0.6123(4) 0.3437(5) 0.9631(2) 0.1154(12) Uani 1 1 d . . . . .
H6 H 0.641507 0.286163 1.014493 0.138 Uiso 1 1 calc R U . . .
C7 C 0.6948(3) 0.4461(5) 0.9385(2) 0.1143(12) Uani 1 1 d . . . . .
H7 H 0.782784 0.458324 0.971566 0.137 Uiso 1 1 calc R U . . .
C8 C 0.6482(3) 0.5334(4) 0.8637(2) 0.0968(8) Uani 1 1 d . . . . .
H8 H 0.702635 0.606387 0.847290 0.116 Uiso 1 1 calc R U . . .
C9 C 0.5188(2) 0.5094(3) 0.81404(17) 0.0770(6) Uani 1 1 d . . . . .
C10 C 0.4603(3) 0.6010(3) 0.7333(2) 0.0851(7) Uani 1 1 d . . . . .
H10A H 0.420980 0.679403 0.763548 0.102 Uiso 1 1 calc R U . . .
H10B H 0.536512 0.630043 0.693621 0.102 Uiso 1 1 calc R U . . .
N1 N 0.4382(2) 0.4061(2) 0.83685(14) 0.0746(5) Uani 1 1 d . . . . .
O1 O 0.3155(6) -0.0226(4) 0.6476(4) 0.1159(15) Uani 0.5 1 d . . P . .
O2 O 0.4555(2) 0.35260(17) 0.56205(16) 0.0873(5) Uani 1 1 d . . . . .
O3 O 0.3249(2) 0.23128(18) 0.66006(14) 0.0844(5) Uani 1 1 d . . . . .
O4 O 0.35466(17) 0.53957(18) 0.67055(13) 0.0704(4) Uani 1 1 d . . . . .
Zn1 Zn 0.250000 0.37621(4) 0.750000 0.06652(17) Uani 1 2 d S T P . .
H4A H 0.384(3) 0.498(3) 0.6389(19) 0.062(8) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.237(3) . ?
C1 O3 1.273(3) . ?
C1 C2 1.498(3) . ?
C2 C3 1.395(3) . ?
C2 C4 1.399(3) . ?
C3 O1 1.346(4) . ?
C3 C4 1.380(3) 3_656 ?
C5 N1 1.344(3) . ?
C5 C6 1.381(5) . ?
C6 C7 1.345(6) . ?
C7 C8 1.387(5) . ?
C8 C9 1.384(4) . ?
C9 N1 1.334(3) . ?
C9 C10 1.503(4) . ?
C10 O4 1.413(3) . ?
N1 Zn1 2.0966(19) . ?
O3 Zn1 2.0462(16) . ?
O4 Zn1 2.2227(17) . ?

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 C1 O3 124.9(2) . . ?
O2 C1 C2 120.2(2) . . ?
O3 C1 C2 114.9(2) . . ?
C3 C2 C4 119.2(2) . . ?
C3 C2 C1 122.0(2) . . ?
C4 C2 C1 118.80(19) . . ?
O1 C3 C4 116.1(3) . 3_656 ?
O1 C3 C2 123.7(3) . . ?
C4 C3 C2 120.1(2) 3_656 . ?
C3 C4 C2 120.7(2) 3_656 . ?
N1 C5 C6 121.9(3) . . ?
C7 C6 C5 119.4(3) . . ?
C6 C7 C8 119.7(3) . . ?
C9 C8 C7 118.5(3) . . ?
N1 C9 C8 121.9(3) . . ?
N1 C9 C10 116.7(2) . . ?
C8 C9 C10 121.4(3) . . ?
O4 C10 C9 112.6(2) . . ?
C9 N1 C5 118.6(2) . . ?
C9 N1 Zn1 117.60(16) . . ?
C5 N1 Zn1 123.7(2) . . ?
C1 O3 Zn1 127.94(16) . . ?
C10 O4 Zn1 110.77(15) . . ?
O3 Zn1 O3 89.52(10) . 2_556 ?
O3 Zn1 N1 96.69(8) . . ?
O3 Zn1 N1 94.94(8) 2_556 . ?
O3 Zn1 N1 94.94(8) . 2_556 ?
O3 Zn1 N1 96.69(8) 2_556 2_556 ?
N1 Zn1 N1 163.60(12) . 2_556 ?
O3 Zn1 O4 93.27(7) . . ?
O3 Zn1 O4 171.60(7) 2_556 . ?
N1 Zn1 O4 76.87(7) . . ?
N1 Zn1 O4 90.97(7) 2_556 . ?
O3 Zn1 O4 171.59(7) . 2_556 ?
O3 Zn1 O4 93.27(7) 2_556 2_556 ?
N1 Zn1 O4 90.97(7) . 2_556 ?
N1 Zn1 O4 76.87(7) 2_556 2_556 ?
O4 Zn1 O4 85.09(10) . 2_556 ?

_refine_diff_density_max         0.361
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.041



####################################################################### 
# 
# 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_4_2628
_database_code_depnum_ccdc_archive 'CCDC 2282118'
loop_
_audit_author_name
_audit_author_address
'Constantina Papatriantafyllopoulou' 'University of Galway'
_audit_update_record             
;
2023-09-17 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H25 N3 Ni O9'
_chemical_formula_weight         546.17

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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'
'-x, -y, -z'

_cell_length_a                   9.6616(13)
_cell_length_b                   10.644(2)
_cell_length_c                   12.4656(15)
_cell_angle_alpha                95.832(14)
_cell_angle_beta                 90.191(11)
_cell_angle_gamma                97.496(15)
_cell_volume                     1264.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293.0(2)
_cell_measurement_reflns_used    1299
_cell_measurement_theta_min      3.8770
_cell_measurement_theta_max      20.2070

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_F_000             568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.823
_shelx_estimated_absorpt_T_min   0.821
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
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.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            8537
_diffrn_reflns_av_unetI/netI     0.3380
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.585
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8537
_reflns_number_gt                2970
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'crysalispro 1.171.42.51a (rigaku od, 2022)'
_computing_cell_refinement       'crysalispro 1.171.42.51a (rigaku od, 2022)'
_computing_data_reduction        'crysalispro 1.171.42.51a (rigaku od, 2022)'
_computing_structure_solution    
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail P. McArdle, J.Appl.Cryst.,2021,54,1535-1541.'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1219P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8537
_refine_ls_number_parameters     332
_refine_ls_number_restraints     264
_refine_ls_R_factor_all          0.2005
_refine_ls_R_factor_gt           0.0815
_refine_ls_wR_factor_ref         0.2209
_refine_ls_wR_factor_gt          0.1818
_refine_ls_goodness_of_fit_ref   0.707
_refine_ls_restrained_S_all      0.701
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.76618(17) 0.62732(15) 0.26243(16) 0.0372(5) Uani 1 1 d . . . . .
O1 O 0.5586(7) 0.6640(10) 0.4687(7) 0.053(3) Uani 1 1 d D . . . .
O2 O 0.7019(7) 0.7701(8) 0.3639(6) 0.046(2) Uani 1 1 d . . . . .
O3 O 0.3059(9) 0.9995(10) 0.6619(8) 0.072(3) Uani 1 1 d . . . . .
H3A H 0.272800 1.066905 0.668915 0.094 Uiso 1 1 calc R U . . .
O4 O 0.8511(7) 0.7685(8) 0.1763(6) 0.043(2) Uani 1 1 d . . . . .
O5 O 0.9838(8) 0.6677(10) 0.0597(7) 0.055(3) Uani 1 1 d . . . . .
O6 O 1.1485(9) 0.8022(8) -0.0602(7) 0.058(3) Uani 1 1 d . . . . .
H6 H 1.117437 0.737696 -0.032809 0.076 Uiso 1 1 calc R U . . .
O7 O 0.8601(7) 0.4886(8) 0.1670(6) 0.034(2) Uani 1 1 d . . . . .
H7A H 0.904731 0.524183 0.120253 0.044 Uiso 1 1 calc R U . . .
O8 O 0.6501(7) 0.4852(9) 0.3400(6) 0.041(2) Uani 1 1 d . . . . .
H8 H 0.619422 0.539956 0.380786 0.053 Uiso 1 1 calc DR U . . .
O9 O 0.2014(16) 0.2288(14) 0.2420(16) 0.174(6) Uani 1 1 d . U . . .
N1 N 0.5811(9) 0.6043(11) 0.1753(8) 0.037(3) Uani 1 1 d . . . . .
N2 N 0.9432(9) 0.6236(10) 0.3518(8) 0.038(3) Uani 1 1 d . . . . .
N3 N 0.224(2) 0.0223(19) 0.2594(16) 0.127(6) Uani 1 1 d . U . . .
C1 C 0.6071(12) 0.7632(14) 0.4307(11) 0.042(3) Uani 1 1 d . . . . .
C2 C 0.5552(10) 0.8840(13) 0.4689(10) 0.039(3) Uani 1 1 d . . . . .
C3 C 0.4587(11) 0.8912(13) 0.5476(10) 0.051(4) Uani 1 1 d . . . . .
H3 H 0.429158 0.818712 0.581569 0.066 Uiso 1 1 calc R U . . .
C4 C 0.4027(11) 1.0021(14) 0.5792(9) 0.047(4) Uani 1 1 d . . . . .
C5 C 0.9320(11) 0.7645(13) 0.0984(10) 0.034(3) Uani 1 1 d . . . . .
C6 C 0.9723(11) 0.8862(11) 0.0463(9) 0.031(3) Uani 1 1 d . . . . .
C7 C 0.9012(11) 0.9901(12) 0.0759(9) 0.039(3) Uani 1 1 d . . . . .
H7 H 0.833640 0.983741 0.128771 0.050 Uiso 1 1 calc R U . . .
C8 C 1.0711(11) 0.8979(13) -0.0285(9) 0.038(3) Uani 1 1 d . . . . .
C9 C 0.9551(11) 0.4326(12) 0.2346(9) 0.044(3) Uani 1 1 d . . . . .
H9A H 0.904985 0.358458 0.263061 0.057 Uiso 1 1 calc R U . . .
H9B H 1.030521 0.404700 0.190956 0.057 Uiso 1 1 calc R U . . .
C10 C 1.0135(13) 0.5240(13) 0.3241(10) 0.041(3) Uani 1 1 d . . . . .
C11 C 1.1414(12) 0.5147(15) 0.3714(11) 0.053(4) Uani 1 1 d . . . . .
H11 H 1.193703 0.449934 0.348495 0.070 Uiso 1 1 calc R U . . .
C12 C 1.1865(15) 0.6070(17) 0.4542(11) 0.069(5) Uani 1 1 d . . . . .
H12 H 1.269859 0.601447 0.489843 0.089 Uiso 1 1 calc R U . . .
C13 C 1.1140(14) 0.7068(16) 0.4864(11) 0.065(4) Uani 1 1 d . . . . .
H13 H 1.146093 0.767673 0.542880 0.084 Uiso 1 1 calc R U . . .
C14 C 0.9920(12) 0.7123(13) 0.4313(9) 0.045(4) Uani 1 1 d . . . . .
H14 H 0.941750 0.779897 0.449919 0.058 Uiso 1 1 calc R U . . .
C15 C 0.5415(12) 0.4191(13) 0.2729(10) 0.051(4) Uani 1 1 d . . . . .
H15A H 0.464046 0.388775 0.316845 0.066 Uiso 1 1 calc R U . . .
H15B H 0.574037 0.345619 0.233279 0.066 Uiso 1 1 calc R U . . .
C16 C 0.4915(13) 0.5041(13) 0.1934(9) 0.038(3) Uani 1 1 d . . . . .
C17 C 0.3619(13) 0.4789(17) 0.1418(11) 0.062(4) Uani 1 1 d . . . . .
H17 H 0.301683 0.406245 0.153634 0.081 Uiso 1 1 calc R U . . .
C18 C 0.3242(14) 0.5594(17) 0.0753(13) 0.071(5) Uani 1 1 d . . . . .
H18 H 0.236185 0.544825 0.042428 0.093 Uiso 1 1 calc R U . . .
C19 C 0.4117(14) 0.6587(16) 0.0566(11) 0.065(5) Uani 1 1 d . . . . .
H19 H 0.387220 0.715144 0.009755 0.084 Uiso 1 1 calc R U . . .
C20 C 0.5438(12) 0.6791(13) 0.1083(9) 0.047(4) Uani 1 1 d . . . . .
H20 H 0.606514 0.749003 0.093691 0.061 Uiso 1 1 calc R U . . .
C21 C 0.096(3) 0.031(3) 0.345(2) 0.247(13) Uani 1 1 d . U . . .
H21A H 0.062475 0.111714 0.344128 0.322 Uiso 1 1 calc R U . . .
H21B H 0.129474 0.022163 0.415866 0.322 Uiso 1 1 calc R U . . .
H21C H 0.021805 -0.036328 0.324064 0.322 Uiso 1 1 calc R U . . .
C22 C 0.2624(18) -0.0921(17) 0.2492(16) 0.126(7) Uani 1 1 d . U . . .
H22A H 0.342220 -0.092798 0.203557 0.163 Uiso 1 1 calc R U . . .
H22B H 0.187074 -0.152475 0.217715 0.163 Uiso 1 1 calc R U . . .
H22C H 0.286135 -0.114833 0.318929 0.163 Uiso 1 1 calc R U . . .
C23 C 0.233(3) 0.122(3) 0.237(3) 0.169(10) Uani 1 1 d . U . . .
H23 H 0.303661 0.124464 0.186078 0.219 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
Ni1 O4 2.024(8) . ?
Ni1 O2 2.038(8) . ?
Ni1 N2 2.045(10) . ?
Ni1 N1 2.062(9) . ?
O1 C1 1.239(15) . ?
O2 C1 1.240(12) . ?
O3 C4 1.395(11) . ?
O3 H3A 0.8200 . ?
O4 C5 1.250(12) . ?
O5 C5 1.256(13) . ?
O6 C8 1.368(13) . ?
O6 H6 0.8200 . ?
O7 C9 1.466(12) . ?
O7 H7A 0.8200 . ?
O8 C15 1.407(12) . ?
O8 H8 0.8200 . ?
O9 C23 1.21(2) . ?
N1 C20 1.292(13) . ?
N1 C16 1.322(14) . ?
N2 C14 1.337(13) . ?
N2 C10 1.348(14) . ?
N3 C23 1.12(3) . ?
N3 C22 1.314(19) . ?
N3 C21 1.64(3) . ?
C1 C2 1.475(18) . ?
C2 C3 1.359(13) . ?
C2 C4 1.420(17) 2_676 ?
C3 C4 1.384(17) . ?
C3 H3 0.9300 . ?
C5 C6 1.514(15) . ?
C6 C8 1.340(13) . ?
C6 C7 1.396(15) . ?
C7 C8 1.380(15) 2_775 ?
C7 H7 0.9300 . ?
C9 C10 1.464(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.387(15) . ?
C11 C12 1.378(18) . ?
C11 H11 0.9300 . ?
C12 C13 1.375(18) . ?
C12 H12 0.9300 . ?
C13 C14 1.373(15) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.525(15) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.387(16) . ?
C17 C18 1.334(19) . ?
C17 H17 0.9300 . ?
C18 C19 1.306(18) . ?
C18 H18 0.9300 . ?
C19 C20 1.410(15) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23 0.9300 . ?

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 Ni1 O2 85.2(3) . . ?
O4 Ni1 N2 94.9(3) . . ?
O2 Ni1 N2 93.1(4) . . ?
O4 Ni1 N1 92.2(4) . . ?
O2 Ni1 N1 91.3(3) . . ?
N2 Ni1 N1 172.0(4) . . ?
C1 O2 Ni1 128.5(9) . . ?
C4 O3 H3A 109.5 . . ?
C5 O4 Ni1 129.9(9) . . ?
C8 O6 H6 109.5 . . ?
C9 O7 H7A 109.5 . . ?
C15 O8 H8 109.5 . . ?
C20 N1 C16 117.7(11) . . ?
C20 N1 Ni1 126.7(10) . . ?
C16 N1 Ni1 115.5(8) . . ?
C14 N2 C10 120.1(12) . . ?
C14 N2 Ni1 124.7(9) . . ?
C10 N2 Ni1 115.2(9) . . ?
C23 N3 C22 151(3) . . ?
C23 N3 C21 98(3) . . ?
C22 N3 C21 111(2) . . ?
O1 C1 O2 124.3(14) . . ?
O1 C1 C2 119.4(12) . . ?
O2 C1 C2 116.2(13) . . ?
C3 C2 C4 116.2(12) . 2_676 ?
C3 C2 C1 122.1(13) . . ?
C4 C2 C1 121.6(11) 2_676 . ?
C2 C3 C4 122.5(12) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C3 C4 O3 117.8(13) . . ?
C3 C4 C2 121.3(10) . 2_676 ?
O3 C4 C2 120.9(12) . 2_676 ?
O4 C5 O5 125.4(13) . . ?
O4 C5 C6 117.6(12) . . ?
O5 C5 C6 117.0(11) . . ?
C8 C6 C7 118.5(11) . . ?
C8 C6 C5 123.0(12) . . ?
C7 C6 C5 118.5(10) . . ?
C8 C7 C6 121.5(10) 2_775 . ?
C8 C7 H7 119.3 2_775 . ?
C6 C7 H7 119.3 . . ?
C6 C8 O6 122.4(12) . . ?
C6 C8 C7 120.1(12) . 2_775 ?
O6 C8 C7 117.5(10) . 2_775 ?
C10 C9 O7 111.4(10) . . ?
C10 C9 H9A 109.3 . . ?
O7 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
O7 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 C11 121.6(13) . . ?
N2 C10 C9 116.8(11) . . ?
C11 C10 C9 121.3(13) . . ?
C12 C11 C10 116.2(14) . . ?
C12 C11 H11 121.9 . . ?
C10 C11 H11 121.9 . . ?
C13 C12 C11 123.0(15) . . ?
C13 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C14 C13 C12 116.8(15) . . ?
C14 C13 H13 121.6 . . ?
C12 C13 H13 121.6 . . ?
N2 C14 C13 122.1(14) . . ?
N2 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
O8 C15 C16 111.4(11) . . ?
O8 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
O8 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
N1 C16 C17 121.5(12) . . ?
N1 C16 C15 115.4(11) . . ?
C17 C16 C15 123.1(13) . . ?
C18 C17 C16 119.7(16) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C19 C18 C17 119.5(16) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C18 C19 C20 119.0(14) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
N1 C20 C19 122.5(13) . . ?
N1 C20 H20 118.7 . . ?
C19 C20 H20 118.7 . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 O9 154(4) . . ?
N3 C23 H23 103.1 . . ?
O9 C23 H23 103.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C1 O1 20.7(19) . . . . ?
Ni1 O2 C1 C2 -162.0(8) . . . . ?
O1 C1 C2 C3 2.3(19) . . . . ?
O2 C1 C2 C3 -175.2(11) . . . . ?
O1 C1 C2 C4 -173.9(11) . . . 2_676 ?
O2 C1 C2 C4 8.7(17) . . . 2_676 ?
C4 C2 C3 C4 1(2) 2_676 . . . ?
C1 C2 C3 C4 -175.8(12) . . . . ?
C2 C3 C4 O3 -179.1(11) . . . . ?
C2 C3 C4 C2 -1(2) . . . 2_676 ?
Ni1 O4 C5 O5 -3.6(17) . . . . ?
Ni1 O4 C5 C6 176.9(7) . . . . ?
O4 C5 C6 C8 171.4(10) . . . . ?
O5 C5 C6 C8 -8.1(17) . . . . ?
O4 C5 C6 C7 -10.0(16) . . . . ?
O5 C5 C6 C7 170.4(11) . . . . ?
C8 C6 C7 C8 1.3(19) . . . 2_775 ?
C5 C6 C7 C8 -177.4(11) . . . 2_775 ?
C7 C6 C8 O6 178.2(11) . . . . ?
C5 C6 C8 O6 -3.2(17) . . . . ?
C7 C6 C8 C7 -1.2(19) . . . 2_775 ?
C5 C6 C8 C7 177.3(11) . . . 2_775 ?
C14 N2 C10 C11 -4.3(17) . . . . ?
Ni1 N2 C10 C11 174.4(9) . . . . ?
C14 N2 C10 C9 -178.6(11) . . . . ?
Ni1 N2 C10 C9 0.2(13) . . . . ?
O7 C9 C10 N2 20.4(15) . . . . ?
O7 C9 C10 C11 -153.8(11) . . . . ?
N2 C10 C11 C12 5.3(18) . . . . ?
C9 C10 C11 C12 179.3(12) . . . . ?
C10 C11 C12 C13 -3(2) . . . . ?
C11 C12 C13 C14 0(2) . . . . ?
C10 N2 C14 C13 0.7(17) . . . . ?
Ni1 N2 C14 C13 -177.9(9) . . . . ?
C12 C13 C14 N2 1.7(19) . . . . ?
C20 N1 C16 C17 0.4(17) . . . . ?
Ni1 N1 C16 C17 178.7(9) . . . . ?
C20 N1 C16 C15 179.8(10) . . . . ?
Ni1 N1 C16 C15 -2.0(13) . . . . ?
O8 C15 C16 N1 21.1(14) . . . . ?
O8 C15 C16 C17 -159.6(11) . . . . ?
N1 C16 C17 C18 -2(2) . . . . ?
C15 C16 C17 C18 178.4(12) . . . . ?
C16 C17 C18 C19 2(2) . . . . ?
C17 C18 C19 C20 -1(2) . . . . ?
C16 N1 C20 C19 1.3(17) . . . . ?
Ni1 N1 C20 C19 -176.7(9) . . . . ?
C18 C19 C20 N1 -1(2) . . . . ?
C22 N3 C23 O9 179(4) . . . . ?
C21 N3 C23 O9 1(7) . . . . ?

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
O3 H3A O2 0.82 1.81 2.517(12) 143.7 2_676 yes
O6 H6 O5 0.82 1.87 2.583(11) 145.2 . yes
O7 H7A O5 0.82 1.85 2.605(12) 152.6 . yes
O8 H8 O1 0.82 1.79 2.609(11) 177.6 . yes
O8 H8 O2 0.82 2.51 2.992(12) 119.2 . yes
C11 H11 O9 0.93 2.59 3.42(2) 147.9 1_655 yes
C14 H14 O2 0.93 2.54 3.079(15) 117.6 . yes
C17 H17 O9 0.93 2.38 3.27(2) 158.7 . yes
C20 H20 O4 0.93 2.55 3.086(15) 117.0 . yes

_refine_diff_density_max         1.078
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.099

####################################################################### 
# 
# 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_6_2637
_database_code_depnum_ccdc_archive 'CCDC 2282119'
loop_
_audit_author_name
_audit_author_address
'Constantina Papatriantafyllopoulou' 'University of Galway'
_audit_update_record             
;
2023-09-17 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H30 N8 Ni O9'
_chemical_formula_weight         657.29

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'

_cell_length_a                   17.2182(10)
_cell_length_b                   10.0832(6)
_cell_length_c                   18.2479(9)
_cell_angle_alpha                90
_cell_angle_beta                 105.108(5)
_cell_angle_gamma                90
_cell_volume                     3058.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293.0(2)
_cell_measurement_reflns_used    3052
_cell_measurement_theta_min      3.7720
_cell_measurement_theta_max      22.7990

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             1368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.698
_shelx_estimated_absorpt_T_min   0.885
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
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.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            21202
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.523
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5571
_reflns_number_gt                3245
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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 1.171.42.51a (rigaku od, 2022)'
_computing_cell_refinement       'crysalispro 1.171.42.51a (rigaku od, 2022)'
_computing_data_reduction        'crysalispro 1.171.42.51a (rigaku od, 2022)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail P. McArdle, J.Appl.Cryst.,2021,54,1535-1541.'
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5571
_refine_ls_number_parameters     421
_refine_ls_number_restraints     346
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0769
_refine_ls_wR_factor_ref         0.2767
_refine_ls_wR_factor_gt          0.2161
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_restrained_S_all      0.848
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.25475(4) 0.42448(7) 0.59179(4) 0.0346(3) Uani 1 1 d . . . . .
O1 O 0.2517(3) 0.5829(4) 0.6606(2) 0.0496(11) Uani 1 1 d . . . . .
O2 O 0.3776(3) 0.6194(5) 0.7254(3) 0.0682(15) Uani 1 1 d . . . . .
O3 O 0.3549(4) 0.9023(8) 0.9394(4) 0.105(2) Uani 1 1 d . . . . .
H3A H 0.332709 0.943204 0.967105 0.137 Uiso 1 1 calc R U . . .
O4 O 0.2430(3) 0.9526(5) 1.0000(2) 0.0511(12) Uani 1 1 d . . . . .
O5 O 0.1160(3) 0.9149(5) 0.9398(3) 0.0644(15) Uani 1 1 d . . . . .
O6 O 0.0687(2) 0.4422(4) 0.5413(2) 0.0523(12) Uani 1 1 d . . . . .
O7 O 0.4356(3) 0.5021(5) 0.6282(3) 0.0635(14) Uani 1 1 d . . . . .
O8 O 0.5148(5) 0.1794(8) 0.4250(5) 0.129(3) Uani 1 1 d . . . . .
O9A O 0.035(2) 0.278(4) 0.808(2) 0.152(15) Uani 0.4 1 d . . P A 1
O9B O 0.0182(12) 0.2087(19) 0.7982(11) 0.095(5) Uani 0.6 1 d . . P A 2
N1 N 0.1373(3) 0.3930(5) 0.5910(3) 0.0402(11) Uani 1 1 d . . . . .
N2 N 0.0492(3) 0.3212(7) 0.6594(3) 0.0695(19) Uani 1 1 d . . . . .
H2A H 0.008172 0.352955 0.626551 0.090 Uiso 1 1 calc R U . . .
H2B H 0.042841 0.281136 0.699038 0.090 Uiso 1 1 calc R U . . .
N3 N 0.2644(3) 0.3078(5) 0.6884(3) 0.0424(12) Uani 1 1 d . . . . .
N4 N 0.2591(3) 0.2618(5) 0.5202(3) 0.0453(12) Uani 1 1 d . . . . .
N5 N 0.3743(3) 0.4148(5) 0.5944(3) 0.0395(11) Uani 1 1 d . . . . .
N6 N 0.4690(4) 0.3307(7) 0.5357(4) 0.077(2) Uani 1 1 d . . . . .
H6A H 0.505087 0.386739 0.557910 0.100 Uiso 1 1 calc R U . . .
H6B H 0.479585 0.273278 0.504808 0.100 Uiso 1 1 calc R U . . .
N7 N 0.6028(4) 0.0832(6) 0.3719(4) 0.0632(16) Uani 1 1 d . . . . .
N8 N -0.0389(6) 0.3352(10) 0.8825(5) 0.104(3) Uani 1 1 d . . . . .
C1 C 0.3039(4) 0.6288(6) 0.7171(3) 0.0428(14) Uani 1 1 d . . . . .
C2 C 0.2731(3) 0.6973(6) 0.7766(3) 0.0389(13) Uani 1 1 d . . . . .
C3 C 0.3277(4) 0.7688(6) 0.8333(3) 0.0428(14) Uani 1 1 d . . . . .
H3 H 0.381841 0.773145 0.833820 0.056 Uiso 1 1 calc R U . . .
C4 C 0.2997(3) 0.8325(6) 0.8882(3) 0.0385(13) Uani 1 1 d . . . . .
C5 C 0.2183(3) 0.8287(6) 0.8878(3) 0.0369(12) Uani 1 1 d . . . . .
C6 C 0.1662(4) 0.7551(6) 0.8324(3) 0.0481(15) Uani 1 1 d . . . . .
H6 H 0.112302 0.749423 0.832248 0.063 Uiso 1 1 calc R U . . .
C7 C 0.1932(4) 0.6893(6) 0.7768(4) 0.0468(15) Uani 1 1 d . . . . .
H7 H 0.157487 0.640040 0.739740 0.061 Uiso 1 1 calc R U . . .
C8 C 0.1891(4) 0.9048(6) 0.9468(3) 0.0373(13) Uani 1 1 d . . . . .
C9 C 0.1225(4) 0.3342(6) 0.6489(3) 0.0406(13) Uani 1 1 d . . . . .
C10 C 0.1945(4) 0.2803(6) 0.7043(3) 0.0452(14) Uani 1 1 d . . . . .
C11 C 0.1909(4) 0.2043(7) 0.7673(4) 0.0582(18) Uani 1 1 d . . . . .
H11 H 0.141939 0.184393 0.777327 0.076 Uiso 1 1 calc R U . . .
C12 C 0.2630(5) 0.1593(7) 0.8147(4) 0.0612(18) Uani 1 1 d . . . . .
H12 H 0.262760 0.107257 0.856673 0.080 Uiso 1 1 calc R U . . .
C13 C 0.3336(5) 0.1911(7) 0.7995(4) 0.0599(18) Uani 1 1 d . . . . .
H13 H 0.382090 0.163619 0.831775 0.078 Uiso 1 1 calc R U . . .
C14 C 0.3326(4) 0.2641(6) 0.7364(3) 0.0477(15) Uani 1 1 d . . . . .
H14 H 0.381382 0.284619 0.726192 0.062 Uiso 1 1 calc R U . . .
C15 C 0.1983(4) 0.1846(7) 0.4860(4) 0.0561(17) Uani 1 1 d . . . . .
H15 H 0.147314 0.202989 0.491901 0.073 Uiso 1 1 calc R U . . .
C16 C 0.2079(5) 0.0776(7) 0.4418(5) 0.069(2) Uani 1 1 d . . . . .
H16 H 0.164204 0.024841 0.418318 0.090 Uiso 1 1 calc R U . . .
C17 C 0.2827(5) 0.0511(8) 0.4333(5) 0.071(2) Uani 1 1 d . . . . .
H17 H 0.290516 -0.021295 0.404477 0.093 Uiso 1 1 calc R U . . .
C18 C 0.3465(5) 0.1310(7) 0.4673(4) 0.0624(18) Uani 1 1 d . . . . .
H18 H 0.397597 0.114434 0.461095 0.081 Uiso 1 1 calc R U . . .
C19 C 0.3333(4) 0.2370(6) 0.5110(3) 0.0456(14) Uani 1 1 d . . . . .
C20 C 0.3966(4) 0.3327(6) 0.5491(4) 0.0463(14) Uani 1 1 d . . . . .
C21 C 0.5443(6) -0.0028(12) 0.3258(7) 0.120(4) Uani 1 1 d . . . . .
H21A H 0.491628 0.022663 0.329234 0.156 Uiso 1 1 calc R U . . .
H21B H 0.554941 -0.092531 0.343220 0.156 Uiso 1 1 calc R U . . .
H21C H 0.546915 0.003428 0.274049 0.156 Uiso 1 1 calc R U . . .
C22 C 0.6852(6) 0.0733(9) 0.3671(6) 0.089(3) Uani 1 1 d . . . . .
H22A H 0.717014 0.140760 0.398053 0.116 Uiso 1 1 calc R U . . .
H22B H 0.686853 0.084952 0.315306 0.116 Uiso 1 1 calc R U . . .
H22C H 0.706276 -0.012471 0.384654 0.116 Uiso 1 1 calc R U . . .
C23 C 0.5810(6) 0.1660(10) 0.4161(5) 0.087(3) Uani 1 1 d . . . . .
H23 H 0.620801 0.221659 0.444266 0.113 Uiso 1 1 calc R U . . .
C24 C -0.0743(9) 0.3142(15) 0.9431(8) 0.157(5) Uani 1 1 d . . . . .
H24A H -0.099421 0.228472 0.937835 0.204 Uiso 1 1 calc R U . . .
H24B H -0.114053 0.381385 0.942199 0.204 Uiso 1 1 calc R U . . .
H24C H -0.033635 0.318426 0.990323 0.204 Uiso 1 1 calc R U . . .
C25A C -0.049(3) 0.480(4) 0.863(3) 0.168(17) Uani 0.4 1 d . . P B 1
H25A H -0.018620 0.502154 0.827357 0.218 Uiso 0.4 1 calc R U P B 1
H25B H -0.030565 0.532323 0.907991 0.218 Uiso 0.4 1 calc R U P B 1
H25C H -0.105066 0.498692 0.840383 0.218 Uiso 0.4 1 calc R U P B 1
C25B C -0.043(3) 0.441(2) 0.8274(16) 0.177(16) Uani 0.6 1 d . . P B 2
H25D H -0.022030 0.521002 0.853266 0.230 Uiso 0.6 1 calc R U P B 2
H25E H -0.098258 0.454298 0.799878 0.230 Uiso 0.6 1 calc R U P B 2
H25F H -0.012230 0.416451 0.792722 0.230 Uiso 0.6 1 calc R U P B 2
C26 C -0.0047(6) 0.2329(13) 0.8564(6) 0.098(3) Uani 1 1 d . . . . .
H26 H -0.008082 0.144614 0.869913 0.128 Uiso 1 1 calc R U . A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.041(4) . ?
Ni1 N1 2.043(5) . ?
Ni1 N5 2.049(5) . ?
Ni1 O4 2.051(4) 2_564 ?
Ni1 N3 2.090(5) . ?
Ni1 N4 2.110(5) . ?
O1 C1 1.265(7) . ?
O2 C1 1.242(7) . ?
O3 C4 1.344(8) . ?
O3 H3A 0.8200 . ?
O4 C8 1.252(7) . ?
O5 C8 1.237(7) . ?
O6 N1 1.380(6) . ?
O7 N5 1.389(6) . ?
O8 C23 1.201(10) . ?
O9A C26 1.32(3) . ?
O9B C26 1.25(2) . ?
N1 C9 1.294(7) . ?
N2 C9 1.331(7) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N3 C10 1.339(7) . ?
N3 C14 1.344(7) . ?
N4 C15 1.324(8) . ?
N4 C19 1.354(7) . ?
N5 C20 1.297(8) . ?
N6 C20 1.331(8) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
N7 C23 1.283(10) . ?
N7 C21 1.426(11) . ?
N7 C22 1.447(10) . ?
N8 C26 1.335(13) . ?
N8 C24 1.410(14) . ?
N8 C25B 1.45(3) . ?
N8 C25A 1.51(4) . ?
C1 C2 1.496(8) . ?
C2 C7 1.378(8) . ?
C2 C3 1.402(8) . ?
C3 C4 1.380(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(8) . ?
C5 C6 1.380(8) . ?
C5 C8 1.511(8) . ?
C6 C7 1.390(8) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C9 C10 1.484(8) . ?
C10 C11 1.397(9) . ?
C11 C12 1.391(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.352(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.363(9) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.382(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.363(11) . ?
C16 H16 0.9300 . ?
C17 C18 1.374(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.486(9) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25A H25A 0.9600 . ?
C25A H25B 0.9600 . ?
C25A H25C 0.9600 . ?
C25B H25D 0.9600 . ?
C25B H25E 0.9600 . ?
C25B H25F 0.9600 . ?
C26 H26 0.9300 . ?

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
O1 Ni1 N1 86.69(19) . . ?
O1 Ni1 N5 102.09(19) . . ?
N1 Ni1 N5 168.3(2) . . ?
O1 Ni1 O4 90.94(19) . 2_564 ?
N1 Ni1 O4 101.63(18) . 2_564 ?
N5 Ni1 O4 86.12(18) . 2_564 ?
O1 Ni1 N3 86.05(18) . . ?
N1 Ni1 N3 77.26(19) . . ?
N5 Ni1 N3 95.44(19) . . ?
O4 Ni1 N3 176.83(19) 2_564 . ?
O1 Ni1 N4 179.3(2) . . ?
N1 Ni1 N4 94.0(2) . . ?
N5 Ni1 N4 77.3(2) . . ?
O4 Ni1 N4 88.6(2) 2_564 . ?
N3 Ni1 N4 94.40(19) . . ?
C1 O1 Ni1 131.4(4) . . ?
C4 O3 H3A 109.5 . . ?
C8 O4 Ni1 139.6(4) . 2_565 ?
C9 N1 O6 112.5(5) . . ?
C9 N1 Ni1 118.1(4) . . ?
O6 N1 Ni1 128.7(4) . . ?
C9 N2 H2A 120.0 . . ?
C9 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C10 N3 C14 118.2(5) . . ?
C10 N3 Ni1 114.9(4) . . ?
C14 N3 Ni1 126.8(4) . . ?
C15 N4 C19 119.2(6) . . ?
C15 N4 Ni1 126.7(5) . . ?
C19 N4 Ni1 114.1(4) . . ?
C20 N5 O7 111.8(5) . . ?
C20 N5 Ni1 118.5(4) . . ?
O7 N5 Ni1 128.5(4) . . ?
C20 N6 H6A 120.0 . . ?
C20 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C23 N7 C21 119.3(8) . . ?
C23 N7 C22 122.4(8) . . ?
C21 N7 C22 118.4(7) . . ?
C26 N8 C24 119.0(10) . . ?
C26 N8 C25B 105.4(16) . . ?
C24 N8 C25B 134.2(19) . . ?
C26 N8 C25A 134(2) . . ?
C24 N8 C25A 107(2) . . ?
O2 C1 O1 123.9(5) . . ?
O2 C1 C2 119.4(5) . . ?
O1 C1 C2 116.8(5) . . ?
C7 C2 C3 120.5(5) . . ?
C7 C2 C1 121.1(5) . . ?
C3 C2 C1 118.4(5) . . ?
C4 C3 C2 118.7(6) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
O3 C4 C3 115.5(6) . . ?
O3 C4 C5 122.9(5) . . ?
C3 C4 C5 121.5(5) . . ?
C6 C5 C4 118.5(5) . . ?
C6 C5 C8 121.5(5) . . ?
C4 C5 C8 120.0(5) . . ?
C5 C6 C7 121.0(6) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C2 C7 C6 119.8(6) . . ?
C2 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
O5 C8 O4 125.3(5) . . ?
O5 C8 C5 119.1(5) . . ?
O4 C8 C5 115.6(5) . . ?
N1 C9 N2 124.0(6) . . ?
N1 C9 C10 114.6(5) . . ?
N2 C9 C10 121.4(5) . . ?
N3 C10 C11 121.8(6) . . ?
N3 C10 C9 114.5(5) . . ?
C11 C10 C9 123.6(6) . . ?
C12 C11 C10 117.8(6) . . ?
C12 C11 H11 121.1 . . ?
C10 C11 H11 121.1 . . ?
C13 C12 C11 120.0(6) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.1(7) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
N3 C14 C13 123.0(6) . . ?
N3 C14 H14 118.5 . . ?
C13 C14 H14 118.5 . . ?
N4 C15 C16 122.2(7) . . ?
N4 C15 H15 118.9 . . ?
C16 C15 H15 118.9 . . ?
C17 C16 C15 118.7(7) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C16 C17 C18 120.2(7) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C19 118.6(7) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
N4 C19 C18 121.0(6) . . ?
N4 C19 C20 114.9(5) . . ?
C18 C19 C20 124.0(6) . . ?
N5 C20 N6 125.0(6) . . ?
N5 C20 C19 114.2(5) . . ?
N6 C20 C19 120.8(6) . . ?
N7 C21 H21A 109.5 . . ?
N7 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N7 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N7 C22 H22A 109.5 . . ?
N7 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N7 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O8 C23 N7 127.1(9) . . ?
O8 C23 H23 116.5 . . ?
N7 C23 H23 116.5 . . ?
N8 C24 H24A 109.5 . . ?
N8 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N8 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N8 C25A H25A 109.5 . . ?
N8 C25A H25B 109.5 . . ?
H25A C25A H25B 109.5 . . ?
N8 C25A H25C 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
N8 C25B H25D 109.5 . . ?
N8 C25B H25E 109.5 . . ?
H25D C25B H25E 109.5 . . ?
N8 C25B H25F 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
O9B C26 N8 136.1(14) . . ?
O9A C26 N8 109(2) . . ?
O9A C26 H26 125.5 . . ?
N8 C26 H26 125.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C1 O2 29.5(10) . . . . ?
Ni1 O1 C1 C2 -150.2(4) . . . . ?
O2 C1 C2 C7 -168.2(6) . . . . ?
O1 C1 C2 C7 11.5(9) . . . . ?
O2 C1 C2 C3 11.0(9) . . . . ?
O1 C1 C2 C3 -169.4(6) . . . . ?
C7 C2 C3 C4 -1.1(9) . . . . ?
C1 C2 C3 C4 179.8(5) . . . . ?
C2 C3 C4 O3 -178.1(6) . . . . ?
C2 C3 C4 C5 -0.9(9) . . . . ?
O3 C4 C5 C6 179.3(7) . . . . ?
C3 C4 C5 C6 2.4(9) . . . . ?
O3 C4 C5 C8 -0.3(10) . . . . ?
C3 C4 C5 C8 -177.2(5) . . . . ?
C4 C5 C6 C7 -1.9(10) . . . . ?
C8 C5 C6 C7 177.7(6) . . . . ?
C3 C2 C7 C6 1.5(10) . . . . ?
C1 C2 C7 C6 -179.3(6) . . . . ?
C5 C6 C7 C2 0.0(10) . . . . ?
Ni1 O4 C8 O5 -7.5(11) 2_565 . . . ?
Ni1 O4 C8 C5 172.9(4) 2_565 . . . ?
C6 C5 C8 O5 -9.1(9) . . . . ?
C4 C5 C8 O5 170.5(6) . . . . ?
C6 C5 C8 O4 170.5(6) . . . . ?
C4 C5 C8 O4 -9.8(8) . . . . ?
O6 N1 C9 N2 0.6(9) . . . . ?
Ni1 N1 C9 N2 172.0(5) . . . . ?
O6 N1 C9 C10 -179.6(5) . . . . ?
Ni1 N1 C9 C10 -8.1(7) . . . . ?
C14 N3 C10 C11 -2.3(9) . . . . ?
Ni1 N3 C10 C11 -179.5(5) . . . . ?
C14 N3 C10 C9 179.0(5) . . . . ?
Ni1 N3 C10 C9 1.9(7) . . . . ?
N1 C9 C10 N3 4.0(8) . . . . ?
N2 C9 C10 N3 -176.2(6) . . . . ?
N1 C9 C10 C11 -174.6(6) . . . . ?
N2 C9 C10 C11 5.2(10) . . . . ?
N3 C10 C11 C12 1.2(10) . . . . ?
C9 C10 C11 C12 179.7(6) . . . . ?
C10 C11 C12 C13 1.0(11) . . . . ?
C11 C12 C13 C14 -1.9(11) . . . . ?
C10 N3 C14 C13 1.4(10) . . . . ?
Ni1 N3 C14 C13 178.1(5) . . . . ?
C12 C13 C14 N3 0.8(11) . . . . ?
C19 N4 C15 C16 1.0(10) . . . . ?
Ni1 N4 C15 C16 -178.1(6) . . . . ?
N4 C15 C16 C17 0.0(12) . . . . ?
C15 C16 C17 C18 -1.0(12) . . . . ?
C16 C17 C18 C19 1.0(12) . . . . ?
C15 N4 C19 C18 -1.0(9) . . . . ?
Ni1 N4 C19 C18 178.2(5) . . . . ?
C15 N4 C19 C20 177.5(6) . . . . ?
Ni1 N4 C19 C20 -3.3(6) . . . . ?
C17 C18 C19 N4 0.0(10) . . . . ?
C17 C18 C19 C20 -178.4(7) . . . . ?
O7 N5 C20 N6 0.0(9) . . . . ?
Ni1 N5 C20 N6 168.6(5) . . . . ?
O7 N5 C20 C19 -179.8(5) . . . . ?
Ni1 N5 C20 C19 -11.2(7) . . . . ?
N4 C19 C20 N5 9.4(8) . . . . ?
C18 C19 C20 N5 -172.2(6) . . . . ?
N4 C19 C20 N6 -170.4(6) . . . . ?
C18 C19 C20 N6 8.1(10) . . . . ?
C21 N7 C23 O8 1.5(16) . . . . ?
C22 N7 C23 O8 -178.4(10) . . . . ?
C24 N8 C26 O9B 164.3(17) . . . . ?
C25B N8 C26 O9B -4(3) . . . . ?
C24 N8 C26 O9A -171(2) . . . . ?
C25A N8 C26 O9A 8(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2A O5 0.86 2.25 3.094(7) 165.8 4_557 yes
N2 H2B O9A^a 0.86 2.03 2.83(3) 152.7 . yes
N2 H2B O9B^b 0.86 2.09 2.948(16) 171.5 . yes
N6 H6A O3 0.86 2.40 3.035(9) 130.6 4_657 yes
N6 H6B O8 0.86 1.96 2.803(8) 166.2 . yes
C11 H11 O9A^a 0.93 2.27 3.07(4) 142.9 . yes
C11 H11 O9B^b 0.93 2.27 3.168(18) 161.3 . yes
C15 H15 N1 0.93 2.67 3.199(8) 116.8 . yes
C18 H18 O8 0.93 2.37 3.223(11) 152.0 . yes
C25B^b H25F^b O9B^b 0.96 2.16 2.68(4) 112.8 . yes

_refine_diff_density_max         1.156
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.089

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

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2282117'
loop_
_audit_author_name
_audit_author_address
'Constantina Papatriantafyllopoulou' 'University of Galway'
_audit_update_record             
;
2023-09-17 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_audit_creation_date             2023-09-06
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H18 Mn N6 O8, C3 H7 N O [+ solvent]'
_chemical_formula_sum            'C23 H25 Mn N7 O9 [+ solvent]'
_chemical_formula_weight         598.44
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.5538(5)
_cell_length_b                   10.0426(5)
_cell_length_c                   15.8933(7)
_cell_angle_alpha                76.086(4)
_cell_angle_beta                 72.980(4)
_cell_angle_gamma                76.741(5)
_cell_volume                     1394.40(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5236
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      74.4440
_cell_measurement_theta_min      4.5620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.380
_oxdiff_exptl_absorpt_empirical_full_max 4.050
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8916
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.992
_diffrn_reflns_theta_max         66.992
_diffrn_reflns_theta_min         4.604
_diffrn_ambient_temperature      175.15
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4292
_reflns_number_total             4956
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4956
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0898
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0888P)²+8.8194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2292
_refine_ls_wR_factor_ref         0.2399
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
 C20(H20), C21(H21)
2.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N5(H5A,H5B)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O5(H5), O8(H8A), 01(H)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8321(7) 0.3812(8) 0.4360(4) 0.0370(16) Uani 1 1 d . . . . .
H1 H 0.730529 0.374852 0.446258 0.044 Uiso 1 1 calc R U . . .
C2 C 0.9096(9) 0.2999(11) 0.4975(6) 0.065(3) Uani 1 1 d . . . . .
H2 H 0.864491 0.236396 0.547327 0.078 Uiso 1 1 calc R U . . .
C3 C 1.0555(10) 0.3156(14) 0.4830(7) 0.090(5) Uani 1 1 d . . . . .
H3 H 1.113050 0.262101 0.523083 0.108 Uiso 1 1 calc R U . . .
C4 C 1.1169(9) 0.4089(11) 0.4104(6) 0.062(3) Uani 1 1 d . . . . .
H4 H 1.215448 0.423542 0.401389 0.075 Uiso 1 1 calc R U . . .
C5 C 1.0332(7) 0.4814(7) 0.3502(4) 0.0293(14) Uani 1 1 d . . . . .
C6 C 1.0909(6) 0.5840(7) 0.2701(4) 0.0245(12) Uani 1 1 d . . . . .
C7 C 0.9662(9) 0.4071(11) 0.1167(6) 0.059(3) Uani 1 1 d . . . . .
H7 H 1.029905 0.474261 0.099969 0.071 Uiso 1 1 calc R U . . .
C8 C 1.0060(10) 0.2961(13) 0.0730(8) 0.083(4) Uani 1 1 d . . . . .
H8 H 1.093451 0.289968 0.025423 0.100 Uiso 1 1 calc R U . . .
C9 C 0.9194(9) 0.1941(10) 0.0979(6) 0.056(2) Uani 1 1 d . . . . .
H9 H 0.947087 0.116646 0.068391 0.068 Uiso 1 1 calc R U . . .
C10 C 0.7907(7) 0.2061(8) 0.1669(5) 0.0355(15) Uani 1 1 d . . . . .
H10 H 0.729402 0.136650 0.186511 0.043 Uiso 1 1 calc R U . . .
C11 C 0.7544(7) 0.3248(7) 0.2065(4) 0.0279(13) Uani 1 1 d . . . . .
C12 C 0.6151(6) 0.3526(6) 0.2758(4) 0.0232(12) Uani 1 1 d . . . . .
C13 C 0.5466(7) 0.7757(7) 0.4024(4) 0.0287(14) Uani 1 1 d . . . . .
C14 C 0.5234(6) 0.8938(7) 0.4515(4) 0.0269(13) Uani 1 1 d . . . . .
C15 C 0.3875(7) 0.9254(7) 0.5129(4) 0.0278(13) Uani 1 1 d . . . . .
H15 H 0.310521 0.874347 0.521618 0.033 Uiso 1 1 calc R U . . .
C16 C 0.3635(7) 1.0297(7) 0.5612(4) 0.0271(13) Uani 1 1 d . . . . .
C17 C 0.7163(6) 0.8522(7) 0.1013(4) 0.0247(13) Uani 1 1 d . . . . .
C18 C 0.6037(6) 0.9279(7) 0.0488(4) 0.0264(13) Uani 1 1 d . . . . .
C19 C 0.4739(7) 0.8768(7) 0.0588(4) 0.0320(14) Uani 1 1 d . . . . .
C20 C 0.3719(7) 0.9495(7) 0.0103(4) 0.0313(14) Uani 1 1 d . . . . .
H20 H 0.283969 0.914259 0.017865 0.038 Uiso 1 1 calc R U . . .
C21 C 0.3804(9) -0.0172(8) 0.2574(6) 0.0475(19) Uani 1 1 d . . . . .
H21 H 0.393881 -0.115638 0.264657 0.057 Uiso 1 1 calc R U . . .
C22 C 0.1263(13) -0.0245(18) 0.2637(9) 0.112(5) Uani 1 1 d . . . . .
H22A H 0.035426 0.044444 0.262473 0.167 Uiso 1 1 calc R U . . .
H22B H 0.151332 -0.072421 0.212947 0.167 Uiso 1 1 calc R U . . .
H22C H 0.110328 -0.092473 0.319816 0.167 Uiso 1 1 calc R U . . .
C23 C 0.205(3) 0.171(3) 0.280(4) 0.40(4) Uani 1 1 d . . . . .
H23A H 0.101405 0.205897 0.276451 0.606 Uiso 1 1 calc R U . . .
H23B H 0.212215 0.164884 0.340633 0.606 Uiso 1 1 calc R U . . .
H23C H 0.268258 0.235313 0.237860 0.606 Uiso 1 1 calc R U . . .
N1 N 0.8925(5) 0.4671(6) 0.3637(3) 0.0264(11) Uani 1 1 d . . . . .
N2 N 0.9943(5) 0.6527(5) 0.2250(3) 0.0250(11) Uani 1 1 d . . . . .
N3 N 1.2322(6) 0.5984(7) 0.2484(4) 0.0442(16) Uani 1 1 d . . . . .
H3A H 1.267038 0.657862 0.200299 0.053 Uiso 1 1 calc R U . . .
H3B H 1.291268 0.548359 0.282050 0.053 Uiso 1 1 calc R U . . .
N4 N 0.8413(6) 0.4244(6) 0.1820(3) 0.0299(12) Uani 1 1 d . . . . .
N5 N 0.5176(6) 0.2661(7) 0.3037(4) 0.0388(14) Uani 1 1 d . . . . .
H5A H 0.434398 0.285147 0.344325 0.047 Uiso 1 1 calc R U . . .
H5B H 0.536263 0.189651 0.281640 0.047 Uiso 1 1 calc R U . . .
N6 N 0.5953(5) 0.4667(5) 0.3052(3) 0.0223(10) Uani 1 1 d . . . . .
N7 N 0.2485(9) 0.0459(11) 0.2575(7) 0.085(3) Uani 1 1 d . . . . .
O2 O 0.4574(5) 0.4858(5) 0.3699(3) 0.0331(10) Uani 1 1 d . . . . .
H2A H 0.447213 0.560095 0.388208 0.050 Uiso 1 1 calc R U . . .
O3 O 0.6758(5) 0.7440(4) 0.3530(3) 0.0297(10) Uani 1 1 d . . . . .
O4 O 0.4395(5) 0.7191(5) 0.4133(3) 0.0349(11) Uani 1 1 d . . . . .
O5 O 0.2287(5) 1.0524(5) 0.6215(3) 0.0338(10) Uani 1 1 d . . . . .
H5 H 0.227401 1.115939 0.647928 0.051 Uiso 1 1 calc R U . . .
O6 O 0.6897(5) 0.7362(5) 0.1524(3) 0.0285(9) Uani 1 1 d . . . . .
O7 O 0.8299(4) 0.8999(5) 0.0904(3) 0.0301(10) Uani 1 1 d . . . . .
O8 O 0.4444(5) 0.7542(6) 0.1152(3) 0.0445(13) Uani 1 1 d . . . . .
H8A H 0.515102 0.718224 0.139197 0.067 Uiso 1 1 calc R U . . .
O9 O 0.4900(6) 0.0277(6) 0.2498(4) 0.0486(13) Uani 1 1 d . . . . .
1 O 1.0588(5) 0.7454(5) 0.1500(3) 0.0370(11) Uani 1 1 d . . . . .
H H 0.992943 0.793629 0.124885 0.056 Uiso 1 1 calc R U . . .
Mn1 Mn 0.76784(9) 0.60327(9) 0.26106(5) 0.0183(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9500 . ?
C1 C2 1.391(9) . ?
C1 N1 1.328(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.375(12) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(9) . ?
C5 C6 1.486(9) . ?
C5 N1 1.333(8) . ?
C6 N2 1.303(7) . ?
C6 N3 1.325(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.376(12) . ?
C7 N4 1.340(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.376(13) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.408(9) . ?
C11 C12 1.477(8) . ?
C11 N4 1.359(9) . ?
C12 N5 1.328(8) . ?
C12 N6 1.293(8) . ?
C13 C14 1.512(9) . ?
C13 O3 1.271(7) . ?
C13 O4 1.231(8) . ?
C14 C15 1.399(8) . ?
C14 C16 1.406(9) 2_676 ?
C15 H15 0.9500 . ?
C15 C16 1.383(9) . ?
C16 O5 1.370(7) . ?
C17 C18 1.509(7) . ?
C17 O6 1.282(8) . ?
C17 O7 1.235(7) . ?
C18 C19 1.401(9) . ?
C18 C20 1.378(9) 2_675 ?
C19 C20 1.386(8) . ?
C19 O8 1.370(8) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C21 N7 1.274(10) . ?
C21 O9 1.196(9) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 N7 1.466(14) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 N7 1.33(3) . ?
N1 Mn1 2.295(5) . ?
N2 1 1.402(7) . ?
N2 Mn1 2.210(5) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N4 Mn1 2.301(5) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N6 O2 1.419(6) . ?
N6 Mn1 2.233(5) . ?
O2 H2A 0.8400 . ?
O3 Mn1 2.139(4) . ?
O5 H5 0.8400 . ?
O6 Mn1 2.123(4) . ?
O8 H8A 0.8400 . ?
1 H 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
C2 C1 H1 118.3 . . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.4(6) . . ?
C1 C2 H2 121.5 . . ?
C3 C2 C1 117.0(7) . . ?
C3 C2 H2 121.5 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.9(7) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(7) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 122.7(6) . . ?
N1 C5 C4 121.4(6) . . ?
N1 C5 C6 115.9(5) . . ?
N2 C6 C5 115.2(5) . . ?
N2 C6 N3 125.0(6) . . ?
N3 C6 C5 119.9(5) . . ?
C8 C7 H7 118.7 . . ?
N4 C7 H7 118.7 . . ?
N4 C7 C8 122.7(8) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.2(8) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 120.5 . . ?
C8 C9 C10 119.0(7) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 H10 121.2 . . ?
C9 C10 C11 117.7(7) . . ?
C11 C10 H10 121.2 . . ?
C10 C11 C12 122.1(6) . . ?
N4 C11 C10 122.9(6) . . ?
N4 C11 C12 115.0(5) . . ?
N5 C12 C11 121.2(6) . . ?
N6 C12 C11 115.3(6) . . ?
N6 C12 N5 123.4(6) . . ?
O3 C13 C14 116.7(6) . . ?
O4 C13 C14 117.7(5) . . ?
O4 C13 O3 125.6(6) . . ?
C15 C14 C13 119.3(6) . . ?
C15 C14 C16 119.0(6) . 2_676 ?
C16 C14 C13 121.6(5) 2_676 . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.1(6) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C14 119.9(6) . 2_676 ?
O5 C16 C14 122.5(6) . 2_676 ?
O5 C16 C15 117.6(6) . . ?
O6 C17 C18 116.3(5) . . ?
O7 C17 C18 119.8(6) . . ?
O7 C17 O6 123.7(5) . . ?
C19 C18 C17 121.6(6) . . ?
C20 C18 C17 119.6(6) 2_675 . ?
C20 C18 C19 118.9(5) 2_675 . ?
C20 C19 C18 120.2(6) . . ?
O8 C19 C18 121.8(5) . . ?
O8 C19 C20 118.0(6) . . ?
C18 C20 C19 120.9(6) 2_675 . ?
C18 C20 H20 119.5 2_675 . ?
C19 C20 H20 119.5 . . ?
N7 C21 H21 114.8 . . ?
O9 C21 H21 114.8 . . ?
O9 C21 N7 130.3(9) . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N7 C22 H22A 109.5 . . ?
N7 C22 H22B 109.5 . . ?
N7 C22 H22C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N7 C23 H23A 109.5 . . ?
N7 C23 H23B 109.5 . . ?
N7 C23 H23C 109.5 . . ?
C1 N1 C5 119.0(5) . . ?
C1 N1 Mn1 124.4(4) . . ?
C5 N1 Mn1 116.6(4) . . ?
C6 N2 1 111.2(5) . . ?
C6 N2 Mn1 121.1(4) . . ?
1 N2 Mn1 127.4(3) . . ?
C6 N3 H3A 120.0 . . ?
C6 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C7 N4 C11 117.5(6) . . ?
C7 N4 Mn1 125.3(5) . . ?
C11 N4 Mn1 117.1(4) . . ?
C12 N5 H5A 120.0 . . ?
C12 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C12 N6 O2 111.1(5) . . ?
C12 N6 Mn1 122.0(4) . . ?
O2 N6 Mn1 126.8(3) . . ?
C21 N7 C22 123.7(11) . . ?
C21 N7 C23 119.1(12) . . ?
C23 N7 C22 114.1(14) . . ?
N6 O2 H2A 109.5 . . ?
C13 O3 Mn1 133.4(4) . . ?
C16 O5 H5 109.5 . . ?
C17 O6 Mn1 135.8(4) . . ?
C19 O8 H8A 109.5 . . ?
N2 1 H 109.5 . . ?
N1 Mn1 N4 88.50(19) . . ?
N2 Mn1 N1 71.16(18) . . ?
N2 Mn1 N4 93.16(18) . . ?
N2 Mn1 N6 156.40(18) . . ?
N6 Mn1 N1 91.25(18) . . ?
N6 Mn1 N4 70.14(18) . . ?
O3 Mn1 N1 87.34(18) . . ?
O3 Mn1 N2 94.68(18) . . ?
O3 Mn1 N4 169.43(18) . . ?
O3 Mn1 N6 100.24(17) . . ?
O6 Mn1 N1 169.99(18) . . ?
O6 Mn1 N2 99.13(17) . . ?
O6 Mn1 N4 89.61(18) . . ?
O6 Mn1 N6 97.35(17) . . ?
O6 Mn1 O3 96.12(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0(2) . . . . ?
C2 C1 N1 C5 -2.7(12) . . . . ?
C2 C1 N1 Mn1 -179.8(7) . . . . ?
C2 C3 C4 C5 -3(2) . . . . ?
C3 C4 C5 C6 180.0(10) . . . . ?
C3 C4 C5 N1 3.0(15) . . . . ?
C4 C5 C6 N2 -173.9(8) . . . . ?
C4 C5 C6 N3 7.3(11) . . . . ?
C4 C5 N1 C1 -0.2(11) . . . . ?
C4 C5 N1 Mn1 177.0(7) . . . . ?
C5 C6 N2 1 -179.1(5) . . . . ?
C5 C6 N2 Mn1 -5.1(7) . . . . ?
C6 C5 N1 C1 -177.4(6) . . . . ?
C6 C5 N1 Mn1 -0.1(7) . . . . ?
C7 C8 C9 C10 0.8(18) . . . . ?
C8 C7 N4 C11 1.9(14) . . . . ?
C8 C7 N4 Mn1 178.6(9) . . . . ?
C8 C9 C10 C11 1.2(14) . . . . ?
C9 C10 C11 C12 175.6(7) . . . . ?
C9 C10 C11 N4 -1.9(10) . . . . ?
C10 C11 C12 N5 0.0(9) . . . . ?
C10 C11 C12 N6 -178.9(5) . . . . ?
C10 C11 N4 C7 0.3(10) . . . . ?
C10 C11 N4 Mn1 -176.6(5) . . . . ?
C11 C12 N6 O2 178.7(4) . . . . ?
C11 C12 N6 Mn1 -4.2(6) . . . . ?
C12 C11 N4 C7 -177.4(7) . . . . ?
C12 C11 N4 Mn1 5.7(6) . . . . ?
C13 C14 C15 C16 178.0(6) . . . . ?
C14 C13 O3 Mn1 -173.7(4) . . . . ?
C14 C15 C16 C14 0.3(10) . . . 2_676 ?
C14 C15 C16 O5 -178.6(6) . . . . ?
C16 C14 C15 C16 -0.3(10) 2_676 . . . ?
C17 C18 C19 C20 179.4(6) . . . . ?
C17 C18 C19 O8 -1.4(10) . . . . ?
C18 C17 O6 Mn1 -163.8(4) . . . . ?
C18 C19 C20 C18 0.4(11) . . . 2_675 ?
C20 C18 C19 C20 -0.4(11) 2_675 . . . ?
C20 C18 C19 O8 178.8(6) 2_675 . . . ?
N1 C1 C2 C3 2.7(16) . . . . ?
N1 C5 C6 N2 3.3(9) . . . . ?
N1 C5 C6 N3 -175.6(6) . . . . ?
N3 C6 N2 1 -0.3(9) . . . . ?
N3 C6 N2 Mn1 173.7(5) . . . . ?
N4 C7 C8 C9 -2.6(19) . . . . ?
N4 C11 C12 N5 177.7(5) . . . . ?
N4 C11 C12 N6 -1.2(7) . . . . ?
N5 C12 N6 O2 -0.2(8) . . . . ?
N5 C12 N6 Mn1 176.9(4) . . . . ?
O3 C13 C14 C15 -174.4(6) . . . . ?
O3 C13 C14 C16 3.8(9) . . . 2_676 ?
O4 C13 C14 C15 5.9(9) . . . . ?
O4 C13 C14 C16 -175.9(6) . . . 2_676 ?
O4 C13 O3 Mn1 6.0(10) . . . . ?
O6 C17 C18 C19 2.8(9) . . . . ?
O6 C17 C18 C20 -177.4(6) . . . 2_675 ?
O7 C17 C18 C19 179.6(6) . . . . ?
O7 C17 C18 C20 -0.6(9) . . . 2_675 ?
O7 C17 O6 Mn1 19.6(9) . . . . ?
O8 C19 C20 C18 -178.8(6) . . . 2_675 ?
O9 C21 N7 C22 177.2(10) . . . . ?
O9 C21 N7 C23 -24(3) . . . . ?

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

data_7_2484
_database_code_depnum_ccdc_archive 'CCDC 2282121'
loop_
_audit_author_name
_audit_author_address
'Constantina Papatriantafyllopoulou' 'University of Galway'
_audit_update_record             
;
2023-09-17 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H74 N14 O24 Zn3'
_chemical_formula_weight         1715.56
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'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'I a'
_space_group_name_Hall           'I -2ya'
_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+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'
_cell_length_a                   18.3768(9)
_cell_length_b                   10.3212(6)
_cell_length_c                   45.523(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.253(4)
_cell_angle_gamma                90
_cell_volume                     8627.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293.0(2)
_cell_measurement_reflns_used    3023
_cell_measurement_theta_min      3.6580
_cell_measurement_theta_max      21.7750
_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             3544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.904
_shelx_estimated_absorpt_T_min   0.661
_shelx_estimated_absorpt_T_max   0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.49395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
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.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            36376
_diffrn_reflns_av_unetI/netI     0.2213
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_theta_min         3.295
_diffrn_reflns_theta_max         29.266
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.774
_diffrn_reflns_point_group_measured_fraction_full 0.927
_reflns_number_total             18203
_reflns_number_gt                6673
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_max     0.672
_reflns_Friedel_fraction_full    0.857
_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 1.171.42.51a (rigaku od, 2022)'
_computing_cell_refinement       'crysalispro 1.171.42.51a (rigaku od, 2022)'
_computing_data_reduction        'crysalispro 1.171.42.51a (rigaku od, 2022)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail P. McArdle, J.Appl.Cryst.,2021,54,1535-1541.'
_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)+(0.1479P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1725 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.48(2)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         18203
_refine_ls_number_parameters     985
_refine_ls_number_restraints     1005
_refine_ls_R_factor_all          0.2556
_refine_ls_R_factor_gt           0.1022
_refine_ls_wR_factor_ref         0.3474
_refine_ls_wR_factor_gt          0.2450
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.962
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
O5 O 0.191(2) 1.038(3) 0.5610(5) 0.211(15) Uani 1 1 d . . . . .
H5B H 0.185517 1.113576 0.566163 0.274 Uiso 1 1 calc R U . . .
O10 O 0.0131(8) 0.6041(15) 0.6011(3) 0.081(5) Uani 1 1 d . . . . .
H10B H 0.002414 0.550721 0.588313 0.106 Uiso 1 1 calc R U . . .
O19 O 0.9629(10) -0.1684(16) 0.2877(4) 0.094(5) Uani 1 1 d . . . . .
H19B H 0.992866 -0.210491 0.297504 0.122 Uiso 1 1 calc R U . . .
Zn1 Zn 0.44720(11) 0.6780(3) 0.50512(5) 0.0431(9) Uani 1 1 d . . . . .
Zn2 Zn 0.35549(10) 0.1773(3) 0.64410(5) 0.0384(8) Uani 1 1 d . . . . .
Zn3 Zn 0.6511(2) 0.32380(15) 0.32455(10) 0.0390(4) Uani 1 1 d . . . . .
O1 O 0.3768(11) 0.8349(18) 0.5051(4) 0.061(5) Uani 1 1 d . . . . .
O2 O 0.3261(12) 0.835(2) 0.4600(4) 0.096(9) Uani 1 1 d . . . . .
O3 O 0.0773(12) 1.190(2) 0.5487(4) 0.073(7) Uani 1 1 d . . . . .
O4 O 0.0306(10) 1.1882(16) 0.5037(4) 0.045(4) Uani 1 1 d . . . . .
O6 O 0.4652(11) 0.710(2) 0.5750(4) 0.083(8) Uani 1 1 d . . . . .
H6 H 0.492206 0.765223 0.568398 0.107 Uiso 1 1 calc R U . . .
O7 O 0.4256(11) 0.706(2) 0.4363(4) 0.065(6) Uani 1 1 d . . . . .
H7 H 0.382974 0.715372 0.440583 0.085 Uiso 1 1 calc R U . . .
O8 O 0.2660(10) 0.2933(18) 0.6433(4) 0.050(4) Uani 1 1 d . . . . .
O9 O 0.2238(10) 0.311(2) 0.5978(4) 0.071(7) Uani 1 1 d . . . . .
O11 O -0.0677(10) 0.6726(15) 0.6440(4) 0.047(4) Uani 1 1 d . . . . .
O12 O -0.0288(11) 0.6528(18) 0.6910(4) 0.067(6) Uani 1 1 d . . . . .
O13 O 0.3696(12) 0.213(2) 0.7128(4) 0.059(5) Uani 1 1 d . . . . .
H13A H 0.398296 0.267828 0.707084 0.076 Uiso 1 1 calc R U . . .
O14 O 0.3352(11) 0.2128(18) 0.5762(4) 0.060(6) Uani 1 1 d . . . . .
H14A H 0.292558 0.220284 0.580635 0.078 Uiso 1 1 calc R U . . .
O15 O 0.6550(9) 0.2735(18) 0.2557(4) 0.049(5) Uani 1 1 d . . . . .
H15A H 0.697332 0.254348 0.260232 0.063 Uiso 1 1 calc R U . . .
O16 O 0.6439(13) 0.278(2) 0.3939(4) 0.083(7) Uani 1 1 d . . . . .
H16 H 0.611006 0.232044 0.387061 0.107 Uiso 1 1 calc R U . . .
O17 O 0.7338(9) 0.1834(16) 0.3241(4) 0.044(4) Uani 1 1 d . . . . .
O18 O 0.7643(13) 0.160(3) 0.2784(5) 0.114(10) Uani 1 1 d . . . . .
O20 O 1.0430(14) -0.146(2) 0.3706(5) 0.105(9) Uani 1 1 d . . . . .
O21 O 1.0686(12) -0.195(2) 0.3256(4) 0.067(6) Uani 1 1 d . . . . .
O22 O 0.4310(12) 0.807(2) 0.7197(5) 0.098(8) Uani 1 1 d . . . . .
N1 N 0.4626(13) 0.642(2) 0.4584(4) 0.046(5) Uani 1 1 d . . . . .
N2 N 0.5198(10) 0.5099(19) 0.5024(4) 0.047(5) Uani 1 1 d . . . . .
N3 N 0.3736(12) 0.1596(18) 0.5986(5) 0.044(5) Uani 1 1 d . . . . .
N4 N 0.4479(12) 0.048(2) 0.6412(5) 0.044(5) Uani 1 1 d . . . . .
N6 N 0.3440(13) 0.141(2) 0.6893(5) 0.047(5) Uani 1 1 d . . . . .
N7 N 0.7342(10) 0.4712(19) 0.3277(4) 0.049(5) Uani 1 1 d . U . . .
N8 N 0.6752(11) 0.347(2) 0.3711(4) 0.042(5) Uani 1 1 d . . . . .
N9 N 0.6272(14) 0.342(2) 0.2773(4) 0.049(5) Uani 1 1 d . . . . .
N11 N 0.3507(11) 0.553(2) 0.5071(4) 0.047(5) Uani 1 1 d . . . . .
N12 N 0.4267(12) 0.649(2) 0.5521(4) 0.051(5) Uani 1 1 d . . . . .
N13 N 0.3564(14) 0.655(3) 0.6987(6) 0.068(7) Uani 1 1 d . . . . .
C1 C 0.3270(18) 0.864(3) 0.4849(7) 0.064(8) Uani 1 1 d . . . . .
C2 C 0.2637(13) 0.946(2) 0.4953(6) 0.057(7) Uani 1 1 d . . . . .
C3 C 0.2148(13) 1.003(3) 0.4771(5) 0.076(9) Uani 1 1 d . . . . .
H3 H 0.220669 0.993476 0.457035 0.099 Uiso 1 1 calc R U . . .
C4 C 0.1570(12) 1.073(2) 0.4859(5) 0.060(8) Uani 1 1 d . . . . .
H4 H 0.123763 1.107731 0.472068 0.078 Uiso 1 1 calc R U . . .
C5 C 0.1482(13) 1.093(2) 0.5160(6) 0.054(6) Uani 1 1 d . . . . .
C6 C 0.1957(14) 1.034(3) 0.5333(5) 0.063(7) Uani 1 1 d . . . . .
C7 C 0.2503(12) 0.957(2) 0.5258(5) 0.055(6) Uani 1 1 d . . . . .
H7A H 0.278444 0.912317 0.539892 0.071 Uiso 1 1 calc R U . . .
C8 C 0.0792(14) 1.167(2) 0.5228(6) 0.035(5) Uani 1 1 d . . . . .
C9 C 0.5143(17) 0.530(3) 0.4208(5) 0.098(12) Uani 1 1 d . . . . .
H9A H 0.560379 0.562257 0.414754 0.127 Uiso 1 1 calc R U . . .
H9B H 0.475703 0.572117 0.409632 0.127 Uiso 1 1 calc R U . . .
H9C H 0.511828 0.438261 0.417452 0.127 Uiso 1 1 calc R U . . .
C10 C 0.5069(14) 0.556(3) 0.4511(5) 0.049(6) Uani 1 1 d . . . . .
C11 C 0.5366(12) 0.481(2) 0.4761(4) 0.042(5) Uani 1 1 d . . . . .
C12 C 0.5847(14) 0.377(2) 0.4723(6) 0.064(7) Uani 1 1 d . . . . .
H12 H 0.598281 0.352068 0.453694 0.083 Uiso 1 1 calc R U . . .
C13 C 0.6092(17) 0.317(3) 0.4954(7) 0.083(10) Uani 1 1 d . . . . .
H13 H 0.641606 0.250192 0.492158 0.108 Uiso 1 1 calc R U . . .
C14 C 0.5951(11) 0.338(2) 0.5218(6) 0.060(6) Uani 1 1 d . . . . .
H14 H 0.613569 0.290844 0.537795 0.077 Uiso 1 1 calc R U . . .
C15 C 0.5481(12) 0.443(3) 0.5236(5) 0.061(7) Uani 1 1 d . . . . .
H15 H 0.535604 0.467320 0.542388 0.079 Uiso 1 1 calc R U . . .
C16 C 0.3422(17) 0.600(3) 0.5880(5) 0.089(12) Uani 1 1 d . . . . .
H16A H 0.350861 0.685319 0.595661 0.116 Uiso 1 1 calc R U . . .
H16B H 0.367703 0.537642 0.600253 0.116 Uiso 1 1 calc R U . . .
H16C H 0.290978 0.581590 0.587686 0.116 Uiso 1 1 calc R U . . .
C17 C 0.3673(15) 0.592(3) 0.5594(5) 0.050(7) Uani 1 1 d . . . . .
C18 C 0.3233(14) 0.538(2) 0.5352(5) 0.042(6) Uani 1 1 d . . . . .
C19 C 0.2623(14) 0.461(3) 0.5398(7) 0.069(8) Uani 1 1 d . . . . .
H19 H 0.242744 0.449668 0.558128 0.089 Uiso 1 1 calc R U . . .
C20 C 0.2337(13) 0.404(3) 0.5143(7) 0.062(7) Uani 1 1 d . . . . .
H20 H 0.194862 0.348060 0.516568 0.080 Uiso 1 1 calc R U . . .
C21 C 0.2547(18) 0.421(3) 0.4869(7) 0.073(10) Uani 1 1 d . . . . .
H21 H 0.229907 0.384564 0.470683 0.095 Uiso 1 1 calc R U . . .
C22 C 0.3136(16) 0.492(3) 0.4848(6) 0.076(10) Uani 1 1 d . . . . .
H22 H 0.331618 0.501024 0.466067 0.099 Uiso 1 1 calc R U . . .
C23 C 0.2227(15) 0.335(3) 0.6243(7) 0.050(6) Uani 1 1 d . U . . .
C24 C 0.1601(7) 0.4140(14) 0.6358(3) 0.030(4) Uani 1 1 d G U . . .
C25 C 0.1459(8) 0.4263(14) 0.6654(3) 0.044(6) Uani 1 1 d G U . . .
H25 H 0.176218 0.386420 0.679517 0.057 Uiso 1 1 calc R U . . .
C26 C 0.0864(9) 0.4982(14) 0.6739(3) 0.043(5) Uani 1 1 d G U . . .
H26 H 0.076828 0.506426 0.693740 0.056 Uiso 1 1 calc R U . . .
C27 C 0.0410(7) 0.5578(14) 0.6528(4) 0.040(5) Uani 1 1 d G U . . .
C28 C 0.0553(8) 0.5454(16) 0.6232(3) 0.055(7) Uani 1 1 d G U . . .
C29 C 0.1148(9) 0.4735(16) 0.6146(2) 0.046(6) Uani 1 1 d G U . . .
H29 H 0.124360 0.465298 0.594822 0.060 Uiso 1 1 calc R U . . .
C30 C -0.0232(14) 0.634(3) 0.6630(7) 0.047(6) Uani 1 1 d . . . . .
C31 C 0.4511(16) 0.086(3) 0.5567(5) 0.088(10) Uani 1 1 d . . . . .
H31A H 0.416105 0.132755 0.544542 0.115 Uiso 1 1 calc R U . . .
H31B H 0.449847 -0.003964 0.551386 0.115 Uiso 1 1 calc R U . . .
H31C H 0.498877 0.120170 0.553794 0.115 Uiso 1 1 calc R U . . .
C32 C 0.4313(14) 0.102(3) 0.5913(5) 0.050(6) Uani 1 1 d . . . . .
C33 C 0.4705(13) 0.035(3) 0.6150(6) 0.045(6) Uani 1 1 d . . . . .
C34 C 0.5365(15) -0.035(2) 0.6106(6) 0.055(7) Uani 1 1 d . . . . .
H34 H 0.550448 -0.044982 0.591358 0.071 Uiso 1 1 calc R U . . .
C35 C 0.5803(17) -0.088(3) 0.6319(6) 0.069(8) Uani 1 1 d . . . . .
H35 H 0.624822 -0.127059 0.628606 0.090 Uiso 1 1 calc R U . . .
C36 C 0.5500(17) -0.076(3) 0.6601(6) 0.067(9) Uani 1 1 d . . . . .
H36 H 0.572893 -0.117900 0.676054 0.088 Uiso 1 1 calc R U . . .
C37 C 0.4833(14) 0.000(2) 0.6649(6) 0.048(6) Uani 1 1 d . . . . .
H37 H 0.466771 0.014432 0.683733 0.062 Uiso 1 1 calc R U . . .
C38 C 0.2781(13) 0.024(3) 0.7303(5) 0.074(9) Uani 1 1 d . . . . .
H38A H 0.321511 0.014502 0.742491 0.097 Uiso 1 1 calc R U . . .
H38B H 0.250027 -0.054296 0.730812 0.097 Uiso 1 1 calc R U . . .
H38C H 0.249710 0.094792 0.737388 0.097 Uiso 1 1 calc R U . . .
C39 C 0.2998(15) 0.053(3) 0.6969(6) 0.055(7) Uani 1 1 d . . . . .
N5 N 0.2809(8) 0.0128(15) 0.6456(4) 0.051(5) Uani 1 1 d G . . . .
C40 C 0.2612(10) -0.0226(18) 0.6737(3) 0.054(7) Uani 1 1 d G . . . .
C41 C 0.2127(10) -0.1242(19) 0.6773(3) 0.067(8) Uani 1 1 d G . . . .
H41 H 0.199541 -0.147903 0.696110 0.087 Uiso 1 1 calc R U . . .
C42 C 0.1839(10) -0.1903(17) 0.6530(5) 0.078(9) Uani 1 1 d G . . . .
H42 H 0.151498 -0.258259 0.655401 0.101 Uiso 1 1 calc R U . . .
C43 C 0.2036(12) -0.155(2) 0.6249(4) 0.118(15) Uani 1 1 d G . . . .
H43 H 0.184379 -0.199109 0.608578 0.153 Uiso 1 1 calc R U . . .
C44 C 0.2521(11) -0.0533(19) 0.6212(3) 0.065(8) Uani 1 1 d G . . . .
H44 H 0.265304 -0.029603 0.602464 0.085 Uiso 1 1 calc R U . . .
C45 C 0.7589(16) 0.414(3) 0.4130(5) 0.078(9) Uani 1 1 d . . . . .
H45A H 0.721595 0.385627 0.425776 0.102 Uiso 1 1 calc R U . . .
H45B H 0.775489 0.498321 0.418853 0.102 Uiso 1 1 calc R U . . .
H45C H 0.798886 0.353892 0.414268 0.102 Uiso 1 1 calc R U . . .
C46 C 0.7261(13) 0.419(3) 0.3794(5) 0.049(6) Uani 1 1 d . . . . .
C47 C 0.7602(14) 0.493(2) 0.3540(5) 0.058(6) Uani 1 1 d . U . . .
C48 C 0.8192(16) 0.574(3) 0.3620(5) 0.083(10) Uani 1 1 d . U . . .
H48 H 0.838550 0.581030 0.381103 0.108 Uiso 1 1 calc R U . . .
C49 C 0.8451(19) 0.641(3) 0.3389(6) 0.122(13) Uani 1 1 d . U . . .
H49 H 0.882615 0.700678 0.342208 0.158 Uiso 1 1 calc R U . . .
C50 C 0.8170(17) 0.624(3) 0.3107(6) 0.100(11) Uani 1 1 d . U . . .
H50 H 0.833141 0.670379 0.294744 0.129 Uiso 1 1 calc R U . . .
C51 C 0.7627(13) 0.531(3) 0.3080(5) 0.071(8) Uani 1 1 d . U . . .
H51 H 0.746007 0.511726 0.288911 0.092 Uiso 1 1 calc R U . . .
C52 C 0.7775(16) 0.144(3) 0.3053(6) 0.056(7) Uani 1 1 d . . . . .
C53 C 0.8396(15) 0.072(3) 0.3137(6) 0.050(6) Uani 1 1 d . U . . .
C54 C 0.8728(13) -0.014(3) 0.2941(5) 0.044(5) Uani 1 1 d . U . . .
H54 H 0.855033 -0.027468 0.274923 0.058 Uiso 1 1 calc R U . . .
C55 C 0.9317(14) -0.075(3) 0.3054(6) 0.048(6) Uani 1 1 d . U . . .
C56 C 0.9653(13) -0.062(2) 0.3336(5) 0.036(5) Uani 1 1 d . U . . .
C57 C 0.9308(14) 0.022(3) 0.3504(6) 0.055(7) Uani 1 1 d . U . . .
H57 H 0.951806 0.038185 0.368930 0.072 Uiso 1 1 calc R U . . .
C58 C 0.8672(14) 0.089(3) 0.3431(6) 0.053(7) Uani 1 1 d . U . . .
H58 H 0.843976 0.140297 0.356602 0.068 Uiso 1 1 calc R U . . .
C59 C 1.0340(14) -0.135(3) 0.3443(6) 0.049(6) Uani 1 1 d . . . . .
C60 C 0.5344(16) 0.406(3) 0.2408(5) 0.070(9) Uani 1 1 d . . . . .
H60A H 0.561609 0.462384 0.228492 0.092 Uiso 1 1 calc R U . . .
H60B H 0.485203 0.437207 0.241543 0.092 Uiso 1 1 calc R U . . .
H60C H 0.534398 0.320077 0.233002 0.092 Uiso 1 1 calc R U . . .
C61 C 0.5662(15) 0.406(2) 0.2690(5) 0.042(5) Uani 1 1 d . . . . .
N10 N 0.5363(10) 0.4879(18) 0.2917(3) 0.073(7) Uani 1 1 d G . . . .
C62 C 0.4811(12) 0.578(2) 0.2867(4) 0.099(13) Uani 1 1 d G . . . .
H62 H 0.461985 0.592309 0.267770 0.128 Uiso 1 1 calc R U . . .
C63 C 0.4544(13) 0.648(2) 0.3101(5) 0.135(17) Uani 1 1 d G . . . .
H63 H 0.417430 0.708332 0.306841 0.175 Uiso 1 1 calc R U . . .
C64 C 0.4829(14) 0.627(2) 0.3385(4) 0.139(18) Uani 1 1 d G . . . .
H64 H 0.465012 0.673475 0.354141 0.181 Uiso 1 1 calc R U . . .
C65 C 0.5381(12) 0.537(2) 0.3434(3) 0.096(12) Uani 1 1 d G . . . .
H65 H 0.557147 0.522594 0.362371 0.125 Uiso 1 1 calc R U . . .
C66 C 0.5648(9) 0.4671(18) 0.3200(3) 0.042(6) Uani 1 1 d G . . . .
C67 C 0.381(2) 0.673(3) 0.6697(8) 0.129(15) Uani 1 1 d . . . . .
H67A H 0.368119 0.759146 0.663047 0.168 Uiso 1 1 calc R U . . .
H67B H 0.357798 0.610843 0.656719 0.168 Uiso 1 1 calc R U . . .
H67C H 0.432587 0.662656 0.669646 0.168 Uiso 1 1 calc R U . . .
C68 C 0.3088(19) 0.553(3) 0.7012(7) 0.112(13) Uani 1 1 d . . . . .
H68A H 0.335245 0.477257 0.707597 0.145 Uiso 1 1 calc R U . . .
H68B H 0.284929 0.536366 0.682419 0.145 Uiso 1 1 calc R U . . .
H68C H 0.273131 0.574263 0.715238 0.145 Uiso 1 1 calc R U . . .
C69 C 0.3781(16) 0.718(3) 0.7184(7) 0.078(8) Uani 1 1 d . . . . .
H69 H 0.355058 0.704735 0.735901 0.101 Uiso 1 1 calc R U . . .
O99 O 0.1308(12) 0.316(2) 0.2267(4) 0.036(5) Uiso 0.5 1 d D U P . .
N99 N 0.110(2) 0.139(3) 0.2596(7) 0.054(10) Uiso 0.5 1 d D U P . .
C99 C 0.0985(15) 0.239(2) 0.2360(6) 0.019(6) Uiso 0.5 1 d D U P . .
H99 H 0.052170 0.234429 0.227042 0.025 Uiso 0.5 1 calc R U P . .
C97 C 0.067(2) 0.048(3) 0.2617(8) 0.051(10) Uiso 0.5 1 d D U P . .
H97A H 0.021529 0.068958 0.251745 0.066 Uiso 0.5 1 calc R U P . .
H97B H 0.059030 0.031236 0.282072 0.066 Uiso 0.5 1 calc R U P . .
H97C H 0.087239 -0.028011 0.252922 0.066 Uiso 0.5 1 calc R U P . .
N98 N 0.4392(17) 0.155(3) 0.4504(6) 0.015(7) Uiso 0.5 1 d D U P . .
C96 C 0.496(3) 0.060(6) 0.4429(14) 0.09(2) Uiso 0.5 1 d D U P . .
H96A H 0.479957 -0.025800 0.447520 0.119 Uiso 0.5 1 calc R U P . .
H96B H 0.540348 0.078807 0.453958 0.119 Uiso 0.5 1 calc R U P . .
H96C H 0.504833 0.065186 0.422231 0.119 Uiso 0.5 1 calc R U P . .
C95 C 0.410(2) 0.181(4) 0.4789(8) 0.036(10) Uiso 0.5 1 d D U P . .
H95A H 0.405528 0.101125 0.489443 0.047 Uiso 0.5 1 calc R U P . .
H95B H 0.362825 0.220648 0.476321 0.047 Uiso 0.5 1 calc R U P . .
H95C H 0.442035 0.238423 0.489776 0.047 Uiso 0.5 1 calc R U P . .
C94 C 0.416(2) 0.239(4) 0.4265(8) 0.032(10) Uiso 0.5 1 d D U P . .
H94 H 0.429940 0.216924 0.407772 0.042 Uiso 0.5 1 calc R U P . .
O98 O 0.3850(17) 0.320(3) 0.4281(6) 0.038(7) Uiso 0.5 1 d D U P . .
C98 C 0.183(3) 0.169(7) 0.2683(15) 0.15(3) Uiso 0.5 1 d D U P . .
H98A H 0.189450 0.158745 0.289244 0.193 Uiso 0.5 1 calc R U P . .
H98B H 0.193647 0.256611 0.263029 0.193 Uiso 0.5 1 calc R U P . .
H98C H 0.215261 0.111152 0.258652 0.193 Uiso 0.5 1 calc R U P . .
O50 O 0.1933(19) 0.163(3) 0.3939(7) 0.195(15) Uiso 1 1 d . . . . .
_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O5 C6 1.27(3) . ?
O5 H5B 0.8200 . ?
O10 C28 1.384(16) . ?
O10 H10B 0.8200 . ?
O19 C55 1.39(3) . ?
O19 H19B 0.8200 . ?
Zn1 O4 2.065(18) 2_575 ?
Zn1 O1 2.073(19) . ?
Zn1 N1 2.19(2) . ?
Zn1 N2 2.196(18) . ?
Zn1 N11 2.20(2) . ?
Zn1 N12 2.20(2) . ?
Zn2 O8 2.034(18) . ?
Zn2 O11 2.095(17) 2_565 ?
Zn2 N6 2.11(2) . ?
Zn2 N3 2.12(2) . ?
Zn2 N4 2.17(2) . ?
Zn2 N5 2.185(13) . ?
Zn3 O21 2.021(19) 2_455 ?
Zn3 O17 2.101(17) . ?
Zn3 N7 2.156(17) . ?
Zn3 N8 2.16(2) . ?
Zn3 C66 2.173(14) . ?
Zn3 N9 2.19(2) . ?
O1 C1 1.31(3) . ?
O2 C1 1.17(3) . ?
O3 C8 1.21(3) . ?
O4 C8 1.24(3) . ?
O6 N12 1.39(3) . ?
O6 H6 0.8200 . ?
O7 N1 1.36(3) . ?
O7 H7 0.8200 . ?
O8 C23 1.23(3) . ?
O9 C23 1.23(3) . ?
O11 C30 1.23(3) . ?
O12 C30 1.30(3) . ?
O13 N6 1.37(3) . ?
O13 H13A 0.8200 . ?
O14 N3 1.33(3) . ?
O14 H14A 0.8200 . ?
O15 N9 1.33(2) . ?
O15 H15A 0.8200 . ?
O16 N8 1.40(2) . ?
O16 H16 0.8200 . ?
O17 C52 1.26(3) . ?
O18 C52 1.25(3) . ?
O20 C59 1.21(3) . ?
O21 C59 1.25(3) . ?
O22 C69 1.34(3) . ?
N1 C10 1.26(3) . ?
N2 C15 1.28(2) . ?
N2 C11 1.28(2) . ?
N3 C32 1.27(3) . ?
N4 C33 1.29(3) . ?
N4 C37 1.33(3) . ?
N6 C39 1.27(3) . ?
N7 C51 1.23(2) . ?
N7 C47 1.29(2) . ?
N8 C46 1.24(3) . ?
N9 C61 1.34(3) . ?
N11 C22 1.36(3) . ?
N11 C18 1.40(3) . ?
N12 C17 1.30(3) . ?
N13 C69 1.17(3) . ?
N13 C68 1.38(4) . ?
N13 C67 1.42(4) . ?
C1 C2 1.53(3) . ?
C2 C3 1.33(3) . ?
C2 C7 1.42(3) . ?
C3 C4 1.36(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.40(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.31(3) . ?
C5 C8 1.52(3) . ?
C6 C7 1.33(3) . ?
C7 H7A 0.9300 . ?
C9 C10 1.42(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.46(3) . ?
C11 C12 1.40(3) . ?
C12 C13 1.28(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.26(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.39(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.40(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.45(3) . ?
C18 C19 1.39(3) . ?
C19 C20 1.39(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.33(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.31(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.52(3) . ?
C24 C25 1.3900 . ?
C24 C29 1.3900 . ?
C25 C26 1.3900 . ?
C25 H25 0.9300 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 C30 1.51(3) . ?
C28 C29 1.3900 . ?
C29 H29 0.9300 . ?
C31 C32 1.64(3) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.45(3) . ?
C33 C34 1.43(3) . ?
C34 C35 1.35(3) . ?
C34 H34 0.9300 . ?
C35 C36 1.42(3) . ?
C35 H35 0.9300 . ?
C36 C37 1.48(4) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 C39 1.62(3) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.47(3) . ?
N5 C40 1.3900 . ?
N5 C44 1.3900 . ?
C40 C41 1.3900 . ?
C41 C42 1.3900 . ?
C41 H41 0.9300 . ?
C42 C43 1.3900 . ?
C42 H42 0.9300 . ?
C43 C44 1.3900 . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 C46 1.62(3) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 C47 1.54(3) . ?
C47 C48 1.40(3) . ?
C48 C49 1.36(3) . ?
C48 H48 0.9300 . ?
C49 C50 1.38(3) . ?
C49 H49 0.9300 . ?
C50 C51 1.38(3) . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
C52 C53 1.40(4) . ?
C53 C54 1.42(3) . ?
C53 C58 1.42(3) . ?
C54 C55 1.34(3) . ?
C54 H54 0.9300 . ?
C55 C56 1.41(3) . ?
C56 C57 1.34(3) . ?
C56 C59 1.53(3) . ?
C57 C58 1.38(3) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?
C60 C61 1.39(3) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 N10 1.46(3) . ?
N10 C62 1.3900 . ?
N10 C66 1.3900 . ?
C62 C63 1.3900 . ?
C62 H62 0.9300 . ?
C63 C64 1.3900 . ?
C63 H63 0.9300 . ?
C64 C65 1.3900 . ?
C64 H64 0.9300 . ?
C65 C66 1.3900 . ?
C65 H65 0.9300 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 H69 0.9300 . ?
O99 C99 1.08(3) . ?
N99 C97 1.23(4) . ?
N99 C98 1.42(3) . ?
N99 C99 1.50(4) . ?
C99 H99 0.9300 . ?
C97 H97A 0.9600 . ?
C97 H97B 0.9600 . ?
C97 H97C 0.9600 . ?
N98 C94 1.44(4) . ?
N98 C95 1.45(4) . ?
N98 C96 1.49(6) . ?
C96 H96A 0.9600 . ?
C96 H96B 0.9600 . ?
C96 H96C 0.9600 . ?
C95 H95A 0.9600 . ?
C95 H95B 0.9600 . ?
C95 H95C 0.9600 . ?
C94 O98 1.00(4) . ?
C94 H94 0.9300 . ?
C98 H98A 0.9600 . ?
C98 H98B 0.9600 . ?
C98 H98C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 O5 H5B 109.5 . . ?
C28 O10 H10B 109.5 . . ?
C55 O19 H19B 109.5 . . ?
O4 Zn1 O1 86.6(7) 2_575 . ?
O4 Zn1 N1 87.7(8) 2_575 . ?
O1 Zn1 N1 103.7(8) . . ?
O4 Zn1 N2 94.2(7) 2_575 . ?
O1 Zn1 N2 176.6(7) . . ?
N1 Zn1 N2 73.0(8) . . ?
O4 Zn1 N11 174.0(8) 2_575 . ?
O1 Zn1 N11 87.4(8) . . ?
N1 Zn1 N11 94.2(8) . . ?
N2 Zn1 N11 91.8(8) . . ?
O4 Zn1 N12 105.9(8) 2_575 . ?
O1 Zn1 N12 88.5(8) . . ?
N1 Zn1 N12 162.4(8) . . ?
N2 Zn1 N12 94.4(8) . . ?
N11 Zn1 N12 73.4(8) . . ?
O8 Zn2 O11 96.3(7) . 2_565 ?
O8 Zn2 N6 90.5(8) . . ?
O11 Zn2 N6 103.1(9) 2_565 . ?
O8 Zn2 N3 101.0(8) . . ?
O11 Zn2 N3 86.0(8) 2_565 . ?
N6 Zn2 N3 164.5(8) . . ?
O8 Zn2 N4 175.1(8) . . ?
O11 Zn2 N4 85.8(8) 2_565 . ?
N6 Zn2 N4 93.3(8) . . ?
N3 Zn2 N4 74.6(8) . . ?
O8 Zn2 N5 87.1(7) . . ?
O11 Zn2 N5 176.2(7) 2_565 . ?
N6 Zn2 N5 75.2(8) . . ?
N3 Zn2 N5 95.0(7) . . ?
N4 Zn2 N5 90.9(7) . . ?
O21 Zn3 O17 95.2(5) 2_455 . ?
O21 Zn3 N7 173.6(8) 2_455 . ?
O17 Zn3 N7 88.7(7) . . ?
O21 Zn3 N8 100.1(8) 2_455 . ?
O17 Zn3 N8 88.0(7) . . ?
N7 Zn3 N8 74.9(8) . . ?
O21 Zn3 C66 84.5(9) 2_455 . ?
O17 Zn3 C66 174.0(7) . . ?
N7 Zn3 C66 92.2(5) . . ?
N8 Zn3 C66 97.9(7) . . ?
O21 Zn3 N9 87.6(8) 2_455 . ?
O17 Zn3 N9 99.7(8) . . ?
N7 Zn3 N9 96.8(8) . . ?
N8 Zn3 N9 168.6(4) . . ?
C66 Zn3 N9 74.3(8) . . ?
C1 O1 Zn1 126.6(19) . . ?
C8 O4 Zn1 127.5(17) . 2_475 ?
N12 O6 H6 109.5 . . ?
N1 O7 H7 109.5 . . ?
C23 O8 Zn2 136.0(19) . . ?
C30 O11 Zn2 131.8(19) . 2_465 ?
N6 O13 H13A 109.5 . . ?
N3 O14 H14A 109.5 . . ?
N9 O15 H15A 109.5 . . ?
N8 O16 H16 109.5 . . ?
C52 O17 Zn3 135.0(19) . . ?
C59 O21 Zn3 138.2(19) . 2 ?
C10 N1 O7 117(2) . . ?
C10 N1 Zn1 119.0(19) . . ?
O7 N1 Zn1 123.6(17) . . ?
C15 N2 C11 118.1(19) . . ?
C15 N2 Zn1 127.8(16) . . ?
C11 N2 Zn1 114.0(15) . . ?
C32 N3 O14 114(2) . . ?
C32 N3 Zn2 117.5(19) . . ?
O14 N3 Zn2 127.8(16) . . ?
C33 N4 C37 123(2) . . ?
C33 N4 Zn2 113.6(18) . . ?
C37 N4 Zn2 122.5(18) . . ?
C39 N6 O13 112(2) . . ?
C39 N6 Zn2 119(2) . . ?
O13 N6 Zn2 128.2(17) . . ?
C51 N7 C47 115.9(19) . . ?
C51 N7 Zn3 128.9(17) . . ?
C47 N7 Zn3 115.0(15) . . ?
C46 N8 O16 114(2) . . ?
C46 N8 Zn3 119.2(18) . . ?
O16 N8 Zn3 126.5(16) . . ?
O15 N9 C61 113(2) . . ?
O15 N9 Zn3 127.7(17) . . ?
C61 N9 Zn3 117.0(17) . . ?
C22 N11 C18 116(2) . . ?
C22 N11 Zn1 128.7(18) . . ?
C18 N11 Zn1 114.9(16) . . ?
C17 N12 O6 115(2) . . ?
C17 N12 Zn1 119.2(18) . . ?
O6 N12 Zn1 124.7(17) . . ?
C69 N13 C68 124(3) . . ?
C69 N13 C67 122(3) . . ?
C68 N13 C67 114(3) . . ?
O2 C1 O1 127(3) . . ?
O2 C1 C2 117(3) . . ?
O1 C1 C2 115(3) . . ?
C3 C2 C7 115.6(19) . . ?
C3 C2 C1 124(2) . . ?
C7 C2 C1 121(2) . . ?
C2 C3 C4 125(2) . . ?
C2 C3 H3 117.7 . . ?
C4 C3 H3 117.7 . . ?
C3 C4 C5 119(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 115(2) . . ?
C6 C5 C8 131(2) . . ?
C4 C5 C8 114(2) . . ?
O5 C6 C5 121(3) . . ?
O5 C6 C7 111(2) . . ?
C5 C6 C7 128(2) . . ?
C6 C7 C2 117(2) . . ?
C6 C7 H7A 121.4 . . ?
C2 C7 H7A 121.4 . . ?
O3 C8 O4 127(3) . . ?
O3 C8 C5 111(2) . . ?
O4 C8 C5 122(2) . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C9 118(3) . . ?
N1 C10 C11 113(2) . . ?
C9 C10 C11 128(2) . . ?
N2 C11 C12 118.0(19) . . ?
N2 C11 C10 120(2) . . ?
C12 C11 C10 122(2) . . ?
C13 C12 C11 118(2) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C14 C13 C12 128(3) . . ?
C14 C13 H13 115.8 . . ?
C12 C13 H13 115.8 . . ?
C13 C14 C15 110(2) . . ?
C13 C14 H14 125.1 . . ?
C15 C14 H14 125.1 . . ?
N2 C15 C14 128(2) . . ?
N2 C15 H15 116.1 . . ?
C14 C15 H15 116.1 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N12 C17 C16 122(2) . . ?
N12 C17 C18 115(2) . . ?
C16 C17 C18 122(2) . . ?
C19 C18 N11 121(2) . . ?
C19 C18 C17 122(2) . . ?
N11 C18 C17 116(2) . . ?
C20 C19 C18 113(3) . . ?
C20 C19 H19 123.4 . . ?
C18 C19 H19 123.4 . . ?
C21 C20 C19 128(3) . . ?
C21 C20 H20 115.9 . . ?
C19 C20 H20 115.9 . . ?
C22 C21 C20 114(3) . . ?
C22 C21 H21 122.9 . . ?
C20 C21 H21 122.9 . . ?
C21 C22 N11 127(3) . . ?
C21 C22 H22 116.7 . . ?
N11 C22 H22 116.7 . . ?
O9 C23 O8 125(3) . . ?
O9 C23 C24 119(2) . . ?
O8 C23 C24 115(2) . . ?
C25 C24 C29 120.0 . . ?
C25 C24 C23 123.9(15) . . ?
C29 C24 C23 116.1(15) . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 C30 118.2(15) . . ?
C28 C27 C30 121.8(15) . . ?
O10 C28 C29 117.1(12) . . ?
O10 C28 C27 122.9(12) . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C24 120.0 . . ?
C28 C29 H29 120.0 . . ?
C24 C29 H29 120.0 . . ?
O11 C30 O12 124(3) . . ?
O11 C30 C27 117(3) . . ?
O12 C30 C27 118(2) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 C33 115(2) . . ?
N3 C32 C31 121(2) . . ?
C33 C32 C31 123(2) . . ?
N4 C33 C34 119(2) . . ?
N4 C33 C32 118(2) . . ?
C34 C33 C32 122(2) . . ?
C35 C34 C33 126(3) . . ?
C35 C34 H34 116.9 . . ?
C33 C34 H34 116.9 . . ?
C34 C35 C36 112(3) . . ?
C34 C35 H35 124.2 . . ?
C36 C35 H35 124.2 . . ?
C35 C36 C37 122(3) . . ?
C35 C36 H36 118.8 . . ?
C37 C36 H36 118.8 . . ?
N4 C37 C36 117(2) . . ?
N4 C37 H37 121.4 . . ?
C36 C37 H37 121.4 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N6 C39 C40 119(2) . . ?
N6 C39 C38 125(3) . . ?
C40 C39 C38 116(2) . . ?
C40 N5 C44 120.0 . . ?
C40 N5 Zn2 114.8(10) . . ?
C44 N5 Zn2 125.2(10) . . ?
C41 C40 N5 120.0 . . ?
C41 C40 C39 127.4(16) . . ?
N5 C40 C39 112.5(16) . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 C44 120.0 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 N5 120.0 . . ?
C43 C44 H44 120.0 . . ?
N5 C44 H44 120.0 . . ?
C46 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C46 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N8 C46 C47 113(2) . . ?
N8 C46 C45 121(2) . . ?
C47 C46 C45 125(2) . . ?
N7 C47 C48 127(2) . . ?
N7 C47 C46 117(2) . . ?
C48 C47 C46 116(2) . . ?
C49 C48 C47 113(2) . . ?
C49 C48 H48 123.4 . . ?
C47 C48 H48 123.4 . . ?
C48 C49 C50 121(2) . . ?
C48 C49 H49 119.3 . . ?
C50 C49 H49 119.3 . . ?
C49 C50 C51 115(2) . . ?
C49 C50 H50 122.6 . . ?
C51 C50 H50 122.6 . . ?
N7 C51 C50 128(2) . . ?
N7 C51 H51 116.2 . . ?
C50 C51 H51 116.2 . . ?
O18 C52 O17 121(3) . . ?
O18 C52 C53 117(3) . . ?
O17 C52 C53 121(3) . . ?
C52 C53 C54 122(3) . . ?
C52 C53 C58 117(2) . . ?
C54 C53 C58 121(3) . . ?
C55 C54 C53 115(3) . . ?
C55 C54 H54 122.7 . . ?
C53 C54 H54 122.7 . . ?
C54 C55 O19 117(2) . . ?
C54 C55 C56 128(3) . . ?
O19 C55 C56 115(2) . . ?
C57 C56 C55 113(2) . . ?
C57 C56 C59 123(3) . . ?
C55 C56 C59 125(2) . . ?
C56 C57 C58 127(3) . . ?
C56 C57 H57 116.5 . . ?
C58 C57 H57 116.5 . . ?
C57 C58 C53 116(2) . . ?
C57 C58 H58 122.2 . . ?
C53 C58 H58 122.2 . . ?
O20 C59 O21 125(3) . . ?
O20 C59 C56 116(3) . . ?
O21 C59 C56 117(3) . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N9 C61 C60 125(2) . . ?
N9 C61 N10 114.8(19) . . ?
C60 C61 N10 120(2) . . ?
C62 N10 C66 120.0 . . ?
C62 N10 C61 124.7(15) . . ?
C66 N10 C61 115.3(15) . . ?
C63 C62 N10 120.0 . . ?
C63 C62 H62 120.0 . . ?
N10 C62 H62 120.0 . . ?
C62 C63 C64 120.0 . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C63 C64 C65 120.0 . . ?
C63 C64 H64 120.0 . . ?
C65 C64 H64 120.0 . . ?
C64 C65 C66 120.0 . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C65 C66 N10 120.0 . . ?
C65 C66 Zn3 123.8(9) . . ?
N10 C66 Zn3 116.2(9) . . ?
N13 C67 H67A 109.5 . . ?
N13 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
N13 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N13 C68 H68A 109.5 . . ?
N13 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
N13 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
N13 C69 O22 130(3) . . ?
N13 C69 H69 114.9 . . ?
O22 C69 H69 114.9 . . ?
C97 N99 C98 138(5) . . ?
C97 N99 C99 121(3) . . ?
C98 N99 C99 99(4) . . ?
O99 C99 N99 136(3) . . ?
O99 C99 H99 112.0 . . ?
N99 C99 H99 112.0 . . ?
N99 C97 H97A 109.5 . . ?
N99 C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
N99 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C94 N98 C95 117(3) . . ?
C94 N98 C96 115(3) . . ?
C95 N98 C96 128(4) . . ?
N98 C96 H96A 109.5 . . ?
N98 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
N98 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
N98 C95 H95A 109.5 . . ?
N98 C95 H95B 109.5 . . ?
H95A C95 H95B 109.5 . . ?
N98 C95 H95C 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?
O98 C94 N98 126(4) . . ?
O98 C94 H94 116.9 . . ?
N98 C94 H94 116.9 . . ?
N99 C98 H98A 109.5 . . ?
N99 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
N99 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 O2 -25(5) . . . . ?
Zn1 O1 C1 C2 155.5(18) . . . . ?
O2 C1 C2 C3 -11(5) . . . . ?
O1 C1 C2 C3 168(3) . . . . ?
O2 C1 C2 C7 164(3) . . . . ?
O1 C1 C2 C7 -17(4) . . . . ?
C7 C2 C3 C4 3(4) . . . . ?
C1 C2 C3 C4 178(3) . . . . ?
C2 C3 C4 C5 2(4) . . . . ?
C3 C4 C5 C6 -4(3) . . . . ?
C3 C4 C5 C8 -177(2) . . . . ?
C4 C5 C6 O5 -176(3) . . . . ?
C8 C5 C6 O5 -5(5) . . . . ?
C4 C5 C6 C7 0(4) . . . . ?
C8 C5 C6 C7 171(3) . . . . ?
O5 C6 C7 C2 -178(3) . . . . ?
C5 C6 C7 C2 6(4) . . . . ?
C3 C2 C7 C6 -7(3) . . . . ?
C1 C2 C7 C6 178(2) . . . . ?
Zn1 O4 C8 O3 24(4) 2_475 . . . ?
Zn1 O4 C8 C5 -163.3(16) 2_475 . . . ?
C6 C5 C8 O3 13(4) . . . . ?
C4 C5 C8 O3 -175(2) . . . . ?
C6 C5 C8 O4 -160(3) . . . . ?
C4 C5 C8 O4 11(3) . . . . ?
O7 N1 C10 C9 -1(4) . . . . ?
Zn1 N1 C10 C9 178(2) . . . . ?
O7 N1 C10 C11 -172(2) . . . . ?
Zn1 N1 C10 C11 6(3) . . . . ?
C15 N2 C11 C12 0(3) . . . . ?
Zn1 N2 C11 C12 178.1(15) . . . . ?
C15 N2 C11 C10 -179(2) . . . . ?
Zn1 N2 C11 C10 -1(2) . . . . ?
N1 C10 C11 N2 -4(3) . . . . ?
C9 C10 C11 N2 -174(2) . . . . ?
N1 C10 C11 C12 177(2) . . . . ?
C9 C10 C11 C12 7(4) . . . . ?
N2 C11 C12 C13 0(3) . . . . ?
C10 C11 C12 C13 179(3) . . . . ?
C11 C12 C13 C14 1(4) . . . . ?
C12 C13 C14 C15 -2(4) . . . . ?
C11 N2 C15 C14 -1(3) . . . . ?
Zn1 N2 C15 C14 -178.6(17) . . . . ?
C13 C14 C15 N2 2(3) . . . . ?
O6 N12 C17 C16 4(4) . . . . ?
Zn1 N12 C17 C16 -164(2) . . . . ?
O6 N12 C17 C18 175(2) . . . . ?
Zn1 N12 C17 C18 7(3) . . . . ?
C22 N11 C18 C19 1(4) . . . . ?
Zn1 N11 C18 C19 180(2) . . . . ?
C22 N11 C18 C17 174(3) . . . . ?
Zn1 N11 C18 C17 -8(3) . . . . ?
N12 C17 C18 C19 173(3) . . . . ?
C16 C17 C18 C19 -16(5) . . . . ?
N12 C17 C18 N11 0(4) . . . . ?
C16 C17 C18 N11 171(3) . . . . ?
N11 C18 C19 C20 0(4) . . . . ?
C17 C18 C19 C20 -172(3) . . . . ?
C18 C19 C20 C21 -4(5) . . . . ?
C19 C20 C21 C22 6(5) . . . . ?
C20 C21 C22 N11 -4(5) . . . . ?
C18 N11 C22 C21 0(5) . . . . ?
Zn1 N11 C22 C21 -178(3) . . . . ?
Zn2 O8 C23 O9 2(5) . . . . ?
Zn2 O8 C23 C24 176.1(14) . . . . ?
O9 C23 C24 C25 167.1(19) . . . . ?
O8 C23 C24 C25 -8(3) . . . . ?
O9 C23 C24 C29 -12(3) . . . . ?
O8 C23 C24 C29 173.7(19) . . . . ?
C29 C24 C25 C26 0.0 . . . . ?
C23 C24 C25 C26 -178.7(18) . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C25 C26 C27 C30 179.5(16) . . . . ?
C26 C27 C28 O10 -178.9(18) . . . . ?
C30 C27 C28 O10 1.7(19) . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C30 C27 C28 C29 -179.5(16) . . . . ?
O10 C28 C29 C24 178.9(17) . . . . ?
C27 C28 C29 C24 0.0 . . . . ?
C25 C24 C29 C28 0.0 . . . . ?
C23 C24 C29 C28 178.8(17) . . . . ?
Zn2 O11 C30 O12 23(4) 2_465 . . . ?
Zn2 O11 C30 C27 -158.4(14) 2_465 . . . ?
C26 C27 C30 O11 -171.4(17) . . . . ?
C28 C27 C30 O11 8(3) . . . . ?
C26 C27 C30 O12 8(3) . . . . ?
C28 C27 C30 O12 -172.8(17) . . . . ?
O14 N3 C32 C33 -176(2) . . . . ?
Zn2 N3 C32 C33 11(3) . . . . ?
O14 N3 C32 C31 -5(4) . . . . ?
Zn2 N3 C32 C31 -178.6(19) . . . . ?
C37 N4 C33 C34 1(4) . . . . ?
Zn2 N4 C33 C34 172.5(19) . . . . ?
C37 N4 C33 C32 -174(2) . . . . ?
Zn2 N4 C33 C32 -3(3) . . . . ?
N3 C32 C33 N4 -5(4) . . . . ?
C31 C32 C33 N4 -176(2) . . . . ?
N3 C32 C33 C34 180(2) . . . . ?
C31 C32 C33 C34 9(4) . . . . ?
N4 C33 C34 C35 -2(4) . . . . ?
C32 C33 C34 C35 173(3) . . . . ?
C33 C34 C35 C36 5(5) . . . . ?
C34 C35 C36 C37 -7(4) . . . . ?
C33 N4 C37 C36 -3(4) . . . . ?
Zn2 N4 C37 C36 -173.8(17) . . . . ?
C35 C36 C37 N4 7(4) . . . . ?
O13 N6 C39 C40 173(2) . . . . ?
Zn2 N6 C39 C40 3(3) . . . . ?
O13 N6 C39 C38 -2(4) . . . . ?
Zn2 N6 C39 C38 -173.0(17) . . . . ?
C44 N5 C40 C41 0.0 . . . . ?
Zn2 N5 C40 C41 178.6(11) . . . . ?
C44 N5 C40 C39 177.0(19) . . . . ?
Zn2 N5 C40 C39 -4.4(17) . . . . ?
N6 C39 C40 C41 178.1(19) . . . . ?
C38 C39 C40 C41 -6(3) . . . . ?
N6 C39 C40 N5 1(3) . . . . ?
C38 C39 C40 N5 177.3(16) . . . . ?
N5 C40 C41 C42 0.0 . . . . ?
C39 C40 C41 C42 -177(2) . . . . ?
C40 C41 C42 C43 0.0 . . . . ?
C41 C42 C43 C44 0.0 . . . . ?
C42 C43 C44 N5 0.0 . . . . ?
C40 N5 C44 C43 0.0 . . . . ?
Zn2 N5 C44 C43 -178.4(13) . . . . ?
O16 N8 C46 C47 180(2) . . . . ?
Zn3 N8 C46 C47 6(3) . . . . ?
O16 N8 C46 C45 8(4) . . . . ?
Zn3 N8 C46 C45 -165.2(18) . . . . ?
C51 N7 C47 C48 -3(4) . . . . ?
Zn3 N7 C47 C48 173(2) . . . . ?
C51 N7 C47 C46 -179(2) . . . . ?
Zn3 N7 C47 C46 -4(3) . . . . ?
N8 C46 C47 N7 -2(4) . . . . ?
C45 C46 C47 N7 169(2) . . . . ?
N8 C46 C47 C48 -179(2) . . . . ?
C45 C46 C47 C48 -8(4) . . . . ?
N7 C47 C48 C49 6(4) . . . . ?
C46 C47 C48 C49 -177(3) . . . . ?
C47 C48 C49 C50 -3(5) . . . . ?
C48 C49 C50 C51 -2(5) . . . . ?
C47 N7 C51 C50 -4(4) . . . . ?
Zn3 N7 C51 C50 -179(2) . . . . ?
C49 C50 C51 N7 6(5) . . . . ?
Zn3 O17 C52 O18 -22(5) . . . . ?
Zn3 O17 C52 C53 163(2) . . . . ?
O18 C52 C53 C54 -20(5) . . . . ?
O17 C52 C53 C54 155(3) . . . . ?
O18 C52 C53 C58 161(3) . . . . ?
O17 C52 C53 C58 -24(4) . . . . ?
C52 C53 C54 C55 180(3) . . . . ?
C58 C53 C54 C55 -1(4) . . . . ?
C53 C54 C55 O19 175(2) . . . . ?
C53 C54 C55 C56 -2(4) . . . . ?
C54 C55 C56 C57 1(4) . . . . ?
O19 C55 C56 C57 -176(2) . . . . ?
C54 C55 C56 C59 -179(3) . . . . ?
O19 C55 C56 C59 4(4) . . . . ?
C55 C56 C57 C58 3(4) . . . . ?
C59 C56 C57 C58 -177(3) . . . . ?
C56 C57 C58 C53 -6(4) . . . . ?
C52 C53 C58 C57 -177(3) . . . . ?
C54 C53 C58 C57 5(4) . . . . ?
Zn3 O21 C59 O20 -2(5) 2 . . . ?
Zn3 O21 C59 C56 -169.8(19) 2 . . . ?
C57 C56 C59 O20 23(4) . . . . ?
C55 C56 C59 O20 -157(3) . . . . ?
C57 C56 C59 O21 -168(3) . . . . ?
C55 C56 C59 O21 11(4) . . . . ?
O15 N9 C61 C60 -2(4) . . . . ?
Zn3 N9 C61 C60 -167(2) . . . . ?
O15 N9 C61 N10 -176.8(18) . . . . ?
Zn3 N9 C61 N10 18(3) . . . . ?
N9 C61 N10 C62 168.9(17) . . . . ?
C60 C61 N10 C62 -6(3) . . . . ?
N9 C61 N10 C66 -14(3) . . . . ?
C60 C61 N10 C66 171(2) . . . . ?
C66 N10 C62 C63 0.0 . . . . ?
C61 N10 C62 C63 177(2) . . . . ?
N10 C62 C63 C64 0.0 . . . . ?
C62 C63 C64 C65 0.0 . . . . ?
C63 C64 C65 C66 0.0 . . . . ?
C64 C65 C66 N10 0.0 . . . . ?
C64 C65 C66 Zn3 179.7(15) . . . . ?
C62 N10 C66 C65 0.0 . . . . ?
C61 N10 C66 C65 -177.5(19) . . . . ?
C62 N10 C66 Zn3 -179.7(14) . . . . ?
C61 N10 C66 Zn3 2.7(19) . . . . ?
C68 N13 C69 O22 170(3) . . . . ?
C67 N13 C69 O22 -7(6) . . . . ?
C97 N99 C99 O99 -166(4) . . . . ?
C98 N99 C99 O99 -1(5) . . . . ?
C95 N98 C94 O98 7(7) . . . . ?
C96 N98 C94 O98 -168(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
O5 H5B O3 0.82 2.25 2.66(4) 110.8 . yes
O5 H5B O9 0.82 2.58 3.32(4) 150.6 1_565 yes
O19 H19B O21 0.82 1.86 2.56(3) 142.8 . yes
O6 H6 O3 0.82 1.89 2.63(3) 150.3 2_575 yes
O7 H7 O2 0.82 1.86 2.54(3) 138.4 . yes
O13 H13A O12 0.82 1.75 2.55(3) 164.4 2_565 yes
O14 H14A O9 0.82 1.78 2.52(3) 149.3 . yes
O15 H15A O18 0.82 1.75 2.51(3) 153.3 . yes
O16 H16 O20 0.82 1.68 2.50(3) 175.1 2_455 yes
C19 H19 O9 0.93 2.34 3.17(4) 147.8 . yes
C34 H34 O3 0.93 2.51 3.35(3) 149.9 2_565 yes
C36 H36 O99 0.93 2.59 3.51(4) 166.7 3_545 yes
C37 H37 N6 0.93 2.63 3.18(3) 118.6 . yes
C38 H38C O99 0.96 2.40 3.17(3) 136.5 4_455 yes
C44 H44 O5 0.93 2.38 3.07(3) 130.0 1_545 yes
C45 H45C O7 0.96 2.57 3.43(4) 149.0 2_565 yes
C48 H48 O98 0.93 2.49 3.38(4) 160.1 2_565 yes
C60 H60A O99 0.96 2.62 3.45(4) 143.9 2_565 yes
C62 H62 O22 0.93 2.47 3.37(3) 162.5 4_464 yes
C69 H69 O18 0.93 2.64 3.56(4) 167.7 3_455 yes
C99 H99 O22 0.93 2.36 3.22(4) 152.5 3_444 yes
C96 H96C O20 0.96 2.61 3.54(7) 163.2 2_455 yes
C98 H98B O99 0.96 2.07 2.58(7) 111.4 . yes
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.123
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2282122'
loop_
_audit_author_name
_audit_author_address
'Constantina Papatriantafyllopoulou' 'University of Galway'
_audit_update_record             
;
2023-09-17 deposited with the CCDC.	2023-10-04 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         ?
_chemical_formula_sum            'C50 H42 Co3 N12 O12'
_chemical_formula_weight         1179.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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'
'-x, -y, -z'

_cell_length_a                   11.1458(8)
_cell_length_b                   14.7658(8)
_cell_length_c                   18.7690(9)
_cell_angle_alpha                81.504(4)
_cell_angle_beta                 89.225(5)
_cell_angle_gamma                86.463(5)
_cell_volume                     3049.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5768
_cell_measurement_theta_min      4.0870
_cell_measurement_theta_max      71.0050

_exptl_crystal_description       Polyhedral
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_F_000             1206
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    6.851
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.42929
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21718
_diffrn_reflns_av_unetI/netI     0.1383
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.569
_diffrn_reflns_theta_max         71.156
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11529
_reflns_number_gt                6904
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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)+(0.1081P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11529
_refine_ls_number_parameters     700
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.2341
_refine_ls_wR_factor_gt          0.2121
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      807.840
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.76440(7) 0.07717(6) 0.78351(4) 0.0147(2) Uani 1 1 d . . . . .
Co2 Co 0.54810(8) 0.25291(6) 0.73787(5) 0.0157(2) Uani 1 1 d . . . . .
Co3 Co 0.33389(7) 0.42849(6) 0.69369(4) 0.0142(2) Uani 1 1 d . . . . .
O1 O 0.5153(3) 0.1106(3) 0.7550(2) 0.0195(8) Uani 1 1 d . . . . .
O2 O 0.6448(3) 0.2300(3) 0.8344(2) 0.0205(8) Uani 1 1 d . . . . .
O3 O 0.6996(3) 0.2271(2) 0.6769(2) 0.0181(8) Uani 1 1 d . . . . .
O4 O 0.4563(3) 0.2801(3) 0.6395(2) 0.0189(8) Uani 1 1 d . . . . .
O5 O 0.3932(3) 0.2732(2) 0.7960(2) 0.0183(8) Uani 1 1 d . . . . .
O6 O 0.5815(3) 0.3954(3) 0.7265(2) 0.0224(8) Uani 1 1 d . . . . .
O7 O 0.9678(5) 0.5942(3) 0.8085(2) 0.0383(11) Uani 1 1 d D . . . .
O8 O 0.9367(5) 0.7101(3) 0.8728(2) 0.0352(11) Uani 1 1 d . . . . .
O9 O 0.9227(4) 0.6763(3) 1.0079(2) 0.0319(10) Uani 1 1 d D . . . .
O10 O 0.8615(4) 0.0970(3) 0.3252(2) 0.0353(10) Uani 1 1 d . . . . .
O11 O 0.8715(4) 0.2097(3) 0.3923(3) 0.0351(10) Uani 1 1 d D . . . .
O12 O 0.9758(4) 0.1814(3) 0.5117(2) 0.0318(10) Uani 1 1 d D . . . .
N1 N 0.7750(4) 0.0007(3) 0.8778(2) 0.0189(9) Uani 1 1 d . . . . .
N2 N 0.5972(4) 0.0625(3) 0.7990(3) 0.0178(9) Uani 1 1 d . . . . .
N3 N 0.9345(4) 0.1029(3) 0.7818(2) 0.0178(9) Uani 1 1 d . . . . .
N4 N 0.7495(4) 0.1870(3) 0.8242(2) 0.0170(9) Uani 1 1 d . . . . .
N5 N 0.1647(4) 0.4016(3) 0.6927(2) 0.0174(9) Uani 1 1 d . . . . .
N6 N 0.3513(4) 0.3223(3) 0.6486(2) 0.0166(9) Uani 1 1 d . . . . .
N7 N 0.3071(4) 0.5308(3) 0.7491(3) 0.0192(9) Uani 1 1 d . . . . .
N8 N 0.3568(4) 0.3602(3) 0.7866(2) 0.0182(9) Uani 1 1 d . . . . .
N9 N 0.3279(4) 0.5111(3) 0.6022(2) 0.0206(10) Uani 1 1 d . . . . .
N10 N 0.5020(4) 0.4467(3) 0.6835(3) 0.0177(9) Uani 1 1 d . . . . .
N11 N 0.7831(4) -0.0294(3) 0.7325(3) 0.0196(9) Uani 1 1 d . . . . .
N12 N 0.7330(4) 0.1407(3) 0.6889(2) 0.0178(9) Uani 1 1 d . . . . .
C1 C 0.8753(5) -0.0309(4) 0.9158(3) 0.0211(11) Uani 1 1 d . . . . .
H1 H 0.949215 -0.009536 0.899993 0.025 Uiso 1 1 calc R U . . .
C2 C 0.8699(6) -0.0939(4) 0.9774(3) 0.0264(12) Uani 1 1 d . . . . .
H2 H 0.939456 -0.114192 1.003262 0.032 Uiso 1 1 calc R U . . .
C3 C 0.7611(6) -0.1267(4) 1.0004(3) 0.0286(13) Uani 1 1 d . . . . .
H3 H 0.757048 -0.170273 1.041462 0.034 Uiso 1 1 calc R U . . .
C4 C 0.6569(6) -0.0948(4) 0.9623(3) 0.0262(12) Uani 1 1 d . . . . .
H4 H 0.582260 -0.115206 0.977702 0.031 Uiso 1 1 calc R U . . .
C5 C 0.6681(5) -0.0310(4) 0.9001(3) 0.0216(11) Uani 1 1 d . . . . .
C6 C 0.5667(5) 0.0119(4) 0.8556(3) 0.0231(12) Uani 1 1 d D . . . .
C7 C 0.4387(6) -0.0021(5) 0.8772(4) 0.0361(15) Uani 1 1 d . . . . .
H7A H 0.435864 -0.034099 0.925527 0.054 Uiso 1 1 calc R U . . .
H7B H 0.403052 -0.037580 0.845060 0.054 Uiso 1 1 calc R U . . .
H7C H 0.395108 0.056379 0.874836 0.054 Uiso 1 1 calc R U . . .
C8 C 1.0260(5) 0.0596(4) 0.7524(3) 0.0227(12) Uani 1 1 d . . . . .
H8 H 1.009921 0.013168 0.726055 0.027 Uiso 1 1 calc R U . . .
C9 C 1.1438(5) 0.0805(4) 0.7592(3) 0.0264(12) Uani 1 1 d . . . . .
H9 H 1.206142 0.047741 0.739078 0.032 Uiso 1 1 calc R U . . .
C10 C 1.1670(5) 0.1520(5) 0.7970(4) 0.0323(15) Uani 1 1 d . . . . .
H10 H 1.245167 0.168949 0.801443 0.039 Uiso 1 1 calc R U . . .
C11 C 1.0729(5) 0.1968(4) 0.8275(3) 0.0253(12) Uani 1 1 d . . . . .
H11 H 1.087786 0.243283 0.854054 0.030 Uiso 1 1 calc R U . . .
C12 C 0.9564(5) 0.1737(4) 0.8192(3) 0.0185(11) Uani 1 1 d . . . . .
C13 C 0.8492(5) 0.2206(4) 0.8439(3) 0.0230(12) Uani 1 1 d . . . . .
C14 C 0.8489(6) 0.3018(5) 0.8820(4) 0.0347(15) Uani 1 1 d . . . . .
H14A H 0.924240 0.302043 0.906093 0.052 Uiso 1 1 calc R U . . .
H14B H 0.784701 0.299249 0.916742 0.052 Uiso 1 1 calc R U . . .
H14C H 0.837422 0.356726 0.847772 0.052 Uiso 1 1 calc R U . . .
C15 C 0.8116(5) -0.1171(4) 0.7589(3) 0.0236(12) Uani 1 1 d . . . . .
H15 H 0.825226 -0.132043 0.808149 0.028 Uiso 1 1 calc R U . . .
C16 C 0.8218(6) -0.1867(4) 0.7173(4) 0.0284(13) Uani 1 1 d . . . . .
H16 H 0.841563 -0.246990 0.737635 0.034 Uiso 1 1 calc R U . . .
C17 C 0.8017(6) -0.1632(4) 0.6442(4) 0.0290(13) Uani 1 1 d . . . . .
H17 H 0.809281 -0.208124 0.614282 0.035 Uiso 1 1 calc R U . . .
C18 C 0.7706(6) -0.0746(4) 0.6159(3) 0.0266(12) Uani 1 1 d . . . . .
H18 H 0.754564 -0.059442 0.566913 0.032 Uiso 1 1 calc R U . . .
C19 C 0.7631(5) -0.0069(4) 0.6604(3) 0.0190(11) Uani 1 1 d . . . . .
C20 C 0.7308(5) 0.0896(4) 0.6375(3) 0.0202(11) Uani 1 1 d . . . . .
C21 C 0.6878(6) 0.1296(4) 0.5639(3) 0.0279(13) Uani 1 1 d . . . . .
H21A H 0.681034 0.081366 0.535314 0.042 Uiso 1 1 calc R U . . .
H21B H 0.743989 0.171900 0.541577 0.042 Uiso 1 1 calc R U . . .
H21C H 0.610585 0.161334 0.567442 0.042 Uiso 1 1 calc R U . . .
C22 C 0.0715(5) 0.4440(3) 0.7234(3) 0.0177(10) Uani 1 1 d . . . . .
H22 H 0.085788 0.490695 0.749825 0.021 Uiso 1 1 calc R U . . .
C23 C -0.0451(5) 0.4195(4) 0.7163(3) 0.0238(12) Uani 1 1 d . . . . .
H23 H -0.108206 0.448965 0.738518 0.029 Uiso 1 1 calc R U . . .
C24 C -0.0674(5) 0.3511(4) 0.6761(3) 0.0246(12) Uani 1 1 d . . . . .
H24 H -0.145455 0.334235 0.670811 0.030 Uiso 1 1 calc R U . . .
C25 C 0.0291(5) 0.3074(4) 0.6433(3) 0.0235(12) Uani 1 1 d . . . . .
H25 H 0.016509 0.261244 0.615984 0.028 Uiso 1 1 calc R U . . .
C26 C 0.1438(5) 0.3348(4) 0.6528(3) 0.0177(10) Uani 1 1 d . . . . .
C27 C 0.2516(5) 0.2903(4) 0.6263(3) 0.0202(11) Uani 1 1 d . . . . .
C28 C 0.2548(6) 0.2124(5) 0.5855(4) 0.0308(14) Uani 1 1 d . . . . .
H28A H 0.191552 0.221849 0.550502 0.046 Uiso 1 1 calc R U . . .
H28B H 0.243812 0.156835 0.618005 0.046 Uiso 1 1 calc R U . . .
H28C H 0.330984 0.207623 0.561516 0.046 Uiso 1 1 calc R U . . .
C29 C 0.2827(5) 0.6196(4) 0.7251(3) 0.0243(12) Uani 1 1 d . . . . .
H29 H 0.280229 0.638766 0.675679 0.029 Uiso 1 1 calc R U . . .
C30 C 0.2609(6) 0.6844(4) 0.7705(4) 0.0295(13) Uani 1 1 d . . . . .
H30 H 0.244188 0.745918 0.752394 0.035 Uiso 1 1 calc R U . . .
C31 C 0.2648(7) 0.6542(5) 0.8444(4) 0.0368(15) Uani 1 1 d . . . . .
H31 H 0.249705 0.695827 0.876553 0.044 Uiso 1 1 calc R U . . .
C32 C 0.2908(6) 0.5638(5) 0.8696(4) 0.0351(15) Uani 1 1 d . . . . .
H32 H 0.294416 0.543855 0.918889 0.042 Uiso 1 1 calc R U . . .
C33 C 0.3116(5) 0.5018(4) 0.8216(3) 0.0228(12) Uani 1 1 d . . . . .
C34 C 0.3415(5) 0.4034(4) 0.8416(3) 0.0237(12) Uani 1 1 d . . . . .
C35 C 0.3612(7) 0.3585(5) 0.9173(3) 0.0363(16) Uani 1 1 d . . . . .
H35A H 0.402240 0.398655 0.943245 0.054 Uiso 1 1 calc R U . . .
H35B H 0.409006 0.302149 0.917552 0.054 Uiso 1 1 calc R U . . .
H35C H 0.285055 0.345940 0.939938 0.054 Uiso 1 1 calc R U . . .
C36 C 0.2303(6) 0.5427(4) 0.5624(3) 0.0262(12) Uani 1 1 d . . . . .
H36 H 0.156005 0.520671 0.576654 0.031 Uiso 1 1 calc R U . . .
C38 C 0.3469(7) 0.6380(5) 0.4796(3) 0.0343(15) Uani 1 1 d . . . . .
H38 H 0.353961 0.677887 0.436654 0.041 Uiso 1 1 calc R U . . .
C39 C 0.4483(6) 0.6099(4) 0.5225(3) 0.0295(14) Uani 1 1 d . . . . .
H39 H 0.522371 0.633656 0.510197 0.035 Uiso 1 1 calc R U . . .
C40 C 0.4356(5) 0.5459(4) 0.5839(3) 0.0208(11) Uani 1 1 d . . . . .
C41 C 0.5346(5) 0.5074(4) 0.6310(3) 0.0227(12) Uani 1 1 d . . . . .
C42 C 0.6613(6) 0.5343(5) 0.6192(4) 0.0332(14) Uani 1 1 d . . . . .
H42A H 0.679493 0.542058 0.568639 0.050 Uiso 1 1 calc R U . . .
H42B H 0.715070 0.487248 0.644151 0.050 Uiso 1 1 calc R U . . .
H42C H 0.670634 0.590971 0.637352 0.050 Uiso 1 1 calc R U . . .
C43 C 0.9615(6) 0.6259(4) 0.8658(3) 0.0249(12) Uani 1 1 d . . . . .
C44 C 0.9820(6) 0.5611(5) 0.9358(3) 0.0262(12) Uani 1 1 d . . . . .
C45 C 1.0218(5) 0.4718(4) 0.9343(3) 0.0209(11) Uani 1 1 d . . . . .
C46 C 0.9573(5) 0.5955(3) 1.0032(3) 0.0234(12) Uani 1 1 d D . . . .
C47 C 0.8871(5) 0.1265(4) 0.3829(3) 0.0244(12) Uani 1 1 d D . . . .
C48 C 0.9426(5) 0.0621(4) 0.4430(3) 0.0231(12) Uani 1 1 d D . . . .
C49 C 0.9843(5) 0.0984(3) 0.5053(3) 0.0238(12) Uani 1 1 d D . . . .
C50 C 1.0419(5) 0.0322(4) 0.5601(3) 0.0214(11) Uani 1 1 d . . . . .
C37 C 0.2369(6) 0.6060(5) 0.5015(3) 0.0304(13) Uani 1 1 d . . . . .
H37 H 0.167998 0.627189 0.475286 0.036 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
Co1 N4 1.890(5) . ?
Co1 N2 1.902(4) . ?
Co1 N12 1.907(5) . ?
Co1 N3 1.955(4) . ?
Co1 N11 1.958(5) . ?
Co1 N1 1.954(5) . ?
Co2 O5 2.060(4) . ?
Co2 O3 2.075(4) . ?
Co2 O2 2.094(4) . ?
Co2 O4 2.098(4) . ?
Co2 O1 2.131(4) . ?
Co2 O6 2.138(4) . ?
Co3 N6 1.888(5) . ?
Co3 N8 1.893(5) . ?
Co3 N10 1.912(5) . ?
Co3 N9 1.953(5) . ?
Co3 N5 1.952(4) . ?
Co3 N7 1.962(5) . ?
O1 N2 1.337(6) . ?
O2 N4 1.319(6) . ?
O3 N12 1.295(6) . ?
O4 N6 1.313(6) . ?
O5 N8 1.310(6) . ?
O6 N10 1.329(6) . ?
O7 C43 1.235(8) . ?
O8 C43 1.282(8) . ?
O9 C46 1.246(4) . ?
O10 C47 1.267(7) . ?
O11 C47 1.267(6) . ?
O12 C49 1.247(4) . ?
N1 C5 1.346(7) . ?
N1 C1 1.355(7) . ?
N2 C6 1.261(8) . ?
N3 C8 1.327(8) . ?
N3 C12 1.378(7) . ?
N4 C13 1.323(7) . ?
N5 C22 1.345(7) . ?
N5 C26 1.356(7) . ?
N6 C27 1.330(7) . ?
N7 C29 1.335(8) . ?
N7 C33 1.367(7) . ?
N8 C34 1.295(8) . ?
N9 C36 1.347(8) . ?
N9 C40 1.355(7) . ?
N10 C41 1.295(7) . ?
N11 C15 1.337(8) . ?
N11 C19 1.365(7) . ?
N12 C20 1.311(7) . ?
C1 C2 1.376(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.375(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.468(8) . ?
C6 C7 1.496(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.379(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.394(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.369(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.449(8) . ?
C13 C14 1.484(9) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.377(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.383(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.363(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.392(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.451(8) . ?
C20 C21 1.494(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.383(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.385(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.401(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.386(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.452(8) . ?
C27 C28 1.470(8) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.380(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.392(10) . ?
C30 H30 0.9300 . ?
C31 C32 1.364(10) . ?
C31 H31 0.9300 . ?
C32 C33 1.383(9) . ?
C32 H32 0.9300 . ?
C33 C34 1.465(9) . ?
C34 C35 1.489(8) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.370(9) . ?
C36 H36 0.9300 . ?
C38 C37 1.377(10) . ?
C38 C39 1.402(10) . ?
C38 H38 0.9300 . ?
C39 C40 1.390(8) . ?
C39 H39 0.9300 . ?
C40 C41 1.457(8) . ?
C41 C42 1.495(8) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.517(8) . ?
C44 C45 1.370(9) . ?
C44 C46 1.449(8) . ?
C45 C46 1.431(7) 2_767 ?
C47 C48 1.479(6) . ?
C48 C50 1.402(8) 2_756 ?
C48 C49 1.449(8) . ?
C49 C50 1.438(8) . ?
C37 H37 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Co1 N2 89.64(19) . . ?
N4 Co1 N12 92.2(2) . . ?
N2 Co1 N12 90.5(2) . . ?
N4 Co1 N3 81.9(2) . . ?
N2 Co1 N3 170.3(2) . . ?
N12 Co1 N3 94.59(19) . . ?
N4 Co1 N11 174.5(2) . . ?
N2 Co1 N11 92.49(19) . . ?
N12 Co1 N11 82.7(2) . . ?
N3 Co1 N11 96.3(2) . . ?
N4 Co1 N1 92.8(2) . . ?
N2 Co1 N1 82.0(2) . . ?
N12 Co1 N1 170.89(19) . . ?
N3 Co1 N1 93.63(19) . . ?
N11 Co1 N1 92.49(19) . . ?
O5 Co2 O3 176.93(15) . . ?
O5 Co2 O2 89.09(16) . . ?
O3 Co2 O2 92.69(16) . . ?
O5 Co2 O4 92.37(15) . . ?
O3 Co2 O4 85.94(15) . . ?
O2 Co2 O4 177.56(16) . . ?
O5 Co2 O1 86.97(15) . . ?
O3 Co2 O1 90.60(15) . . ?
O2 Co2 O1 87.64(15) . . ?
O4 Co2 O1 94.39(15) . . ?
O5 Co2 O6 91.58(15) . . ?
O3 Co2 O6 90.93(15) . . ?
O2 Co2 O6 89.81(16) . . ?
O4 Co2 O6 88.20(15) . . ?
O1 Co2 O6 177.08(16) . . ?
N6 Co3 N8 92.6(2) . . ?
N6 Co3 N10 91.38(19) . . ?
N8 Co3 N10 91.5(2) . . ?
N6 Co3 N9 93.3(2) . . ?
N8 Co3 N9 171.31(19) . . ?
N10 Co3 N9 81.9(2) . . ?
N6 Co3 N5 81.81(19) . . ?
N8 Co3 N5 92.29(19) . . ?
N10 Co3 N5 172.3(2) . . ?
N9 Co3 N5 94.9(2) . . ?
N6 Co3 N7 173.85(19) . . ?
N8 Co3 N7 82.5(2) . . ?
N10 Co3 N7 92.38(19) . . ?
N9 Co3 N7 92.1(2) . . ?
N5 Co3 N7 94.70(19) . . ?
N2 O1 Co2 111.2(3) . . ?
N4 O2 Co2 109.6(3) . . ?
N12 O3 Co2 109.9(3) . . ?
N6 O4 Co2 109.7(3) . . ?
N8 O5 Co2 110.5(3) . . ?
N10 O6 Co2 112.0(3) . . ?
C5 N1 C1 119.4(5) . . ?
C5 N1 Co1 112.1(4) . . ?
C1 N1 Co1 127.9(4) . . ?
C6 N2 O1 121.3(5) . . ?
C6 N2 Co1 117.3(4) . . ?
O1 N2 Co1 121.1(3) . . ?
C8 N3 C12 119.3(5) . . ?
C8 N3 Co1 128.5(4) . . ?
C12 N3 Co1 112.2(4) . . ?
O2 N4 C13 119.4(5) . . ?
O2 N4 Co1 122.8(3) . . ?
C13 N4 Co1 117.8(4) . . ?
C22 N5 C26 119.4(5) . . ?
C22 N5 Co3 127.6(4) . . ?
C26 N5 Co3 112.9(4) . . ?
O4 N6 C27 120.2(5) . . ?
O4 N6 Co3 122.5(3) . . ?
C27 N6 Co3 117.3(4) . . ?
C29 N7 C33 119.1(5) . . ?
C29 N7 Co3 129.0(4) . . ?
C33 N7 Co3 111.9(4) . . ?
C34 N8 O5 120.0(5) . . ?
C34 N8 Co3 117.9(4) . . ?
O5 N8 Co3 122.0(3) . . ?
C36 N9 C40 119.4(5) . . ?
C36 N9 Co3 127.8(4) . . ?
C40 N9 Co3 112.3(4) . . ?
C41 N10 O6 122.0(5) . . ?
C41 N10 Co3 117.2(4) . . ?
O6 N10 Co3 120.8(3) . . ?
C15 N11 C19 118.5(5) . . ?
C15 N11 Co1 129.0(4) . . ?
C19 N11 Co1 112.4(4) . . ?
O3 N12 C20 120.9(5) . . ?
O3 N12 Co1 122.4(4) . . ?
C20 N12 Co1 116.0(4) . . ?
N1 C1 C2 121.3(5) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C1 C2 C3 119.6(6) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 120.0(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 117.8(5) . . ?
C3 C4 H4 121.1 . . ?
C5 C4 H4 121.1 . . ?
N1 C5 C4 121.9(5) . . ?
N1 C5 C6 113.6(5) . . ?
C4 C5 C6 124.5(5) . . ?
N2 C6 C5 114.2(5) . . ?
N2 C6 C7 123.5(6) . . ?
C5 C6 C7 122.3(5) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C9 122.9(6) . . ?
N3 C8 H8 118.5 . . ?
C9 C8 H8 118.5 . . ?
C8 C9 C10 118.3(6) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C11 C10 C9 119.0(5) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 120.7(6) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.7 . . ?
N3 C12 C11 119.7(5) . . ?
N3 C12 C13 114.4(5) . . ?
C11 C12 C13 125.8(5) . . ?
N4 C13 C12 112.3(5) . . ?
N4 C13 C14 122.9(6) . . ?
C12 C13 C14 124.6(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N11 C15 C16 123.7(6) . . ?
N11 C15 H15 118.1 . . ?
C16 C15 H15 118.1 . . ?
C15 C16 C17 117.4(6) . . ?
C15 C16 H16 121.3 . . ?
C17 C16 H16 121.3 . . ?
C18 C17 C16 120.3(6) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 119.8(6) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
N11 C19 C18 120.2(5) . . ?
N11 C19 C20 114.1(5) . . ?
C18 C19 C20 125.6(5) . . ?
N12 C20 C19 114.5(5) . . ?
N12 C20 C21 120.6(5) . . ?
C19 C20 C21 124.7(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 121.4(5) . . ?
N5 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C24 C23 C22 119.7(5) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 119.2(5) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C26 C25 C24 118.2(5) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
N5 C26 C25 122.1(5) . . ?
N5 C26 C27 114.4(5) . . ?
C25 C26 C27 123.3(5) . . ?
N6 C27 C26 112.2(5) . . ?
N6 C27 C28 122.1(5) . . ?
C26 C27 C28 125.5(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N7 C29 C30 123.0(6) . . ?
N7 C29 H29 118.5 . . ?
C30 C29 H29 118.5 . . ?
C29 C30 C31 117.5(6) . . ?
C29 C30 H30 121.2 . . ?
C31 C30 H30 121.2 . . ?
C32 C31 C30 120.1(6) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 119.9(6) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
N7 C33 C32 120.3(6) . . ?
N7 C33 C34 114.4(5) . . ?
C32 C33 C34 125.3(6) . . ?
N8 C34 C33 113.2(5) . . ?
N8 C34 C35 123.2(6) . . ?
C33 C34 C35 123.4(5) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N9 C36 C37 122.2(6) . . ?
N9 C36 H36 118.9 . . ?
C37 C36 H36 118.9 . . ?
C37 C38 C39 119.4(6) . . ?
C37 C38 H38 120.3 . . ?
C39 C38 H38 120.3 . . ?
C40 C39 C38 118.6(6) . . ?
C40 C39 H39 120.7 . . ?
C38 C39 H39 120.7 . . ?
N9 C40 C39 121.1(6) . . ?
N9 C40 C41 114.8(5) . . ?
C39 C40 C41 124.1(6) . . ?
N10 C41 C40 113.1(5) . . ?
N10 C41 C42 123.5(6) . . ?
C40 C41 C42 123.4(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O7 C43 O8 126.0(6) . . ?
O7 C43 C44 118.7(5) . . ?
O8 C43 C44 115.2(5) . . ?
C45 C44 C46 121.3(5) . . ?
C45 C44 C43 120.0(5) . . ?
C46 C44 C43 118.7(6) . . ?
C44 C45 C46 124.8(5) . 2_767 ?
O9 C46 C45 121.9(5) . 2_767 ?
O9 C46 C44 124.1(5) . . ?
C45 C46 C44 114.0(5) 2_767 . ?
O10 C47 O11 124.0(5) . . ?
O10 C47 C48 119.3(5) . . ?
O11 C47 C48 116.7(5) . . ?
C50 C48 C49 119.8(5) 2_756 . ?
C50 C48 C47 121.4(5) 2_756 . ?
C49 C48 C47 118.8(5) . . ?
O12 C49 C50 120.6(6) . . ?
O12 C49 C48 123.8(6) . . ?
C50 C49 C48 115.6(4) . . ?
C48 C50 C49 124.6(5) 2_756 . ?
C36 C37 C38 119.2(6) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co2 O1 N2 C6 124.8(5) . . . . ?
Co2 O1 N2 Co1 -49.1(4) . . . . ?
Co2 O2 N4 C13 128.1(4) . . . . ?
Co2 O2 N4 Co1 -52.9(4) . . . . ?
N2 Co1 N4 O2 -14.8(4) . . . . ?
N12 Co1 N4 O2 75.6(4) . . . . ?
N3 Co1 N4 O2 170.0(4) . . . . ?
N1 Co1 N4 O2 -96.8(4) . . . . ?
N2 Co1 N4 C13 164.2(4) . . . . ?
N12 Co1 N4 C13 -105.3(4) . . . . ?
N3 Co1 N4 C13 -11.0(4) . . . . ?
N1 Co1 N4 C13 82.3(4) . . . . ?
Co2 O4 N6 C27 -127.7(4) . . . . ?
Co2 O4 N6 Co3 51.8(4) . . . . ?
N8 Co3 N6 O4 -76.2(4) . . . . ?
N10 Co3 N6 O4 15.4(4) . . . . ?
N9 Co3 N6 O4 97.3(4) . . . . ?
N5 Co3 N6 O4 -168.2(4) . . . . ?
N8 Co3 N6 C27 103.2(4) . . . . ?
N10 Co3 N6 C27 -165.2(4) . . . . ?
N9 Co3 N6 C27 -83.2(4) . . . . ?
N5 Co3 N6 C27 11.3(4) . . . . ?
Co2 O5 N8 C34 -123.6(4) . . . . ?
Co2 O5 N8 Co3 52.8(4) . . . . ?
N6 Co3 N8 C34 -173.4(4) . . . . ?
N10 Co3 N8 C34 95.1(4) . . . . ?
N5 Co3 N8 C34 -91.5(4) . . . . ?
N7 Co3 N8 C34 2.9(4) . . . . ?
N6 Co3 N8 O5 10.1(4) . . . . ?
N10 Co3 N8 O5 -81.3(4) . . . . ?
N5 Co3 N8 O5 92.0(4) . . . . ?
N7 Co3 N8 O5 -173.5(4) . . . . ?
Co2 O6 N10 C41 -130.4(4) . . . . ?
Co2 O6 N10 Co3 46.0(5) . . . . ?
Co2 O3 N12 C20 115.9(4) . . . . ?
Co2 O3 N12 Co1 -54.7(4) . . . . ?
C5 N1 C1 C2 -0.9(8) . . . . ?
Co1 N1 C1 C2 -171.4(4) . . . . ?
N1 C1 C2 C3 1.0(9) . . . . ?
C1 C2 C3 C4 -1.3(10) . . . . ?
C2 C3 C4 C5 1.4(10) . . . . ?
C1 N1 C5 C4 1.1(9) . . . . ?
Co1 N1 C5 C4 173.1(5) . . . . ?
C1 N1 C5 C6 177.6(5) . . . . ?
Co1 N1 C5 C6 -10.4(6) . . . . ?
C3 C4 C5 N1 -1.4(9) . . . . ?
C3 C4 C5 C6 -177.5(6) . . . . ?
O1 N2 C6 C5 -176.1(5) . . . . ?
Co1 N2 C6 C5 -2.0(7) . . . . ?
O1 N2 C6 C7 2.4(9) . . . . ?
Co1 N2 C6 C7 176.5(5) . . . . ?
N1 C5 C6 N2 8.4(8) . . . . ?
C4 C5 C6 N2 -175.2(6) . . . . ?
N1 C5 C6 C7 -170.1(6) . . . . ?
C4 C5 C6 C7 6.3(10) . . . . ?
C12 N3 C8 C9 1.9(8) . . . . ?
Co1 N3 C8 C9 -175.3(4) . . . . ?
N3 C8 C9 C10 -1.8(9) . . . . ?
C8 C9 C10 C11 1.8(9) . . . . ?
C9 C10 C11 C12 -2.0(9) . . . . ?
C8 N3 C12 C11 -1.9(8) . . . . ?
Co1 N3 C12 C11 175.7(4) . . . . ?
C8 N3 C12 C13 175.3(5) . . . . ?
Co1 N3 C12 C13 -7.1(6) . . . . ?
C10 C11 C12 N3 2.0(9) . . . . ?
C10 C11 C12 C13 -174.9(6) . . . . ?
O2 N4 C13 C12 -171.2(4) . . . . ?
Co1 N4 C13 C12 9.7(6) . . . . ?
O2 N4 C13 C14 4.4(8) . . . . ?
Co1 N4 C13 C14 -174.7(5) . . . . ?
N3 C12 C13 N4 -1.3(7) . . . . ?
C11 C12 C13 N4 175.7(5) . . . . ?
N3 C12 C13 C14 -176.7(5) . . . . ?
C11 C12 C13 C14 0.3(9) . . . . ?
C19 N11 C15 C16 -0.1(8) . . . . ?
Co1 N11 C15 C16 179.8(4) . . . . ?
N11 C15 C16 C17 0.2(9) . . . . ?
C15 C16 C17 C18 -1.2(9) . . . . ?
C16 C17 C18 C19 2.1(10) . . . . ?
C15 N11 C19 C18 0.9(8) . . . . ?
Co1 N11 C19 C18 -179.0(4) . . . . ?
C15 N11 C19 C20 179.0(5) . . . . ?
Co1 N11 C19 C20 -0.9(6) . . . . ?
C17 C18 C19 N11 -2.0(9) . . . . ?
C17 C18 C19 C20 -179.8(6) . . . . ?
O3 N12 C20 C19 -176.1(4) . . . . ?
Co1 N12 C20 C19 -5.0(6) . . . . ?
O3 N12 C20 C21 -1.1(8) . . . . ?
Co1 N12 C20 C21 170.0(4) . . . . ?
N11 C19 C20 N12 3.8(7) . . . . ?
C18 C19 C20 N12 -178.3(5) . . . . ?
N11 C19 C20 C21 -171.0(5) . . . . ?
C18 C19 C20 C21 6.9(9) . . . . ?
C26 N5 C22 C23 1.4(8) . . . . ?
Co3 N5 C22 C23 177.8(4) . . . . ?
N5 C22 C23 C24 -1.0(9) . . . . ?
C22 C23 C24 C25 0.3(9) . . . . ?
C23 C24 C25 C26 0.1(9) . . . . ?
C22 N5 C26 C25 -1.0(8) . . . . ?
Co3 N5 C26 C25 -178.0(4) . . . . ?
C22 N5 C26 C27 -176.4(5) . . . . ?
Co3 N5 C26 C27 6.7(6) . . . . ?
C24 C25 C26 N5 0.3(9) . . . . ?
C24 C25 C26 C27 175.2(5) . . . . ?
O4 N6 C27 C26 169.1(4) . . . . ?
Co3 N6 C27 C26 -10.4(6) . . . . ?
O4 N6 C27 C28 -5.3(8) . . . . ?
Co3 N6 C27 C28 175.2(5) . . . . ?
N5 C26 C27 N6 2.0(7) . . . . ?
C25 C26 C27 N6 -173.2(5) . . . . ?
N5 C26 C27 C28 176.2(6) . . . . ?
C25 C26 C27 C28 0.9(9) . . . . ?
C33 N7 C29 C30 -0.4(9) . . . . ?
Co3 N7 C29 C30 177.3(5) . . . . ?
N7 C29 C30 C31 -0.1(10) . . . . ?
C29 C30 C31 C32 0.7(10) . . . . ?
C30 C31 C32 C33 -0.9(11) . . . . ?
C29 N7 C33 C32 0.2(9) . . . . ?
Co3 N7 C33 C32 -177.8(5) . . . . ?
C29 N7 C33 C34 -178.8(5) . . . . ?
Co3 N7 C33 C34 3.1(6) . . . . ?
C31 C32 C33 N7 0.4(10) . . . . ?
C31 C32 C33 C34 179.3(6) . . . . ?
O5 N8 C34 C33 174.6(4) . . . . ?
Co3 N8 C34 C33 -1.9(7) . . . . ?
O5 N8 C34 C35 -1.1(9) . . . . ?
Co3 N8 C34 C35 -177.6(5) . . . . ?
N7 C33 C34 N8 -0.9(7) . . . . ?
C32 C33 C34 N8 -180.0(6) . . . . ?
N7 C33 C34 C35 174.7(6) . . . . ?
C32 C33 C34 C35 -4.3(10) . . . . ?
C40 N9 C36 C37 3.1(9) . . . . ?
Co3 N9 C36 C37 175.1(5) . . . . ?
C37 C38 C39 C40 4.0(10) . . . . ?
C36 N9 C40 C39 -3.4(8) . . . . ?
Co3 N9 C40 C39 -176.5(4) . . . . ?
C36 N9 C40 C41 179.5(5) . . . . ?
Co3 N9 C40 C41 6.4(6) . . . . ?
C38 C39 C40 N9 -0.1(9) . . . . ?
C38 C39 C40 C41 176.7(6) . . . . ?
O6 N10 C41 C40 171.0(5) . . . . ?
Co3 N10 C41 C40 -5.5(6) . . . . ?
O6 N10 C41 C42 -8.1(9) . . . . ?
Co3 N10 C41 C42 175.4(5) . . . . ?
N9 C40 C41 N10 -0.8(7) . . . . ?
C39 C40 C41 N10 -177.8(5) . . . . ?
N9 C40 C41 C42 178.3(5) . . . . ?
C39 C40 C41 C42 1.3(9) . . . . ?
O7 C43 C44 C45 8.3(9) . . . . ?
O8 C43 C44 C45 -172.9(6) . . . . ?
O7 C43 C44 C46 -171.0(6) . . . . ?
O8 C43 C44 C46 7.9(9) . . . . ?
C46 C44 C45 C46 0.0(10) . . . 2_767 ?
C43 C44 C45 C46 -179.2(5) . . . 2_767 ?
C45 C44 C46 O9 178.9(6) . . . . ?
C43 C44 C46 O9 -1.9(9) . . . . ?
C45 C44 C46 C45 0.0(9) . . . 2_767 ?
C43 C44 C46 C45 179.2(5) . . . 2_767 ?
O10 C47 C48 C50 -5.5(8) . . . 2_756 ?
O11 C47 C48 C50 176.5(5) . . . 2_756 ?
O10 C47 C48 C49 172.9(5) . . . . ?
O11 C47 C48 C49 -5.1(8) . . . . ?
C50 C48 C49 O12 178.8(5) 2_756 . . . ?
C47 C48 C49 O12 0.4(9) . . . . ?
C50 C48 C49 C50 1.0(9) 2_756 . . . ?
C47 C48 C49 C50 -177.4(5) . . . . ?
O12 C49 C50 C48 -178.9(5) . . . 2_756 ?
C48 C49 C50 C48 -1.1(9) . . . 2_756 ?
N9 C36 C37 C38 0.8(10) . . . . ?
C39 C38 C37 C36 -4.3(10) . . . . ?

_refine_diff_density_max         0.918
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.118



# start Validation Reply Form
_vrf_PLAT602_shelx               
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PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check 
RESPONSE: Due to squeeze 
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