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

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

data_L1
_database_code_depnum_ccdc_archive 'CCDC 1406627'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_audit_creation_date             2015-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H32 N2 O8'
_chemical_formula_sum            'C34 H32 N2 O8'
_chemical_formula_weight         596.61
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   6.8880(14)
_cell_length_b                   9.5160(19)
_cell_length_c                   22.333(5)
_cell_angle_alpha                91.24(3)
_cell_angle_beta                 94.48(3)
_cell_angle_gamma                94.64(3)
_cell_volume                     1454.0(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      0.915
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27935
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.992
_diffrn_reflns_theta_min         0.915
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5785
_reflns_number_total             6926
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6926
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0507
_refine_ls_restrained_S_all      1.037
_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)+(0.0810P)²+0.4400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1421
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H35A,H35B} of C35, {H10A,H10B} of C10, {H12A,H12B} of C12,
   {H25A,H25B} of C25, {H23A,H23B} of C23, {H22A,H22B} of C22
 At 1.5 times of:
  All O(H) groups, {H1,H33} of C30
2. Restrained distances
 H1-O1
 0.84 with sigma of 0.02
 H33-O33
 0.84 with sigma of 0.02
 H20-O20
 0.84 with sigma of 0.02
 O43-H43
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,
 H25B), C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17), C18(H18),
 C27(H27), C28(H28), C30(H30), C31(H31), C37(H37), C38(H38), C40(H40), C41(H41)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
O1 O 0.64983(16) 1.11225(12) 0.04432(5) 0.0255(2) Uani 1 1 d D . . . .
C2 C 0.7336(2) 1.04430(14) 0.08602(6) 0.0192(3) Uani 1 1 d . . . . .
O3 O 0.91716(16) 1.04200(13) 0.09438(5) 0.0308(3) Uani 1 1 d . . . . .
C4 C 0.6083(2) 0.96625(14) 0.12728(6) 0.0178(3) Uani 1 1 d . . . . .
C5 C 0.4063(2) 0.94829(14) 0.11418(6) 0.0184(3) Uani 1 1 d . . . . .
H5 H 0.3489 0.9824 0.0778 0.022 Uiso 1 1 calc R . . . .
C6 C 0.2893(2) 0.88027(14) 0.15452(6) 0.0182(3) Uani 1 1 d . . . . .
H6 H 0.1522 0.8658 0.1450 0.022 Uiso 1 1 calc R . . . .
C7 C 0.37122(19) 0.83304(13) 0.20879(6) 0.0159(3) Uani 1 1 d . . . . .
C8 C 0.5742(2) 0.84866(14) 0.22086(6) 0.0176(3) Uani 1 1 d . . . . .
H8 H 0.6318 0.8142 0.2571 0.021 Uiso 1 1 calc R . . . .
C9 C 0.6920(2) 0.91396(14) 0.18041(6) 0.0184(3) Uani 1 1 d . . . . .
H9 H 0.8299 0.9232 0.1888 0.022 Uiso 1 1 calc R . . . .
C10 C 0.2418(2) 0.77305(14) 0.25568(6) 0.0176(3) Uani 1 1 d . . . . .
H10A H 0.2201 0.8490 0.2848 0.021 Uiso 1 1 calc R . . . .
H10B H 0.1132 0.7375 0.2358 0.021 Uiso 1 1 calc R . . . .
N11 N 0.32888(17) 0.65862(11) 0.28773(5) 0.0161(2) Uani 1 1 d . . . . .
C12 C 0.2421(2) 0.63192(14) 0.34451(6) 0.0184(3) Uani 1 1 d . . . . .
H12A H 0.1075 0.5872 0.3362 0.022 Uiso 1 1 calc R . . . .
H12B H 0.2342 0.7226 0.3664 0.022 Uiso 1 1 calc R . . . .
C13 C 0.3610(2) 0.53686(14) 0.38339(6) 0.0172(3) Uani 1 1 d . . . . .
C14 C 0.5592(2) 0.57500(14) 0.39844(6) 0.0185(3) Uani 1 1 d . . . . .
H14 H 0.6166 0.6618 0.3852 0.022 Uiso 1 1 calc R . . . .
C15 C 0.6730(2) 0.48786(14) 0.43250(6) 0.0181(3) Uani 1 1 d . . . . .
H15 H 0.8080 0.5143 0.4422 0.022 Uiso 1 1 calc R . . . .
C16 C 0.5880(2) 0.36052(14) 0.45262(6) 0.0171(3) Uani 1 1 d . . . . .
C17 C 0.3892(2) 0.32329(14) 0.43933(6) 0.0192(3) Uani 1 1 d . . . . .
H17 H 0.3305 0.2382 0.4538 0.023 Uiso 1 1 calc R . . . .
C18 C 0.2773(2) 0.41140(14) 0.40475(6) 0.0186(3) Uani 1 1 d . . . . .
H18 H 0.1419 0.3857 0.3955 0.022 Uiso 1 1 calc R . . . .
C19 C 0.7121(2) 0.26727(14) 0.48812(6) 0.0179(3) Uani 1 1 d . . . . .
O20 O 0.62062(16) 0.15842(11) 0.51111(5) 0.0235(2) Uani 1 1 d D . . . .
H20 H 0.702(3) 0.112(2) 0.5336(9) 0.035 Uiso 1 1 d DR . . . .
O21 O 0.89219(16) 0.29296(12) 0.49452(5) 0.0270(2) Uani 1 1 d . . . . .
C22 C 0.3245(2) 0.53094(14) 0.24913(6) 0.0177(3) Uani 1 1 d . . . . .
H22A H 0.2749 0.5524 0.2078 0.021 Uiso 1 1 calc R . . . .
H22B H 0.2331 0.4567 0.2642 0.021 Uiso 1 1 calc R . . . .
C23 C 0.52700(19) 0.47533(13) 0.24747(6) 0.0167(3) Uani 1 1 d . . . . .
H23A H 0.6159 0.5494 0.2312 0.020 Uiso 1 1 calc R . . . .
H23B H 0.5781 0.4592 0.2892 0.020 Uiso 1 1 calc R . . . .
N24 N 0.53332(17) 0.34511(11) 0.21192(5) 0.0160(2) Uani 1 1 d . . . . .
C25 C 0.45993(19) 0.35465(14) 0.14895(6) 0.0170(3) Uani 1 1 d . . . . .
H25A H 0.3247 0.3834 0.1470 0.020 Uiso 1 1 calc R . . . .
H25B H 0.4568 0.2607 0.1288 0.020 Uiso 1 1 calc R . . . .
C26 C 0.5865(2) 0.45973(14) 0.11643(6) 0.0175(3) Uani 1 1 d . . . . .
C27 C 0.5051(2) 0.55904(15) 0.07960(6) 0.0208(3) Uani 1 1 d . . . . .
H27 H 0.3678 0.5654 0.0770 0.025 Uiso 1 1 calc R . . . .
C28 C 0.6217(2) 0.64932(15) 0.04650(6) 0.0210(3) Uani 1 1 d . . . . .
H28 H 0.5636 0.7159 0.0212 0.025 Uiso 1 1 calc R . . . .
C29 C 0.8221(2) 0.64207(15) 0.05046(6) 0.0193(3) Uani 1 1 d . . . . .
C30 C 0.9055(2) 0.5448(2) 0.08842(8) 0.0335(4) Uani 1 1 d . . . . .
H30 H 1.0432 0.5404 0.0920 0.040 Uiso 1 1 calc R . . . .
H1 H 0.728(3) 1.164(2) 0.0215(10) 0.050 Uiso 1 1 d DR . . . .
H33 H 0.947(3) 0.856(2) -0.0489(9) 0.050 Uiso 1 1 d DR . . . .
C31 C 0.7887(2) 0.45493(19) 0.12081(8) 0.0321(4) Uani 1 1 d . . . . .
H31 H 0.8470 0.3890 0.1464 0.039 Uiso 1 1 calc R . . . .
C32 C 0.9464(2) 0.73380(15) 0.01378(6) 0.0198(3) Uani 1 1 d . . . . .
O33 O 0.86230(17) 0.81087(13) -0.02460(5) 0.0317(3) Uani 1 1 d D . . . .
O34 O 1.12950(16) 0.73019(14) 0.02093(5) 0.0315(3) Uani 1 1 d . . . . .
C35 C 0.45037(19) 0.22103(13) 0.24094(6) 0.0170(3) Uani 1 1 d . . . . .
H35A H 0.4155 0.1447 0.2102 0.020 Uiso 1 1 calc R . . . .
H35B H 0.3286 0.2442 0.2584 0.020 Uiso 1 1 calc R . . . .
C36 C 0.58761(19) 0.16795(13) 0.29007(6) 0.0164(3) Uani 1 1 d . . . . .
C37 C 0.7902(2) 0.19155(14) 0.28981(6) 0.0193(3) Uani 1 1 d . . . . .
H37 H 0.8447 0.2526 0.2613 0.023 Uiso 1 1 calc R . . . .
C38 C 0.9125(2) 0.12643(14) 0.33090(6) 0.0197(3) Uani 1 1 d . . . . .
H38 H 1.0502 0.1438 0.3306 0.024 Uiso 1 1 calc R . . . .
C39 C 0.8338(2) 0.03538(14) 0.37270(6) 0.0171(3) Uani 1 1 d . . . . .
C40 C 0.6314(2) 0.01506(14) 0.37455(6) 0.0177(3) Uani 1 1 d . . . . .
H40 H 0.5767 -0.0447 0.4035 0.021 Uiso 1 1 calc R . . . .
C41 C 0.51069(19) 0.08253(14) 0.33388(6) 0.0174(3) Uani 1 1 d . . . . .
H41 H 0.3731 0.0703 0.3359 0.021 Uiso 1 1 calc R . . . .
C42 C 0.9648(2) -0.04085(14) 0.41383(6) 0.0179(3) Uani 1 1 d . . . . .
O43 O 0.87706(16) -0.13106(12) 0.44778(5) 0.0267(2) Uani 1 1 d D . . . .
H43 H 0.958(3) -0.184(2) 0.4667(9) 0.040 Uiso 1 1 d DR . . . .
O44 O 1.14542(15) -0.02044(11) 0.41473(5) 0.0231(2) 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
O1 C2 1.2731(17) . ?
O1 H1 0.897(16) . ?
C2 O3 1.2657(18) . ?
C2 C4 1.4816(19) . ?
C4 C5 1.3952(19) . ?
C4 C9 1.3975(19) . ?
C5 H5 0.9500 . ?
C5 C6 1.3907(19) . ?
C6 H6 0.9500 . ?
C6 C7 1.3954(18) . ?
C7 C8 1.3983(19) . ?
C7 C10 1.5187(18) . ?
C8 H8 0.9500 . ?
C8 C9 1.3848(19) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 N11 1.4595(17) . ?
N11 C12 1.4621(16) . ?
N11 C22 1.4714(17) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.5122(18) . ?
C13 C14 1.3965(19) . ?
C13 C18 1.3934(19) . ?
C14 H14 0.9500 . ?
C14 C15 1.3859(19) . ?
C15 H15 0.9500 . ?
C15 C16 1.4011(19) . ?
C16 C17 1.3938(19) . ?
C16 C19 1.4811(19) . ?
C17 H17 0.9500 . ?
C17 C18 1.3902(19) . ?
C18 H18 0.9500 . ?
C19 O20 1.3045(17) . ?
C19 O21 1.2411(18) . ?
O20 H20 0.880(15) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.5342(18) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 N24 1.4626(16) . ?
N24 C25 1.4641(17) . ?
N24 C35 1.4568(16) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.5089(18) . ?
C26 C27 1.3894(19) . ?
C26 C31 1.393(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.3919(19) . ?
C28 H28 0.9500 . ?
C28 C29 1.3838(19) . ?
C29 C30 1.396(2) . ?
C29 C32 1.4786(19) . ?
C30 H30 0.9500 . ?
C30 C31 1.381(2) . ?
C31 H31 0.9500 . ?
C32 O33 1.2754(18) . ?
C32 O34 1.2618(18) . ?
O33 H33 0.914(16) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.5137(19) . ?
C36 C37 1.3961(19) . ?
C36 C41 1.3946(18) . ?
C37 H37 0.9500 . ?
C37 C38 1.3871(19) . ?
C38 H38 0.9500 . ?
C38 C39 1.3980(18) . ?
C39 C40 1.3955(19) . ?
C39 C42 1.4798(19) . ?
C40 H40 0.9500 . ?
C40 C41 1.3864(19) . ?
C41 H41 0.9500 . ?
C42 O43 1.3013(17) . ?
C42 O44 1.2417(17) . ?
O43 H43 0.870(15) . ?

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 O1 H1 116.5(16) . . ?
O1 C2 C4 117.79(12) . . ?
O3 C2 O1 123.40(13) . . ?
O3 C2 C4 118.80(12) . . ?
C5 C4 C2 120.26(12) . . ?
C5 C4 C9 119.79(12) . . ?
C9 C4 C2 119.92(12) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.77(12) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.69(13) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 C8 119.05(12) . . ?
C6 C7 C10 120.63(12) . . ?
C8 C7 C10 120.23(11) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.55(12) . . ?
C9 C8 H8 119.7 . . ?
C4 C9 H9 120.0 . . ?
C8 C9 C4 120.08(13) . . ?
C8 C9 H9 120.0 . . ?
C7 C10 H10A 109.3 . . ?
C7 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
N11 C10 C7 111.71(11) . . ?
N11 C10 H10A 109.3 . . ?
N11 C10 H10B 109.3 . . ?
C10 N11 C12 111.82(10) . . ?
C10 N11 C22 111.44(10) . . ?
C12 N11 C22 112.82(11) . . ?
N11 C12 H12A 109.4 . . ?
N11 C12 H12B 109.4 . . ?
N11 C12 C13 111.30(11) . . ?
H12A C12 H12B 108.0 . . ?
C13 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
C14 C13 C12 119.61(12) . . ?
C18 C13 C12 121.43(12) . . ?
C18 C13 C14 118.96(12) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.83(12) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.63(13) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C19 119.06(12) . . ?
C17 C16 C15 120.03(13) . . ?
C17 C16 C19 120.91(12) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.61(12) . . ?
C18 C17 H17 120.2 . . ?
C13 C18 H18 119.6 . . ?
C17 C18 C13 120.90(13) . . ?
C17 C18 H18 119.6 . . ?
O20 C19 C16 115.97(12) . . ?
O21 C19 C16 120.80(12) . . ?
O21 C19 O20 123.23(13) . . ?
C19 O20 H20 110.8(14) . . ?
N11 C22 H22A 109.2 . . ?
N11 C22 H22B 109.2 . . ?
N11 C22 C23 112.17(11) . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
C22 C23 H23A 108.4 . . ?
C22 C23 H23B 108.4 . . ?
H23A C23 H23B 107.5 . . ?
N24 C23 C22 115.45(11) . . ?
N24 C23 H23A 108.4 . . ?
N24 C23 H23B 108.4 . . ?
C23 N24 C25 113.92(10) . . ?
C35 N24 C23 112.93(10) . . ?
C35 N24 C25 113.43(11) . . ?
N24 C25 H25A 109.4 . . ?
N24 C25 H25B 109.4 . . ?
N24 C25 C26 111.37(11) . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
C27 C26 C25 121.30(12) . . ?
C27 C26 C31 118.44(13) . . ?
C31 C26 C25 120.21(12) . . ?
C26 C27 H27 119.5 . . ?
C26 C27 C28 121.04(13) . . ?
C28 C27 H27 119.5 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 120.01(13) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 119.33(13) . . ?
C28 C29 C32 120.45(12) . . ?
C30 C29 C32 120.21(13) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.29(14) . . ?
C31 C30 H30 119.9 . . ?
C26 C31 H31 119.6 . . ?
C30 C31 C26 120.87(14) . . ?
C30 C31 H31 119.6 . . ?
O33 C32 C29 118.00(13) . . ?
O34 C32 C29 118.81(12) . . ?
O34 C32 O33 123.17(13) . . ?
C32 O33 H33 113.1(15) . . ?
N24 C35 H35A 108.9 . . ?
N24 C35 H35B 108.9 . . ?
N24 C35 C36 113.25(11) . . ?
H35A C35 H35B 107.7 . . ?
C36 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
C37 C36 C35 121.84(12) . . ?
C41 C36 C35 119.11(12) . . ?
C41 C36 C37 118.81(12) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 C36 120.46(12) . . ?
C38 C37 H37 119.8 . . ?
C37 C38 H38 119.9 . . ?
C37 C38 C39 120.21(13) . . ?
C39 C38 H38 119.9 . . ?
C38 C39 C42 119.94(12) . . ?
C40 C39 C38 119.61(13) . . ?
C40 C39 C42 120.44(12) . . ?
C39 C40 H40 120.2 . . ?
C41 C40 C39 119.63(12) . . ?
C41 C40 H40 120.2 . . ?
C36 C41 H41 119.4 . . ?
C40 C41 C36 121.16(12) . . ?
C40 C41 H41 119.4 . . ?
O43 C42 C39 115.18(12) . . ?
O44 C42 C39 121.68(12) . . ?
O44 C42 O43 123.13(13) . . ?
C42 O43 H43 112.4(15) . . ?

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
O20 H20 O44 0.880(15) 1.785(15) 2.6613(17) 174(2) 2_756
O1 H1 O34 0.897(16) 1.703(16) 2.5987(17) 177(2) 2_775
O33 H33 O3 0.914(16) 1.702(17) 2.6108(17) 172(2) 2_775
O43 H43 O21 0.870(15) 1.723(16) 2.5926(17) 177(2) 2_756

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
O1 C2 C4 C5 10.91(19) . . . . ?
O1 C2 C4 C9 -167.20(13) . . . . ?
C2 C4 C5 C6 -177.18(12) . . . . ?
C2 C4 C9 C8 175.99(12) . . . . ?
O3 C2 C4 C5 -170.12(13) . . . . ?
O3 C2 C4 C9 11.8(2) . . . . ?
C4 C5 C6 C7 1.7(2) . . . . ?
C5 C4 C9 C8 -2.1(2) . . . . ?
C5 C6 C7 C8 -3.18(19) . . . . ?
C5 C6 C7 C10 173.39(12) . . . . ?
C6 C7 C8 C9 1.97(19) . . . . ?
C6 C7 C10 N11 144.79(12) . . . . ?
C7 C8 C9 C4 0.7(2) . . . . ?
C7 C10 N11 C12 161.22(11) . . . . ?
C7 C10 N11 C22 -71.47(14) . . . . ?
C8 C7 C10 N11 -38.68(17) . . . . ?
C9 C4 C5 C6 0.9(2) . . . . ?
C10 C7 C8 C9 -174.62(12) . . . . ?
C10 N11 C12 C13 -167.57(11) . . . . ?
C10 N11 C22 C23 126.83(12) . . . . ?
N11 C12 C13 C14 55.76(16) . . . . ?
N11 C12 C13 C18 -124.27(14) . . . . ?
N11 C22 C23 N24 177.62(10) . . . . ?
C12 N11 C22 C23 -106.41(13) . . . . ?
C12 C13 C14 C15 -178.05(12) . . . . ?
C12 C13 C18 C17 178.52(12) . . . . ?
C13 C14 C15 C16 -0.6(2) . . . . ?
C14 C13 C18 C17 -1.5(2) . . . . ?
C14 C15 C16 C17 -1.22(19) . . . . ?
C14 C15 C16 C19 178.99(12) . . . . ?
C15 C16 C17 C18 1.7(2) . . . . ?
C15 C16 C19 O20 172.64(12) . . . . ?
C15 C16 C19 O21 -7.90(19) . . . . ?
C16 C17 C18 C13 -0.3(2) . . . . ?
C17 C16 C19 O20 -7.15(18) . . . . ?
C17 C16 C19 O21 172.31(13) . . . . ?
C18 C13 C14 C15 1.98(19) . . . . ?
C19 C16 C17 C18 -178.53(12) . . . . ?
C22 N11 C12 C13 65.88(15) . . . . ?
C22 C23 N24 C25 57.79(15) . . . . ?
C22 C23 N24 C35 -73.51(14) . . . . ?
C23 N24 C25 C26 64.37(14) . . . . ?
C23 N24 C35 C36 -78.54(14) . . . . ?
N24 C25 C26 C27 -133.76(13) . . . . ?
N24 C25 C26 C31 49.02(18) . . . . ?
N24 C35 C36 C37 -26.54(17) . . . . ?
N24 C35 C36 C41 159.26(11) . . . . ?
C25 N24 C35 C36 149.91(11) . . . . ?
C25 C26 C27 C28 -175.55(13) . . . . ?
C25 C26 C31 C30 176.03(16) . . . . ?
C26 C27 C28 C29 -0.7(2) . . . . ?
C27 C26 C31 C30 -1.3(3) . . . . ?
C27 C28 C29 C30 -0.8(2) . . . . ?
C27 C28 C29 C32 177.71(13) . . . . ?
C28 C29 C30 C31 1.2(3) . . . . ?
C28 C29 C32 O33 -5.4(2) . . . . ?
C28 C29 C32 O34 176.08(13) . . . . ?
C29 C30 C31 C26 -0.2(3) . . . . ?
C30 C29 C32 O33 173.12(15) . . . . ?
C30 C29 C32 O34 -5.4(2) . . . . ?
C31 C26 C27 C28 1.7(2) . . . . ?
C32 C29 C30 C31 -177.28(16) . . . . ?
C35 N24 C25 C26 -164.57(10) . . . . ?
C35 C36 C37 C38 -171.60(12) . . . . ?
C35 C36 C41 C40 170.68(12) . . . . ?
C36 C37 C38 C39 0.6(2) . . . . ?
C37 C36 C41 C40 -3.70(19) . . . . ?
C37 C38 C39 C40 -2.7(2) . . . . ?
C37 C38 C39 C42 176.08(13) . . . . ?
C38 C39 C40 C41 1.7(2) . . . . ?
C38 C39 C42 O43 -174.92(13) . . . . ?
C38 C39 C42 O44 4.1(2) . . . . ?
C39 C40 C41 C36 1.6(2) . . . . ?
C40 C39 C42 O43 3.88(19) . . . . ?
C40 C39 C42 O44 -177.09(13) . . . . ?
C41 C36 C37 C38 2.6(2) . . . . ?
C42 C39 C40 C41 -177.13(12) . . . . ?

_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_1
_database_code_depnum_ccdc_archive 'CCDC 1406628'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_audit_creation_date             2015-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H66 N4 Ni3 O20, 2(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C74 H84 N6 Ni3 O24'
_chemical_formula_weight         1617.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3410 1.1070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.878(2)
_cell_length_b                   11.944(2)
_cell_length_c                   13.199(3)
_cell_angle_alpha                76.18(3)
_cell_angle_beta                 79.76(3)
_cell_angle_gamma                75.16(3)
_cell_volume                     1744.1(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8335
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      1.79
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58284
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.947
_diffrn_reflns_theta_min         1.788
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7763
_reflns_number_total             8335
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8335
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0530P)²+1.5500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0960
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N13-H13
 0.88 with sigma of 0.02
 O49-H49A = O49-H49B
 0.84 with sigma of 0.02
 H47A-O47
 0.84 with sigma of 0.02
 O47-H47B
 0.84 with sigma of 0.02
 H48A-O48
 0.84 with sigma of 0.02
 O48-H48B
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C12(H12A,H12B), C27(H27A,H27B), C37(H37A,H37B), C25(H25A,
 H25B), C24(H24A,H24B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C30(H30), C11(H11), C19(H19), C33(H33), C43(H43), C8(H8), C10(H10),
 C40(H40), C17(H17), C20(H20), C32(H32), C42(H42), C51(H51), C39(H39), C16(H16),
  C29(H29)
3.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.5000 0.5000 0.0000 0.00949(7) Uani 1 2 d S T P . .
Ni1 Ni 0.19503(2) 0.52768(2) 0.01708(2) 0.01021(6) Uani 1 1 d . . . . .
O48 O 0.02025(10) 0.58459(11) 0.07740(9) 0.0135(2) Uani 1 1 d D . . . .
O5 O 0.42703(11) 0.48783(14) 0.15425(10) 0.0227(3) Uani 1 1 d . . . . .
O22 O 0.22296(11) 0.69321(11) -0.00973(10) 0.0162(2) Uani 1 1 d . . . . .
O47 O 0.36245(10) 0.46308(10) -0.04649(9) 0.0117(2) Uani 1 1 d D . . . .
O46 O -0.34188(11) -0.25362(11) 0.97405(10) 0.0183(2) Uani 1 1 d . . . . .
O35 O -0.30802(11) 0.41281(11) 0.22655(9) 0.0169(2) Uani 1 1 d . . . . .
O23 O 0.41905(11) 0.67495(11) -0.02622(12) 0.0227(3) Uani 1 1 d . . . . .
O45 O -0.15721(10) -0.35866(10) 0.95367(9) 0.0140(2) Uani 1 1 d . . . . .
O3 O 0.23531(11) 0.48867(11) 0.16532(9) 0.0169(2) Uani 1 1 d . . . . .
O36 O -0.13490(10) 0.43052(10) 0.13160(9) 0.0137(2) Uani 1 1 d . . . . .
C7 C 0.41250(15) 0.43301(16) 0.37377(13) 0.0170(3) Uani 1 1 d . . . . .
H7 H 0.4890 0.4211 0.3359 0.020 Uiso 1 1 calc R . . . .
C4 C 0.32673(14) 0.48515(14) 0.20235(13) 0.0136(3) Uani 1 1 d . . . . .
N26 N 0.02126(13) 0.15889(12) 0.67349(11) 0.0148(3) Uani 1 1 d . . . . .
C14 C 0.25619(15) 0.23873(14) 0.81452(12) 0.0146(3) Uani 1 1 d . . . . .
H14A H 0.3111 0.2695 0.8431 0.017 Uiso 1 1 calc R . . . .
H14B H 0.1754 0.2808 0.8362 0.017 Uiso 1 1 calc R . . . .
C9 C 0.28620(15) 0.43037(14) 0.53890(13) 0.0149(3) Uani 1 1 d . . . . .
C6 C 0.31411(15) 0.47382(14) 0.31978(13) 0.0144(3) Uani 1 1 d . . . . .
C30 C -0.19955(16) 0.26291(16) 0.39394(14) 0.0185(3) Uani 1 1 d . . . . .
H30 H -0.2798 0.2657 0.3919 0.022 Uiso 1 1 calc R . . . .
C11 C 0.20273(15) 0.49896(14) 0.37524(13) 0.0150(3) Uani 1 1 d . . . . .
H11 H 0.1359 0.5293 0.3385 0.018 Uiso 1 1 calc R . . . .
C12 C 0.26824(16) 0.39607(14) 0.65694(13) 0.0153(3) Uani 1 1 d . . . . .
H12A H 0.1892 0.4379 0.6834 0.018 Uiso 1 1 calc R . . . .
H12B H 0.3267 0.4215 0.6860 0.018 Uiso 1 1 calc R . . . .
C19 C 0.18661(15) -0.06243(15) 0.93178(13) 0.0149(3) Uani 1 1 d . . . . .
H19 H 0.1197 -0.0959 0.9548 0.018 Uiso 1 1 calc R . . . .
C33 C 0.03199(15) 0.26015(15) 0.40389(13) 0.0165(3) Uani 1 1 d . . . . .
H33 H 0.1106 0.2616 0.4080 0.020 Uiso 1 1 calc R . . . .
N52 N 0.45729(16) 0.07908(16) 0.34500(14) 0.0279(4) Uani 1 1 d . . . . .
O50 O 0.52938(15) -0.11958(15) 0.39030(12) 0.0361(4) Uani 1 1 d . . . . .
N13 N 0.28006(12) 0.26416(12) 0.69523(11) 0.0128(3) Uani 1 1 d D . . . .
C27 C 0.03372(16) 0.11226(15) 0.57755(13) 0.0165(3) Uani 1 1 d . . . . .
H27A H 0.0046 0.0384 0.5970 0.020 Uiso 1 1 calc R . . . .
H27B H 0.1185 0.0907 0.5523 0.020 Uiso 1 1 calc R . . . .
C43 C -0.24800(15) 0.05867(15) 0.81358(14) 0.0179(3) Uani 1 1 d . . . . .
H43 H -0.3063 0.1296 0.7993 0.021 Uiso 1 1 calc R . . . .
C15 C 0.26983(15) 0.10863(14) 0.86017(13) 0.0147(3) Uani 1 1 d . . . . .
C8 C 0.39806(15) 0.40982(15) 0.48311(13) 0.0169(3) Uani 1 1 d . . . . .
H8 H 0.4649 0.3798 0.5199 0.020 Uiso 1 1 calc R . . . .
C10 C 0.18894(15) 0.47977(15) 0.48426(13) 0.0158(3) Uani 1 1 d . . . . .
H10 H 0.1131 0.5003 0.5217 0.019 Uiso 1 1 calc R . . . .
C18 C 0.29867(14) 0.86508(14) -0.06326(13) 0.0135(3) Uani 1 1 d . . . . .
C40 C -0.07825(14) -0.15006(15) 0.85390(13) 0.0143(3) Uani 1 1 d . . . . .
H40 H -0.0199 -0.2211 0.8672 0.017 Uiso 1 1 calc R . . . .
O49 O 0.48372(14) 0.70362(15) 0.18843(14) 0.0316(3) Uani 1 1 d D . . . .
C17 C 0.39667(15) -0.08476(15) 0.90768(13) 0.0158(3) Uani 1 1 d . . . . .
H17 H 0.4732 -0.1334 0.9136 0.019 Uiso 1 1 calc R . . . .
C20 C 0.17229(15) 0.05871(15) 0.89329(13) 0.0152(3) Uani 1 1 d . . . . .
H20 H 0.0956 0.1076 0.8896 0.018 Uiso 1 1 calc R . . . .
C38 C -0.13021(15) 0.05968(15) 0.78140(13) 0.0152(3) Uani 1 1 d . . . . .
C44 C -0.23465(14) -0.26239(14) 0.94183(13) 0.0133(3) Uani 1 1 d . . . . .
C32 C -0.02118(15) 0.32572(15) 0.31594(13) 0.0162(3) Uani 1 1 d . . . . .
H32 H 0.0218 0.3696 0.2597 0.019 Uiso 1 1 calc R . . . .
C42 C -0.28070(15) -0.04581(15) 0.86660(14) 0.0177(3) Uani 1 1 d . . . . .
H42 H -0.3612 -0.0456 0.8896 0.021 Uiso 1 1 calc R . . . .
C34 C -0.19853(14) 0.39473(14) 0.21556(13) 0.0131(3) Uani 1 1 d . . . . .
C37 C -0.09662(15) 0.17637(15) 0.73023(14) 0.0170(3) Uani 1 1 d . . . . .
H37A H -0.1533 0.2232 0.6809 0.020 Uiso 1 1 calc R . . . .
H37B H -0.1009 0.2218 0.7850 0.020 Uiso 1 1 calc R . . . .
C51 C 0.45052(19) -0.03320(19) 0.36324(16) 0.0285(4) Uani 1 1 d . . . . .
H51 H 0.3784 -0.0484 0.3547 0.034 Uiso 1 1 calc R . . . .
C41 C -0.19607(15) -0.15110(14) 0.88635(13) 0.0142(3) Uani 1 1 d . . . . .
C25 C 0.07745(15) 0.25757(15) 0.66025(13) 0.0155(3) Uani 1 1 d . . . . .
H25A H 0.0556 0.2927 0.7237 0.019 Uiso 1 1 calc R . . . .
H25B H 0.0514 0.3195 0.5991 0.019 Uiso 1 1 calc R . . . .
C39 C -0.04591(15) -0.04520(15) 0.80212(13) 0.0154(3) Uani 1 1 d . . . . .
H39 H 0.0347 -0.0450 0.7806 0.018 Uiso 1 1 calc R . . . .
C31 C -0.13738(15) 0.32711(14) 0.31018(13) 0.0142(3) Uani 1 1 d . . . . .
C28 C -0.02804(15) 0.19206(15) 0.48647(13) 0.0159(3) Uani 1 1 d . . . . .
C24 C 0.21024(15) 0.21092(15) 0.64279(13) 0.0150(3) Uani 1 1 d . . . . .
H24A H 0.2280 0.1242 0.6689 0.018 Uiso 1 1 calc R . . . .
H24B H 0.2365 0.2259 0.5662 0.018 Uiso 1 1 calc R . . . .
C16 C 0.38197(15) 0.03658(15) 0.87007(13) 0.0156(3) Uani 1 1 d . . . . .
H16 H 0.4487 0.0707 0.8510 0.019 Uiso 1 1 calc R . . . .
C21 C 0.31450(15) 0.73234(14) -0.02945(13) 0.0136(3) Uani 1 1 d . . . . .
C29 C -0.14489(17) 0.19502(16) 0.48017(14) 0.0201(3) Uani 1 1 d . . . . .
H29 H -0.1876 0.1500 0.5357 0.024 Uiso 1 1 calc R . . . .
C53 C 0.5636(2) 0.1133(3) 0.3541(2) 0.0402(5) Uani 1 1 d . . . . .
H53A H 0.6253 0.0423 0.3717 0.060 Uiso 1 1 calc GR . . . .
H53B H 0.5475 0.1591 0.4096 0.060 Uiso 1 1 calc GR . . . .
H53C H 0.5894 0.1618 0.2871 0.060 Uiso 1 1 calc GR . . . .
C54 C 0.3588(2) 0.1746(2) 0.3145(2) 0.0381(5) Uani 1 1 d . . . . .
H54A H 0.3817 0.2226 0.2463 0.057 Uiso 1 1 calc GR . . . .
H54B H 0.3350 0.2242 0.3675 0.057 Uiso 1 1 calc GR . . . .
H54C H 0.2930 0.1417 0.3092 0.057 Uiso 1 1 calc GR . . . .
H13 H 0.3569(17) 0.228(3) 0.682(2) 0.046 Uiso 1 1 d DR . . . .
H47A H 0.353(2) 0.496(2) -0.1098(15) 0.036(7) Uiso 1 1 d D . . . .
H47B H 0.362(3) 0.3902(17) -0.028(2) 0.045(8) Uiso 1 1 d D . . . .
H48A H -0.022(2) 0.619(3) 0.029(2) 0.046(8) Uiso 1 1 d D . . . .
H48B H -0.010(3) 0.527(2) 0.107(2) 0.048(9) Uiso 1 1 d D . . . .
H49A H 0.468(4) 0.635(2) 0.208(4) 0.103(16) Uiso 1 1 d D . . . .
H49B H 0.484(4) 0.732(4) 0.1221(17) 0.109(18) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 O5 2.0526(14) . ?
Ni2 O5 2.0526(14) 2_665 ?
Ni2 O47 2.0237(12) 2_665 ?
Ni2 O47 2.0237(12) . ?
Ni2 O23 2.0382(14) 2_665 ?
Ni2 O23 2.0382(14) . ?
Ni1 O48 2.0866(13) . ?
Ni1 O22 2.0260(13) . ?
Ni1 O47 2.0455(13) . ?
Ni1 O45 2.1111(12) 2_556 ?
Ni1 O3 2.0144(13) . ?
Ni1 O36 2.1114(13) 2_565 ?
O48 H48A 0.843(18) . ?
O48 H48B 0.841(18) . ?
O5 C4 1.251(2) . ?
O22 C21 1.253(2) . ?
O47 H47A 0.848(17) . ?
O47 H47B 0.848(17) . ?
O46 C44 1.255(2) . ?
O35 C34 1.250(2) . ?
O23 C21 1.258(2) . ?
O45 Ni1 2.1111(12) 2_556 ?
O45 C44 1.271(2) . ?
O3 C4 1.255(2) . ?
O36 Ni1 2.1114(13) 2_565 ?
O36 C34 1.274(2) . ?
C7 H7 0.9500 . ?
C7 C6 1.396(2) . ?
C7 C8 1.391(2) . ?
C4 C6 1.507(2) . ?
N26 C27 1.471(2) . ?
N26 C37 1.455(2) . ?
N26 C25 1.459(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 N13 1.519(2) . ?
C14 C15 1.504(2) . ?
C9 C12 1.504(2) . ?
C9 C8 1.393(2) . ?
C9 C10 1.395(2) . ?
C6 C11 1.391(2) . ?
C30 H30 0.9500 . ?
C30 C31 1.397(2) . ?
C30 C29 1.388(2) . ?
C11 H11 0.9500 . ?
C11 C10 1.388(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 N13 1.513(2) . ?
C19 H19 0.9500 . ?
C19 C18 1.392(2) 1_546 ?
C19 C20 1.391(2) . ?
C33 H33 0.9500 . ?
C33 C32 1.390(2) . ?
C33 C28 1.398(2) . ?
N52 C51 1.326(3) . ?
N52 C53 1.455(3) . ?
N52 C54 1.448(3) . ?
O50 C51 1.232(3) . ?
N13 C24 1.502(2) . ?
N13 H13 0.909(17) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.517(2) . ?
C43 H43 0.9500 . ?
C43 C38 1.390(2) . ?
C43 C42 1.390(2) . ?
C15 C20 1.392(2) . ?
C15 C16 1.398(2) . ?
C8 H8 0.9500 . ?
C10 H10 0.9500 . ?
C18 C19 1.392(2) 1_564 ?
C18 C17 1.396(2) 1_564 ?
C18 C21 1.512(2) . ?
C40 H40 0.9500 . ?
C40 C41 1.391(2) . ?
C40 C39 1.388(2) . ?
O49 H49A 0.856(19) . ?
O49 H49B 0.860(19) . ?
C17 C18 1.396(2) 1_546 ?
C17 H17 0.9500 . ?
C17 C16 1.391(2) . ?
C20 H20 0.9500 . ?
C38 C37 1.516(2) . ?
C38 C39 1.392(2) . ?
C44 C41 1.497(2) . ?
C32 H32 0.9500 . ?
C32 C31 1.391(2) . ?
C42 H42 0.9500 . ?
C42 C41 1.396(2) . ?
C34 C31 1.510(2) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C51 H51 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.528(2) . ?
C39 H39 0.9500 . ?
C28 C29 1.396(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C16 H16 0.9500 . ?
C29 H29 0.9500 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Ni2 O5 180.0 . 2_665 ?
O47 Ni2 O5 94.15(5) . . ?
O47 Ni2 O5 85.85(5) . 2_665 ?
O47 Ni2 O5 94.15(5) 2_665 2_665 ?
O47 Ni2 O5 85.85(5) 2_665 . ?
O47 Ni2 O47 180.0 . 2_665 ?
O47 Ni2 O23 90.44(6) . 2_665 ?
O47 Ni2 O23 89.56(6) 2_665 2_665 ?
O47 Ni2 O23 89.56(6) . . ?
O47 Ni2 O23 90.44(6) 2_665 . ?
O23 Ni2 O5 88.21(7) 2_665 2_665 ?
O23 Ni2 O5 88.21(7) . . ?
O23 Ni2 O5 91.79(7) . 2_665 ?
O23 Ni2 O5 91.79(7) 2_665 . ?
O23 Ni2 O23 180.0 2_665 . ?
O48 Ni1 O45 85.63(6) . 2_556 ?
O48 Ni1 O36 86.50(5) . 2_565 ?
O22 Ni1 O48 91.68(6) . . ?
O22 Ni1 O47 91.84(6) . . ?
O22 Ni1 O45 177.25(5) . 2_556 ?
O22 Ni1 O36 88.85(6) . 2_565 ?
O47 Ni1 O48 175.75(5) . . ?
O47 Ni1 O45 90.82(6) . 2_556 ?
O47 Ni1 O36 91.18(5) . 2_565 ?
O45 Ni1 O36 90.43(5) 2_556 2_565 ?
O3 Ni1 O48 87.90(6) . . ?
O3 Ni1 O22 92.85(6) . . ?
O3 Ni1 O47 94.31(6) . . ?
O3 Ni1 O45 87.61(6) . 2_556 ?
O3 Ni1 O36 174.19(5) . 2_565 ?
Ni1 O48 H48A 111(2) . . ?
Ni1 O48 H48B 111(2) . . ?
H48A O48 H48B 103(3) . . ?
C4 O5 Ni2 134.98(12) . . ?
C21 O22 Ni1 132.69(12) . . ?
Ni2 O47 Ni1 119.96(6) . . ?
Ni2 O47 H47A 112.3(19) . . ?
Ni2 O47 H47B 112(2) . . ?
Ni1 O47 H47A 96.5(19) . . ?
Ni1 O47 H47B 98(2) . . ?
H47A O47 H47B 118(3) . . ?
C21 O23 Ni2 135.01(12) . . ?
C44 O45 Ni1 123.83(10) . 2_556 ?
C4 O3 Ni1 132.43(11) . . ?
C34 O36 Ni1 121.64(10) . 2_565 ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C8 C7 C6 119.78(16) . . ?
O5 C4 O3 128.13(16) . . ?
O5 C4 C6 116.19(15) . . ?
O3 C4 C6 115.67(15) . . ?
C37 N26 C27 114.64(14) . . ?
C37 N26 C25 114.24(14) . . ?
C25 N26 C27 114.06(14) . . ?
H14A C14 H14B 107.9 . . ?
N13 C14 H14A 109.2 . . ?
N13 C14 H14B 109.2 . . ?
C15 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C15 C14 N13 112.15(14) . . ?
C8 C9 C12 121.02(15) . . ?
C8 C9 C10 119.47(15) . . ?
C10 C9 C12 119.47(16) . . ?
C7 C6 C4 120.67(15) . . ?
C11 C6 C7 119.82(15) . . ?
C11 C6 C4 119.44(15) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C29 C30 C31 120.44(16) . . ?
C6 C11 H11 119.9 . . ?
C10 C11 C6 120.14(16) . . ?
C10 C11 H11 119.9 . . ?
C9 C12 H12A 109.2 . . ?
C9 C12 H12B 109.2 . . ?
C9 C12 N13 112.16(14) . . ?
H12A C12 H12B 107.9 . . ?
N13 C12 H12A 109.2 . . ?
N13 C12 H12B 109.2 . . ?
C18 C19 H19 119.9 1_546 . ?
C20 C19 H19 119.9 . . ?
C20 C19 C18 120.26(16) . 1_546 ?
C32 C33 H33 119.4 . . ?
C32 C33 C28 121.27(16) . . ?
C28 C33 H33 119.4 . . ?
C51 N52 C53 122.1(2) . . ?
C51 N52 C54 121.6(2) . . ?
C54 N52 C53 116.3(2) . . ?
C14 N13 H13 103.5(19) . . ?
C12 N13 C14 108.32(13) . . ?
C12 N13 H13 108(2) . . ?
C24 N13 C14 114.24(13) . . ?
C24 N13 C12 114.42(13) . . ?
C24 N13 H13 107(2) . . ?
N26 C27 H27A 107.9 . . ?
N26 C27 H27B 107.9 . . ?
N26 C27 C28 117.46(14) . . ?
H27A C27 H27B 107.2 . . ?
C28 C27 H27A 107.9 . . ?
C28 C27 H27B 107.9 . . ?
C38 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C42 C43 C38 120.20(16) . . ?
C20 C15 C14 121.02(15) . . ?
C20 C15 C16 119.33(15) . . ?
C16 C15 C14 119.65(15) . . ?
C7 C8 C9 120.35(16) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.15(16) . . ?
C11 C10 H10 119.9 . . ?
C19 C18 C17 119.69(15) 1_564 1_564 ?
C19 C18 C21 120.24(15) 1_564 . ?
C17 C18 C21 120.05(15) 1_564 . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C39 C40 C41 120.03(16) . . ?
H49A O49 H49B 114(4) . . ?
C18 C17 H17 120.1 1_546 . ?
C16 C17 C18 119.83(16) . 1_546 ?
C16 C17 H17 120.1 . . ?
C19 C20 C15 120.28(16) . . ?
C19 C20 H20 119.9 . . ?
C15 C20 H20 119.9 . . ?
C43 C38 C37 118.98(15) . . ?
C43 C38 C39 119.20(16) . . ?
C39 C38 C37 121.72(15) . . ?
O46 C44 O45 124.55(15) . . ?
O46 C44 C41 117.25(15) . . ?
O45 C44 C41 118.20(15) . . ?
C33 C32 H32 120.0 . . ?
C33 C32 C31 120.03(16) . . ?
C31 C32 H32 120.0 . . ?
C43 C42 H42 119.8 . . ?
C43 C42 C41 120.48(16) . . ?
C41 C42 H42 119.8 . . ?
O35 C34 O36 125.22(15) . . ?
O35 C34 C31 117.18(15) . . ?
O36 C34 C31 117.59(14) . . ?
N26 C37 C38 111.69(14) . . ?
N26 C37 H37A 109.3 . . ?
N26 C37 H37B 109.3 . . ?
C38 C37 H37A 109.3 . . ?
C38 C37 H37B 109.3 . . ?
H37A C37 H37B 107.9 . . ?
N52 C51 H51 117.1 . . ?
O50 C51 N52 125.8(2) . . ?
O50 C51 H51 117.1 . . ?
C40 C41 C44 121.70(15) . . ?
C40 C41 C42 119.27(15) . . ?
C42 C41 C44 119.03(15) . . ?
N26 C25 H25A 110.0 . . ?
N26 C25 H25B 110.0 . . ?
N26 C25 C24 108.28(14) . . ?
H25A C25 H25B 108.4 . . ?
C24 C25 H25A 110.0 . . ?
C24 C25 H25B 110.0 . . ?
C40 C39 C38 120.81(16) . . ?
C40 C39 H39 119.6 . . ?
C38 C39 H39 119.6 . . ?
C30 C31 C34 118.63(15) . . ?
C32 C31 C30 119.18(15) . . ?
C32 C31 C34 122.18(15) . . ?
C33 C28 C27 120.99(15) . . ?
C29 C28 C33 118.12(15) . . ?
C29 C28 C27 120.82(15) . . ?
N13 C24 C25 114.89(14) . . ?
N13 C24 H24A 108.5 . . ?
N13 C24 H24B 108.5 . . ?
C25 C24 H24A 108.5 . . ?
C25 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.48(16) . . ?
C17 C16 H16 119.8 . . ?
O22 C21 O23 128.19(15) . . ?
O22 C21 C18 116.51(15) . . ?
O23 C21 C18 115.29(15) . . ?
C30 C29 C28 120.89(16) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
N52 C53 H53A 109.5 . . ?
N52 C53 H53B 109.5 . . ?
N52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N52 C54 H54A 109.5 . . ?
N52 C54 H54B 109.5 . . ?
N52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N13 H13 O50 0.909(17) 1.91(2) 2.720(2) 147(3) 2_656
O47 H47A O35 0.848(17) 1.744(18) 2.5761(19) 167(3) 2_565
O47 H47B O46 0.848(17) 1.675(18) 2.5139(18) 170(3) 2_556
O48 H48A O45 0.843(18) 1.97(2) 2.7446(18) 153(3) 1_564
O48 H48B O36 0.841(18) 2.04(2) 2.8168(18) 154(3) .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni2 O5 C4 O3 0.6(3) . . . . ?
Ni2 O5 C4 C6 179.30(12) . . . . ?
Ni2 O23 C21 O22 4.8(3) . . . . ?
Ni2 O23 C21 C18 -174.06(12) . . . . ?
Ni1 O22 C21 O23 -9.1(3) . . . . ?
Ni1 O22 C21 C18 169.74(11) . . . . ?
Ni1 O45 C44 O46 21.1(2) 2_556 . . . ?
Ni1 O45 C44 C41 -159.35(11) 2_556 . . . ?
Ni1 O3 C4 O5 -12.3(3) . . . . ?
Ni1 O3 C4 C6 169.01(11) . . . . ?
Ni1 O36 C34 O35 -22.5(2) 2_565 . . . ?
Ni1 O36 C34 C31 158.76(11) 2_565 . . . ?
O5 C4 C6 C7 -18.7(2) . . . . ?
O5 C4 C6 C11 164.37(16) . . . . ?
O46 C44 C41 C40 175.62(16) . . . . ?
O46 C44 C41 C42 -4.5(2) . . . . ?
O35 C34 C31 C30 16.4(2) . . . . ?
O35 C34 C31 C32 -164.34(16) . . . . ?
O45 C44 C41 C40 -4.0(2) . . . . ?
O45 C44 C41 C42 175.92(15) . . . . ?
O3 C4 C6 C7 160.10(16) . . . . ?
O3 C4 C6 C11 -16.8(2) . . . . ?
O36 C34 C31 C30 -164.76(16) . . . . ?
O36 C34 C31 C32 14.5(2) . . . . ?
C7 C6 C11 C10 -2.2(2) . . . . ?
C4 C6 C11 C10 174.76(15) . . . . ?
N26 C27 C28 C33 96.7(2) . . . . ?
N26 C27 C28 C29 -86.5(2) . . . . ?
N26 C25 C24 N13 -141.48(14) . . . . ?
C14 N13 C24 C25 63.25(18) . . . . ?
C14 C15 C20 C19 177.66(15) . . . . ?
C14 C15 C16 C17 -177.10(15) . . . . ?
C9 C12 N13 C14 -177.95(13) . . . . ?
C9 C12 N13 C24 -49.24(19) . . . . ?
C6 C7 C8 C9 -1.9(3) . . . . ?
C6 C11 C10 C9 -2.8(2) . . . . ?
C12 C9 C8 C7 174.69(16) . . . . ?
C12 C9 C10 C11 -172.38(15) . . . . ?
C12 N13 C24 C25 -62.42(18) . . . . ?
C19 C18 C21 O22 1.9(2) 1_564 . . . ?
C19 C18 C21 O23 -179.09(16) 1_564 . . . ?
C33 C32 C31 C30 0.6(3) . . . . ?
C33 C32 C31 C34 -178.69(16) . . . . ?
C33 C28 C29 C30 0.5(3) . . . . ?
N13 C14 C15 C20 -100.93(18) . . . . ?
N13 C14 C15 C16 79.39(19) . . . . ?
C27 N26 C37 C38 69.84(18) . . . . ?
C27 N26 C25 C24 -68.46(17) . . . . ?
C27 C28 C29 C30 -176.33(17) . . . . ?
C43 C38 C37 N26 -162.57(15) . . . . ?
C43 C38 C39 C40 0.2(3) . . . . ?
C43 C42 C41 C40 1.0(3) . . . . ?
C43 C42 C41 C44 -178.84(16) . . . . ?
C15 C14 N13 C12 -178.15(13) . . . . ?
C15 C14 N13 C24 53.05(18) . . . . ?
C8 C7 C6 C4 -172.39(15) . . . . ?
C8 C7 C6 C11 4.5(3) . . . . ?
C8 C9 C12 N13 -75.7(2) . . . . ?
C8 C9 C10 C11 5.4(2) . . . . ?
C10 C9 C12 N13 102.09(18) . . . . ?
C10 C9 C8 C7 -3.1(3) . . . . ?
C18 C19 C20 C15 -0.5(3) 1_546 . . . ?
C18 C17 C16 C15 -0.6(3) 1_546 . . . ?
C17 C18 C21 O22 -176.42(15) 1_564 . . . ?
C17 C18 C21 O23 2.6(2) 1_564 . . . ?
C20 C15 C16 C17 3.2(3) . . . . ?
C38 C43 C42 C41 -1.2(3) . . . . ?
C32 C33 C28 C27 174.49(16) . . . . ?
C32 C33 C28 C29 -2.4(3) . . . . ?
C42 C43 C38 C37 -175.98(16) . . . . ?
C42 C43 C38 C39 0.6(3) . . . . ?
C37 N26 C27 C28 67.49(19) . . . . ?
C37 N26 C25 C24 156.96(14) . . . . ?
C37 C38 C39 C40 176.68(16) . . . . ?
C41 C40 C39 C38 -0.4(3) . . . . ?
C25 N26 C27 C28 -66.90(19) . . . . ?
C25 N26 C37 C38 -155.84(14) . . . . ?
C39 C40 C41 C44 179.64(15) . . . . ?
C39 C40 C41 C42 -0.2(3) . . . . ?
C39 C38 C37 N26 21.0(2) . . . . ?
C31 C30 C29 C28 1.8(3) . . . . ?
C28 C33 C32 C31 1.8(3) . . . . ?
C16 C15 C20 C19 -2.7(2) . . . . ?
C29 C30 C31 C32 -2.4(3) . . . . ?
C29 C30 C31 C34 176.91(17) . . . . ?
C53 N52 C51 O50 0.9(3) . . . . ?
C54 N52 C51 O50 -179.3(2) . . . . ?

_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_2
_database_code_depnum_ccdc_archive 'CCDC 1406629'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_audit_creation_date             2015-06-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H14 N O4 Zn, C3 H7 N O'
_chemical_formula_sum            'C20 H21 N2 O5 Zn'
_chemical_formula_weight         434.76
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 0.2920 1.4260 '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                   5.9540(12)
_cell_length_b                   13.521(3)
_cell_length_c                   13.942(3)
_cell_angle_alpha                95.02(3)
_cell_angle_beta                 94.33(3)
_cell_angle_gamma                99.72(3)
_cell_volume                     1097.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      1.473
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             450
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2155
_diffrn_reflns_av_unetI/netI     0.1260
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18152
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         1.473
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3087
_reflns_number_total             3987
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         2.031
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0835
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1356P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2199
_refine_special_details          
;
The material contains significant regions of diffuse electron density
corresponding to highly disordered lattice solvent; as such, the SQUEEZE 
routine was employed to provide accurate statistics for the refinement of the
framework atoms. Because of the uncertainty associated with solvation in
the freshly isolated crystal compared with bulk phase analysis, in which
solvent molecules are frequently observed to exchange with atmospheric water,
the crystallographic formula is presented for crystallographically located
framework atoms only, and as such, the values for density, F000 and absorption
coefficients do not include contributions from unmodelled solvent.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C33, C32}
{C25, C29}
3. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C32)
Uanis(C25) = Uanis(C29)
4. Others
 Fixed Sof: O24(0.5) C25(0.5) H25(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
 O31(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5) H33(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C23(H23A,H23B)
5.b Me refined with riding coordinates:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C15(H15), C16(H16), C18(H18), C19(H19),
 C25(H25), C33(H33)
;
_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
Zn1 Zn 1.27390(10) 1.05515(4) 0.50156(4) 0.0413(3) Uani 1 1 d . . . . .
O2 O 1.2438(6) 0.9493(3) 0.3939(3) 0.0461(9) Uani 1 1 d . . . . .
C3 C 1.2941(9) 0.8625(4) 0.3977(4) 0.0416(11) Uani 1 1 d . . . . .
O4 O 1.4608(6) 0.8443(3) 0.4520(3) 0.0489(9) Uani 1 1 d . . . . .
C5 C 1.1498(9) 0.7754(4) 0.3364(4) 0.0467(12) Uani 1 1 d . . . . .
C6 C 0.9394(10) 0.7847(5) 0.2925(4) 0.0488(12) Uani 1 1 d . . . . .
H6 H 0.8883 0.8476 0.2992 0.059 Uiso 1 1 calc R . . . .
C7 C 0.8025(9) 0.7022(5) 0.2387(4) 0.0492(12) Uani 1 1 d . . . . .
H7 H 0.6564 0.7087 0.2103 0.059 Uiso 1 1 calc R . . . .
C8 C 0.8758(9) 0.6106(4) 0.2260(4) 0.0462(12) Uani 1 1 d . . . . .
C9 C 1.0901(11) 0.6024(5) 0.2673(5) 0.0545(14) Uani 1 1 d . . . . .
H9 H 1.1447 0.5406 0.2573 0.065 Uiso 1 1 calc R . . . .
C10 C 1.2260(10) 0.6841(5) 0.3233(5) 0.0517(13) Uani 1 1 d . . . . .
H10 H 1.3712 0.6774 0.3526 0.062 Uiso 1 1 calc R . . . .
C11 C 0.7226(10) 0.5180(5) 0.1720(5) 0.0532(14) Uani 1 1 d . . . . .
H11A H 0.6584 0.4730 0.2193 0.064 Uiso 1 1 calc R . . . .
H11B H 0.5935 0.5392 0.1350 0.064 Uiso 1 1 calc R . . . .
N12 N 0.8449(8) 0.4629(3) 0.1065(3) 0.0435(10) Uani 1 1 d . . . . .
C13 C 0.7215(11) 0.3577(4) 0.0828(4) 0.0495(13) Uani 1 1 d . . . . .
H13A H 0.7717 0.3288 0.0220 0.059 Uiso 1 1 calc R . . . .
H13B H 0.5553 0.3578 0.0722 0.059 Uiso 1 1 calc R . . . .
C14 C 0.7645(9) 0.2927(4) 0.1620(4) 0.0461(12) Uani 1 1 d . . . . .
C15 C 0.9841(10) 0.3034(5) 0.2110(4) 0.0507(13) Uani 1 1 d . . . . .
H15 H 1.1053 0.3517 0.1934 0.061 Uiso 1 1 calc R . . . .
C16 C 1.0251(9) 0.2458(4) 0.2829(4) 0.0473(12) Uani 1 1 d . . . . .
H16 H 1.1731 0.2562 0.3167 0.057 Uiso 1 1 calc R . . . .
C17 C 0.8521(9) 0.1705(4) 0.3083(4) 0.0428(11) Uani 1 1 d . . . . .
C18 C 0.6357(9) 0.1597(4) 0.2610(4) 0.0456(12) Uani 1 1 d . . . . .
H18 H 0.5161 0.1099 0.2775 0.055 Uiso 1 1 calc R . . . .
C19 C 0.5921(9) 0.2204(4) 0.1901(4) 0.0448(12) Uani 1 1 d . . . . .
H19 H 0.4413 0.2129 0.1595 0.054 Uiso 1 1 calc R . . . .
C20 C 0.9009(9) 0.1068(4) 0.3849(4) 0.0428(11) Uani 1 1 d . . . . .
O21 O 1.0771(7) 0.1375(3) 0.4436(3) 0.0478(9) Uani 1 1 d . . . . .
O22 O 0.7681(6) 0.0218(3) 0.3868(3) 0.0437(8) Uani 1 1 d . . . . .
C23 C 0.8959(10) 0.5152(4) 0.0218(4) 0.0468(12) Uani 1 1 d . . . . .
H23A H 0.9251 0.5889 0.0403 0.056 Uiso 1 1 calc R . . . .
H23B H 0.7622 0.4989 -0.0271 0.056 Uiso 1 1 calc R . . . .
O24 O 0.5639(17) 0.8657(10) 0.0498(9) 0.082(3) Uani 0.5 1 d . . P A 2
C25 C 0.7146(15) 0.9313(8) 0.0983(7) 0.086(2) Uani 0.5 1 d . . P A 2
H25 H 0.6757 0.9862 0.1370 0.103 Uiso 0.5 1 calc R . P A 2
N26 N 0.9368(10) 0.9197(4) 0.0925(4) 0.0604(13) Uani 1 1 d . . . . .
C28 C 1.1175(14) 0.9915(6) 0.1458(6) 0.0715(19) Uani 1 1 d . . . . .
H28A H 1.2652 0.9723 0.1337 0.107 Uiso 1 1 calc R . . . .
H28B H 1.1132 1.0586 0.1250 0.107 Uiso 1 1 calc R . . . .
H28C H 1.0979 0.9927 0.2150 0.107 Uiso 1 1 calc R . . . .
C29 C 0.7146(15) 0.9313(8) 0.0983(7) 0.086(2) Uani 0.5 1 d . . P A 1
H29A H 0.7103 0.9950 0.1370 0.129 Uiso 0.5 1 calc R . P A 1
H29B H 0.6411 0.9323 0.0331 0.129 Uiso 0.5 1 calc R . P A 1
H29C H 0.6329 0.8751 0.1289 0.129 Uiso 0.5 1 calc R . P A 1
O31 O 0.817(2) 0.7711(9) 0.0014(9) 0.081(3) Uani 0.5 1 d . . P A 1
C32 C 0.9910(15) 0.8353(6) 0.0413(6) 0.0729(19) Uani 0.5 1 d . . P A 2
H32A H 1.1576 0.8402 0.0453 0.109 Uiso 0.5 1 calc R . P A 2
H32B H 0.9227 0.7744 0.0692 0.109 Uiso 0.5 1 calc R . P A 2
H32C H 0.9309 0.8317 -0.0265 0.109 Uiso 0.5 1 calc R . P A 2
C33 C 0.9910(15) 0.8353(6) 0.0413(6) 0.0729(19) Uani 0.5 1 d . . P A 1
H33 H 1.1442 0.8256 0.0363 0.087 Uiso 0.5 1 calc R . P 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
Zn1 O2 1.958(4) . ?
Zn1 O4 1.931(4) 2_876 ?
Zn1 O21 1.929(4) 1_565 ?
Zn1 O22 1.955(4) 2_766 ?
O2 C3 1.263(7) . ?
C3 O4 1.273(6) . ?
C3 C5 1.492(8) . ?
O4 Zn1 1.931(4) 2_876 ?
C5 C6 1.382(8) . ?
C5 C10 1.388(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(9) . ?
C8 C9 1.386(8) . ?
C8 C11 1.520(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.392(8) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 N12 1.443(8) . ?
N12 C13 1.483(7) . ?
N12 C23 1.454(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.504(7) . ?
C14 C15 1.407(8) . ?
C14 C19 1.397(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.354(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.409(8) . ?
C17 C18 1.381(8) . ?
C17 C20 1.471(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.376(8) . ?
C19 H19 0.9500 . ?
C20 O21 1.268(7) . ?
C20 O22 1.284(7) . ?
O21 Zn1 1.929(4) 1_545 ?
O22 Zn1 1.955(4) 2_766 ?
C23 C23 1.521(12) 2_765 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
O24 C25 1.258(14) . ?
C25 H25 0.9500 . ?
C25 N26 1.366(11) . ?
N26 C28 1.432(9) . ?
N26 C29 1.366(11) . ?
N26 C32 1.391(10) . ?
N26 C33 1.391(10) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O31 C33 1.289(14) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zn1 O2 128.06(18) 2_876 . ?
O4 Zn1 O22 101.72(17) 2_876 2_766 ?
O21 Zn1 O2 97.91(16) 1_565 . ?
O21 Zn1 O4 100.86(17) 1_565 2_876 ?
O21 Zn1 O22 129.23(17) 1_565 2_766 ?
O22 Zn1 O2 102.72(17) 2_766 . ?
C3 O2 Zn1 126.4(4) . . ?
O2 C3 O4 123.7(5) . . ?
O2 C3 C5 118.8(5) . . ?
O4 C3 C5 117.5(5) . . ?
C3 O4 Zn1 123.2(4) . 2_876 ?
C6 C5 C3 120.5(5) . . ?
C6 C5 C10 119.4(5) . . ?
C10 C5 C3 120.0(5) . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.1(6) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 121.0(5) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C9 118.9(5) . . ?
C7 C8 C11 121.6(5) . . ?
C9 C8 C11 119.5(5) . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.5(6) . . ?
C10 C9 H9 119.8 . . ?
C5 C10 C9 120.1(5) . . ?
C5 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C8 C11 H11A 109.2 . . ?
C8 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N12 C11 C8 112.1(5) . . ?
N12 C11 H11A 109.2 . . ?
N12 C11 H11B 109.2 . . ?
C11 N12 C13 110.3(5) . . ?
C11 N12 C23 112.1(5) . . ?
C23 N12 C13 113.5(4) . . ?
N12 C13 H13A 109.3 . . ?
N12 C13 H13B 109.3 . . ?
N12 C13 C14 111.8(4) . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
C15 C14 C13 120.2(5) . . ?
C19 C14 C13 122.2(5) . . ?
C19 C14 C15 117.5(5) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.9(5) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.2(5) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 C20 120.5(5) . . ?
C18 C17 C16 118.3(5) . . ?
C18 C17 C20 121.1(5) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 C17 120.5(5) . . ?
C19 C18 H18 119.7 . . ?
C14 C19 H19 119.2 . . ?
C18 C19 C14 121.5(5) . . ?
C18 C19 H19 119.2 . . ?
O21 C20 C17 118.0(5) . . ?
O21 C20 O22 123.4(5) . . ?
O22 C20 C17 118.6(5) . . ?
C20 O21 Zn1 126.6(3) . 1_545 ?
C20 O22 Zn1 126.7(3) . 2_766 ?
N12 C23 C23 111.1(5) . 2_765 ?
N12 C23 H23A 109.4 . . ?
N12 C23 H23B 109.4 . . ?
C23 C23 H23A 109.4 2_765 . ?
C23 C23 H23B 109.4 2_765 . ?
H23A C23 H23B 108.0 . . ?
O24 C25 H25 121.7 . . ?
O24 C25 N26 116.7(10) . . ?
N26 C25 H25 121.7 . . ?
C25 N26 C28 119.8(7) . . ?
C25 N26 C32 121.2(7) . . ?
C29 N26 C28 119.8(7) . . ?
C29 N26 C33 121.2(7) . . ?
C32 N26 C28 118.9(6) . . ?
C33 N26 C28 118.9(6) . . ?
N26 C28 H28A 109.5 . . ?
N26 C28 H28B 109.5 . . ?
N26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N26 C29 H29A 109.5 . . ?
N26 C29 H29B 109.5 . . ?
N26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N26 C32 H32A 109.5 . . ?
N26 C32 H32B 109.5 . . ?
N26 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N26 C33 H33 122.6 . . ?
O31 C33 N26 114.7(9) . . ?
O31 C33 H33 122.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O2 C3 O4 -35.0(8) . . . . ?
Zn1 O2 C3 C5 144.4(4) . . . . ?
O2 C3 O4 Zn1 -24.3(8) . . . 2_876 ?
O2 C3 C5 C6 -13.8(8) . . . . ?
O2 C3 C5 C10 166.5(6) . . . . ?
C3 C5 C6 C7 -177.4(5) . . . . ?
C3 C5 C10 C9 179.0(5) . . . . ?
O4 C3 C5 C6 165.6(5) . . . . ?
O4 C3 C5 C10 -14.1(8) . . . . ?
C5 C3 O4 Zn1 156.3(4) . . . 2_876 ?
C5 C6 C7 C8 -1.7(9) . . . . ?
C6 C5 C10 C9 -0.7(9) . . . . ?
C6 C7 C8 C9 -0.5(9) . . . . ?
C6 C7 C8 C11 176.5(5) . . . . ?
C7 C8 C9 C10 2.1(9) . . . . ?
C7 C8 C11 N12 136.7(6) . . . . ?
C8 C9 C10 C5 -1.5(10) . . . . ?
C8 C11 N12 C13 159.6(5) . . . . ?
C8 C11 N12 C23 -72.8(6) . . . . ?
C9 C8 C11 N12 -46.3(8) . . . . ?
C10 C5 C6 C7 2.3(9) . . . . ?
C11 C8 C9 C10 -175.0(6) . . . . ?
C11 N12 C13 C14 -79.4(6) . . . . ?
C11 N12 C23 C23 154.8(6) . . . 2_765 ?
N12 C13 C14 C15 -39.6(8) . . . . ?
N12 C13 C14 C19 140.4(6) . . . . ?
C13 N12 C23 C23 -79.4(7) . . . 2_765 ?
C13 C14 C15 C16 179.7(6) . . . . ?
C13 C14 C19 C18 178.2(6) . . . . ?
C14 C15 C16 C17 2.6(10) . . . . ?
C15 C14 C19 C18 -1.8(9) . . . . ?
C15 C16 C17 C18 -2.8(9) . . . . ?
C15 C16 C17 C20 178.4(6) . . . . ?
C16 C17 C18 C19 0.7(9) . . . . ?
C16 C17 C20 O21 18.5(8) . . . . ?
C16 C17 C20 O22 -159.2(5) . . . . ?
C17 C18 C19 C14 1.6(9) . . . . ?
C17 C20 O21 Zn1 -144.9(4) . . . 1_545 ?
C17 C20 O22 Zn1 -158.0(4) . . . 2_766 ?
C18 C17 C20 O21 -160.2(5) . . . . ?
C18 C17 C20 O22 22.1(8) . . . . ?
C19 C14 C15 C16 -0.3(9) . . . . ?
C20 C17 C18 C19 179.5(5) . . . . ?
O21 C20 O22 Zn1 24.4(8) . . . 2_766 ?
O22 C20 O21 Zn1 32.7(8) . . . 1_545 ?
C23 N12 C13 C14 153.9(5) . . . . ?
O24 C25 N26 C28 -180.0(10) . . . . ?
O24 C25 N26 C32 -4.8(13) . . . . ?
C28 N26 C33 O31 175.2(8) . . . . ?
C29 N26 C33 O31 0.0(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_RINTA01_2                   
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Crystals were of extremely poor quality and suffered beam damage
from synchrotron radiation. Complete dataset was obtained by merging data
from three partial collections.
;
_vrf_PLAT020_2                   
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.215 Report
RESPONSE: As above
;
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1406630'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_audit_creation_date             2015-03-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H52 N2 O12 S4 Zn2'
_chemical_formula_sum            'C42 H52 N2 O12 S4 Zn2'
_chemical_formula_weight         1035.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2920 1.4260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.437(3)
_cell_length_b                   15.586(3)
_cell_length_c                   30.335(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.86(3)
_cell_angle_gamma                90
_cell_volume                     5880(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.845
_cell_measurement_theta_min      1.469
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35387
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        22.800
_diffrn_reflns_theta_max         22.845
_diffrn_reflns_theta_min         1.469
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5655
_reflns_number_total             7986
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         7986
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0842
_refine_ls_restrained_S_all      1.047
_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)+(0.1372P)²+10.8942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2305
_refine_ls_wR_factor_ref         0.2541
_refine_special_details          
;
The material contains significant regions of diffuse electron density
corresponding to highly disordered lattice solvent; as such, the SQUEEZE 
routine was employed to provide accurate statistics for the refinement of the
framework atoms. Because of the uncertainty associated with solvation in
the freshly isolated crystal compared with bulk phase analysis, in which
solvent molecules are frequently observed to exchange with atmospheric water,
the crystallographic formula is presented for crystallographically located
framework atoms only, and as such, the values for density, F000 and absorption
coefficients do not include contributions from unmodelled solvent.
The structure model appears to contain additional non-crystallographic symmetry 
from an orthorhombic cell (beta = 90.83 degrees), although we were unable to 
index a higher symmetry unit cell, nor could any twin law be determined. 
No distance or Uij restraints were necessary to retain sensible
chemical structures for the framework atoms. Each of the four DMSO ligands
displayed disorder over at least two positions, and so DFIX restraints were used
to retain sensible chemical structures. ISOR and RIGU restraints were used in some
cases on the disordered DMSO species to prevent the emergence of non-positive
definite Uij tensors.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All C(H,H,H,H,H,H,H,H,H)
  groups
2. Restrained distances
 S62-C65
 1.75 with sigma of 0.02
 C66-S63
 1.75 with sigma of 0.02
 C64-S63
 1.75 with sigma of 0.02
 S62-C64
 1.75 with sigma of 0.02
 S69-C70
 1.75 with sigma of 0.02
 S68-C70
 1.75 with sigma of 0.02
 S69-C71
 1.75 with sigma of 0.02
 S68-C71
 1.75 with sigma of 0.02
 S56-C57
 1.75 with sigma of 0.02
 S55-C57
 1.75 with sigma of 0.02
 S54-C57
 1.75 with sigma of 0.02
 C58-S56
 1.75 with sigma of 0.02
 S55-C59
 1.75 with sigma of 0.02
 C60-S54
 1.75 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S63, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S62, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: S48(0.5) H49A(0.5) H49B(0.5) H49C(0.5) H49D(0.5) H49E(0.5)
 H49F(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) S51(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) S54(0.33333) S55(0.33333) S56(0.33333) H57G(0.33333)
 H57H(0.33333) H57I(0.33333) H57A(0.33333) H57B(0.33333) H57C(0.33333)
 H57D(0.33333) H57E(0.33333) H57F(0.33333) C58(0.33333) H58A(0.33333)
 H58B(0.33333) H58C(0.33333) C59(0.33333) H59A(0.33333) H59B(0.33333)
 H59C(0.33333) C60(0.33333) H60A(0.33333) H60B(0.33333) H60C(0.33333) S62(0.5)
 S63(0.5) H64D(0.5) H64E(0.5) H64F(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C65(0.5)
 H65A(0.5) H65B(0.5) H65C(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) S68(0.5)
 S69(0.5) H70A(0.5) H70B(0.5) H70C(0.5) H70D(0.5) H70E(0.5) H70F(0.5) H71A(0.5)
 H71B(0.5) H71C(0.5) H71D(0.5) H71E(0.5) H71F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C24(H24A,H24B), C34(H34A,H34B), C36(H36A,
 H36B), C46(H46A,H46B)
6.b Me refined with riding coordinates:
 C49(H49A,H49B,H49C), C49(H49D,H49E,H49F), C57(H57G,H57H,H57I), C57(H57A,H57B,
 H57C), C57(H57D,H57E,H57F), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C64(H64D,H64E,H64F), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C),
 C70(H70D,H70E,H70F), C71(H71A,H71B,H71C), C71(H71D,H71E,H71F)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C16(H16), C17(H17), C19(H19), C20(H20),
 C29(H29), C30(H30), C32(H32), C33(H33), C38(H38), C39(H39), C41(H41), C42(H42)
6.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C)
;
_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
Zn1 Zn 0.76480(7) 0.99948(6) 0.29258(3) 0.0829(3) Uani 1 1 d . . . . .
Zn2 Zn 0.74569(8) 0.80992(6) -0.26536(3) 0.0957(4) Uani 1 1 d . . . . .
O3 O 0.7953(4) 0.9728(5) 0.22897(18) 0.1105(19) Uani 1 1 d . . . . .
C4 C 0.6984(6) 0.9613(5) 0.2160(3) 0.083(2) Uani 1 1 d . . . . .
O5 O 0.6244(4) 0.9671(4) 0.24203(17) 0.1009(16) Uani 1 1 d . . . . .
C6 C 0.6797(5) 0.9386(5) 0.1691(2) 0.085(2) Uani 1 1 d . . . . .
C7 C 0.7583(7) 0.9335(7) 0.1404(3) 0.115(3) Uani 1 1 d . . . . .
H7 H 0.8288 0.9494 0.1497 0.137 Uiso 1 1 calc R . . . .
C8 C 0.7430(7) 0.9067(7) 0.0981(3) 0.117(3) Uani 1 1 d . . . . .
H8 H 0.8029 0.9030 0.0791 0.140 Uiso 1 1 calc R . . . .
C9 C 0.6407(7) 0.8843(7) 0.0820(3) 0.120(3) Uani 1 1 d . . . . .
C10 C 0.5566(7) 0.8933(9) 0.1115(3) 0.153(5) Uani 1 1 d . . . . .
H10 H 0.4851 0.8801 0.1024 0.184 Uiso 1 1 calc R . . . .
C11 C 0.5770(7) 0.9215(7) 0.1539(3) 0.119(3) Uani 1 1 d . . . . .
H11 H 0.5184 0.9294 0.1732 0.143 Uiso 1 1 calc R . . . .
C12 C 0.6148(11) 0.8474(10) 0.0360(3) 0.164(6) Uani 1 1 d . . . . .
H12A H 0.6774 0.8564 0.0167 0.197 Uiso 1 1 calc R . . . .
H12B H 0.6027 0.7849 0.0386 0.197 Uiso 1 1 calc R . . . .
N13 N 0.5210(7) 0.8868(7) 0.0160(3) 0.131(3) Uani 1 1 d . . . . .
C14 C 0.4671(10) 0.8338(9) -0.0165(3) 0.147(5) Uani 1 1 d . . . . .
H14A H 0.3961 0.8597 -0.0232 0.177 Uiso 1 1 calc R . . . .
H14B H 0.4539 0.7769 -0.0031 0.177 Uiso 1 1 calc R . . . .
C15 C 0.5241(11) 0.8199(10) -0.0595(4) 0.137(5) Uani 1 1 d . . . . .
C16 C 0.6068(12) 0.7605(9) -0.0634(4) 0.139(4) Uani 1 1 d . . . . .
H16 H 0.6283 0.7284 -0.0381 0.167 Uiso 1 1 calc R . . . .
C17 C 0.6602(10) 0.7460(7) -0.1036(3) 0.138(4) Uani 1 1 d . . . . .
H17 H 0.7153 0.7041 -0.1058 0.166 Uiso 1 1 calc R . . . .
C18 C 0.6295(10) 0.7945(7) -0.1392(3) 0.115(3) Uani 1 1 d . . . . .
C19 C 0.5516(9) 0.8536(8) -0.1352(3) 0.119(3) Uani 1 1 d . . . . .
H19 H 0.5334 0.8877 -0.1602 0.143 Uiso 1 1 calc R . . . .
C20 C 0.4951(8) 0.8675(8) -0.0956(3) 0.127(4) Uani 1 1 d . . . . .
H20 H 0.4388 0.9086 -0.0942 0.152 Uiso 1 1 calc R . . . .
C21 C 0.6885(10) 0.7788(8) -0.1821(4) 0.116(3) Uani 1 1 d . . . . .
O22 O 0.6697(6) 0.8350(4) -0.2117(2) 0.123(2) Uani 1 1 d . . . . .
O23 O 0.7461(7) 0.7173(5) -0.1878(2) 0.129(2) Uani 1 1 d . . . . .
C24 C 0.5481(7) 0.9724(8) 0.0020(3) 0.129(4) Uani 1 1 d . . . . .
H24A H 0.5841 0.9696 -0.0268 0.154 Uiso 1 1 calc R . . . .
H24B H 0.5991 0.9980 0.0236 0.154 Uiso 1 1 calc R . . . .
O25 O 0.6887(4) 0.9598(3) 0.34543(16) 0.0830(13) Uani 1 1 d . . . . .
C26 C 0.7138(6) 0.8803(5) 0.3456(2) 0.0783(19) Uani 1 1 d . . . . .
O27 O 0.7714(5) 0.8470(3) 0.31735(17) 0.0924(15) Uani 1 1 d . . . . .
C28 C 0.6674(6) 0.8254(4) 0.3820(2) 0.0778(18) Uani 1 1 d . . . . .
C29 C 0.7003(6) 0.7420(5) 0.3883(2) 0.0803(19) Uani 1 1 d . . . . .
H29 H 0.7557 0.7190 0.3706 0.096 Uiso 1 1 calc R . . . .
C30 C 0.6540(7) 0.6916(4) 0.4198(2) 0.085(2) Uani 1 1 d . . . . .
H30 H 0.6785 0.6344 0.4241 0.102 Uiso 1 1 calc R . . . .
C31 C 0.5717(7) 0.7233(4) 0.4457(2) 0.090(2) Uani 1 1 d . . . . .
C32 C 0.5403(8) 0.8067(5) 0.4398(3) 0.107(3) Uani 1 1 d . . . . .
H32 H 0.4842 0.8294 0.4573 0.129 Uiso 1 1 calc R . . . .
C33 C 0.5885(7) 0.8579(5) 0.4093(3) 0.093(2) Uani 1 1 d . . . . .
H33 H 0.5678 0.9164 0.4067 0.111 Uiso 1 1 calc R . . . .
C34 C 0.5193(10) 0.6664(5) 0.4802(3) 0.120(4) Uani 1 1 d . . . . .
H34A H 0.5732 0.6504 0.5032 0.144 Uiso 1 1 calc R . . . .
H34B H 0.4604 0.6980 0.4946 0.144 Uiso 1 1 calc R . . . .
N35 N 0.4763(6) 0.5883(4) 0.45883(19) 0.0892(19) Uani 1 1 d . . . . .
C36 C 0.3862(7) 0.6054(6) 0.4300(3) 0.098(2) Uani 1 1 d . . . . .
H36A H 0.4015 0.6570 0.4121 0.117 Uiso 1 1 calc R . . . .
H36B H 0.3220 0.6175 0.4479 0.117 Uiso 1 1 calc R . . . .
C37 C 0.3629(6) 0.5308(6) 0.3999(2) 0.088(2) Uani 1 1 d . . . . .
C38 C 0.2611(7) 0.5036(8) 0.3895(3) 0.112(3) Uani 1 1 d . . . . .
H38 H 0.2012 0.5322 0.4018 0.135 Uiso 1 1 calc R . . . .
C39 C 0.2440(8) 0.4333(9) 0.3607(4) 0.128(4) Uani 1 1 d . . . . .
H39 H 0.1726 0.4143 0.3549 0.154 Uiso 1 1 calc R . . . .
C40 C 0.3247(7) 0.3938(7) 0.3419(3) 0.107(3) Uani 1 1 d . . . . .
C41 C 0.4262(8) 0.4200(8) 0.3524(3) 0.137(4) Uani 1 1 d . . . . .
H41 H 0.4856 0.3918 0.3394 0.165 Uiso 1 1 calc R . . . .
C42 C 0.4450(7) 0.4860(7) 0.3814(4) 0.136(4) Uani 1 1 d . . . . .
H42 H 0.5171 0.5010 0.3888 0.163 Uiso 1 1 calc R . . . .
C43 C 0.3185(7) 0.3072(7) 0.3095(3) 0.097(3) Uani 1 1 d . . . . .
O44 O 0.3939(8) 0.2760(6) 0.2958(3) 0.162(3) Uani 1 1 d . . . . .
O45 O 0.2194(7) 0.2938(5) 0.3021(3) 0.146(3) Uani 1 1 d . . . . .
C46 C 0.4513(7) 0.5232(4) 0.4927(2) 0.087(2) Uani 1 1 d . . . . .
H46A H 0.4186 0.5518 0.5184 0.104 Uiso 1 1 calc R . . . .
H46B H 0.3984 0.4818 0.4805 0.104 Uiso 1 1 calc R . . . .
O47 O 0.9122(5) 1.0265(5) 0.3157(2) 0.128(2) Uani 1 1 d . . . . .
S48 S 0.9984(5) 0.9305(4) 0.3157(3) 0.136(2) Uani 0.5 1 d . . P A 2
C49 C 1.0432(13) 0.9393(10) 0.2703(5) 0.189(6) Uani 1 1 d . . . . .
H49A H 1.1177 0.9190 0.2694 0.283 Uiso 0.5 1 calc R . P A 1
H49B H 0.9944 0.8900 0.2704 0.283 Uiso 0.5 1 calc R . P A 1
H49C H 1.0279 0.9749 0.2443 0.283 Uiso 0.5 1 calc R . P A 1
H49D H 0.9893 0.9208 0.2485 0.283 Uiso 0.5 1 calc R . P A 2
H49E H 1.0621 0.9994 0.2649 0.283 Uiso 0.5 1 calc R . P A 2
H49F H 1.1077 0.9035 0.2679 0.283 Uiso 0.5 1 calc R . P A 2
C50 C 1.1086(19) 0.9671(18) 0.3476(8) 0.161(11) Uani 0.5 1 d . . P A 2
H50A H 1.1221 1.0277 0.3410 0.242 Uiso 0.5 1 calc GR . P A 2
H50B H 1.1725 0.9332 0.3406 0.242 Uiso 0.5 1 calc GR . P A 2
H50C H 1.0926 0.9609 0.3790 0.242 Uiso 0.5 1 calc GR . P A 2
S51 S 1.0232(3) 1.0052(3) 0.32211(17) 0.0977(13) Uani 0.5 1 d . . P A 1
C52 C 1.012(2) 0.9319(18) 0.3658(9) 0.162(10) Uani 0.5 1 d . . P A 1
H52A H 0.9649 0.9557 0.3883 0.243 Uiso 0.5 1 calc GR . P A 1
H52B H 1.0835 0.9211 0.3788 0.243 Uiso 0.5 1 calc GR . P A 1
H52C H 0.9818 0.8779 0.3547 0.243 Uiso 0.5 1 calc GR . P A 1
O53 O 0.7221(7) 1.1223(4) 0.2929(2) 0.123(2) Uani 1 1 d . U . . .
S54 S 0.7101(6) 1.1842(5) 0.2596(3) 0.109(2) Uani 0.3333 1 d D . P B 1
S55 S 0.6335(13) 1.1507(12) 0.2902(4) 0.085(5) Uani 0.3333 1 d D . P B 2
S56 S 0.6010(13) 1.1541(10) 0.2916(5) 0.079(4) Uani 0.3333 1 d D . P B 3
C57 C 0.5912(7) 1.1873(8) 0.2357(4) 0.159(5) Uani 1 1 d D . . . .
H57G H 0.5186 1.2093 0.2296 0.239 Uiso 0.3333 1 calc R . P B 3
H57H H 0.6440 1.2326 0.2303 0.239 Uiso 0.3333 1 calc R . P B 3
H57I H 0.6054 1.1383 0.2164 0.239 Uiso 0.3333 1 calc R . P B 3
H57A H 0.5901 1.2321 0.2131 0.239 Uiso 0.3333 1 calc R . P B 1
H57B H 0.5755 1.1316 0.2221 0.239 Uiso 0.3333 1 calc R . P B 1
H57C H 0.5367 1.2000 0.2578 0.239 Uiso 0.3333 1 calc R . P B 1
H57D H 0.5175 1.2094 0.2370 0.239 Uiso 0.3333 1 calc R . P B 2
H57E H 0.6394 1.2329 0.2259 0.239 Uiso 0.3333 1 calc R . P B 2
H57F H 0.5938 1.1392 0.2149 0.239 Uiso 0.3333 1 calc R . P B 2
C58 C 0.613(3) 1.241(2) 0.3278(12) 0.142(12) Uani 0.3333 1 d D U P B 3
H58A H 0.5427 1.2688 0.3308 0.213 Uiso 0.3333 1 calc R . P B 3
H58B H 0.6380 1.2205 0.3567 0.213 Uiso 0.3333 1 calc R . P B 3
H58C H 0.6647 1.2823 0.3162 0.213 Uiso 0.3333 1 calc R . P B 3
C59 C 0.663(4) 1.2570(18) 0.3010(15) 0.133(16) Uani 0.3333 1 d D U P B 2
H59A H 0.5971 1.2909 0.3000 0.199 Uiso 0.3333 1 calc R . P B 2
H59B H 0.6970 1.2618 0.3303 0.199 Uiso 0.3333 1 calc R . P B 2
H59C H 0.7131 1.2785 0.2787 0.199 Uiso 0.3333 1 calc R . P B 2
C60 C 0.673(3) 1.2812(15) 0.2847(11) 0.101(10) Uani 0.3333 1 d D U P B 1
H60A H 0.6644 1.3257 0.2621 0.151 Uiso 0.3333 1 calc R . P B 1
H60B H 0.6053 1.2734 0.3002 0.151 Uiso 0.3333 1 calc R . P B 1
H60C H 0.7295 1.2986 0.3058 0.151 Uiso 0.3333 1 calc R . P B 1
O61 O 0.8940(5) 0.8466(5) -0.2536(3) 0.131(2) Uani 1 1 d . . . . .
S62 S 0.9649(4) 0.7734(3) -0.2319(2) 0.0983(13) Uani 0.5 1 d D U P C 2
S63 S 1.0161(6) 0.8351(5) -0.2503(3) 0.166(3) Uani 0.5 1 d D U P C 1
C64 C 1.0500(14) 0.7455(12) -0.2746(7) 0.349(18) Uani 1 1 d D . . . .
H64D H 1.0986 0.6997 -0.2647 0.523 Uiso 0.5 1 calc R . P C 2
H64E H 1.0071 0.7254 -0.3000 0.523 Uiso 0.5 1 calc R . P C 2
H64F H 1.0922 0.7957 -0.2833 0.523 Uiso 0.5 1 calc R . P C 2
H64A H 1.1282 0.7381 -0.2726 0.523 Uiso 0.5 1 calc R . P C 1
H64B H 1.0146 0.6972 -0.2601 0.523 Uiso 0.5 1 calc R . P C 1
H64C H 1.0275 0.7476 -0.3057 0.523 Uiso 0.5 1 calc R . P C 1
C65 C 1.044(3) 0.8522(15) -0.2016(8) 0.212(17) Uani 0.5 1 d D U P C 2
H65A H 1.1192 0.8496 -0.2113 0.318 Uiso 0.5 1 calc GR . P C 2
H65B H 1.0416 0.8397 -0.1700 0.318 Uiso 0.5 1 calc GR . P C 2
H65C H 1.0154 0.9097 -0.2073 0.318 Uiso 0.5 1 calc GR . P C 2
C66 C 0.9750(12) 0.8072(12) -0.1993(6) 0.108(5) Uani 0.5 1 d D U P C 1
H66A H 0.9474 0.7483 -0.1999 0.162 Uiso 0.5 1 calc GR . P C 1
H66B H 0.9179 0.8464 -0.1900 0.162 Uiso 0.5 1 calc GR . P C 1
H66C H 1.0358 0.8109 -0.1785 0.162 Uiso 0.5 1 calc GR . P C 1
O67 O 0.6976(6) 0.9065(5) -0.3034(3) 0.153(3) Uani 1 1 d . . . . .
S68 S 0.7004(3) 0.9907(3) -0.30752(14) 0.0910(11) Uani 0.5 1 d D . P D 2
S69 S 0.6046(3) 0.9564(3) -0.28837(14) 0.0882(11) Uani 0.5 1 d D . P D 1
C70 C 0.5893(10) 1.0306(9) -0.3367(4) 0.185(6) Uani 1 1 d D . . . .
H70A H 0.5288 1.0695 -0.3319 0.278 Uiso 0.5 1 calc R . P D 1
H70B H 0.6554 1.0640 -0.3400 0.278 Uiso 0.5 1 calc R . P D 1
H70C H 0.5758 0.9969 -0.3635 0.278 Uiso 0.5 1 calc R . P D 1
H70D H 0.5949 1.0931 -0.3389 0.278 Uiso 0.5 1 calc R . P D 2
H70E H 0.5873 1.0056 -0.3663 0.278 Uiso 0.5 1 calc R . P D 2
H70F H 0.5234 1.0154 -0.3212 0.278 Uiso 0.5 1 calc R . P D 2
C71 C 0.6435(9) 1.0330(7) -0.2551(3) 0.143(4) Uani 1 1 d D . . . .
H71A H 0.5807 1.0656 -0.2454 0.214 Uiso 0.5 1 calc R . P D 1
H71B H 0.6804 1.0081 -0.2294 0.214 Uiso 0.5 1 calc R . P D 1
H71C H 0.6927 1.0714 -0.2705 0.214 Uiso 0.5 1 calc R . P D 1
H71D H 0.6432 1.0959 -0.2559 0.214 Uiso 0.5 1 calc R . P D 2
H71E H 0.5698 1.0120 -0.2519 0.214 Uiso 0.5 1 calc R . P D 2
H71F H 0.6877 1.0134 -0.2301 0.214 Uiso 0.5 1 calc R . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 2.015(6) . ?
Zn1 C4 2.526(7) . ?
Zn1 O5 2.361(5) . ?
Zn1 O25 1.973(5) . ?
Zn1 C26 2.544(7) . ?
Zn1 O47 1.998(6) . ?
Zn1 O53 1.986(7) . ?
Zn2 O22 1.934(6) . ?
Zn2 C43 2.393(9) 3_665 ?
Zn2 O44 2.368(8) 3_665 ?
Zn2 O45 2.015(9) 3_665 ?
Zn2 O61 1.958(7) . ?
Zn2 O67 1.984(7) . ?
O3 C4 1.276(8) . ?
C4 O5 1.226(9) . ?
C4 C6 1.479(11) . ?
C6 C7 1.322(11) . ?
C6 C11 1.378(10) . ?
C7 H7 0.9500 . ?
C7 C8 1.360(12) . ?
C8 H8 0.9500 . ?
C8 C9 1.399(12) . ?
C9 C10 1.393(12) . ?
C9 C12 1.539(13) . ?
C10 H10 0.9500 . ?
C10 C11 1.380(12) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 N13 1.445(17) . ?
N13 C14 1.443(12) . ?
N13 C24 1.441(15) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.508(15) . ?
C15 C16 1.390(17) . ?
C15 C20 1.368(16) . ?
C16 H16 0.9500 . ?
C16 C17 1.416(15) . ?
C17 H17 0.9500 . ?
C17 C18 1.367(15) . ?
C18 C19 1.344(15) . ?
C18 C21 1.524(14) . ?
C19 H19 0.9500 . ?
C19 C20 1.419(13) . ?
C20 H20 0.9500 . ?
C21 O22 1.274(13) . ?
C21 O23 1.210(13) . ?
C24 C24 1.48(2) 3_675 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
O25 C26 1.279(9) . ?
C26 O27 1.239(9) . ?
C26 C28 1.518(10) . ?
C28 C29 1.375(10) . ?
C28 C33 1.389(10) . ?
C29 H29 0.9500 . ?
C29 C30 1.371(10) . ?
C30 H30 0.9500 . ?
C30 C31 1.390(11) . ?
C31 C32 1.367(10) . ?
C31 C34 1.527(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.368(10) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 N35 1.476(10) . ?
N35 C36 1.435(11) . ?
N35 C46 1.481(8) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.505(12) . ?
C37 C38 1.366(12) . ?
C37 C42 1.364(11) . ?
C38 H38 0.9500 . ?
C38 C39 1.415(14) . ?
C39 H39 0.9500 . ?
C39 C40 1.316(14) . ?
C40 C41 1.360(12) . ?
C40 C43 1.671(14) . ?
C41 H41 0.9500 . ?
C41 C42 1.371(12) . ?
C42 H42 0.9500 . ?
C43 Zn2 2.394(9) 3_665 ?
C43 O44 1.141(12) . ?
C43 O45 1.267(10) . ?
O44 Zn2 2.368(8) 3_665 ?
O45 Zn2 2.015(9) 3_665 ?
C46 C46 1.473(16) 3_666 ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
O47 S48 1.839(10) . ?
O47 S51 1.431(7) . ?
S48 C49 1.500(17) . ?
S48 C50 1.76(2) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C49 H49D 0.9800 . ?
C49 H49E 0.9800 . ?
C49 H49F 0.9800 . ?
C49 S51 1.896(14) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
S51 C52 1.76(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
O53 S54 1.404(9) . ?
O53 S55 1.189(18) . ?
O53 S56 1.585(16) . ?
S54 C57 1.638(10) . ?
S54 C60 1.757(18) . ?
S55 C57 1.817(14) . ?
S55 C59 1.728(19) . ?
S56 C57 1.773(15) . ?
S56 C58 1.749(18) . ?
C57 H57G 0.9800 . ?
C57 H57H 0.9800 . ?
C57 H57I 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C57 H57D 0.9800 . ?
C57 H57E 0.9800 . ?
C57 H57F 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
O61 S62 1.579(8) . ?
O61 S63 1.532(9) . ?
S62 C64 1.741(16) . ?
S62 C65 1.817(16) . ?
S63 C64 1.637(13) . ?
S63 C66 1.695(16) . ?
C64 H64D 0.9800 . ?
C64 H64E 0.9800 . ?
C64 H64F 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
O67 S68 1.319(8) . ?
O67 S69 1.472(7) . ?
S68 C70 1.744(10) . ?
S68 C71 1.871(10) . ?
S69 C70 1.874(12) . ?
S69 C71 1.632(10) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C70 H70D 0.9800 . ?
C70 H70E 0.9800 . ?
C70 H70F 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C71 H71D 0.9800 . ?
C71 H71E 0.9800 . ?
C71 H71F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 C4 30.0(2) . . ?
O3 Zn1 O5 58.8(2) . . ?
O3 Zn1 C26 120.5(3) . . ?
C4 Zn1 C26 109.2(3) . . ?
O5 Zn1 C4 28.8(2) . . ?
O5 Zn1 C26 93.8(2) . . ?
O25 Zn1 O3 144.4(2) . . ?
O25 Zn1 C4 121.3(2) . . ?
O25 Zn1 O5 95.8(2) . . ?
O25 Zn1 C26 29.6(2) . . ?
O25 Zn1 O47 103.3(2) . . ?
O25 Zn1 O53 99.5(3) . . ?
O47 Zn1 O3 101.2(2) . . ?
O47 Zn1 C4 131.2(3) . . ?
O47 Zn1 O5 159.9(2) . . ?
O47 Zn1 C26 99.6(3) . . ?
O53 Zn1 O3 104.9(3) . . ?
O53 Zn1 C4 98.5(3) . . ?
O53 Zn1 O5 90.8(3) . . ?
O53 Zn1 C26 129.1(3) . . ?
O53 Zn1 O47 92.3(3) . . ?
O22 Zn2 C43 117.5(3) . 3_665 ?
O22 Zn2 O44 94.5(3) . 3_665 ?
O22 Zn2 O45 137.7(3) . 3_665 ?
O22 Zn2 O61 104.9(3) . . ?
O22 Zn2 O67 100.9(3) . . ?
O44 Zn2 C43 27.7(3) 3_665 3_665 ?
O45 Zn2 C43 32.0(3) 3_665 3_665 ?
O45 Zn2 O44 59.6(3) 3_665 3_665 ?
O61 Zn2 C43 129.0(3) . 3_665 ?
O61 Zn2 O44 156.8(3) . 3_665 ?
O61 Zn2 O45 97.2(3) . 3_665 ?
O61 Zn2 O67 99.2(3) . . ?
O67 Zn2 C43 99.1(4) . 3_665 ?
O67 Zn2 O44 89.4(4) . 3_665 ?
O67 Zn2 O45 110.7(3) . 3_665 ?
C4 O3 Zn1 97.7(5) . . ?
O3 C4 Zn1 52.2(4) . . ?
O3 C4 C6 117.7(7) . . ?
O5 C4 Zn1 68.1(4) . . ?
O5 C4 O3 120.3(7) . . ?
O5 C4 C6 122.0(7) . . ?
C6 C4 Zn1 169.9(6) . . ?
C4 O5 Zn1 83.1(4) . . ?
C7 C6 C4 122.8(7) . . ?
C7 C6 C11 117.3(8) . . ?
C11 C6 C4 119.9(7) . . ?
C6 C7 H7 118.4 . . ?
C6 C7 C8 123.1(8) . . ?
C8 C7 H7 118.4 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.2(7) . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C12 125.7(8) . . ?
C10 C9 C8 116.1(8) . . ?
C10 C9 C12 118.1(9) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0(8) . . ?
C11 C10 H10 120.0 . . ?
C6 C11 C10 122.0(8) . . ?
C6 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C9 C12 H12A 109.1 . . ?
C9 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
N13 C12 C9 112.3(11) . . ?
N13 C12 H12A 109.1 . . ?
N13 C12 H12B 109.1 . . ?
C14 N13 C12 114.1(12) . . ?
C24 N13 C12 109.0(8) . . ?
C24 N13 C14 116.0(9) . . ?
N13 C14 H14A 108.1 . . ?
N13 C14 H14B 108.1 . . ?
N13 C14 C15 116.9(8) . . ?
H14A C14 H14B 107.3 . . ?
C15 C14 H14A 108.1 . . ?
C15 C14 H14B 108.1 . . ?
C16 C15 C14 121.8(13) . . ?
C20 C15 C14 119.5(15) . . ?
C20 C15 C16 118.7(11) . . ?
C15 C16 H16 118.8 . . ?
C15 C16 C17 122.5(13) . . ?
C17 C16 H16 118.8 . . ?
C16 C17 H17 121.2 . . ?
C18 C17 C16 117.6(13) . . ?
C18 C17 H17 121.2 . . ?
C17 C18 C21 117.0(13) . . ?
C19 C18 C17 120.1(10) . . ?
C19 C18 C21 122.9(11) . . ?
C18 C19 H19 118.4 . . ?
C18 C19 C20 123.2(11) . . ?
C20 C19 H19 118.4 . . ?
C15 C20 C19 117.9(13) . . ?
C15 C20 H20 121.1 . . ?
C19 C20 H20 121.1 . . ?
O22 C21 C18 114.0(12) . . ?
O23 C21 C18 122.8(12) . . ?
O23 C21 O22 123.2(10) . . ?
C21 O22 Zn2 111.5(7) . . ?
N13 C24 C24 111.8(10) . 3_675 ?
N13 C24 H24A 109.3 . . ?
N13 C24 H24B 109.3 . . ?
C24 C24 H24A 109.3 3_675 . ?
C24 C24 H24B 109.3 3_675 . ?
H24A C24 H24B 107.9 . . ?
C26 O25 Zn1 100.7(4) . . ?
O25 C26 Zn1 49.7(3) . . ?
O25 C26 C28 117.0(7) . . ?
O27 C26 Zn1 73.5(4) . . ?
O27 C26 O25 123.2(6) . . ?
O27 C26 C28 119.9(7) . . ?
C28 C26 Zn1 166.6(6) . . ?
C29 C28 C26 121.2(7) . . ?
C29 C28 C33 118.2(7) . . ?
C33 C28 C26 120.5(6) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 C28 120.8(7) . . ?
C30 C29 H29 119.6 . . ?
C29 C30 H30 119.7 . . ?
C29 C30 C31 120.7(7) . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C34 120.4(7) . . ?
C32 C31 C30 118.5(7) . . ?
C32 C31 C34 121.2(8) . . ?
C31 C32 H32 119.5 . . ?
C31 C32 C33 121.0(8) . . ?
C33 C32 H32 119.5 . . ?
C28 C33 H33 119.6 . . ?
C32 C33 C28 120.8(7) . . ?
C32 C33 H33 119.6 . . ?
C31 C34 H34A 109.8 . . ?
C31 C34 H34B 109.8 . . ?
H34A C34 H34B 108.2 . . ?
N35 C34 C31 109.4(6) . . ?
N35 C34 H34A 109.8 . . ?
N35 C34 H34B 109.8 . . ?
C34 N35 C46 109.7(6) . . ?
C36 N35 C34 112.9(7) . . ?
C36 N35 C46 112.3(7) . . ?
N35 C36 H36A 109.3 . . ?
N35 C36 H36B 109.3 . . ?
N35 C36 C37 111.6(6) . . ?
H36A C36 H36B 108.0 . . ?
C37 C36 H36A 109.3 . . ?
C37 C36 H36B 109.3 . . ?
C38 C37 C36 123.3(8) . . ?
C42 C37 C36 120.4(8) . . ?
C42 C37 C38 116.3(9) . . ?
C37 C38 H38 119.6 . . ?
C37 C38 C39 120.8(8) . . ?
C39 C38 H38 119.6 . . ?
C38 C39 H39 119.3 . . ?
C40 C39 C38 121.4(9) . . ?
C40 C39 H39 119.3 . . ?
C39 C40 C41 118.0(10) . . ?
C39 C40 C43 127.2(9) . . ?
C41 C40 C43 114.6(9) . . ?
C40 C41 H41 119.2 . . ?
C40 C41 C42 121.6(9) . . ?
C42 C41 H41 119.2 . . ?
C37 C42 C41 121.8(8) . . ?
C37 C42 H42 119.1 . . ?
C41 C42 H42 119.1 . . ?
C40 C43 Zn2 163.2(7) . 3_665 ?
O44 C43 Zn2 74.9(7) . 3_665 ?
O44 C43 C40 121.8(8) . . ?
O44 C43 O45 131.9(11) . . ?
O45 C43 Zn2 57.3(5) . 3_665 ?
O45 C43 C40 105.9(9) . . ?
C43 O44 Zn2 77.4(6) . 3_665 ?
C43 O45 Zn2 90.7(7) . 3_665 ?
N35 C46 H46A 109.4 . . ?
N35 C46 H46B 109.4 . . ?
C46 C46 N35 111.4(8) 3_666 . ?
C46 C46 H46A 109.4 3_666 . ?
C46 C46 H46B 109.4 3_666 . ?
H46A C46 H46B 108.0 . . ?
S48 O47 Zn1 111.1(4) . . ?
S51 O47 Zn1 151.4(6) . . ?
C49 S48 O47 98.7(6) . . ?
C49 S48 C50 100.2(11) . . ?
C50 S48 O47 100.7(11) . . ?
S48 C49 H49D 109.5 . . ?
S48 C49 H49E 109.5 . . ?
S48 C49 H49F 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
H49D C49 H49E 109.5 . . ?
H49D C49 H49F 109.5 . . ?
H49E C49 H49F 109.5 . . ?
S51 C49 H49A 109.5 . . ?
S51 C49 H49B 109.5 . . ?
S51 C49 H49C 109.5 . . ?
S48 C50 H50A 109.5 . . ?
S48 C50 H50B 109.5 . . ?
S48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O47 S51 C49 98.7(6) . . ?
O47 S51 C52 99.5(9) . . ?
C52 S51 C49 106.6(11) . . ?
S51 C52 H52A 109.5 . . ?
S51 C52 H52B 109.5 . . ?
S51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
S54 O53 Zn1 133.2(6) . . ?
S55 O53 Zn1 127.3(10) . . ?
S56 O53 Zn1 123.8(7) . . ?
O53 S54 C57 115.0(6) . . ?
O53 S54 C60 107.8(13) . . ?
C57 S54 C60 85.8(14) . . ?
O53 S55 C57 115.9(11) . . ?
O53 S55 C59 98(2) . . ?
C59 S55 C57 86.0(17) . . ?
O53 S56 C57 99.7(9) . . ?
O53 S56 C58 98.9(15) . . ?
C58 S56 C57 112.2(16) . . ?
S54 C57 H57A 109.5 . . ?
S54 C57 H57B 109.5 . . ?
S54 C57 H57C 109.5 . . ?
S55 C57 H57D 109.5 . . ?
S55 C57 H57E 109.5 . . ?
S55 C57 H57F 109.5 . . ?
S56 C57 H57G 109.5 . . ?
S56 C57 H57H 109.5 . . ?
S56 C57 H57I 109.5 . . ?
H57G C57 H57H 109.5 . . ?
H57G C57 H57I 109.5 . . ?
H57H C57 H57I 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
H57D C57 H57E 109.5 . . ?
H57D C57 H57F 109.5 . . ?
H57E C57 H57F 109.5 . . ?
S56 C58 H58A 109.5 . . ?
S56 C58 H58B 109.5 . . ?
S56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
S55 C59 H59A 109.5 . . ?
S55 C59 H59B 109.5 . . ?
S55 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
S54 C60 H60A 109.5 . . ?
S54 C60 H60B 109.5 . . ?
S54 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
S62 O61 Zn2 112.6(4) . . ?
S63 O61 Zn2 155.2(6) . . ?
O61 S62 C64 102.3(9) . . ?
O61 S62 C65 91.1(10) . . ?
C64 S62 C65 102.3(14) . . ?
O61 S63 C64 109.4(8) . . ?
O61 S63 C66 77.0(7) . . ?
C64 S63 C66 106.0(11) . . ?
S62 C64 H64D 109.5 . . ?
S62 C64 H64E 109.5 . . ?
S62 C64 H64F 109.5 . . ?
S63 C64 H64A 109.5 . . ?
S63 C64 H64B 109.5 . . ?
S63 C64 H64C 109.5 . . ?
H64D C64 H64E 109.5 . . ?
H64D C64 H64F 109.5 . . ?
H64E C64 H64F 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
S62 C65 H65A 109.5 . . ?
S62 C65 H65B 109.5 . . ?
S62 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
S63 C66 H66A 109.5 . . ?
S63 C66 H66B 109.5 . . ?
S63 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
S68 O67 Zn2 143.3(7) . . ?
S69 O67 Zn2 116.9(4) . . ?
O67 S68 C70 112.3(7) . . ?
O67 S68 C71 105.0(5) . . ?
C70 S68 C71 89.9(6) . . ?
O67 S69 C70 98.9(5) . . ?
O67 S69 C71 110.6(6) . . ?
C71 S69 C70 93.4(6) . . ?
S68 C70 H70D 109.5 . . ?
S68 C70 H70E 109.5 . . ?
S68 C70 H70F 109.5 . . ?
S69 C70 H70A 109.5 . . ?
S69 C70 H70B 109.5 . . ?
S69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
H70D C70 H70E 109.5 . . ?
H70D C70 H70F 109.5 . . ?
H70E C70 H70F 109.5 . . ?
S68 C71 H71D 109.5 . . ?
S68 C71 H71E 109.5 . . ?
S68 C71 H71F 109.5 . . ?
S69 C71 H71A 109.5 . . ?
S69 C71 H71B 109.5 . . ?
S69 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
H71D C71 H71E 109.5 . . ?
H71D C71 H71F 109.5 . . ?
H71E C71 H71F 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 O3 C4 O5 -1.1(9) . . . . ?
Zn1 O3 C4 C6 -179.6(6) . . . . ?
Zn1 C4 C6 C7 -5(4) . . . . ?
Zn1 C4 C6 C11 175(3) . . . . ?
Zn1 O25 C26 O27 -0.3(8) . . . . ?
Zn1 O25 C26 C28 -178.8(5) . . . . ?
Zn1 C26 C28 C29 -175.5(18) . . . . ?
Zn1 C26 C28 C33 6(3) . . . . ?
Zn1 O47 S48 C49 89.6(7) . . . . ?
Zn1 O47 S48 C50 -168.2(9) . . . . ?
Zn1 O47 S51 C49 30.7(12) . . . . ?
Zn1 O47 S51 C52 -77.9(14) . . . . ?
Zn1 O53 S54 C57 88.0(10) . . . . ?
Zn1 O53 S54 C60 -178.4(15) . . . . ?
Zn1 O53 S55 C57 -98.6(13) . . . . ?
Zn1 O53 S55 C59 171.7(16) . . . . ?
Zn1 O53 S56 C57 -104.0(8) . . . . ?
Zn1 O53 S56 C58 141.5(15) . . . . ?
Zn2 O61 S62 C64 108.8(7) . . . . ?
Zn2 O61 S62 C65 -148.4(12) . . . . ?
Zn2 O61 S63 C64 12.7(19) . . . . ?
Zn2 O61 S63 C66 -90.0(15) . . . . ?
Zn2 O67 S68 C70 -152.6(8) . . . . ?
Zn2 O67 S68 C71 -56.3(9) . . . . ?
Zn2 O67 S69 C70 -176.3(7) . . . . ?
Zn2 O67 S69 C71 86.7(7) . . . . ?
O3 C4 O5 Zn1 1.0(8) . . . . ?
O3 C4 C6 C7 -2.9(13) . . . . ?
O3 C4 C6 C11 177.0(9) . . . . ?
C4 C6 C7 C8 175.0(9) . . . . ?
C4 C6 C11 C10 -174.6(11) . . . . ?
O5 C4 C6 C7 178.7(9) . . . . ?
O5 C4 C6 C11 -1.4(13) . . . . ?
C6 C4 O5 Zn1 179.3(8) . . . . ?
C6 C7 C8 C9 1.5(17) . . . . ?
C7 C6 C11 C10 5.3(17) . . . . ?
C7 C8 C9 C10 1.5(17) . . . . ?
C7 C8 C9 C12 -175.6(12) . . . . ?
C8 C9 C10 C11 -1.0(19) . . . . ?
C8 C9 C12 N13 -136.4(12) . . . . ?
C9 C10 C11 C6 -2(2) . . . . ?
C9 C12 N13 C14 -155.2(8) . . . . ?
C9 C12 N13 C24 73.4(10) . . . . ?
C10 C9 C12 N13 46.6(16) . . . . ?
C11 C6 C7 C8 -4.9(16) . . . . ?
C12 C9 C10 C11 176.3(13) . . . . ?
C12 N13 C14 C15 -70.7(15) . . . . ?
C12 N13 C24 C24 -157.2(10) . . . 3_675 ?
N13 C14 C15 C16 79.7(16) . . . . ?
N13 C14 C15 C20 -99.4(14) . . . . ?
C14 N13 C24 C24 72.5(13) . . . 3_675 ?
C14 C15 C16 C17 179.2(8) . . . . ?
C14 C15 C20 C19 179.1(8) . . . . ?
C15 C16 C17 C18 1.6(15) . . . . ?
C16 C15 C20 C19 -0.1(15) . . . . ?
C16 C17 C18 C19 0.2(14) . . . . ?
C16 C17 C18 C21 179.4(8) . . . . ?
C17 C18 C19 C20 -2.0(15) . . . . ?
C17 C18 C21 O22 -168.7(8) . . . . ?
C17 C18 C21 O23 12.8(14) . . . . ?
C18 C19 C20 C15 2.0(14) . . . . ?
C18 C21 O22 Zn2 -179.2(6) . . . . ?
C19 C18 C21 O22 10.5(13) . . . . ?
C19 C18 C21 O23 -168.1(10) . . . . ?
C20 C15 C16 C17 -1.6(16) . . . . ?
C21 C18 C19 C20 178.8(8) . . . . ?
O23 C21 O22 Zn2 -0.7(13) . . . . ?
C24 N13 C14 C15 57.2(17) . . . . ?
O25 C26 C28 C29 -171.7(7) . . . . ?
O25 C26 C28 C33 9.7(10) . . . . ?
C26 C28 C29 C30 -176.7(7) . . . . ?
C26 C28 C33 C32 174.7(8) . . . . ?
O27 C26 C28 C29 9.7(11) . . . . ?
O27 C26 C28 C33 -168.9(7) . . . . ?
C28 C29 C30 C31 1.0(12) . . . . ?
C29 C28 C33 C32 -3.8(12) . . . . ?
C29 C30 C31 C32 -2.0(13) . . . . ?
C29 C30 C31 C34 179.1(8) . . . . ?
C30 C31 C32 C33 0.1(14) . . . . ?
C30 C31 C34 N35 -56.9(12) . . . . ?
C31 C32 C33 C28 2.9(15) . . . . ?
C31 C34 N35 C36 -68.5(10) . . . . ?
C31 C34 N35 C46 165.4(7) . . . . ?
C32 C31 C34 N35 124.2(9) . . . . ?
C33 C28 C29 C30 1.9(11) . . . . ?
C34 C31 C32 C33 179.0(9) . . . . ?
C34 N35 C36 C37 164.8(6) . . . . ?
C34 N35 C46 C46 -80.7(10) . . . 3_666 ?
N35 C36 C37 C38 139.6(8) . . . . ?
N35 C36 C37 C42 -40.1(11) . . . . ?
C36 N35 C46 C46 152.8(8) . . . 3_666 ?
C36 C37 C38 C39 179.6(8) . . . . ?
C36 C37 C42 C41 -177.4(10) . . . . ?
C37 C38 C39 C40 -2.2(15) . . . . ?
C38 C37 C42 C41 2.9(17) . . . . ?
C38 C39 C40 C41 2.8(16) . . . . ?
C38 C39 C40 C43 176.4(8) . . . . ?
C39 C40 C41 C42 -0.6(18) . . . . ?
C39 C40 C43 Zn2 6(3) . . . 3_665 ?
C39 C40 C43 O44 -177.6(11) . . . . ?
C39 C40 C43 O45 8.2(12) . . . . ?
C40 C41 C42 C37 -2(2) . . . . ?
C40 C43 O44 Zn2 -178.9(8) . . . 3_665 ?
C40 C43 O45 Zn2 -179.3(5) . . . 3_665 ?
C41 C40 C43 Zn2 179.9(19) . . . 3_665 ?
C41 C40 C43 O44 -3.8(14) . . . . ?
C41 C40 C43 O45 -178.0(9) . . . . ?
C42 C37 C38 C39 -0.7(14) . . . . ?
C43 C40 C41 C42 -175.0(11) . . . . ?
O44 C43 O45 Zn2 7.3(13) . . . 3_665 ?
O45 C43 O44 Zn2 -6.4(12) . . . 3_665 ?
C46 N35 C36 C37 -70.5(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_THETM01_3                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystals were small and displayed poor diffraction characteristics, 
partially due to the very large volume occupied by diffuse solvent molecules,
with the result that only a relatively low-resolution dataset could be
obtained (theta max 22.8 degrees), even with high intensity synchrotron 
radiation. This structure is presented as a connectivity model of the 
material only. 
;
_vrf_PLAT027_3                   
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      22.80 Degree
RESPONSE: See above
;
_vrf_PLAT241_3                   
;
PROBLEM: High      Ueq as Compared to Neighbors for .....        C64 Check 
RESPONSE: Each of the four uniquely modelled coordinating DMSO molecules displayed
disorder over at least two positions sharing coordinating oxygen atoms. Carbon atom
C64 was best described as an elongated elliptical distribution of electron density 
shared between two half-occupancy sulfur atoms, rather than modelling as independent
disordered atoms, which required excessive ADP restraints to prevent the emergence of
non-positive definite Uij tensors. The remaining atoms displaying high relative Ueq
values due to this disorder were either allowed to refine freely or applied mild ISOR 
restraints, and DFIX restraints were applied as necessary to maintain chemically 
sensible molecular geometries.
;
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1406631'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_audit_creation_date             2015-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C50 H50 N4 O10 S2 Zn2'
_chemical_formula_sum            'C50 H50 N4 O10 S2 Zn2'
_chemical_formula_weight         1061.80
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2910 1.4390 '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                   7.6120(15)
_cell_length_b                   13.231(3)
_cell_length_c                   14.107(3)
_cell_angle_alpha                81.58(3)
_cell_angle_beta                 84.39(3)
_cell_angle_gamma                84.86(3)
_cell_volume                     1394.6(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6608
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      1.56
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26320
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.969
_diffrn_reflns_theta_min         1.561
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6071
_reflns_number_total             6608
_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       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6608
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0382
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0454P)²+1.0732P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.0992
_refine_special_details          
;
The material contains significant regions of diffuse electron density
corresponding to highly disordered lattice solvent; as such, the SQUEEZE 
routine was employed to provide accurate statistics for the refinement of the
framework atoms. Because of the uncertainty associated with solvation in
the freshly isolated crystal compared with bulk phase analysis, in which
solvent molecules are frequently observed to exchange with atmospheric water,
the crystallographic formula is presented for crystallographically located
framework atoms only, and as such, the values for density, F000 and absorption
coefficients do not include contributions from unmodelled solvent.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C15(H15), C16(H16), C18(H18), C19(H19),
 C25(H25), C26(H26), C28(H28), C29(H29), C30(H30)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34C,H34A,H34B)
;
_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
Zn1 Zn 1.22388(3) 0.77517(2) 0.96748(2) 0.02681(8) Uani 1 1 d . . . . .
O2 O 1.00535(19) 0.77523(12) 0.90904(10) 0.0331(3) Uani 1 1 d . . . . .
C3 C 1.0328(3) 0.74051(16) 0.82773(14) 0.0310(4) Uani 1 1 d . . . . .
O4 O 1.1779(2) 0.70195(16) 0.79802(12) 0.0466(4) Uani 1 1 d . . . . .
C5 C 0.8785(3) 0.75058(15) 0.76783(13) 0.0270(4) Uani 1 1 d . . . . .
C6 C 0.8911(3) 0.70214(17) 0.68588(14) 0.0339(4) Uani 1 1 d . . . . .
H6 H 0.9968 0.6626 0.6688 0.041 Uiso 1 1 calc R . . . .
C7 C 0.7496(3) 0.71139(17) 0.62886(14) 0.0334(4) Uani 1 1 d . . . . .
H7 H 0.7596 0.6782 0.5730 0.040 Uiso 1 1 calc R . . . .
C8 C 0.5942(3) 0.76861(14) 0.65294(13) 0.0268(4) Uani 1 1 d . . . . .
C9 C 0.5820(3) 0.81591(15) 0.73577(14) 0.0302(4) Uani 1 1 d . . . . .
H9 H 0.4759 0.8548 0.7534 0.036 Uiso 1 1 calc R . . . .
C10 C 0.7222(3) 0.80691(15) 0.79245(13) 0.0290(4) Uani 1 1 d . . . . .
H10 H 0.7116 0.8395 0.8487 0.035 Uiso 1 1 calc R . . . .
C11 C 0.4380(3) 0.78042(15) 0.59262(13) 0.0293(4) Uani 1 1 d . . . . .
H11A H 0.4718 0.7494 0.5331 0.035 Uiso 1 1 calc R . . . .
H11B H 0.3391 0.7438 0.6289 0.035 Uiso 1 1 calc R . . . .
N12 N 0.3799(2) 0.88899(12) 0.56753(11) 0.0260(3) Uani 1 1 d . . . . .
C13 C 0.1987(2) 0.90376(16) 0.53596(13) 0.0278(4) Uani 1 1 d . . . . .
H13A H 0.1594 0.9776 0.5314 0.033 Uiso 1 1 calc R . . . .
H13B H 0.1187 0.8666 0.5860 0.033 Uiso 1 1 calc R . . . .
C14 C 0.1782(2) 0.86806(16) 0.44015(13) 0.0280(4) Uani 1 1 d . . . . .
C15 C 0.1457(3) 0.76664(17) 0.43520(15) 0.0363(4) Uani 1 1 d . . . . .
H15 H 0.1303 0.7200 0.4928 0.044 Uiso 1 1 calc R . . . .
C16 C 0.1356(3) 0.73307(18) 0.34711(16) 0.0406(5) Uani 1 1 d . . . . .
H16 H 0.1124 0.6641 0.3450 0.049 Uiso 1 1 calc R . . . .
C17 C 0.1594(3) 0.80026(17) 0.26189(14) 0.0341(4) Uani 1 1 d . . . . .
C18 C 0.1907(3) 0.90132(16) 0.26604(14) 0.0322(4) Uani 1 1 d . . . . .
H18 H 0.2069 0.9477 0.2083 0.039 Uiso 1 1 calc R . . . .
C19 C 0.1983(3) 0.93481(16) 0.35458(14) 0.0303(4) Uani 1 1 d . . . . .
H19 H 0.2177 1.0044 0.3566 0.036 Uiso 1 1 calc R . . . .
C20 C 0.1511(4) 0.76279(19) 0.16646(16) 0.0423(5) Uani 1 1 d . . . . .
O21 O 0.1163(5) 0.6753(2) 0.16375(15) 0.1062(12) Uani 1 1 d . . . . .
O22 O 0.1888(2) 0.82644(13) 0.09230(10) 0.0423(4) Uani 1 1 d . . . . .
C23 C 0.5120(2) 0.94218(14) 0.50058(13) 0.0270(4) Uani 1 1 d . . . . .
H23A H 0.5026 0.9260 0.4350 0.032 Uiso 1 1 calc R . . . .
H23B H 0.6319 0.9170 0.5193 0.032 Uiso 1 1 calc R . . . .
N24 N 1.4427(2) 0.67772(12) 0.97087(12) 0.0268(3) Uani 1 1 d . . . . .
C25 C 1.5540(3) 0.68202(15) 1.03877(14) 0.0303(4) Uani 1 1 d . . . . .
H25 H 1.5189 0.7250 1.0867 0.036 Uiso 1 1 calc R . . . .
C26 C 1.7157(3) 0.62708(15) 1.04165(15) 0.0321(4) Uani 1 1 d . . . . .
H26 H 1.7912 0.6336 1.0899 0.039 Uiso 1 1 calc R . . . .
C27 C 1.7685(3) 0.56133(14) 0.97291(14) 0.0279(4) Uani 1 1 d . . . . .
C28 C 1.6518(3) 0.55627(14) 0.90420(14) 0.0290(4) Uani 1 1 d . . . . .
H28 H 1.6815 0.5121 0.8568 0.035 Uiso 1 1 calc R . . . .
C29 C 1.4928(3) 0.61526(14) 0.90465(14) 0.0286(4) Uani 1 1 d . . . . .
H29 H 1.4160 0.6115 0.8563 0.034 Uiso 1 1 calc R . . . .
C30 C 1.9373(3) 0.49875(14) 0.97049(14) 0.0296(4) Uani 1 1 d . . . . .
H30 H 1.9588 0.4533 0.9236 0.036 Uiso 1 1 calc R . . . .
O31 O 1.3226(2) 0.90675(11) 0.89900(11) 0.0352(3) Uani 1 1 d . . . . .
S32 S 1.19629(7) 1.00174(4) 0.88159(4) 0.03857(13) Uani 1 1 d . . . . .
C33 C 1.2782(4) 1.0622(3) 0.7673(3) 0.0719(10) Uani 1 1 d . . . . .
H33A H 1.4046 1.0709 0.7678 0.108 Uiso 1 1 calc GR . . . .
H33B H 1.2139 1.1294 0.7529 0.108 Uiso 1 1 calc GR . . . .
H33C H 1.2614 1.0197 0.7180 0.108 Uiso 1 1 calc GR . . . .
C34 C 1.2606(5) 1.0837(3) 0.9579(3) 0.0787(12) Uani 1 1 d . . . . .
H34C H 1.3889 1.0886 0.9479 0.118 Uiso 1 1 calc GR . . . .
H34A H 1.2284 1.0561 1.0251 0.118 Uiso 1 1 calc GR . . . .
H34B H 1.2001 1.1520 0.9432 0.118 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O2 1.9273(15) . ?
Zn1 O22 1.9641(15) 1_656 ?
Zn1 N24 2.0129(17) . ?
Zn1 O31 2.0320(17) . ?
O2 C3 1.289(2) . ?
C3 O4 1.236(3) . ?
C3 C5 1.498(3) . ?
C5 C6 1.393(3) . ?
C5 C10 1.388(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.392(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.387(3) . ?
C8 C9 1.396(3) . ?
C8 C11 1.513(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(3) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 N12 1.467(3) . ?
N12 C13 1.478(2) . ?
N12 C23 1.465(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.522(2) . ?
C14 C15 1.399(3) . ?
C14 C19 1.392(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.393(3) . ?
C17 C18 1.390(3) . ?
C17 C20 1.510(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.393(3) . ?
C19 H19 0.9500 . ?
C20 O21 1.217(3) . ?
C20 O22 1.270(3) . ?
O22 Zn1 1.9640(15) 1_454 ?
C23 C23 1.522(4) 2_676 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
N24 C25 1.350(2) . ?
N24 C29 1.342(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.373(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.403(3) . ?
C27 C28 1.390(3) . ?
C27 C30 1.465(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.380(3) . ?
C29 H29 0.9500 . ?
C30 C30 1.332(4) 2_967 ?
C30 H30 0.9500 . ?
O31 S32 1.5179(16) . ?
S32 C33 1.773(3) . ?
S32 C34 1.765(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O22 112.59(7) . 1_656 ?
O2 Zn1 N24 132.18(7) . . ?
O2 Zn1 O31 102.18(7) . . ?
O22 Zn1 N24 106.85(7) 1_656 . ?
O22 Zn1 O31 93.01(7) 1_656 . ?
N24 Zn1 O31 101.63(7) . . ?
C3 O2 Zn1 111.03(13) . . ?
O2 C3 C5 116.54(18) . . ?
O4 C3 O2 123.21(19) . . ?
O4 C3 C5 120.24(18) . . ?
C6 C5 C3 119.54(18) . . ?
C10 C5 C3 121.39(17) . . ?
C10 C5 C6 119.07(18) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.34(18) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.54(18) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C9 118.75(18) . . ?
C7 C8 C11 121.97(17) . . ?
C9 C8 C11 119.28(17) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.83(18) . . ?
C10 C9 H9 119.6 . . ?
C5 C10 H10 119.8 . . ?
C9 C10 C5 120.46(17) . . ?
C9 C10 H10 119.8 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
N12 C11 C8 110.66(15) . . ?
N12 C11 H11A 109.5 . . ?
N12 C11 H11B 109.5 . . ?
C11 N12 C13 112.40(15) . . ?
C23 N12 C11 111.08(15) . . ?
C23 N12 C13 114.21(15) . . ?
N12 C13 H13A 108.4 . . ?
N12 C13 H13B 108.4 . . ?
N12 C13 C14 115.32(15) . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
C15 C14 C13 121.13(18) . . ?
C19 C14 C13 120.61(18) . . ?
C19 C14 C15 118.22(17) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 120.9(2) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.2(2) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 C20 119.9(2) . . ?
C18 C17 C16 119.30(18) . . ?
C18 C17 C20 120.80(19) . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.20(19) . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 121.11(19) . . ?
C14 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
O21 C20 C17 120.3(2) . . ?
O21 C20 O22 123.9(2) . . ?
O22 C20 C17 115.8(2) . . ?
C20 O22 Zn1 117.73(14) . 1_454 ?
N12 C23 C23 112.05(19) . 2_676 ?
N12 C23 H23A 109.2 . . ?
N12 C23 H23B 109.2 . . ?
C23 C23 H23A 109.2 2_676 . ?
C23 C23 H23B 109.2 2_676 . ?
H23A C23 H23B 107.9 . . ?
C25 N24 Zn1 117.95(13) . . ?
C29 N24 Zn1 123.97(13) . . ?
C29 N24 C25 117.79(17) . . ?
N24 C25 H25 118.5 . . ?
N24 C25 C26 122.96(18) . . ?
C26 C25 H25 118.5 . . ?
C25 C26 H26 120.2 . . ?
C25 C26 C27 119.51(18) . . ?
C27 C26 H26 120.2 . . ?
C26 C27 C30 123.65(18) . . ?
C28 C27 C26 117.08(18) . . ?
C28 C27 C30 119.27(17) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 C27 120.20(17) . . ?
C29 C28 H28 119.9 . . ?
N24 C29 C28 122.43(18) . . ?
N24 C29 H29 118.8 . . ?
C28 C29 H29 118.8 . . ?
C27 C30 H30 117.8 . . ?
C30 C30 C27 124.4(2) 2_967 . ?
C30 C30 H30 117.8 2_967 . ?
S32 O31 Zn1 118.45(9) . . ?
O31 S32 C33 103.20(13) . . ?
O31 S32 C34 103.73(15) . . ?
C34 S32 C33 101.2(2) . . ?
S32 C33 H33A 109.5 . . ?
S32 C33 H33B 109.5 . . ?
S32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
S32 C34 H34C 109.5 . . ?
S32 C34 H34A 109.5 . . ?
S32 C34 H34B 109.5 . . ?
H34C C34 H34A 109.5 . . ?
H34C C34 H34B 109.5 . . ?
H34A C34 H34B 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 O2 C3 O4 7.6(3) . . . . ?
Zn1 O2 C3 C5 -171.33(13) . . . . ?
Zn1 N24 C25 C26 -172.98(17) . . . . ?
Zn1 N24 C29 C28 173.90(15) . . . . ?
Zn1 O31 S32 C33 -143.43(17) . . . . ?
Zn1 O31 S32 C34 111.32(16) . . . . ?
O2 C3 C5 C6 -171.02(19) . . . . ?
O2 C3 C5 C10 8.7(3) . . . . ?
C3 C5 C6 C7 -179.43(19) . . . . ?
C3 C5 C10 C9 179.48(18) . . . . ?
O4 C3 C5 C6 10.0(3) . . . . ?
O4 C3 C5 C10 -170.3(2) . . . . ?
C5 C6 C7 C8 -0.2(3) . . . . ?
C6 C5 C10 C9 -0.8(3) . . . . ?
C6 C7 C8 C9 -0.6(3) . . . . ?
C6 C7 C8 C11 179.93(19) . . . . ?
C7 C8 C9 C10 0.6(3) . . . . ?
C7 C8 C11 N12 -127.6(2) . . . . ?
C8 C9 C10 C5 0.1(3) . . . . ?
C8 C11 N12 C13 -162.11(15) . . . . ?
C8 C11 N12 C23 68.53(19) . . . . ?
C9 C8 C11 N12 52.8(2) . . . . ?
C10 C5 C6 C7 0.9(3) . . . . ?
C11 C8 C9 C10 -179.87(18) . . . . ?
C11 N12 C13 C14 -68.2(2) . . . . ?
C11 N12 C23 C23 -160.70(18) . . . 2_676 ?
N12 C13 C14 C15 87.1(2) . . . . ?
N12 C13 C14 C19 -90.3(2) . . . . ?
C13 N12 C23 C23 70.9(2) . . . 2_676 ?
C13 C14 C15 C16 -176.8(2) . . . . ?
C13 C14 C19 C18 176.00(18) . . . . ?
C14 C15 C16 C17 0.6(4) . . . . ?
C15 C14 C19 C18 -1.5(3) . . . . ?
C15 C16 C17 C18 -0.9(4) . . . . ?
C15 C16 C17 C20 179.0(2) . . . . ?
C16 C17 C18 C19 0.1(3) . . . . ?
C16 C17 C20 O21 3.1(4) . . . . ?
C16 C17 C20 O22 -174.4(2) . . . . ?
C17 C18 C19 C14 1.1(3) . . . . ?
C17 C20 O22 Zn1 168.85(15) . . . 1_454 ?
C18 C17 C20 O21 -176.9(3) . . . . ?
C18 C17 C20 O22 5.6(3) . . . . ?
C19 C14 C15 C16 0.7(3) . . . . ?
C20 C17 C18 C19 -179.9(2) . . . . ?
O21 C20 O22 Zn1 -8.5(4) . . . 1_454 ?
C23 N12 C13 C14 59.5(2) . . . . ?
N24 C25 C26 C27 -1.5(3) . . . . ?
C25 N24 C29 C28 0.1(3) . . . . ?
C25 C26 C27 C28 0.4(3) . . . . ?
C25 C26 C27 C30 -179.4(2) . . . . ?
C26 C27 C28 C29 0.8(3) . . . . ?
C26 C27 C30 C30 -3.7(4) . . . 2_967 ?
C27 C28 C29 N24 -1.1(3) . . . . ?
C28 C27 C30 C30 176.5(3) . . . 2_967 ?
C29 N24 C25 C26 1.2(3) . . . . ?
C30 C27 C28 C29 -179.41(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
