# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_rm145a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 Cu N2 O5, H2 O'
_chemical_formula_sum            'C34 H38 Cu N2 O6'
_chemical_formula_weight         634.20

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8156(8)
_cell_length_b                   10.3153(17)
_cell_length_c                   20.747(2)
_cell_angle_alpha                101.272(11)
_cell_angle_beta                 100.209(8)
_cell_angle_gamma                97.106(12)
_cell_volume                     1592.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             666
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.7583
_exptl_absorpt_correction_T_max  0.8857
_exptl_absorpt_process_details   'North et al., 1968'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6028
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         24.96
_reflns_number_total             5582
_reflns_number_gt                4148
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0678P)²+1.0377P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5582
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.73607(6) 0.16796(4) 0.37228(2) 0.04151(16) Uani 1 1 d . . .
N1 N 0.7131(4) 0.2417(3) 0.46710(14) 0.0450(7) Uani 1 1 d . . .
N2 N 0.7721(4) 0.0043(3) 0.41076(13) 0.0402(6) Uani 1 1 d . . .
O1 O 0.7247(3) 0.0691(3) 0.28218(12) 0.0555(7) Uani 1 1 d . . .
O2 O 0.9967(4) 0.1312(3) 0.26925(14) 0.0668(8) Uani 1 1 d . . .
O3 O 0.5874(3) 0.2872(3) 0.33724(13) 0.0574(7) Uani 1 1 d . . .
O4 O 0.7861(4) 0.4585(3) 0.33461(16) 0.0691(8) Uani 1 1 d . . .
O5 O 1.0049(4) 0.2998(3) 0.38621(14) 0.0503(7) Uani 1 1 d . . .
O6 O 0.3186(5) 0.0179(4) 0.25104(19) 0.0866(10) Uani 1 1 d . . .
C1 C 0.8439(5) 0.0732(3) 0.24730(17) 0.0417(8) Uani 1 1 d . . .
C2 C 0.7879(4) -0.0027(3) 0.17579(16) 0.0414(8) Uani 1 1 d . . .
C3 C 0.6312(5) -0.0895(4) 0.15251(18) 0.0591(10) Uani 1 1 d . . .
H3 H 0.5563 -0.1010 0.1819 0.071 Uiso 1 1 calc R . .
C4 C 0.5825(6) -0.1597(5) 0.0868(2) 0.0698(12) Uani 1 1 d . . .
H4 H 0.4755 -0.2178 0.0730 0.084 Uiso 1 1 calc R . .
C5 C 0.6876(5) -0.1467(4) 0.04053(18) 0.0542(9) Uani 1 1 d . . .
C6 C 0.8448(6) -0.0604(5) 0.06487(19) 0.0678(12) Uani 1 1 d . . .
H6 H 0.9199 -0.0484 0.0356 0.081 Uiso 1 1 calc R . .
C7 C 0.8956(5) 0.0092(4) 0.13090(19) 0.0634(11) Uani 1 1 d . . .
H7 H 1.0043 0.0651 0.1452 0.076 Uiso 1 1 calc R . .
C8 C 0.6321(7) -0.2258(5) -0.0323(2) 0.0734(13) Uani 1 1 d . . .
C9 C 0.4393(9) -0.2295(10) -0.0590(3) 0.170(4) Uani 1 1 d . . .
H9A H 0.3716 -0.2667 -0.0307 0.255 Uiso 1 1 calc R . .
H9B H 0.4060 -0.2839 -0.1038 0.255 Uiso 1 1 calc R . .
H9C H 0.4174 -0.1401 -0.0596 0.255 Uiso 1 1 calc R . .
C10 C 0.647(2) -0.3655(9) -0.0346(4) 0.295(9) Uani 1 1 d . . .
H10A H 0.5842 -0.3972 -0.0034 0.443 Uiso 1 1 calc R . .
H10B H 0.7687 -0.3739 -0.0228 0.443 Uiso 1 1 calc R . .
H10C H 0.5971 -0.4178 -0.0792 0.443 Uiso 1 1 calc R . .
C11 C 0.7211(14) -0.1671(12) -0.0773(3) 0.269(8) Uani 1 1 d . . .
H11A H 0.7089 -0.0743 -0.0717 0.404 Uiso 1 1 calc R . .
H11B H 0.6700 -0.2134 -0.1228 0.404 Uiso 1 1 calc R . .
H11C H 0.8438 -0.1744 -0.0675 0.404 Uiso 1 1 calc R . .
C12 C 0.6348(5) 0.3962(3) 0.32026(17) 0.0440(8) Uani 1 1 d . . .
C13 C 0.4886(4) 0.4493(3) 0.28129(16) 0.0389(7) Uani 1 1 d . . .
C14 C 0.5244(5) 0.5588(4) 0.25405(18) 0.0470(8) Uani 1 1 d . . .
H14 H 0.6405 0.5996 0.2592 0.056 Uiso 1 1 calc R . .
C15 C 0.3886(5) 0.6087(4) 0.21895(18) 0.0502(9) Uani 1 1 d . . .
H15 H 0.4161 0.6820 0.2006 0.060 Uiso 1 1 calc R . .
C16 C 0.2137(4) 0.5526(3) 0.21050(17) 0.0425(8) Uani 1 1 d . . .
C17 C 0.1796(5) 0.4431(4) 0.23846(19) 0.0508(9) Uani 1 1 d . . .
H17 H 0.0635 0.4030 0.2340 0.061 Uiso 1 1 calc R . .
C18 C 0.3145(5) 0.3920(3) 0.27289(18) 0.0469(8) Uani 1 1 d . . .
H18 H 0.2874 0.3177 0.2907 0.056 Uiso 1 1 calc R . .
C19 C 0.0623(5) 0.6108(4) 0.1744(2) 0.0559(10) Uani 1 1 d . . .
C20 C 0.1215(7) 0.6889(6) 0.1250(3) 0.0947(17) Uani 1 1 d . . .
H20A H 0.0236 0.7236 0.1035 0.142 Uiso 1 1 calc R . .
H20B H 0.1645 0.6306 0.0917 0.142 Uiso 1 1 calc R . .
H20C H 0.2138 0.7617 0.1486 0.142 Uiso 1 1 calc R . .
C21 C -0.0003(6) 0.7074(5) 0.2285(3) 0.0814(14) Uani 1 1 d . . .
H21A H -0.0953 0.7457 0.2076 0.122 Uiso 1 1 calc R . .
H21B H 0.0956 0.7776 0.2520 0.122 Uiso 1 1 calc R . .
H21C H -0.0402 0.6592 0.2597 0.122 Uiso 1 1 calc R . .
C22 C -0.0931(7) 0.5021(5) 0.1377(3) 0.105(2) Uani 1 1 d . . .
H22A H -0.1850 0.5420 0.1158 0.158 Uiso 1 1 calc R . .
H22B H -0.1366 0.4571 0.1693 0.158 Uiso 1 1 calc R . .
H22C H -0.0559 0.4387 0.1048 0.158 Uiso 1 1 calc R . .
C23 C 0.6909(6) 0.3644(4) 0.4944(2) 0.0621(11) Uani 1 1 d . . .
H23 H 0.6864 0.4281 0.4683 0.075 Uiso 1 1 calc R . .
C24 C 0.6740(6) 0.4007(4) 0.5611(2) 0.0708(12) Uani 1 1 d . . .
H24 H 0.6616 0.4882 0.5791 0.085 Uiso 1 1 calc R . .
C25 C 0.6756(5) 0.3085(4) 0.59979(19) 0.0609(11) Uani 1 1 d . . .
H25 H 0.6620 0.3319 0.6440 0.073 Uiso 1 1 calc R . .
C26 C 0.6980(5) 0.1773(4) 0.57235(17) 0.0480(9) Uani 1 1 d . . .
C27 C 0.7190(4) 0.1504(3) 0.50601(16) 0.0391(7) Uani 1 1 d . . .
C28 C 0.7045(5) 0.0731(4) 0.60844(18) 0.0552(10) Uani 1 1 d . . .
H28 H 0.6870 0.0892 0.6523 0.066 Uiso 1 1 calc R . .
C29 C 0.7355(5) -0.0481(4) 0.58005(19) 0.0557(10) Uani 1 1 d . . .
H29 H 0.7398 -0.1141 0.6048 0.067 Uiso 1 1 calc R . .
C30 C 0.7624(4) -0.0783(4) 0.51205(17) 0.0456(8) Uani 1 1 d . . .
C31 C 0.7514(4) 0.0209(3) 0.47526(15) 0.0376(7) Uani 1 1 d . . .
C32 C 0.7996(5) -0.2015(4) 0.4792(2) 0.0553(10) Uani 1 1 d . . .
H32 H 0.8105 -0.2706 0.5018 0.066 Uiso 1 1 calc R . .
C33 C 0.8195(5) -0.2189(4) 0.4142(2) 0.0578(10) Uani 1 1 d . . .
H33 H 0.8438 -0.3000 0.3922 0.069 Uiso 1 1 calc R . .
C34 C 0.8033(5) -0.1139(4) 0.38092(18) 0.0503(9) Uani 1 1 d . . .
H34 H 0.8148 -0.1275 0.3363 0.060 Uiso 1 1 calc R . .
H5A H 0.967(6) 0.355(4) 0.378(2) 0.055(15) Uiso 1 1 d . . .
H5B H 1.025(8) 0.244(6) 0.357(3) 0.12(2) Uiso 1 1 d . . .
H6A H 0.413(7) 0.082(5) 0.255(3) 0.100 Uiso 1 1 d . . .
H6B H 0.197(7) 0.064(5) 0.245(2) 0.100 Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.928(2) . ?
Cu1 O3 1.948(2) . ?
Cu1 N1 2.013(3) . ?
Cu1 N2 2.033(3) . ?
Cu1 O5 2.296(3) . ?
N1 C23 1.328(5) . ?
N1 C27 1.355(4) . ?
N2 C34 1.327(4) . ?
N2 C31 1.357(4) . ?
O1 C1 1.279(4) . ?
O2 C1 1.231(4) . ?
O3 C12 1.275(4) . ?
O4 C12 1.229(4) . ?
O5 H5A 0.71(4) . ?
O5 H5B 0.81(6) . ?
O6 H6A 0.90(5) . ?
O6 H6B 1.11(5) . ?
C1 C2 1.495(5) . ?
C2 C3 1.373(5) . ?
C2 C7 1.374(5) . ?
C3 C4 1.375(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.375(6) . ?
C5 C8 1.529(5) . ?
C6 C7 1.379(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C11 1.438(8) . ?
C8 C10 1.452(9) . ?
C8 C9 1.504(8) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.503(5) . ?
C13 C14 1.379(5) . ?
C13 C18 1.381(5) . ?
C14 C15 1.389(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.383(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.386(5) . ?
C16 C19 1.536(5) . ?
C17 C18 1.385(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.520(6) . ?
C19 C22 1.521(6) . ?
C19 C21 1.541(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.394(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.360(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.407(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.393(5) . ?
C26 C28 1.426(5) . ?
C27 C31 1.436(5) . ?
C28 C29 1.344(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.442(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.394(5) . ?
C30 C32 1.409(5) . ?
C32 C33 1.364(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.401(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O3 90.24(12) . . ?
O1 Cu1 N1 168.97(11) . . ?
O3 Cu1 N1 91.95(11) . . ?
O1 Cu1 N2 91.91(11) . . ?
O3 Cu1 N2 152.13(11) . . ?
N1 Cu1 N2 81.15(11) . . ?
O1 Cu1 O5 97.51(11) . . ?
O3 Cu1 O5 98.35(12) . . ?
N1 Cu1 O5 92.86(11) . . ?
N2 Cu1 O5 108.89(11) . . ?
C23 N1 C27 118.0(3) . . ?
C23 N1 Cu1 128.4(3) . . ?
C27 N1 Cu1 113.6(2) . . ?
C34 N2 C31 117.9(3) . . ?
C34 N2 Cu1 129.3(2) . . ?
C31 N2 Cu1 112.7(2) . . ?
C1 O1 Cu1 127.9(2) . . ?
C12 O3 Cu1 128.2(2) . . ?
Cu1 O5 H5A 94(4) . . ?
Cu1 O5 H5B 87(4) . . ?
H5A O5 H5B 120(5) . . ?
H6A O6 H6B 109(4) . . ?
O2 C1 O1 124.5(3) . . ?
O2 C1 C2 120.2(3) . . ?
O1 C1 C2 115.3(3) . . ?
C3 C2 C7 117.2(3) . . ?
C3 C2 C1 122.2(3) . . ?
C7 C2 C1 120.6(3) . . ?
C2 C3 C4 121.5(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 122.1(4) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C6 C5 C4 115.6(3) . . ?
C6 C5 C8 122.8(4) . . ?
C4 C5 C8 121.6(4) . . ?
C5 C6 C7 122.6(4) . . ?
C5 C6 H6 118.7 . . ?
C7 C6 H6 118.7 . . ?
C2 C7 C6 121.0(4) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C11 C8 C10 114.5(8) . . ?
C11 C8 C9 105.0(7) . . ?
C10 C8 C9 103.7(7) . . ?
C11 C8 C5 113.1(4) . . ?
C10 C8 C5 109.1(4) . . ?
C9 C8 C5 110.9(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O4 C12 O3 124.8(3) . . ?
O4 C12 C13 120.2(3) . . ?
O3 C12 C13 114.9(3) . . ?
C14 C13 C18 118.0(3) . . ?
C14 C13 C12 120.7(3) . . ?
C18 C13 C12 121.2(3) . . ?
C13 C14 C15 120.5(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C16 C15 C14 122.0(3) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C15 C16 C17 116.8(3) . . ?
C15 C16 C19 122.3(3) . . ?
C17 C16 C19 120.8(3) . . ?
C18 C17 C16 121.5(3) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C13 C18 C17 121.2(3) . . ?
C13 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C20 C19 C22 109.3(4) . . ?
C20 C19 C16 112.0(3) . . ?
C22 C19 C16 111.8(3) . . ?
C20 C19 C21 108.4(4) . . ?
C22 C19 C21 108.0(4) . . ?
C16 C19 C21 107.3(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 C24 122.1(4) . . ?
N1 C23 H23 119.0 . . ?
C24 C23 H23 119.0 . . ?
C25 C24 C23 120.1(4) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 119.4(4) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C27 C26 C25 116.9(3) . . ?
C27 C26 C28 118.8(3) . . ?
C25 C26 C28 124.3(3) . . ?
N1 C27 C26 123.6(3) . . ?
N1 C27 C31 116.0(3) . . ?
C26 C27 C31 120.4(3) . . ?
C29 C28 C26 121.0(3) . . ?
C29 C28 H28 119.5 . . ?
C26 C28 H28 119.5 . . ?
C28 C29 C30 121.6(3) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C31 C30 C32 116.6(3) . . ?
C31 C30 C29 118.3(3) . . ?
C32 C30 C29 125.1(3) . . ?
N2 C31 C30 123.8(3) . . ?
N2 C31 C27 116.3(3) . . ?
C30 C31 C27 119.8(3) . . ?
C33 C32 C30 119.7(3) . . ?
C33 C32 H32 120.2 . . ?
C30 C32 H32 120.2 . . ?
C32 C33 C34 119.6(3) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
N2 C34 C33 122.3(3) . . ?
N2 C34 H34 118.9 . . ?
C33 C34 H34 118.9 . . ?

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 Cu1 N1 C23 -131.7(6) . . . . ?
O3 Cu1 N1 C23 -30.4(4) . . . . ?
N2 Cu1 N1 C23 176.8(4) . . . . ?
O5 Cu1 N1 C23 68.1(4) . . . . ?
O1 Cu1 N1 C27 47.1(7) . . . . ?
O3 Cu1 N1 C27 148.5(2) . . . . ?
N2 Cu1 N1 C27 -4.4(2) . . . . ?
O5 Cu1 N1 C27 -113.1(2) . . . . ?
O1 Cu1 N2 C34 9.3(3) . . . . ?
O3 Cu1 N2 C34 103.5(4) . . . . ?
N1 Cu1 N2 C34 -179.3(3) . . . . ?
O5 Cu1 N2 C34 -89.3(3) . . . . ?
O1 Cu1 N2 C31 -167.1(2) . . . . ?
O3 Cu1 N2 C31 -73.0(3) . . . . ?
N1 Cu1 N2 C31 4.3(2) . . . . ?
O5 Cu1 N2 C31 94.3(2) . . . . ?
O3 Cu1 O1 C1 104.2(3) . . . . ?
N1 Cu1 O1 C1 -154.3(5) . . . . ?
N2 Cu1 O1 C1 -103.6(3) . . . . ?
O5 Cu1 O1 C1 5.8(3) . . . . ?
O1 Cu1 O3 C12 -89.9(3) . . . . ?
N1 Cu1 O3 C12 100.9(3) . . . . ?
N2 Cu1 O3 C12 175.5(3) . . . . ?
O5 Cu1 O3 C12 7.7(3) . . . . ?
Cu1 O1 C1 O2 9.0(5) . . . . ?
Cu1 O1 C1 C2 -172.8(2) . . . . ?
O2 C1 C2 C3 167.2(4) . . . . ?
O1 C1 C2 C3 -11.1(5) . . . . ?
O2 C1 C2 C7 -10.9(5) . . . . ?
O1 C1 C2 C7 170.8(4) . . . . ?
C7 C2 C3 C4 -1.1(6) . . . . ?
C1 C2 C3 C4 -179.3(4) . . . . ?
C2 C3 C4 C5 -0.3(7) . . . . ?
C3 C4 C5 C6 0.8(7) . . . . ?
C3 C4 C5 C8 179.8(4) . . . . ?
C4 C5 C6 C7 -0.1(7) . . . . ?
C8 C5 C6 C7 -179.0(4) . . . . ?
C3 C2 C7 C6 1.9(6) . . . . ?
C1 C2 C7 C6 -180.0(4) . . . . ?
C5 C6 C7 C2 -1.3(7) . . . . ?
C6 C5 C8 C11 -22.0(9) . . . . ?
C4 C5 C8 C11 159.2(8) . . . . ?
C6 C5 C8 C10 106.7(8) . . . . ?
C4 C5 C8 C10 -72.1(9) . . . . ?
C6 C5 C8 C9 -139.6(6) . . . . ?
C4 C5 C8 C9 41.5(7) . . . . ?
Cu1 O3 C12 O4 -14.1(5) . . . . ?
Cu1 O3 C12 C13 167.3(2) . . . . ?
O4 C12 C13 C14 8.0(5) . . . . ?
O3 C12 C13 C14 -173.4(3) . . . . ?
O4 C12 C13 C18 -170.6(3) . . . . ?
O3 C12 C13 C18 8.0(5) . . . . ?
C18 C13 C14 C15 -0.4(5) . . . . ?
C12 C13 C14 C15 -179.0(3) . . . . ?
C13 C14 C15 C16 0.8(6) . . . . ?
C14 C15 C16 C17 -0.4(5) . . . . ?
C14 C15 C16 C19 177.3(3) . . . . ?
C15 C16 C17 C18 -0.3(5) . . . . ?
C19 C16 C17 C18 -178.1(3) . . . . ?
C14 C13 C18 C17 -0.3(5) . . . . ?
C12 C13 C18 C17 178.3(3) . . . . ?
C16 C17 C18 C13 0.7(6) . . . . ?
C15 C16 C19 C20 25.2(5) . . . . ?
C17 C16 C19 C20 -157.2(4) . . . . ?
C15 C16 C19 C22 148.1(4) . . . . ?
C17 C16 C19 C22 -34.2(5) . . . . ?
C15 C16 C19 C21 -93.7(4) . . . . ?
C17 C16 C19 C21 84.0(4) . . . . ?
C27 N1 C23 C24 0.1(6) . . . . ?
Cu1 N1 C23 C24 178.9(3) . . . . ?
N1 C23 C24 C25 -1.7(7) . . . . ?
C23 C24 C25 C26 1.3(7) . . . . ?
C24 C25 C26 C27 0.5(6) . . . . ?
C24 C25 C26 C28 179.0(4) . . . . ?
C23 N1 C27 C26 1.9(5) . . . . ?
Cu1 N1 C27 C26 -177.1(3) . . . . ?
C23 N1 C27 C31 -177.2(3) . . . . ?
Cu1 N1 C27 C31 3.8(4) . . . . ?
C25 C26 C27 N1 -2.2(5) . . . . ?
C28 C26 C27 N1 179.3(3) . . . . ?
C25 C26 C27 C31 176.9(3) . . . . ?
C28 C26 C27 C31 -1.7(5) . . . . ?
C27 C26 C28 C29 2.0(6) . . . . ?
C25 C26 C28 C29 -176.5(4) . . . . ?
C26 C28 C29 C30 -0.4(6) . . . . ?
C28 C29 C30 C31 -1.5(5) . . . . ?
C28 C29 C30 C32 178.4(4) . . . . ?
C34 N2 C31 C30 0.5(5) . . . . ?
Cu1 N2 C31 C30 177.4(3) . . . . ?
C34 N2 C31 C27 179.6(3) . . . . ?
Cu1 N2 C31 C27 -3.5(4) . . . . ?
C32 C30 C31 N2 0.9(5) . . . . ?
C29 C30 C31 N2 -179.2(3) . . . . ?
C32 C30 C31 C27 -178.2(3) . . . . ?
C29 C30 C31 C27 1.7(5) . . . . ?
N1 C27 C31 N2 -0.2(4) . . . . ?
C26 C27 C31 N2 -179.3(3) . . . . ?
N1 C27 C31 C30 178.9(3) . . . . ?
C26 C27 C31 C30 -0.2(5) . . . . ?
C31 C30 C32 C33 -1.2(5) . . . . ?
C29 C30 C32 C33 178.9(3) . . . . ?
C30 C32 C33 C34 0.2(6) . . . . ?
C31 N2 C34 C33 -1.6(5) . . . . ?
Cu1 N2 C34 C33 -177.9(3) . . . . ?
C32 C33 C34 N2 1.3(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.96
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 993872'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_RK1-141

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H68 Mn2 N4 O8, 2(C H4 O)'
_chemical_formula_sum            'C70 H76 Mn2 N4 O10'
_chemical_formula_weight         1243.23

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   31.05(14)
_cell_length_b                   9.83(4)
_cell_length_c                   20.58(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.19(8)
_cell_angle_gamma                90.00
_cell_volume                     6161(46)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3904
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      25.4

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2616
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21924
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5412
_reflns_number_gt                4397
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0904P)²+9.5989P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5412
_refine_ls_number_parameters     454
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1628
_refine_ls_wR_factor_gt          0.1522
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.89815(12) -0.0436(3) 0.05556(18) 0.0338(8) Uani 1 1 d . . .
C2 C 0.85987(11) -0.0714(3) 0.00079(15) 0.0265(7) Uani 1 1 d . . .
C3 C 0.86510(11) -0.0827(3) -0.06476(17) 0.0287(7) Uani 1 1 d . . .
C4 C 0.82894(12) -0.1013(3) -0.11530(17) 0.0312(8) Uani 1 1 d . . .
C5 C 0.78653(11) -0.1112(3) -0.10219(17) 0.0324(8) Uani 1 1 d . . .
C6 C 0.74679(13) -0.1305(4) -0.15879(18) 0.0421(9) Uani 1 1 d . . .
C7 C 0.7443(2) -0.0175(6) -0.2071(3) 0.0818(18) Uani 1 1 d . . .
H7A H 0.7430 0.0695 -0.1843 0.123 Uiso 1 1 calc R . .
H7B H 0.7179 -0.0282 -0.2416 0.123 Uiso 1 1 calc R . .
H7C H 0.7703 -0.0192 -0.2274 0.123 Uiso 1 1 calc R . .
C8 C 0.74869(17) -0.2702(5) -0.1891(3) 0.0739(16) Uani 1 1 d . . .
H8A H 0.7503 -0.3396 -0.1545 0.111 Uiso 1 1 calc R . .
H8B H 0.7747 -0.2765 -0.2092 0.111 Uiso 1 1 calc R . .
H8C H 0.7223 -0.2848 -0.2231 0.111 Uiso 1 1 calc R . .
C9 C 0.70244(16) -0.1319(8) -0.1334(3) 0.0856(19) Uani 1 1 d . . .
H9A H 0.7030 -0.2051 -0.1009 0.128 Uiso 1 1 calc R . .
H9B H 0.6781 -0.1471 -0.1708 0.128 Uiso 1 1 calc R . .
H9C H 0.6984 -0.0443 -0.1126 0.128 Uiso 1 1 calc R . .
C10 C 0.78228(12) -0.1025(4) -0.03682(19) 0.0366(9) Uani 1 1 d . . .
C11 C 0.81780(12) -0.0817(4) 0.01382(18) 0.0365(8) Uani 1 1 d . . .
C12 C 0.94795(10) -0.1120(3) 0.30057(16) 0.0228(7) Uani 1 1 d . . .
C13 C 0.92064(9) -0.1735(3) 0.34544(15) 0.0208(6) Uani 1 1 d . . .
C14 C 0.87677(10) -0.2105(3) 0.32179(16) 0.0232(7) Uani 1 1 d . . .
C15 C 0.85318(10) -0.2739(3) 0.36286(16) 0.0250(7) Uani 1 1 d . . .
C16 C 0.87099(10) -0.3017(3) 0.42934(15) 0.0225(6) Uani 1 1 d . . .
C17 C 0.84474(10) -0.3788(3) 0.47310(16) 0.0284(7) Uani 1 1 d . . .
C18 C 0.80118(12) -0.3048(4) 0.4732(2) 0.0424(9) Uani 1 1 d . . .
H18A H 0.7844 -0.3544 0.5012 0.064 Uiso 1 1 calc R . .
H18B H 0.7842 -0.3002 0.4278 0.064 Uiso 1 1 calc R . .
H18C H 0.8072 -0.2124 0.4905 0.064 Uiso 1 1 calc R . .
C19 C 0.83542(15) -0.5230(4) 0.4456(2) 0.0482(10) Uani 1 1 d . . .
H19A H 0.8186 -0.5731 0.4735 0.072 Uiso 1 1 calc R . .
H19B H 0.8632 -0.5700 0.4456 0.072 Uiso 1 1 calc R . .
H19C H 0.8185 -0.5180 0.4003 0.072 Uiso 1 1 calc R . .
C20 C 0.86951(13) -0.3890(5) 0.54471(19) 0.0503(11) Uani 1 1 d . . .
H20A H 0.8517 -0.4391 0.5710 0.075 Uiso 1 1 calc R . .
H20B H 0.8754 -0.2974 0.5630 0.075 Uiso 1 1 calc R . .
H20C H 0.8973 -0.4370 0.5460 0.075 Uiso 1 1 calc R . .
C21 C 0.91422(10) -0.2588(3) 0.45307(15) 0.0232(7) Uani 1 1 d . . .
C22 C 0.93851(10) -0.1963(3) 0.41200(15) 0.0226(6) Uani 1 1 d . . .
C23 C 0.91202(10) 0.2244(3) 0.26159(15) 0.0267(7) Uani 1 1 d . . .
C24 C 0.89855(11) 0.3502(4) 0.28363(17) 0.0309(7) Uani 1 1 d . . .
C25 C 0.91203(11) 0.4680(3) 0.25885(17) 0.0311(8) Uani 1 1 d . . .
C26 C 0.93929(11) 0.4625(3) 0.21109(16) 0.0265(7) Uani 1 1 d . . .
C27 C 0.95492(12) 0.5815(3) 0.18289(17) 0.0331(8) Uani 1 1 d . . .
C28 C 0.98178(12) 0.5709(3) 0.13816(17) 0.0325(8) Uani 1 1 d . . .
C29 C 0.99438(10) 0.4397(3) 0.11714(16) 0.0265(7) Uani 1 1 d . . .
C30 C 1.02198(11) 0.4219(4) 0.07132(16) 0.0303(8) Uani 1 1 d . . .
C31 C 1.03107(11) 0.2935(4) 0.05143(16) 0.0283(7) Uani 1 1 d . . .
C32 C 1.01257(10) 0.1814(3) 0.07807(15) 0.0251(7) Uani 1 1 d . . .
C33 C 0.97864(10) 0.3216(3) 0.14276(14) 0.0222(6) Uani 1 1 d . . .
C34 C 0.95087(10) 0.3328(3) 0.19207(14) 0.0224(6) Uani 1 1 d . . .
C35 C 0.80832(18) 0.1519(6) 0.1595(3) 0.0754(15) Uani 1 1 d . . .
H35A H 0.7818 0.1712 0.1770 0.113 Uiso 1 1 calc R . .
H35B H 0.8002 0.1319 0.1120 0.113 Uiso 1 1 calc R . .
H35C H 0.8278 0.2312 0.1663 0.113 Uiso 1 1 calc R . .
N1 N 0.93789(8) 0.2156(2) 0.21700(12) 0.0216(5) Uani 1 1 d . . .
N2 N 0.98717(8) 0.1936(2) 0.12305(12) 0.0214(5) Uani 1 1 d . . .
O1 O 0.93620(8) -0.0691(3) 0.04900(14) 0.0450(7) Uani 1 1 d . . .
O2 O 0.89019(9) 0.0076(3) 0.10856(12) 0.0455(7) Uani 1 1 d . . .
O3 O 0.93042(7) -0.0929(2) 0.24096(11) 0.0289(5) Uani 1 1 d . . .
O4 O 1.01268(7) -0.0853(2) 0.17401(11) 0.0326(6) Uani 1 1 d . . .
O5 O 0.83011(11) 0.0387(4) 0.19282(17) 0.0660(9) Uani 1 1 d . . .
H5 H 0.8534 0.0242 0.1790 0.099 Uiso 1 1 calc R . .
Mn1 Mn 0.954217(14) 0.01878(4) 0.16672(2) 0.02129(18) Uani 1 1 d . . .
H3 H 0.8929(11) -0.074(4) -0.0726(16) 0.027(9) Uiso 1 1 d . . .
H4 H 0.8353(12) -0.107(4) -0.1628(19) 0.044(11) Uiso 1 1 d . . .
H10 H 0.7583(14) -0.110(5) -0.0294(19) 0.045(12) Uiso 1 1 d . . .
H11 H 0.8124(15) -0.066(5) 0.057(2) 0.063(14) Uiso 1 1 d . . .
H14 H 0.8638(12) -0.188(4) 0.2757(18) 0.034(10) Uiso 1 1 d . . .
H15 H 0.8243(13) -0.288(4) 0.3446(18) 0.034(10) Uiso 1 1 d . . .
H21 H 0.9287(11) -0.275(4) 0.5044(18) 0.032(9) Uiso 1 1 d . . .
H22 H 0.9674(12) -0.169(4) 0.4323(16) 0.027(9) Uiso 1 1 d . . .
H23 H 0.9001(11) 0.137(4) 0.2803(16) 0.027(9) Uiso 1 1 d . . .
H24 H 0.8802(11) 0.353(4) 0.3130(17) 0.030(9) Uiso 1 1 d . . .
H25 H 0.9062(12) 0.560(4) 0.2731(18) 0.036(10) Uiso 1 1 d . . .
H27 H 0.9457(11) 0.674(4) 0.1964(17) 0.032(9) Uiso 1 1 d . . .
H28 H 0.9916(10) 0.649(4) 0.1221(15) 0.021(8) Uiso 1 1 d . . .
H30 H 1.0331(11) 0.495(4) 0.0571(17) 0.023(9) Uiso 1 1 d . . .
H31 H 1.0501(11) 0.278(4) 0.0225(17) 0.031(9) Uiso 1 1 d . . .
H32 H 1.0192(10) 0.086(4) 0.0628(15) 0.024(8) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.241(7) . ?
C1 O2 1.268(6) . ?
C1 C2 1.496(7) . ?
C2 C11 1.387(8) . ?
C2 C3 1.394(7) . ?
C3 C4 1.387(7) . ?
C3 H3 0.91(3) . ?
C4 C5 1.398(8) . ?
C4 H4 1.04(4) . ?
C5 C10 1.380(8) . ?
C5 C6 1.536(7) . ?
C6 C7 1.483(8) . ?
C6 C8 1.513(8) . ?
C6 C9 1.565(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.378(7) . ?
C10 H10 0.79(4) . ?
C11 H11 0.95(5) . ?
C12 O3 1.256(6) . ?
C12 O4 1.261(6) 2_755 ?
C12 C13 1.497(6) . ?
C13 C22 1.393(7) . ?
C13 C14 1.403(7) . ?
C14 C15 1.371(6) . ?
C14 H14 0.98(4) . ?
C15 C16 1.399(7) . ?
C15 H15 0.91(4) . ?
C16 C21 1.401(7) . ?
C16 C17 1.528(6) . ?
C17 C20 1.528(8) . ?
C17 C19 1.532(7) . ?
C17 C18 1.536(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.381(6) . ?
C21 H21 1.08(4) . ?
C22 H22 0.95(4) . ?
C23 N1 1.334(6) . ?
C23 C24 1.408(6) . ?
C23 H23 1.04(4) . ?
C24 C25 1.363(7) . ?
C24 H24 0.91(4) . ?
C25 C26 1.417(7) . ?
C25 H25 0.98(4) . ?
C26 C34 1.401(6) . ?
C26 C27 1.431(6) . ?
C27 C28 1.361(7) . ?
C27 H27 1.00(4) . ?
C28 C29 1.439(7) . ?
C28 H28 0.91(4) . ?
C29 C33 1.401(6) . ?
C29 C30 1.403(7) . ?
C30 C31 1.373(7) . ?
C30 H30 0.87(4) . ?
C31 C32 1.402(6) . ?
C31 H31 0.93(4) . ?
C32 N2 1.333(6) . ?
C32 H32 1.02(4) . ?
C33 N2 1.363(6) . ?
C33 C34 1.458(6) . ?
C34 N1 1.354(6) . ?
C35 O5 1.409(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
N1 Mn1 2.296(7) . ?
N2 Mn1 2.273(7) . ?
O2 Mn1 2.115(8) . ?
O3 Mn1 2.127(6) . ?
O4 C12 1.261(6) 2_755 ?
O4 Mn1 2.063(8) . ?
O5 H5 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 121.5(3) . . ?
O1 C1 C2 121.0(4) . . ?
O2 C1 C2 117.5(4) . . ?
C11 C2 C3 118.2(3) . . ?
C11 C2 C1 120.5(4) . . ?
C3 C2 C1 121.3(4) . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 122(2) . . ?
C2 C3 H3 117(2) . . ?
C3 C4 C5 121.4(4) . . ?
C3 C4 H4 116(2) . . ?
C5 C4 H4 123(2) . . ?
C10 C5 C4 117.1(3) . . ?
C10 C5 C6 122.2(4) . . ?
C4 C5 C6 120.7(4) . . ?
C7 C6 C8 113.8(5) . . ?
C7 C6 C5 110.3(4) . . ?
C8 C6 C5 109.6(3) . . ?
C7 C6 C9 107.2(5) . . ?
C8 C6 C9 103.7(4) . . ?
C5 C6 C9 112.2(5) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C5 122.2(4) . . ?
C11 C10 H10 121(3) . . ?
C5 C10 H10 117(3) . . ?
C10 C11 C2 120.7(4) . . ?
C10 C11 H11 118(3) . . ?
C2 C11 H11 121(3) . . ?
O3 C12 O4 125.2(3) . 2_755 ?
O3 C12 C13 118.2(4) . . ?
O4 C12 C13 116.6(4) 2_755 . ?
C22 C13 C14 118.3(3) . . ?
C22 C13 C12 120.4(4) . . ?
C14 C13 C12 121.3(4) . . ?
C15 C14 C13 120.2(4) . . ?
C15 C14 H14 122(2) . . ?
C13 C14 H14 118(2) . . ?
C14 C15 C16 122.3(4) . . ?
C14 C15 H15 115(2) . . ?
C16 C15 H15 123(2) . . ?
C15 C16 C21 116.9(3) . . ?
C15 C16 C17 121.2(4) . . ?
C21 C16 C17 121.9(4) . . ?
C20 C17 C16 112.0(4) . . ?
C20 C17 C19 108.6(3) . . ?
C16 C17 C19 109.0(3) . . ?
C20 C17 C18 108.0(3) . . ?
C16 C17 C18 109.6(4) . . ?
C19 C17 C18 109.6(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C16 121.4(4) . . ?
C22 C21 H21 119.5(19) . . ?
C16 C21 H21 119.1(19) . . ?
C21 C22 C13 120.8(4) . . ?
C21 C22 H22 116(2) . . ?
C13 C22 H22 123(2) . . ?
N1 C23 C24 122.3(3) . . ?
N1 C23 H23 120.4(19) . . ?
C24 C23 H23 117.2(19) . . ?
C25 C24 C23 119.5(4) . . ?
C25 C24 H24 120(2) . . ?
C23 C24 H24 120(2) . . ?
C24 C25 C26 119.7(3) . . ?
C24 C25 H25 126(2) . . ?
C26 C25 H25 114(2) . . ?
C34 C26 C25 116.6(3) . . ?
C34 C26 C27 120.3(4) . . ?
C25 C26 C27 123.1(3) . . ?
C28 C27 C26 120.9(4) . . ?
C28 C27 H27 120(2) . . ?
C26 C27 H27 119(2) . . ?
C27 C28 C29 120.7(3) . . ?
C27 C28 H28 118(2) . . ?
C29 C28 H28 121(2) . . ?
C33 C29 C30 116.9(3) . . ?
C33 C29 C28 119.6(4) . . ?
C30 C29 C28 123.5(3) . . ?
C31 C30 C29 120.2(3) . . ?
C31 C30 H30 123(2) . . ?
C29 C30 H30 117(2) . . ?
C30 C31 C32 118.8(4) . . ?
C30 C31 H31 123(2) . . ?
C32 C31 H31 119(2) . . ?
N2 C32 C31 122.9(3) . . ?
N2 C32 H32 118.6(19) . . ?
C31 C32 H32 118.4(19) . . ?
N2 C33 C29 123.4(4) . . ?
N2 C33 C34 116.9(3) . . ?
C29 C33 C34 119.8(3) . . ?
N1 C34 C26 123.8(4) . . ?
N1 C34 C33 117.4(3) . . ?
C26 C34 C33 118.8(3) . . ?
O5 C35 H35A 109.5 . . ?
O5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C23 N1 C34 118.0(3) . . ?
C23 N1 Mn1 125.4(2) . . ?
C34 N1 Mn1 116.0(3) . . ?
C32 N2 C33 117.7(3) . . ?
C32 N2 Mn1 125.4(3) . . ?
C33 N2 Mn1 116.8(3) . . ?
C1 O2 Mn1 100.9(3) . . ?
C12 O3 Mn1 129.3(3) . . ?
C12 O4 Mn1 154.4(2) 2_755 . ?
C35 O5 H5 109.5 . . ?
O4 Mn1 O2 137.1(2) . . ?
O4 Mn1 O3 96.6(2) . . ?
O2 Mn1 O3 87.7(3) . . ?
O4 Mn1 N2 86.9(3) . . ?
O2 Mn1 N2 105.2(2) . . ?
O3 Mn1 N2 156.95(10) . . ?
O4 Mn1 N1 130.74(13) . . ?
O2 Mn1 N1 91.9(2) . . ?
O3 Mn1 N1 88.4(3) . . ?
N2 Mn1 N1 72.4(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
O1 C1 C2 C11 160.7(3) . . . . ?
O2 C1 C2 C11 -19.6(5) . . . . ?
O1 C1 C2 C3 -21.6(5) . . . . ?
O2 C1 C2 C3 158.0(3) . . . . ?
C11 C2 C3 C4 1.1(5) . . . . ?
C1 C2 C3 C4 -176.6(3) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C3 C4 C5 C10 -0.4(5) . . . . ?
C3 C4 C5 C6 179.5(3) . . . . ?
C10 C5 C6 C7 122.0(5) . . . . ?
C4 C5 C6 C7 -57.8(5) . . . . ?
C10 C5 C6 C8 -111.9(5) . . . . ?
C4 C5 C6 C8 68.2(5) . . . . ?
C10 C5 C6 C9 2.6(6) . . . . ?
C4 C5 C6 C9 -177.2(4) . . . . ?
C4 C5 C10 C11 1.6(5) . . . . ?
C6 C5 C10 C11 -178.3(4) . . . . ?
C5 C10 C11 C2 -1.4(6) . . . . ?
C3 C2 C11 C10 0.0(5) . . . . ?
C1 C2 C11 C10 177.7(3) . . . . ?
O3 C12 C13 C22 -179.7(3) . . . . ?
O4 C12 C13 C22 1.3(4) 2_755 . . . ?
O3 C12 C13 C14 0.7(4) . . . . ?
O4 C12 C13 C14 -178.3(3) 2_755 . . . ?
C22 C13 C14 C15 -3.4(4) . . . . ?
C12 C13 C14 C15 176.2(3) . . . . ?
C13 C14 C15 C16 1.4(5) . . . . ?
C14 C15 C16 C21 1.4(5) . . . . ?
C14 C15 C16 C17 -176.9(3) . . . . ?
C15 C16 C17 C20 -176.2(3) . . . . ?
C21 C16 C17 C20 5.6(4) . . . . ?
C15 C16 C17 C19 63.6(4) . . . . ?
C21 C16 C17 C19 -114.6(4) . . . . ?
C15 C16 C17 C18 -56.4(4) . . . . ?
C21 C16 C17 C18 125.4(4) . . . . ?
C15 C16 C21 C22 -2.2(4) . . . . ?
C17 C16 C21 C22 176.1(3) . . . . ?
C16 C21 C22 C13 0.2(5) . . . . ?
C14 C13 C22 C21 2.6(4) . . . . ?
C12 C13 C22 C21 -177.0(3) . . . . ?
N1 C23 C24 C25 0.2(5) . . . . ?
C23 C24 C25 C26 0.2(5) . . . . ?
C24 C25 C26 C34 0.0(5) . . . . ?
C24 C25 C26 C27 -179.8(3) . . . . ?
C34 C26 C27 C28 -1.1(5) . . . . ?
C25 C26 C27 C28 178.6(3) . . . . ?
C26 C27 C28 C29 1.3(5) . . . . ?
C27 C28 C29 C33 0.3(5) . . . . ?
C27 C28 C29 C30 -179.9(3) . . . . ?
C33 C29 C30 C31 2.6(5) . . . . ?
C28 C29 C30 C31 -177.2(3) . . . . ?
C29 C30 C31 C32 -0.4(5) . . . . ?
C30 C31 C32 N2 -1.4(5) . . . . ?
C30 C29 C33 N2 -3.2(5) . . . . ?
C28 C29 C33 N2 176.6(3) . . . . ?
C30 C29 C33 C34 178.2(3) . . . . ?
C28 C29 C33 C34 -2.1(4) . . . . ?
C25 C26 C34 N1 -0.6(5) . . . . ?
C27 C26 C34 N1 179.2(3) . . . . ?
C25 C26 C34 C33 179.6(3) . . . . ?
C27 C26 C34 C33 -0.6(4) . . . . ?
N2 C33 C34 N1 3.6(4) . . . . ?
C29 C33 C34 N1 -177.6(3) . . . . ?
N2 C33 C34 C26 -176.6(3) . . . . ?
C29 C33 C34 C26 2.2(4) . . . . ?
C24 C23 N1 C34 -0.8(4) . . . . ?
C24 C23 N1 Mn1 -171.0(2) . . . . ?
C26 C34 N1 C23 1.0(4) . . . . ?
C33 C34 N1 C23 -179.2(3) . . . . ?
C26 C34 N1 Mn1 172.2(2) . . . . ?
C33 C34 N1 Mn1 -8.0(3) . . . . ?
C31 C32 N2 C33 1.0(4) . . . . ?
C31 C32 N2 Mn1 178.1(2) . . . . ?
C29 C33 N2 C32 1.4(4) . . . . ?
C34 C33 N2 C32 -179.9(2) . . . . ?
C29 C33 N2 Mn1 -176.0(2) . . . . ?
C34 C33 N2 Mn1 2.7(3) . . . . ?
O1 C1 O2 Mn1 -1.8(4) . . . . ?
C2 C1 O2 Mn1 178.6(2) . . . . ?
O4 C12 O3 Mn1 -12.1(4) 2_755 . . . ?
C13 C12 O3 Mn1 169.09(19) . . . . ?
C12 O4 Mn1 O2 -175.0(4) 2_755 . . . ?
C12 O4 Mn1 O3 -81.2(6) 2_755 . . . ?
C12 O4 Mn1 N2 75.9(6) 2_755 . . . ?
C12 O4 Mn1 N1 12.5(5) 2_755 . . . ?
C1 O2 Mn1 O4 -28.5(3) . . . . ?
C1 O2 Mn1 O3 -125.8(3) . . . . ?
C1 O2 Mn1 N2 73.6(3) . . . . ?
C1 O2 Mn1 N1 145.9(2) . . . . ?
C12 O3 Mn1 O4 56.3(3) . . . . ?
C12 O3 Mn1 O2 -166.6(3) . . . . ?
C12 O3 Mn1 N2 -41.5(4) . . . . ?
C12 O3 Mn1 N1 -74.6(3) . . . . ?
C32 N2 Mn1 O4 43.2(3) . . . . ?
C33 N2 Mn1 O4 -139.6(3) . . . . ?
C32 N2 Mn1 O2 -95.0(4) . . . . ?
C33 N2 Mn1 O2 82.2(3) . . . . ?
C32 N2 Mn1 O3 142.9(3) . . . . ?
C33 N2 Mn1 O3 -39.9(4) . . . . ?
C32 N2 Mn1 N1 177.9(3) . . . . ?
C33 N2 Mn1 N1 -5.0(2) . . . . ?
C23 N1 Mn1 O4 -113.1(4) . . . . ?
C34 N1 Mn1 O4 76.5(3) . . . . ?
C23 N1 Mn1 O2 72.0(4) . . . . ?
C34 N1 Mn1 O2 -98.4(3) . . . . ?
C23 N1 Mn1 O3 -15.7(2) . . . . ?
C34 N1 Mn1 O3 173.9(2) . . . . ?
C23 N1 Mn1 N2 177.3(3) . . . . ?
C34 N1 Mn1 N2 6.88(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 993873'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rk1-139

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H68 N4 O10 Zn2, 2(C H4 O)'
_chemical_formula_sum            'C68 H76 N4 O12 Zn2'
_chemical_formula_weight         1272.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   31.01(7)
_cell_length_b                   9.72(2)
_cell_length_c                   20.78(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.99(3)
_cell_angle_gamma                90.00
_cell_volume                     6126(24)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6155
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      31.3

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2672
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8417
_exptl_absorpt_correction_T_max  0.9668
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22418
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5404
_reflns_number_gt                5180
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0700P)²+13.9863P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5404
_refine_ls_number_parameters     424
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.1456
_refine_ls_wR_factor_gt          0.1346
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_restrained_S_all      1.193
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.51065(10) 0.1806(4) 0.58304(15) 0.0234(7) Uani 1 1 d . . .
H1 H 0.5168 0.0913 0.5687 0.028 Uiso 1 1 calc R . .
C2 C 0.52792(11) 0.2944(4) 0.55653(16) 0.0278(8) Uani 1 1 d . . .
H2 H 0.5464 0.2823 0.5258 0.033 Uiso 1 1 calc R . .
C3 C 0.51802(11) 0.4246(4) 0.57506(16) 0.0291(8) Uani 1 1 d . . .
H3 H 0.5296 0.5029 0.5571 0.035 Uiso 1 1 calc R . .
C4 C 0.49070(11) 0.4412(4) 0.62069(17) 0.0263(7) Uani 1 1 d . . .
C5 C 0.47711(13) 0.5723(4) 0.64103(19) 0.0338(8) Uani 1 1 d . . .
H5 H 0.4867 0.6540 0.6233 0.041 Uiso 1 1 calc R . .
C6 C 0.45066(13) 0.5810(4) 0.68540(19) 0.0352(9) Uani 1 1 d . . .
H6 H 0.4418 0.6689 0.6979 0.042 Uiso 1 1 calc R . .
C7 C 0.43590(12) 0.4601(4) 0.71361(18) 0.0282(8) Uani 1 1 d . . .
C8 C 0.40920(13) 0.4622(4) 0.76057(19) 0.0342(9) Uani 1 1 d . . .
H8 H 0.3998 0.5476 0.7753 0.041 Uiso 1 1 calc R . .
C9 C 0.39669(12) 0.3416(4) 0.78512(19) 0.0336(8) Uani 1 1 d . . .
H9 H 0.3785 0.3424 0.8167 0.040 Uiso 1 1 calc R . .
C10 C 0.41100(11) 0.2169(4) 0.76321(16) 0.0270(7) Uani 1 1 d . . .
H10 H 0.4023 0.1334 0.7806 0.032 Uiso 1 1 calc R . .
C11 C 0.44873(10) 0.3302(3) 0.69453(15) 0.0206(7) Uani 1 1 d . . .
C12 C 0.47597(10) 0.3203(3) 0.64596(15) 0.0208(7) Uani 1 1 d . . .
C13 C 0.40812(11) -0.0517(3) 0.54881(16) 0.0220(7) Uani 1 1 d . . .
C14 C 0.36655(10) -0.0744(3) 0.49819(15) 0.0210(7) Uani 1 1 d . . .
C15 C 0.36832(11) -0.0779(4) 0.43170(16) 0.0243(7) Uani 1 1 d . . .
H15 H 0.3960 -0.0698 0.4192 0.029 Uiso 1 1 calc R . .
C16 C 0.33058(11) -0.0928(4) 0.38389(16) 0.0261(7) Uani 1 1 d . . .
H16 H 0.3328 -0.0944 0.3390 0.031 Uiso 1 1 calc R . .
C17 C 0.28919(11) -0.1057(4) 0.39964(16) 0.0259(7) Uani 1 1 d . A .
C18 C 0.24755(11) -0.1179(4) 0.34540(18) 0.0349(9) Uani 1 1 d D . .
C22 C 0.28787(11) -0.1066(4) 0.46621(18) 0.0321(8) Uani 1 1 d . . .
H22 H 0.2604 -0.1186 0.4788 0.039 Uiso 1 1 calc R A .
C23 C 0.32557(11) -0.0904(4) 0.51444(17) 0.0299(8) Uani 1 1 d . A .
H23 H 0.3235 -0.0902 0.5594 0.036 Uiso 1 1 calc R . .
C24 C 0.55841(10) -0.2004(3) 0.58989(15) 0.0199(7) Uani 1 1 d . . .
H24 H 0.5288 -0.1747 0.5716 0.024 Uiso 1 1 calc R . .
C25 C 0.58357(10) -0.2626(3) 0.55091(15) 0.0216(7) Uani 1 1 d . . .
H25 H 0.5709 -0.2786 0.5058 0.026 Uiso 1 1 calc R . .
C26 C 0.62716(10) -0.3029(3) 0.57563(15) 0.0202(7) Uani 1 1 d . . .
C27 C 0.64472(10) -0.2726(3) 0.64157(16) 0.0224(7) Uani 1 1 d . . .
H27 H 0.6745 -0.2964 0.6597 0.027 Uiso 1 1 calc R . .
C28 C 0.61997(10) -0.2091(3) 0.68119(15) 0.0200(7) Uani 1 1 d . . .
H28 H 0.6329 -0.1888 0.7257 0.024 Uiso 1 1 calc R . .
C29 C 0.65488(11) -0.3774(4) 0.53374(17) 0.0276(8) Uani 1 1 d . . .
C30 C 0.6657(2) -0.5207(5) 0.5613(3) 0.0678(16) Uani 1 1 d . . .
H30A H 0.6835 -0.5691 0.5346 0.102 Uiso 1 1 calc R . .
H30B H 0.6383 -0.5716 0.5603 0.102 Uiso 1 1 calc R . .
H30C H 0.6823 -0.5139 0.6068 0.102 Uiso 1 1 calc R . .
C31 C 0.69742(13) -0.2973(5) 0.5346(2) 0.0483(11) Uani 1 1 d . . .
H31A H 0.7151 -0.3454 0.5077 0.073 Uiso 1 1 calc R . .
H31B H 0.7143 -0.2902 0.5800 0.073 Uiso 1 1 calc R . .
H31C H 0.6902 -0.2048 0.5168 0.073 Uiso 1 1 calc R . .
C32 C 0.63088(15) -0.3885(7) 0.4618(2) 0.0657(17) Uani 1 1 d . . .
H32A H 0.6497 -0.4367 0.4366 0.099 Uiso 1 1 calc R . .
H32B H 0.6242 -0.2961 0.4436 0.099 Uiso 1 1 calc R . .
H32C H 0.6034 -0.4398 0.4591 0.099 Uiso 1 1 calc R . .
C33 C 0.31249(18) 0.1308(7) 0.6521(3) 0.0699(16) Uani 1 1 d . . .
H33A H 0.3322 0.2103 0.6548 0.105 Uiso 1 1 calc R . .
H33B H 0.2879 0.1534 0.6731 0.105 Uiso 1 1 calc R . .
H33C H 0.3011 0.1073 0.6058 0.105 Uiso 1 1 calc R . .
C34 C 0.57608(9) -0.1748(3) 0.65608(15) 0.0170(6) Uani 1 1 d . . .
N1 N 0.48574(8) 0.1926(3) 0.62792(12) 0.0194(6) Uani 1 1 d . . .
N2 N 0.43629(9) 0.2107(3) 0.71895(13) 0.0210(6) Uani 1 1 d . . .
O1 O 0.40245(8) -0.0148(2) 0.60653(11) 0.0255(5) Uani 1 1 d . . .
O2 O 0.44416(8) -0.0658(3) 0.53452(12) 0.0332(6) Uani 1 1 d . . .
O003 O 0.54810(11) -0.1104(3) 0.69876(16) 0.0525(8) Uani 1 1 d . . .
O3 O 0.50874(7) -0.0860(3) 0.67182(11) 0.0264(5) Uani 1 1 d . . .
O4 O 0.43373(7) -0.0861(2) 0.74208(10) 0.0238(5) Uani 1 1 d . . .
O5 O 0.33569(10) 0.0191(4) 0.68429(17) 0.0536(8) Uani 1 1 d . . .
H5A H 0.3558 -0.0036 0.6648 0.080 Uiso 1 1 calc R . .
Zn1 Zn 0.455729(11) 0.02718(4) 0.672840(16) 0.01697(15) Uani 1 1 d . . .
C19A C 0.2494(2) -0.2589(7) 0.3099(3) 0.053(2) Uani 0.717(8) 1 d PD A 1
H19A H 0.2232 -0.2686 0.2744 0.080 Uiso 0.717(8) 1 calc PR A 1
H19B H 0.2501 -0.3340 0.3416 0.080 Uiso 0.717(8) 1 calc PR A 1
H19C H 0.2760 -0.2626 0.2914 0.080 Uiso 0.717(8) 1 calc PR A 1
C20A C 0.2458(2) -0.0040(7) 0.2949(3) 0.055(2) Uani 0.717(8) 1 d PD A 1
H20A H 0.2736 -0.0017 0.2796 0.083 Uiso 0.717(8) 1 calc PR A 1
H20B H 0.2412 0.0846 0.3149 0.083 Uiso 0.717(8) 1 calc PR A 1
H20C H 0.2214 -0.0215 0.2575 0.083 Uiso 0.717(8) 1 calc PR A 1
C21A C 0.2049(2) -0.1153(12) 0.3708(4) 0.064(3) Uani 0.717(8) 1 d PD A 1
H21A H 0.1797 -0.1236 0.3337 0.096 Uiso 0.717(8) 1 calc PR A 1
H21B H 0.2028 -0.0284 0.3938 0.096 Uiso 0.717(8) 1 calc PR A 1
H21C H 0.2047 -0.1923 0.4012 0.096 Uiso 0.717(8) 1 calc PR A 1
C19C C 0.2577(5) -0.129(2) 0.2774(6) 0.052(5) Uani 0.283(8) 1 d PD A 2
H19D H 0.2735 -0.0469 0.2681 0.079 Uiso 0.283(8) 1 calc PR A 2
H19E H 0.2300 -0.1379 0.2447 0.079 Uiso 0.283(8) 1 calc PR A 2
H19F H 0.2760 -0.2107 0.2754 0.079 Uiso 0.283(8) 1 calc PR A 2
C20C C 0.2257(5) 0.0280(15) 0.3445(8) 0.050(5) Uani 0.283(8) 1 d PD A 2
H20D H 0.2471 0.0987 0.3387 0.075 Uiso 0.283(8) 1 calc PR A 2
H20E H 0.2164 0.0434 0.3861 0.075 Uiso 0.283(8) 1 calc PR A 2
H20F H 0.2000 0.0329 0.3080 0.075 Uiso 0.283(8) 1 calc PR A 2
C21C C 0.2161(7) -0.220(3) 0.3640(11) 0.091(10) Uani 0.283(8) 1 d PD A 2
H21D H 0.1868 -0.2074 0.3359 0.136 Uiso 0.283(8) 1 calc PR A 2
H21E H 0.2144 -0.2066 0.4101 0.136 Uiso 0.283(8) 1 calc PR A 2
H21F H 0.2266 -0.3137 0.3582 0.136 Uiso 0.283(8) 1 calc PR A 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
C1 N1 1.334(5) . ?
C1 C2 1.391(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.376(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.406(6) . ?
C3 H3 0.9500 . ?
C4 C12 1.402(5) . ?
C4 C5 1.433(6) . ?
C5 C6 1.358(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.430(6) . ?
C6 H6 0.9500 . ?
C7 C11 1.405(5) . ?
C7 C8 1.405(6) . ?
C8 C9 1.367(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.399(5) . ?
C9 H9 0.9500 . ?
C10 N2 1.328(5) . ?
C10 H10 0.9500 . ?
C11 N2 1.355(5) . ?
C11 C12 1.448(5) . ?
C12 N1 1.349(5) . ?
C13 O2 1.222(5) . ?
C13 O1 1.298(5) . ?
C13 C14 1.501(5) . ?
C14 C23 1.390(5) . ?
C14 C15 1.395(6) . ?
C15 C16 1.376(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.394(6) . ?
C16 H16 0.9500 . ?
C17 C22 1.392(6) . ?
C17 C18 1.532(5) . ?
C18 C21C 1.499(15) . ?
C18 C19C 1.515(13) . ?
C18 C20A 1.519(8) . ?
C18 C21A 1.522(8) . ?
C18 C19A 1.564(7) . ?
C18 C20C 1.569(13) . ?
C22 C23 1.382(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.376(5) . ?
C24 C34 1.393(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.399(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.397(5) . ?
C26 C29 1.527(5) . ?
C27 C28 1.382(5) . ?
C27 H27 0.9500 . ?
C28 C34 1.393(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.517(7) . ?
C29 C31 1.528(6) . ?
C29 C32 1.529(6) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 O5 1.394(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 O003 1.500(5) . ?
N1 Zn1 2.164(4) . ?
N2 Zn1 2.169(4) . ?
O1 Zn1 1.962(4) . ?
O003 O3 1.255(5) . ?
O003 O4 1.264(5) 2_656 ?
O3 Zn1 1.982(4) . ?
O4 O003 1.264(5) 2_656 ?
O4 Zn1 2.039(4) . ?
O5 H5A 0.8400 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C19C H19D 0.9800 . ?
C19C H19E 0.9800 . ?
C19C H19F 0.9800 . ?
C20C H20D 0.9800 . ?
C20C H20E 0.9800 . ?
C20C H20F 0.9800 . ?
C21C H21D 0.9800 . ?
C21C H21E 0.9800 . ?
C21C H21F 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
N1 C1 C2 122.3(3) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C12 C4 C3 116.5(3) . . ?
C12 C4 C5 119.7(4) . . ?
C3 C4 C5 123.8(3) . . ?
C6 C5 C4 120.8(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 121.1(4) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C11 C7 C8 116.9(3) . . ?
C11 C7 C6 119.3(4) . . ?
C8 C7 C6 123.9(3) . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 122.5(3) . . ?
N2 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
N2 C11 C7 123.0(3) . . ?
N2 C11 C12 117.2(3) . . ?
C7 C11 C12 119.8(3) . . ?
N1 C12 C4 123.9(3) . . ?
N1 C12 C11 116.9(3) . . ?
C4 C12 C11 119.2(3) . . ?
O2 C13 O1 124.2(3) . . ?
O2 C13 C14 120.6(3) . . ?
O1 C13 C14 115.3(3) . . ?
C23 C14 C15 117.7(3) . . ?
C23 C14 C13 122.8(3) . . ?
C15 C14 C13 119.5(3) . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 121.7(3) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C22 C17 C16 116.9(3) . . ?
C22 C17 C18 122.4(3) . . ?
C16 C17 C18 120.7(3) . . ?
C21C C18 C19C 117.6(13) . . ?
C21C C18 C20A 136.9(9) . . ?
C19C C18 C20A 52.6(8) . . ?
C21C C18 C21A 42.5(12) . . ?
C19C C18 C21A 133.5(6) . . ?
C20A C18 C21A 108.6(5) . . ?
C21C C18 C17 110.8(8) . . ?
C19C C18 C17 112.7(6) . . ?
C20A C18 C17 110.9(4) . . ?
C21A C18 C17 113.8(4) . . ?
C21C C18 C19A 68.2(13) . . ?
C19C C18 C19A 57.3(8) . . ?
C20A C18 C19A 108.2(5) . . ?
C21A C18 C19A 107.3(5) . . ?
C17 C18 C19A 107.9(3) . . ?
C21C C18 C20C 107.5(14) . . ?
C19C C18 C20C 103.1(10) . . ?
C20A C18 C20C 51.7(7) . . ?
C21A C18 C20C 65.5(8) . . ?
C17 C18 C20C 103.6(6) . . ?
C19A C18 C20C 147.6(6) . . ?
C23 C22 C17 121.7(3) . . ?
C23 C22 H22 119.2 . . ?
C17 C22 H22 119.2 . . ?
C22 C23 C14 121.0(4) . . ?
C22 C23 H23 119.5 . . ?
C14 C23 H23 119.5 . . ?
C25 C24 C34 120.3(3) . . ?
C25 C24 H24 119.8 . . ?
C34 C24 H24 119.8 . . ?
C24 C25 C26 122.0(3) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C27 C26 C25 116.8(3) . . ?
C27 C26 C29 120.6(3) . . ?
C25 C26 C29 122.6(3) . . ?
C28 C27 C26 121.8(3) . . ?
C28 C27 H27 119.1 . . ?
C26 C27 H27 119.1 . . ?
C27 C28 C34 120.3(3) . . ?
C27 C28 H28 119.9 . . ?
C34 C28 H28 119.9 . . ?
C30 C29 C26 109.0(3) . . ?
C30 C29 C31 109.9(4) . . ?
C26 C29 C31 109.8(3) . . ?
C30 C29 C32 109.2(4) . . ?
C26 C29 C32 111.9(3) . . ?
C31 C29 C32 106.9(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O5 C33 H33A 109.5 . . ?
O5 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O5 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C28 C34 C24 118.7(3) . . ?
C28 C34 O003 121.2(3) . . ?
C24 C34 O003 120.1(3) . . ?
C1 N1 C12 118.1(3) . . ?
C1 N1 Zn1 126.9(2) . . ?
C12 N1 Zn1 115.0(2) . . ?
C10 N2 C11 118.4(3) . . ?
C10 N2 Zn1 126.9(2) . . ?
C11 N2 Zn1 114.4(2) . . ?
C13 O1 Zn1 116.8(2) . . ?
O3 O003 O4 126.4(3) . 2_656 ?
O3 O003 C34 116.3(3) . . ?
O4 O003 C34 117.2(3) 2_656 . ?
O003 O3 Zn1 146.3(2) . . ?
O003 O4 Zn1 129.9(2) 2_656 . ?
C33 O5 H5A 109.5 . . ?
O1 Zn1 O3 117.14(16) . . ?
O1 Zn1 O4 91.55(18) . . ?
O3 Zn1 O4 96.18(15) . . ?
O1 Zn1 N1 103.08(16) . . ?
O3 Zn1 N1 88.62(17) . . ?
O4 Zn1 N1 160.50(10) . . ?
O1 Zn1 N2 102.17(15) . . ?
O3 Zn1 N2 140.23(11) . . ?
O4 Zn1 N2 88.16(18) . . ?
N1 Zn1 N2 76.31(18) . . ?
C18 C19A H19A 109.5 . . ?
C18 C19A H19B 109.5 . . ?
C18 C19A H19C 109.5 . . ?
C18 C20A H20A 109.5 . . ?
C18 C20A H20B 109.5 . . ?
C18 C20A H20C 109.5 . . ?
C18 C21A H21A 109.5 . . ?
C18 C21A H21B 109.5 . . ?
C18 C21A H21C 109.5 . . ?
C18 C19C H19D 109.5 . . ?
C18 C19C H19E 109.5 . . ?
H19D C19C H19E 109.5 . . ?
C18 C19C H19F 109.5 . . ?
H19D C19C H19F 109.5 . . ?
H19E C19C H19F 109.5 . . ?
C18 C20C H20D 109.5 . . ?
C18 C20C H20E 109.5 . . ?
H20D C20C H20E 109.5 . . ?
C18 C20C H20F 109.5 . . ?
H20D C20C H20F 109.5 . . ?
H20E C20C H20F 109.5 . . ?
C18 C21C H21D 109.5 . . ?
C18 C21C H21E 109.5 . . ?
H21D C21C H21E 109.5 . . ?
C18 C21C H21F 109.5 . . ?
H21D C21C H21F 109.5 . . ?
H21E C21C H21F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -2.3(5) . . . . ?
C1 C2 C3 C4 0.2(5) . . . . ?
C2 C3 C4 C12 1.6(5) . . . . ?
C2 C3 C4 C5 -177.4(3) . . . . ?
C12 C4 C5 C6 1.1(5) . . . . ?
C3 C4 C5 C6 -180.0(3) . . . . ?
C4 C5 C6 C7 0.6(6) . . . . ?
C5 C6 C7 C11 -0.6(5) . . . . ?
C5 C6 C7 C8 178.8(4) . . . . ?
C11 C7 C8 C9 -0.4(5) . . . . ?
C6 C7 C8 C9 -179.8(4) . . . . ?
C7 C8 C9 C10 0.4(6) . . . . ?
C8 C9 C10 N2 -0.3(5) . . . . ?
C8 C7 C11 N2 0.4(5) . . . . ?
C6 C7 C11 N2 179.9(3) . . . . ?
C8 C7 C11 C12 179.5(3) . . . . ?
C6 C7 C11 C12 -1.0(5) . . . . ?
C3 C4 C12 N1 -1.5(5) . . . . ?
C5 C4 C12 N1 177.5(3) . . . . ?
C3 C4 C12 C11 178.3(3) . . . . ?
C5 C4 C12 C11 -2.7(5) . . . . ?
N2 C11 C12 N1 1.6(4) . . . . ?
C7 C11 C12 N1 -177.5(3) . . . . ?
N2 C11 C12 C4 -178.2(3) . . . . ?
C7 C11 C12 C4 2.7(5) . . . . ?
O2 C13 C14 C23 165.1(3) . . . . ?
O1 C13 C14 C23 -16.0(5) . . . . ?
O2 C13 C14 C15 -15.9(5) . . . . ?
O1 C13 C14 C15 163.0(3) . . . . ?
C23 C14 C15 C16 1.7(5) . . . . ?
C13 C14 C15 C16 -177.3(3) . . . . ?
C14 C15 C16 C17 -0.3(5) . . . . ?
C15 C16 C17 C22 -1.7(5) . . . . ?
C15 C16 C17 C18 178.1(3) . . . . ?
C22 C17 C18 C21C -39.8(15) . . . . ?
C16 C17 C18 C21C 140.3(15) . . . . ?
C22 C17 C18 C19C -174.0(9) . . . . ?
C16 C17 C18 C19C 6.1(10) . . . . ?
C22 C17 C18 C20A 129.0(5) . . . . ?
C16 C17 C18 C20A -50.9(5) . . . . ?
C22 C17 C18 C21A 6.2(7) . . . . ?
C16 C17 C18 C21A -173.6(6) . . . . ?
C22 C17 C18 C19A -112.7(5) . . . . ?
C16 C17 C18 C19A 67.4(5) . . . . ?
C22 C17 C18 C20C 75.2(9) . . . . ?
C16 C17 C18 C20C -104.7(8) . . . . ?
C16 C17 C22 C23 2.3(6) . . . . ?
C18 C17 C22 C23 -177.6(4) . . . . ?
C17 C22 C23 C14 -0.9(6) . . . . ?
C15 C14 C23 C22 -1.2(5) . . . . ?
C13 C14 C23 C22 177.8(3) . . . . ?
C34 C24 C25 C26 0.3(5) . . . . ?
C24 C25 C26 C27 -2.2(5) . . . . ?
C24 C25 C26 C29 177.4(3) . . . . ?
C25 C26 C27 C28 1.6(5) . . . . ?
C29 C26 C27 C28 -178.0(3) . . . . ?
C26 C27 C28 C34 0.8(5) . . . . ?
C27 C26 C29 C30 64.2(5) . . . . ?
C25 C26 C29 C30 -115.4(4) . . . . ?
C27 C26 C29 C31 -56.2(4) . . . . ?
C25 C26 C29 C31 124.2(4) . . . . ?
C27 C26 C29 C32 -174.8(4) . . . . ?
C25 C26 C29 C32 5.6(5) . . . . ?
C27 C28 C34 C24 -2.7(5) . . . . ?
C27 C28 C34 O003 177.8(3) . . . . ?
C25 C24 C34 C28 2.2(5) . . . . ?
C25 C24 C34 O003 -178.3(3) . . . . ?
C2 C1 N1 C12 2.4(5) . . . . ?
C2 C1 N1 Zn1 179.1(2) . . . . ?
C4 C12 N1 C1 -0.5(4) . . . . ?
C11 C12 N1 C1 179.7(3) . . . . ?
C4 C12 N1 Zn1 -177.5(2) . . . . ?
C11 C12 N1 Zn1 2.7(3) . . . . ?
C9 C10 N2 C11 0.3(5) . . . . ?
C9 C10 N2 Zn1 -173.4(3) . . . . ?
C7 C11 N2 C10 -0.4(5) . . . . ?
C12 C11 N2 C10 -179.5(3) . . . . ?
C7 C11 N2 Zn1 174.1(2) . . . . ?
C12 C11 N2 Zn1 -5.1(3) . . . . ?
O2 C13 O1 Zn1 2.5(4) . . . . ?
C14 C13 O1 Zn1 -176.3(2) . . . . ?
C28 C34 O003 O3 -178.6(3) . . . . ?
C24 C34 O003 O3 1.9(4) . . . . ?
C28 C34 O003 O4 1.4(4) . . . 2_656 ?
C24 C34 O003 O4 -178.1(3) . . . 2_656 ?
O4 O003 O3 Zn1 24.6(6) 2_656 . . . ?
C34 O003 O3 Zn1 -155.3(3) . . . . ?
C13 O1 Zn1 O3 -36.3(3) . . . . ?
C13 O1 Zn1 O4 -134.0(3) . . . . ?
C13 O1 Zn1 N1 59.0(3) . . . . ?
C13 O1 Zn1 N2 137.5(2) . . . . ?
O003 O3 Zn1 O1 -177.7(4) . . . . ?
O003 O3 Zn1 O4 -82.8(4) . . . . ?
O003 O3 Zn1 N1 78.3(4) . . . . ?
O003 O3 Zn1 N2 11.8(5) . . . . ?
O003 O4 Zn1 O1 178.9(3) 2_656 . . . ?
O003 O4 Zn1 O3 61.4(3) 2_656 . . . ?
O003 O4 Zn1 N1 -42.1(4) 2_656 . . . ?
O003 O4 Zn1 N2 -79.0(3) 2_656 . . . ?
C1 N1 Zn1 O1 -81.2(3) . . . . ?
C12 N1 Zn1 O1 95.6(3) . . . . ?
C1 N1 Zn1 O3 36.4(3) . . . . ?
C12 N1 Zn1 O3 -146.8(2) . . . . ?
C1 N1 Zn1 O4 141.1(3) . . . . ?
C12 N1 Zn1 O4 -42.1(4) . . . . ?
C1 N1 Zn1 N2 179.3(3) . . . . ?
C12 N1 Zn1 N2 -4.0(2) . . . . ?
C10 N2 Zn1 O1 78.0(3) . . . . ?
C11 N2 Zn1 O1 -95.9(3) . . . . ?
C10 N2 Zn1 O3 -110.7(3) . . . . ?
C11 N2 Zn1 O3 75.4(3) . . . . ?
C10 N2 Zn1 O4 -13.2(3) . . . . ?
C11 N2 Zn1 O4 172.9(2) . . . . ?
C10 N2 Zn1 N1 178.7(3) . . . . ?
C11 N2 Zn1 N1 4.8(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.557
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.142
_database_code_depnum_ccdc_archive 'CCDC 993874'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sg

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 Mn N2 O5'
_chemical_formula_sum            'C32 H32 Mn N2 O5'
_chemical_formula_weight         579.54

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41
_symmetry_space_group_name_Hall  'I 4bw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'

_cell_length_a                   20.2631(3)
_cell_length_b                   20.2631(3)
_cell_length_c                   13.8155(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5672.6(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6536
_cell_measurement_theta_min      1.78
_cell_measurement_theta_max      27.53

_exptl_crystal_description       plates
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2424
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8223
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_process_details   'Flack H D (1983), Acta Cryst. A39, 876-881'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'STOE AED2 four circle diffractometer'
_diffrn_measurement_method       'profile fitted theta omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29272
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         27.53
_reflns_number_total             6536
_reflns_number_gt                6021
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0341P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(9)
_refine_ls_number_reflns         6536
_refine_ls_number_parameters     489
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0614
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.349055(11) 0.367178(11) 0.783541(16) 0.01614(6) Uani 1 1 d . . .
O1 O 0.41848(6) 0.37910(6) 0.67217(9) 0.0262(3) Uani 1 1 d . . .
O2 O 0.42000(8) 0.27624(7) 0.61515(10) 0.0393(4) Uani 1 1 d . . .
O3 O 0.26516(6) 0.38900(5) 0.68894(8) 0.0204(2) Uani 1 1 d . . .
O4 O 0.42991(6) 0.32879(6) 0.87999(8) 0.0211(2) Uani 1 1 d . . .
O5 O 0.33074(7) 0.26066(6) 0.75730(11) 0.0226(3) Uani 1 1 d . . .
N1 N 0.29625(6) 0.37716(7) 0.92578(10) 0.0180(3) Uani 1 1 d . . .
N2 N 0.37705(6) 0.46699(7) 0.84068(10) 0.0185(3) Uani 1 1 d . . .
C1 C 0.43787(9) 0.33494(9) 0.61430(13) 0.0256(4) Uani 1 1 d . . .
C2 C 0.48583(9) 0.35689(9) 0.53725(15) 0.0288(4) Uani 1 1 d . . .
C3 C 0.46280(10) 0.39458(10) 0.46076(14) 0.0321(4) Uani 1 1 d . . .
C4 C 0.50687(12) 0.41411(11) 0.38827(16) 0.0402(5) Uani 1 1 d . . .
C5 C 0.57306(12) 0.39770(12) 0.39247(16) 0.0462(6) Uani 1 1 d . . .
C6 C 0.59451(12) 0.36018(13) 0.46940(17) 0.0463(6) Uani 1 1 d . . .
C7 C 0.55238(10) 0.33886(11) 0.54298(15) 0.0382(5) Uani 1 1 d . . .
C8 C 0.39220(12) 0.41624(12) 0.45352(16) 0.0393(5) Uani 1 1 d . . .
C9 C 0.61985(15) 0.42349(17) 0.3160(2) 0.0611(9) Uani 1 1 d . . .
C10 C 0.57768(14) 0.30030(15) 0.6273(2) 0.0513(6) Uani 1 1 d . . .
C11 C 0.21978(8) 0.43211(8) 0.68571(11) 0.0173(3) Uani 1 1 d . . .
C12 C 0.22501(8) 0.49170(8) 0.75090(12) 0.0180(3) Uani 1 1 d . . .
C13 C 0.19020(8) 0.49411(8) 0.83792(12) 0.0203(3) Uani 1 1 d . . .
C14 C 0.19724(9) 0.54976(9) 0.89659(13) 0.0251(4) Uani 1 1 d . . .
C15 C 0.23579(9) 0.60283(9) 0.86833(14) 0.0273(4) Uani 1 1 d . . .
C16 C 0.26784(8) 0.59983(8) 0.77922(15) 0.0271(4) Uani 1 1 d . . .
C17 C 0.26377(8) 0.54482(8) 0.72034(12) 0.0223(3) Uani 1 1 d . . .
C18 C 0.14456(9) 0.43929(10) 0.86716(14) 0.0272(4) Uani 1 1 d . . .
C19 C 0.24272(13) 0.66314(11) 0.9318(2) 0.0420(5) Uani 1 1 d . . .
C20 C 0.29976(12) 0.54213(12) 0.62615(15) 0.0344(5) Uani 1 1 d . . .
C21 C 0.25940(8) 0.33186(9) 0.96859(13) 0.0222(3) Uani 1 1 d . . .
C22 C 0.23314(9) 0.33997(9) 1.06139(13) 0.0270(4) Uani 1 1 d . . .
C23 C 0.24681(9) 0.39667(10) 1.11116(13) 0.0281(4) Uani 1 1 d . . .
C24 C 0.28533(9) 0.44576(9) 1.06821(12) 0.0237(4) Uani 1 1 d . . .
C25 C 0.30975(8) 0.43369(8) 0.97449(11) 0.0187(3) Uani 1 1 d . . .
C26 C 0.30123(10) 0.50706(10) 1.11461(14) 0.0318(4) Uani 1 1 d . . .
C27 C 0.34056(10) 0.55160(10) 1.07215(14) 0.0321(4) Uani 1 1 d . . .
C28 C 0.36839(9) 0.53964(9) 0.97884(12) 0.0248(4) Uani 1 1 d . . .
C29 C 0.35253(8) 0.48124(8) 0.92935(12) 0.0191(3) Uani 1 1 d . . .
C30 C 0.41271(9) 0.58339(9) 0.93361(15) 0.0293(4) Uani 1 1 d . . .
C31 C 0.43816(9) 0.56818(9) 0.84535(14) 0.0281(4) Uani 1 1 d . . .
C32 C 0.41858(8) 0.50933(8) 0.80049(13) 0.0228(3) Uani 1 1 d . . .
H4A H 0.4901(11) 0.4395(11) 0.3367(17) 0.034(6) Uiso 1 1 d . . .
H5A H 0.3563(12) 0.2558(12) 0.7177(19) 0.039(7) Uiso 1 1 d . . .
H5B H 0.3463(11) 0.2465(11) 0.8081(18) 0.034(6) Uiso 1 1 d . . .
H6A H 0.6359(13) 0.3504(13) 0.473(2) 0.051(8) Uiso 1 1 d . . .
H8A H 0.3880(11) 0.4629(13) 0.4811(16) 0.040(6) Uiso 1 1 d . . .
H8B H 0.3644(16) 0.3900(17) 0.483(3) 0.083(10) Uiso 1 1 d . . .
H8C H 0.3737(13) 0.4140(13) 0.382(2) 0.059(8) Uiso 1 1 d . . .
H9A H 0.5865(16) 0.4446(16) 0.252(3) 0.084(10) Uiso 1 1 d . . .
H9B H 0.6459(13) 0.4638(13) 0.346(2) 0.054(7) Uiso 1 1 d . . .
H9C H 0.6506(13) 0.3868(13) 0.3087(18) 0.047(7) Uiso 1 1 d . . .
H10A H 0.5480(12) 0.2688(11) 0.6439(16) 0.038(6) Uiso 1 1 d . . .
H10B H 0.5791(14) 0.3275(13) 0.686(2) 0.064(8) Uiso 1 1 d . . .
H10C H 0.6239(16) 0.2862(15) 0.615(3) 0.076(9) Uiso 1 1 d . . .
H14 H 0.1766(9) 0.5519(9) 0.9612(13) 0.015(4) Uiso 1 1 d . . .
H16 H 0.2965(11) 0.6355(11) 0.7556(16) 0.037(6) Uiso 1 1 d . . .
H18A H 0.1018(13) 0.4461(12) 0.8355(19) 0.050(7) Uiso 1 1 d . . .
H18B H 0.1401(11) 0.4353(11) 0.9391(18) 0.039(6) Uiso 1 1 d . . .
H18C H 0.1576(11) 0.3934(12) 0.8430(16) 0.040(6) Uiso 1 1 d . . .
H19A H 0.2100(14) 0.6943(14) 0.921(2) 0.063(8) Uiso 1 1 d . . .
H19B H 0.2373(14) 0.6555(14) 0.996(3) 0.068(9) Uiso 1 1 d . . .
H19C H 0.2861(16) 0.6815(15) 0.928(2) 0.073(9) Uiso 1 1 d . . .
H20A H 0.3367(16) 0.5727(16) 0.620(2) 0.077(9) Uiso 1 1 d . . .
H20B H 0.2738(14) 0.5293(14) 0.579(2) 0.056(7) Uiso 1 1 d . . .
H20C H 0.3255(15) 0.5035(15) 0.622(2) 0.068(9) Uiso 1 1 d . . .
H21 H 0.2508(9) 0.2939(9) 0.9301(13) 0.015(4) Uiso 1 1 d . . .
H22 H 0.2071(10) 0.3057(10) 1.0909(15) 0.030(5) Uiso 1 1 d . . .
H23 H 0.2311(11) 0.4030(11) 1.1726(17) 0.035(5) Uiso 1 1 d . . .
H26 H 0.2814(13) 0.5134(13) 1.178(2) 0.061(8) Uiso 1 1 d . . .
H27 H 0.3546(10) 0.5971(11) 1.1037(16) 0.034(6) Uiso 1 1 d . . .
H30 H 0.4264(11) 0.6263(12) 0.9700(16) 0.040(6) Uiso 1 1 d . . .
H31 H 0.4682(11) 0.5959(11) 0.8135(15) 0.035(6) Uiso 1 1 d . . .
H32 H 0.4369(9) 0.4996(10) 0.7395(15) 0.023(5) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.0987(12) . ?
Mn1 O3 2.1895(11) . ?
Mn1 O5 2.2199(13) . ?
Mn1 N2 2.2440(13) . ?
Mn1 N1 2.2467(14) . ?
Mn1 O4 2.2505(12) . ?
O1 C1 1.263(2) . ?
O2 C1 1.243(2) . ?
O3 C11 1.2691(19) . ?
O4 C11 1.250(2) 8_454 ?
O5 H5A 0.76(3) . ?
O5 H5B 0.82(3) . ?
N1 C21 1.323(2) . ?
N1 C25 1.356(2) . ?
N2 C32 1.324(2) . ?
N2 C29 1.353(2) . ?
C1 C2 1.508(2) . ?
C2 C3 1.385(3) . ?
C2 C7 1.399(3) . ?
C3 C4 1.399(3) . ?
C3 C8 1.500(3) . ?
C4 C5 1.383(4) . ?
C4 H4A 0.94(2) . ?
C5 C6 1.377(4) . ?
C5 C9 1.513(3) . ?
C6 C7 1.396(3) . ?
C6 H6A 0.86(3) . ?
C7 C10 1.493(4) . ?
C8 H8A 1.02(3) . ?
C8 H8B 0.88(4) . ?
C8 H8C 1.06(3) . ?
C9 H9A 1.19(4) . ?
C9 H9B 1.06(3) . ?
C9 H9C 0.97(3) . ?
C10 H10A 0.91(2) . ?
C10 H10B 0.98(3) . ?
C10 H10C 0.99(3) . ?
C11 O4 1.250(2) 7_544 ?
C11 C12 1.510(2) . ?
C12 C13 1.395(2) . ?
C12 C17 1.398(2) . ?
C13 C14 1.396(2) . ?
C13 C18 1.501(3) . ?
C14 C15 1.385(3) . ?
C14 H14 0.987(18) . ?
C15 C16 1.393(3) . ?
C15 C19 1.511(3) . ?
C16 C17 1.382(2) . ?
C16 H16 0.98(2) . ?
C17 C20 1.493(3) . ?
C18 H18A 0.98(3) . ?
C18 H18B 1.00(2) . ?
C18 H18C 1.02(2) . ?
C19 H19A 0.93(3) . ?
C19 H19B 0.91(3) . ?
C19 H19C 0.96(3) . ?
C20 H20A 0.98(3) . ?
C20 H20B 0.88(3) . ?
C20 H20C 0.94(3) . ?
C21 C22 1.398(2) . ?
C21 H21 0.952(18) . ?
C22 C23 1.367(3) . ?
C22 H22 0.96(2) . ?
C23 C24 1.397(3) . ?
C23 H23 0.92(2) . ?
C24 C25 1.408(2) . ?
C24 C26 1.434(3) . ?
C25 C29 1.438(2) . ?
C26 C27 1.339(3) . ?
C26 H26 0.97(3) . ?
C27 C28 1.428(3) . ?
C27 H27 1.06(2) . ?
C28 C29 1.404(2) . ?
C28 C30 1.408(3) . ?
C30 C31 1.359(3) . ?
C30 H30 1.04(2) . ?
C31 C32 1.401(3) . ?
C31 H31 0.94(2) . ?
C32 H32 0.94(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O3 93.41(5) . . ?
O1 Mn1 O5 95.98(5) . . ?
O3 Mn1 O5 88.23(5) . . ?
O1 Mn1 N2 89.12(5) . . ?
O3 Mn1 N2 102.96(5) . . ?
O5 Mn1 N2 167.44(5) . . ?
O1 Mn1 N1 161.83(5) . . ?
O3 Mn1 N1 97.71(5) . . ?
O5 Mn1 N1 98.67(5) . . ?
N2 Mn1 N1 74.43(5) . . ?
O1 Mn1 O4 89.19(5) . . ?
O3 Mn1 O4 171.30(4) . . ?
O5 Mn1 O4 83.24(5) . . ?
N2 Mn1 O4 85.37(4) . . ?
N1 Mn1 O4 81.95(5) . . ?
C1 O1 Mn1 126.24(11) . . ?
C11 O3 Mn1 136.27(10) . . ?
C11 O4 Mn1 131.50(10) 8_454 . ?
Mn1 O5 H5A 97.4(19) . . ?
Mn1 O5 H5B 97.8(16) . . ?
H5A O5 H5B 108(2) . . ?
C21 N1 C25 118.56(15) . . ?
C21 N1 Mn1 126.69(12) . . ?
C25 N1 Mn1 114.45(11) . . ?
C32 N2 C29 118.35(14) . . ?
C32 N2 Mn1 126.68(11) . . ?
C29 N2 Mn1 114.70(11) . . ?
O2 C1 O1 125.55(16) . . ?
O2 C1 C2 118.45(15) . . ?
O1 C1 C2 116.00(15) . . ?
C3 C2 C7 120.79(18) . . ?
C3 C2 C1 118.94(17) . . ?
C7 C2 C1 120.27(19) . . ?
C2 C3 C4 119.2(2) . . ?
C2 C3 C8 122.26(17) . . ?
C4 C3 C8 118.6(2) . . ?
C5 C4 C3 121.4(2) . . ?
C5 C4 H4A 120.8(13) . . ?
C3 C4 H4A 117.8(14) . . ?
C6 C5 C4 118.1(2) . . ?
C6 C5 C9 122.1(3) . . ?
C4 C5 C9 119.7(3) . . ?
C5 C6 C7 122.7(2) . . ?
C5 C6 H6A 118.2(19) . . ?
C7 C6 H6A 119.1(19) . . ?
C6 C7 C2 117.9(2) . . ?
C6 C7 C10 121.3(2) . . ?
C2 C7 C10 120.8(2) . . ?
C3 C8 H8A 108.9(13) . . ?
C3 C8 H8B 114(2) . . ?
H8A C8 H8B 109(3) . . ?
C3 C8 H8C 112.7(15) . . ?
H8A C8 H8C 111.1(19) . . ?
H8B C8 H8C 101(3) . . ?
C5 C9 H9A 106.6(16) . . ?
C5 C9 H9B 108.0(15) . . ?
H9A C9 H9B 107(2) . . ?
C5 C9 H9C 102.1(15) . . ?
H9A C9 H9C 124(2) . . ?
H9B C9 H9C 108(2) . . ?
C7 C10 H10A 109.8(15) . . ?
C7 C10 H10B 111.1(17) . . ?
H10A C10 H10B 102(2) . . ?
C7 C10 H10C 109.8(19) . . ?
H10A C10 H10C 118(2) . . ?
H10B C10 H10C 106(3) . . ?
O4 C11 O3 124.57(15) 7_544 . ?
O4 C11 C12 116.81(14) 7_544 . ?
O3 C11 C12 118.59(14) . . ?
C13 C12 C17 121.18(15) . . ?
C13 C12 C11 120.43(14) . . ?
C17 C12 C11 118.36(14) . . ?
C12 C13 C14 118.49(16) . . ?
C12 C13 C18 121.18(15) . . ?
C14 C13 C18 120.30(16) . . ?
C15 C14 C13 121.40(17) . . ?
C15 C14 H14 117.4(10) . . ?
C13 C14 H14 121.2(11) . . ?
C14 C15 C16 118.56(16) . . ?
C14 C15 C19 121.1(2) . . ?
C16 C15 C19 120.33(19) . . ?
C17 C16 C15 121.82(16) . . ?
C17 C16 H16 115.7(13) . . ?
C15 C16 H16 122.4(13) . . ?
C16 C17 C12 118.47(16) . . ?
C16 C17 C20 120.88(17) . . ?
C12 C17 C20 120.65(16) . . ?
C13 C18 H18A 108.7(15) . . ?
C13 C18 H18B 112.5(13) . . ?
H18A C18 H18B 112(2) . . ?
C13 C18 H18C 115.2(13) . . ?
H18A C18 H18C 102.1(19) . . ?
H18B C18 H18C 105.9(18) . . ?
C15 C19 H19A 112.7(18) . . ?
C15 C19 H19B 114.8(19) . . ?
H19A C19 H19B 101(2) . . ?
C15 C19 H19C 111.8(18) . . ?
H19A C19 H19C 113(2) . . ?
H19B C19 H19C 103(3) . . ?
C17 C20 H20A 115(2) . . ?
C17 C20 H20B 111.7(17) . . ?
H20A C20 H20B 126(3) . . ?
C17 C20 H20C 111.0(19) . . ?
H20A C20 H20C 96(2) . . ?
H20B C20 H20C 92(2) . . ?
N1 C21 C22 122.91(17) . . ?
N1 C21 H21 114.5(11) . . ?
C22 C21 H21 122.5(11) . . ?
C23 C22 C21 118.89(17) . . ?
C23 C22 H22 120.2(12) . . ?
C21 C22 H22 120.8(12) . . ?
C22 C23 C24 119.86(16) . . ?
C22 C23 H23 121.0(14) . . ?
C24 C23 H23 119.2(14) . . ?
C23 C24 C25 117.61(16) . . ?
C23 C24 C26 123.53(17) . . ?
C25 C24 C26 118.86(17) . . ?
N1 C25 C24 122.15(15) . . ?
N1 C25 C29 118.18(14) . . ?
C24 C25 C29 119.62(15) . . ?
C27 C26 C24 121.43(18) . . ?
C27 C26 H26 123.5(16) . . ?
C24 C26 H26 115.1(16) . . ?
C26 C27 C28 121.07(17) . . ?
C26 C27 H27 124.5(12) . . ?
C28 C27 H27 114.4(12) . . ?
C29 C28 C30 117.42(16) . . ?
C29 C28 C27 119.50(17) . . ?
C30 C28 C27 123.07(17) . . ?
N2 C29 C28 122.46(16) . . ?
N2 C29 C25 118.09(15) . . ?
C28 C29 C25 119.43(15) . . ?
C31 C30 C28 119.82(17) . . ?
C31 C30 H30 121.4(12) . . ?
C28 C30 H30 118.7(12) . . ?
C30 C31 C32 118.84(17) . . ?
C30 C31 H31 122.0(13) . . ?
C32 C31 H31 119.1(13) . . ?
N2 C32 C31 123.09(17) . . ?
N2 C32 H32 119.3(12) . . ?
C31 C32 H32 117.6(12) . . ?

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
O3 Mn1 O1 C1 -87.98(15) . . . . ?
O5 Mn1 O1 C1 0.59(15) . . . . ?
N2 Mn1 O1 C1 169.09(15) . . . . ?
N1 Mn1 O1 C1 144.24(17) . . . . ?
O4 Mn1 O1 C1 83.71(15) . . . . ?
O1 Mn1 O3 C11 -119.29(15) . . . . ?
O5 Mn1 O3 C11 144.82(16) . . . . ?
N2 Mn1 O3 C11 -29.41(16) . . . . ?
N1 Mn1 O3 C11 46.31(16) . . . . ?
O4 Mn1 O3 C11 133.5(3) . . . . ?
O1 Mn1 O4 C11 -134.77(14) . . . 8_454 ?
O3 Mn1 O4 C11 -27.2(4) . . . 8_454 ?
O5 Mn1 O4 C11 -38.65(14) . . . 8_454 ?
N2 Mn1 O4 C11 136.05(14) . . . 8_454 ?
N1 Mn1 O4 C11 61.15(14) . . . 8_454 ?
O1 Mn1 N1 C21 -150.82(16) . . . . ?
O3 Mn1 N1 C21 81.95(14) . . . . ?
O5 Mn1 N1 C21 -7.43(14) . . . . ?
N2 Mn1 N1 C21 -176.68(14) . . . . ?
O4 Mn1 N1 C21 -89.28(14) . . . . ?
O1 Mn1 N1 C25 22.7(2) . . . . ?
O3 Mn1 N1 C25 -104.55(11) . . . . ?
O5 Mn1 N1 C25 166.07(11) . . . . ?
N2 Mn1 N1 C25 -3.18(10) . . . . ?
O4 Mn1 N1 C25 84.22(11) . . . . ?
O1 Mn1 N2 C32 4.88(13) . . . . ?
O3 Mn1 N2 C32 -88.42(13) . . . . ?
O5 Mn1 N2 C32 119.1(2) . . . . ?
N1 Mn1 N2 C32 177.06(14) . . . . ?
O4 Mn1 N2 C32 94.14(13) . . . . ?
O1 Mn1 N2 C29 -169.00(11) . . . . ?
O3 Mn1 N2 C29 97.70(11) . . . . ?
O5 Mn1 N2 C29 -54.8(3) . . . . ?
N1 Mn1 N2 C29 3.18(11) . . . . ?
O4 Mn1 N2 C29 -79.74(11) . . . . ?
Mn1 O1 C1 O2 -1.7(3) . . . . ?
Mn1 O1 C1 C2 177.11(12) . . . . ?
O2 C1 C2 C3 105.5(2) . . . . ?
O1 C1 C2 C3 -73.4(2) . . . . ?
O2 C1 C2 C7 -74.0(2) . . . . ?
O1 C1 C2 C7 107.1(2) . . . . ?
C7 C2 C3 C4 0.6(3) . . . . ?
C1 C2 C3 C4 -178.92(17) . . . . ?
C7 C2 C3 C8 -178.44(19) . . . . ?
C1 C2 C3 C8 2.1(3) . . . . ?
C2 C3 C4 C5 -1.3(3) . . . . ?
C8 C3 C4 C5 177.7(2) . . . . ?
C3 C4 C5 C6 1.3(3) . . . . ?
C3 C4 C5 C9 -176.1(2) . . . . ?
C4 C5 C6 C7 -0.6(3) . . . . ?
C9 C5 C6 C7 176.7(2) . . . . ?
C5 C6 C7 C2 -0.1(3) . . . . ?
C5 C6 C7 C10 -177.7(2) . . . . ?
C3 C2 C7 C6 0.1(3) . . . . ?
C1 C2 C7 C6 179.61(17) . . . . ?
C3 C2 C7 C10 177.76(19) . . . . ?
C1 C2 C7 C10 -2.7(3) . . . . ?
Mn1 O3 C11 O4 -170.56(11) . . . 7_544 ?
Mn1 O3 C11 C12 11.5(2) . . . . ?
O4 C11 C12 C13 82.93(19) 7_544 . . . ?
O3 C11 C12 C13 -98.96(18) . . . . ?
O4 C11 C12 C17 -95.08(18) 7_544 . . . ?
O3 C11 C12 C17 83.03(19) . . . . ?
C17 C12 C13 C14 -3.0(2) . . . . ?
C11 C12 C13 C14 179.09(15) . . . . ?
C17 C12 C13 C18 175.29(16) . . . . ?
C11 C12 C13 C18 -2.7(2) . . . . ?
C12 C13 C14 C15 2.4(2) . . . . ?
C18 C13 C14 C15 -175.86(16) . . . . ?
C13 C14 C15 C16 0.0(3) . . . . ?
C13 C14 C15 C19 179.48(17) . . . . ?
C14 C15 C16 C17 -2.0(3) . . . . ?
C19 C15 C16 C17 178.51(18) . . . . ?
C15 C16 C17 C12 1.5(2) . . . . ?
C15 C16 C17 C20 -178.63(17) . . . . ?
C13 C12 C17 C16 1.1(2) . . . . ?
C11 C12 C17 C16 179.04(15) . . . . ?
C13 C12 C17 C20 -178.82(17) . . . . ?
C11 C12 C17 C20 -0.8(2) . . . . ?
C25 N1 C21 C22 0.7(2) . . . . ?
Mn1 N1 C21 C22 174.00(12) . . . . ?
N1 C21 C22 C23 -1.1(3) . . . . ?
C21 C22 C23 C24 1.3(3) . . . . ?
C22 C23 C24 C25 -1.2(3) . . . . ?
C22 C23 C24 C26 179.06(18) . . . . ?
C21 N1 C25 C24 -0.7(2) . . . . ?
Mn1 N1 C25 C24 -174.72(12) . . . . ?
C21 N1 C25 C29 176.96(14) . . . . ?
Mn1 N1 C25 C29 2.89(18) . . . . ?
C23 C24 C25 N1 0.9(2) . . . . ?
C26 C24 C25 N1 -179.36(16) . . . . ?
C23 C24 C25 C29 -176.69(15) . . . . ?
C26 C24 C25 C29 3.1(2) . . . . ?
C23 C24 C26 C27 177.26(18) . . . . ?
C25 C24 C26 C27 -2.5(3) . . . . ?
C24 C26 C27 C28 -0.1(3) . . . . ?
C26 C27 C28 C29 2.1(3) . . . . ?
C26 C27 C28 C30 -176.56(19) . . . . ?
C32 N2 C29 C28 1.4(2) . . . . ?
Mn1 N2 C29 C28 175.86(12) . . . . ?
C32 N2 C29 C25 -177.28(14) . . . . ?
Mn1 N2 C29 C25 -2.85(18) . . . . ?
C30 C28 C29 N2 -1.4(2) . . . . ?
C27 C28 C29 N2 179.82(15) . . . . ?
C30 C28 C29 C25 177.29(15) . . . . ?
C27 C28 C29 C25 -1.5(2) . . . . ?
N1 C25 C29 N2 0.0(2) . . . . ?
C24 C25 C29 N2 177.64(14) . . . . ?
N1 C25 C29 C28 -178.79(15) . . . . ?
C24 C25 C29 C28 -1.1(2) . . . . ?
C29 C28 C30 C31 0.1(3) . . . . ?
C27 C28 C30 C31 178.83(18) . . . . ?
C28 C30 C31 C32 1.1(3) . . . . ?
C29 N2 C32 C31 -0.2(2) . . . . ?
Mn1 N2 C32 C31 -173.85(12) . . . . ?
C30 C31 C32 N2 -1.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.036
_database_code_depnum_ccdc_archive 'CCDC 993875'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rm116b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 Cu N2 O5'
_chemical_formula_sum            'C32 H32 Cu N2 O5'
_chemical_formula_weight         588.14

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41 '
_symmetry_space_group_name_Hall  'I 4bw '

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

_cell_length_a                   20.5720(8)
_cell_length_b                   20.5720(14)
_cell_length_c                   13.725(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5808.5(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2837
_cell_measurement_theta_min      1.40
_cell_measurement_theta_max      24.98

_exptl_crystal_description       Prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2456
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'STOE AED2 four circle diffractometer'
_diffrn_measurement_method       'profile fitted theta omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2837
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2679
_reflns_number_gt                1871
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0508P)²+2.2694P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_number_reflns         2679
_refine_ls_number_parameters     377
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1063
_refine_ls_wR_factor_gt          0.0910
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4198(4) 0.1653(4) 0.9873(6) 0.068(2) Uani 1 1 d . . .
C2 C 0.4680(5) 0.1446(6) 1.0642(9) 0.094(3) Uani 1 1 d . . .
C3 C 0.5328(5) 0.1669(8) 1.0523(13) 0.144(7) Uani 1 1 d . . .
C4 C 0.5771(8) 0.1444(12) 1.1276(14) 0.198(14) Uani 1 1 d . . .
H4 H 0.613(7) 0.155(3) 1.1250(16) 0.238 Uiso 1 1 calc R . .
C5 C 0.5583(12) 0.1055(13) 1.2017(15) 0.205(15) Uani 1 1 d . . .
C6 C 0.4959(9) 0.0875(7) 1.2116(10) 0.162(8) Uani 1 1 d . . .
H6 H 0.4830 0.0630 1.2652 0.195 Uiso 1 1 calc R . .
C7 C 0.4496(7) 0.1060(6) 1.1396(11) 0.116(5) Uani 1 1 d . . .
C8 C 0.5530(6) 0.2076(9) 0.9697(14) 0.180(9) Uani 1 1 d . . .
H8A H 0.5986 0.2168 0.9748 0.270 Uiso 1 1 calc R . .
H8B H 0.5289 0.2475 0.9704 0.270 Uiso 1 1 calc R . .
H8C H 0.5446 0.1849 0.9098 0.270 Uiso 1 1 calc R . .
C9 C 0.6111(8) 0.0824(9) 1.2770(13) 0.320(17) Uani 1 1 d . . .
H9A H 0.5910 0.0557 1.3258 0.481 Uiso 1 1 calc R . .
H9B H 0.6306 0.1196 1.3074 0.481 Uiso 1 1 calc R . .
H9C H 0.6439 0.0577 1.2437 0.481 Uiso 1 1 calc R . .
C10 C 0.3813(7) 0.0843(5) 1.1522(8) 0.128(5) Uani 1 1 d . . .
H10A H 0.3782 0.0573 1.2091 0.192 Uiso 1 1 calc R . .
H10B H 0.3680 0.0599 1.0960 0.192 Uiso 1 1 calc R . .
H10C H 0.3536 0.1215 1.1597 0.192 Uiso 1 1 calc R . .
C11 C 0.4437(3) 0.2171(3) 0.6669(5) 0.0494(17) Uani 1 1 d . . .
C12 C 0.5008(3) 0.2264(3) 0.5975(5) 0.0458(17) Uani 1 1 d . . .
C13 C 0.5014(3) 0.1952(3) 0.5080(6) 0.0522(18) Uani 1 1 d . . .
C14 C 0.5536(4) 0.2046(4) 0.4473(7) 0.068(2) Uani 1 1 d . . .
H14 H 0.5531(4) 0.1868(18) 0.389(6) 0.081 Uiso 1 1 calc R . .
C15 C 0.6068(4) 0.2410(4) 0.4748(8) 0.075(3) Uani 1 1 d . . .
C16 C 0.6063(4) 0.2701(4) 0.5640(9) 0.077(3) Uani 1 1 d . . .
H16 H 0.639(3) 0.292(2) 0.581(2) 0.092 Uiso 1 1 calc R . .
C17 C 0.5540(4) 0.2644(4) 0.6272(6) 0.064(2) Uani 1 1 d . . .
C18 C 0.4467(4) 0.1507(4) 0.4784(6) 0.063(2) Uani 1 1 d . . .
H18A H 0.4144 0.1499 0.5288 0.094 Uiso 1 1 calc R . .
H18B H 0.4634 0.1076 0.4684 0.094 Uiso 1 1 calc R . .
H18C H 0.4276 0.1663 0.4190 0.094 Uiso 1 1 calc R . .
C19 C 0.6653(4) 0.2507(5) 0.4054(9) 0.123(4) Uani 1 1 d . . .
H19A H 0.6580 0.2271 0.3461 0.184 Uiso 1 1 calc R . .
H19B H 0.7042 0.2350 0.4362 0.184 Uiso 1 1 calc R . .
H19C H 0.6702 0.2961 0.3910 0.184 Uiso 1 1 calc R . .
C20 C 0.5539(5) 0.2966(5) 0.7243(8) 0.100(3) Uani 1 1 d . . .
H20A H 0.5138 0.2873 0.7572 0.150 Uiso 1 1 calc R . .
H20B H 0.5582 0.3428 0.7158 0.150 Uiso 1 1 calc R . .
H20C H 0.5897 0.2807 0.7623 0.150 Uiso 1 1 calc R . .
C21 C 0.2685(4) 0.1686(4) 0.6395(6) 0.058(2) Uani 1 1 d . . .
H21 H 0.2596(6) 0.210(3) 0.675(2) 0.070 Uiso 1 1 calc R . .
C22 C 0.2418(4) 0.1602(4) 0.5455(6) 0.068(3) Uani 1 1 d . . .
H22 H 0.220(2) 0.186(3) 0.523(2) 0.082 Uiso 1 1 calc R . .
C23 C 0.2563(4) 0.1045(5) 0.4952(6) 0.073(3) Uani 1 1 d . . .
H23 H 0.2428(16) 0.0996(8) 0.443(6) 0.087 Uiso 1 1 calc R . .
C24 C 0.2950(4) 0.0571(4) 0.5366(5) 0.059(2) Uani 1 1 d . . .
C25 C 0.3183(3) 0.0686(3) 0.6312(5) 0.0504(18) Uani 1 1 d . . .
C26 C 0.3144(4) -0.0029(4) 0.4912(7) 0.076(3) Uani 1 1 d . . .
H26 H 0.3013(16) -0.0107(9) 0.435(7) 0.092 Uiso 1 1 calc R . .
C27 C 0.3525(5) -0.0468(5) 0.5354(7) 0.082(3) Uani 1 1 d . . .
H27 H 0.3637(11) -0.091(4) 0.499(3) 0.099 Uiso 1 1 calc R . .
C28 C 0.3781(4) -0.0350(4) 0.6303(7) 0.063(2) Uani 1 1 d . . .
C29 C 0.3595(3) 0.0225(3) 0.6784(5) 0.0482(17) Uani 1 1 d . . .
C30 C 0.4191(4) -0.0762(4) 0.6808(8) 0.073(3) Uani 1 1 d . . .
H30 H 0.4341(13) -0.117(3) 0.649(3) 0.088 Uiso 1 1 calc R . .
C31 C 0.4395(4) -0.0623(4) 0.7733(7) 0.068(3) Uani 1 1 d . . .
H31 H 0.467(2) -0.092(2) 0.808(3) 0.082 Uiso 1 1 calc R . .
C32 C 0.4184(3) -0.0039(3) 0.8157(7) 0.0592(18) Uani 1 1 d . . .
H32 H 0.4326(12) 0.0066(9) 0.881(5) 0.071 Uiso 1 1 calc R . .
N1 N 0.3045(3) 0.1240(3) 0.6818(4) 0.0442(13) Uani 1 1 d . . .
N2 N 0.3796(2) 0.0378(3) 0.7691(4) 0.0478(14) Uani 1 1 d . . .
O1 O 0.4078(2) 0.1222(2) 0.9240(4) 0.0628(14) Uani 1 1 d . . .
O2 O 0.3945(3) 0.2198(3) 0.9916(4) 0.0812(18) Uani 1 1 d . . .
O3 O 0.4448(2) 0.1672(2) 0.7184(4) 0.0605(13) Uani 1 1 d . . .
O4 O 0.3997(2) 0.2605(2) 0.6672(4) 0.0544(12) Uani 1 1 d . . .
O5 O 0.3294(2) 0.2227(2) 0.8267(4) 0.0498(12) Uani 1 1 d D . .
H5B H 0.3466 0.2367 0.8763 0.075 Uiso 1 1 calc R . .
Cu1 Cu 0.35257(4) 0.12873(4) 0.80940(7) 0.0487(2) Uani 1 1 d . . .
H5A H 0.352(4) 0.238(4) 0.786(5) 0.09(4) 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
C1 O2 1.238(9) . ?
C1 O1 1.265(9) . ?
C1 C2 1.510(12) . ?
C2 C7 1.357(18) . ?
C2 C3 1.419(17) . ?
C3 C4 1.45(2) . ?
C3 C8 1.47(2) . ?
C4 C5 1.35(4) . ?
C4 H4 0.7730 . ?
C5 C6 1.34(3) . ?
C5 C9 1.57(2) . ?
C6 C7 1.426(15) . ?
C6 H6 0.9300 . ?
C7 C10 1.484(18) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 O3 1.247(8) . ?
C11 O4 1.271(8) . ?
C11 C12 1.523(10) . ?
C12 C13 1.386(10) . ?
C12 C17 1.405(10) . ?
C13 C14 1.372(10) . ?
C13 C18 1.506(10) . ?
C14 C15 1.378(12) . ?
C14 H14 0.8759 . ?
C15 C16 1.363(14) . ?
C15 C19 1.548(12) . ?
C16 C17 1.387(12) . ?
C16 H16 0.8442 . ?
C17 C20 1.488(12) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N1 1.314(8) . ?
C21 C22 1.412(11) . ?
C21 H21 0.9981 . ?
C22 C23 1.370(11) . ?
C22 H22 0.7670 . ?
C23 C24 1.381(11) . ?
C23 H23 0.7731 . ?
C24 C25 1.403(10) . ?
C24 C26 1.439(10) . ?
C25 N1 1.364(8) . ?
C25 C29 1.428(10) . ?
C26 C27 1.341(12) . ?
C26 H26 0.8348 . ?
C27 C28 1.425(12) . ?
C27 H27 1.0603 . ?
C28 C30 1.382(12) . ?
C28 C29 1.407(10) . ?
C29 N2 1.349(9) . ?
C30 C31 1.367(12) . ?
C30 H30 0.9978 . ?
C31 C32 1.404(10) . ?
C31 H31 0.9574 . ?
C32 N2 1.335(9) . ?
C32 H32 0.9672 . ?
N1 Cu1 2.014(5) . ?
N2 Cu1 2.027(5) . ?
O1 Cu1 1.946(5) . ?
O3 Cu1 2.406(5) . ?
O5 Cu1 2.005(5) . ?
O5 H5B 0.8200 . ?
O5 H5A 0.80(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 125.9(7) . . ?
O2 C1 C2 119.9(7) . . ?
O1 C1 C2 114.2(7) . . ?
C7 C2 C3 122.6(13) . . ?
C7 C2 C1 121.0(10) . . ?
C3 C2 C1 116.4(13) . . ?
C2 C3 C4 113.9(18) . . ?
C2 C3 C8 122.6(13) . . ?
C4 C3 C8 123.5(15) . . ?
C5 C4 C3 123(2) . . ?
C5 C4 H4 118.5 . . ?
C3 C4 H4 118.5 . . ?
C6 C5 C4 121(2) . . ?
C6 C5 C9 121(2) . . ?
C4 C5 C9 118(3) . . ?
C5 C6 C7 119.6(19) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C2 C7 C6 120.0(15) . . ?
C2 C7 C10 121.9(9) . . ?
C6 C7 C10 118.1(16) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 C11 O4 126.0(7) . . ?
O3 C11 C12 116.4(6) . . ?
O4 C11 C12 117.6(6) . . ?
C13 C12 C17 120.4(7) . . ?
C13 C12 C11 120.2(6) . . ?
C17 C12 C11 119.3(6) . . ?
C14 C13 C12 118.7(7) . . ?
C14 C13 C18 120.4(7) . . ?
C12 C13 C18 120.9(6) . . ?
C13 C14 C15 122.1(9) . . ?
C13 C14 H14 119.0 . . ?
C15 C14 H14 119.0 . . ?
C16 C15 C14 118.6(8) . . ?
C16 C15 C19 120.1(9) . . ?
C14 C15 C19 121.3(10) . . ?
C15 C16 C17 122.0(8) . . ?
C15 C16 H16 119.0 . . ?
C17 C16 H16 119.0 . . ?
C16 C17 C12 118.1(8) . . ?
C16 C17 C20 121.5(8) . . ?
C12 C17 C20 120.4(7) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19A 109.5 . . ?
C15 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C15 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C21 C22 122.5(8) . . ?
N1 C21 H21 118.8 . . ?
C22 C21 H21 118.8 . . ?
C23 C22 C21 118.5(8) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C22 C23 C24 120.6(8) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C25 117.2(7) . . ?
C23 C24 C26 126.0(8) . . ?
C25 C24 C26 116.8(8) . . ?
N1 C25 C24 122.7(7) . . ?
N1 C25 C29 116.5(6) . . ?
C24 C25 C29 120.7(7) . . ?
C27 C26 C24 122.9(8) . . ?
C27 C26 H26 118.5 . . ?
C24 C26 H26 118.5 . . ?
C26 C27 C28 120.9(9) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C30 C28 C29 116.4(8) . . ?
C30 C28 C27 125.4(8) . . ?
C29 C28 C27 118.2(9) . . ?
N2 C29 C28 123.1(7) . . ?
N2 C29 C25 116.5(6) . . ?
C28 C29 C25 120.4(7) . . ?
C31 C30 C28 121.7(8) . . ?
C31 C30 H30 119.1 . . ?
C28 C30 H30 119.1 . . ?
C30 C31 C32 117.9(8) . . ?
C30 C31 H31 121.0 . . ?
C32 C31 H31 121.0 . . ?
N2 C32 C31 122.5(9) . . ?
N2 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
C21 N1 C25 118.4(6) . . ?
C21 N1 Cu1 128.9(5) . . ?
C25 N1 Cu1 112.4(5) . . ?
C32 N2 C29 118.3(6) . . ?
C32 N2 Cu1 128.8(5) . . ?
C29 N2 Cu1 112.5(5) . . ?
C1 O1 Cu1 128.3(5) . . ?
C11 O3 Cu1 123.5(4) . . ?
Cu1 O5 H5B 109.5 . . ?
Cu1 O5 H5A 99(6) . . ?
H5B O5 H5A 100.6 . . ?
O1 Cu1 O5 96.3(2) . . ?
O1 Cu1 N1 170.7(2) . . ?
O5 Cu1 N1 91.9(2) . . ?
O1 Cu1 N2 89.8(2) . . ?
O5 Cu1 N2 170.6(2) . . ?
N1 Cu1 N2 81.5(2) . . ?
O1 Cu1 O3 88.9(2) . . ?
O5 Cu1 O3 86.0(2) . . ?
N1 Cu1 O3 87.3(2) . . ?
N2 Cu1 O3 86.9(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C7 99.3(13) . . . . ?
O1 C1 C2 C7 -78.7(11) . . . . ?
O2 C1 C2 C3 -81.6(11) . . . . ?
O1 C1 C2 C3 100.4(10) . . . . ?
C7 C2 C3 C4 0.3(16) . . . . ?
C1 C2 C3 C4 -178.9(10) . . . . ?
C7 C2 C3 C8 178.7(12) . . . . ?
C1 C2 C3 C8 -0.4(16) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C8 C3 C4 C5 -178.1(18) . . . . ?
C3 C4 C5 C6 -3(3) . . . . ?
C3 C4 C5 C9 178.0(10) . . . . ?
C4 C5 C6 C7 4(3) . . . . ?
C9 C5 C6 C7 -176.5(11) . . . . ?
C3 C2 C7 C6 1.2(16) . . . . ?
C1 C2 C7 C6 -179.6(8) . . . . ?
C3 C2 C7 C10 178.7(9) . . . . ?
C1 C2 C7 C10 -2.2(16) . . . . ?
C5 C6 C7 C2 -3.4(19) . . . . ?
C5 C6 C7 C10 179.0(13) . . . . ?
O3 C11 C12 C13 82.5(8) . . . . ?
O4 C11 C12 C13 -97.5(7) . . . . ?
O3 C11 C12 C17 -94.6(8) . . . . ?
O4 C11 C12 C17 85.4(8) . . . . ?
C17 C12 C13 C14 -2.9(10) . . . . ?
C11 C12 C13 C14 -179.9(6) . . . . ?
C17 C12 C13 C18 175.7(7) . . . . ?
C11 C12 C13 C18 -1.2(10) . . . . ?
C12 C13 C14 C15 3.6(11) . . . . ?
C18 C13 C14 C15 -175.1(7) . . . . ?
C13 C14 C15 C16 -2.0(12) . . . . ?
C13 C14 C15 C19 179.7(7) . . . . ?
C14 C15 C16 C17 -0.3(13) . . . . ?
C19 C15 C16 C17 178.0(7) . . . . ?
C15 C16 C17 C12 0.9(12) . . . . ?
C15 C16 C17 C20 -179.7(8) . . . . ?
C13 C12 C17 C16 0.8(10) . . . . ?
C11 C12 C17 C16 177.8(7) . . . . ?
C13 C12 C17 C20 -178.6(8) . . . . ?
C11 C12 C17 C20 -1.6(11) . . . . ?
N1 C21 C22 C23 -2.8(11) . . . . ?
C21 C22 C23 C24 1.5(11) . . . . ?
C22 C23 C24 C25 0.0(11) . . . . ?
C22 C23 C24 C26 -179.2(7) . . . . ?
C23 C24 C25 N1 -0.4(11) . . . . ?
C26 C24 C25 N1 178.9(7) . . . . ?
C23 C24 C25 C29 -178.8(7) . . . . ?
C26 C24 C25 C29 0.5(10) . . . . ?
C23 C24 C26 C27 179.6(8) . . . . ?
C25 C24 C26 C27 0.3(13) . . . . ?
C24 C26 C27 C28 -2.3(14) . . . . ?
C26 C27 C28 C30 -178.2(9) . . . . ?
C26 C27 C28 C29 3.3(12) . . . . ?
C30 C28 C29 N2 -0.3(10) . . . . ?
C27 C28 C29 N2 178.3(7) . . . . ?
C30 C28 C29 C25 178.8(7) . . . . ?
C27 C28 C29 C25 -2.5(10) . . . . ?
N1 C25 C29 N2 1.3(9) . . . . ?
C24 C25 C29 N2 179.9(6) . . . . ?
N1 C25 C29 C28 -177.8(6) . . . . ?
C24 C25 C29 C28 0.7(10) . . . . ?
C29 C28 C30 C31 1.1(12) . . . . ?
C27 C28 C30 C31 -177.4(8) . . . . ?
C28 C30 C31 C32 -1.1(12) . . . . ?
C30 C31 C32 N2 0.2(12) . . . . ?
C22 C21 N1 C25 2.4(10) . . . . ?
C22 C21 N1 Cu1 174.7(5) . . . . ?
C24 C25 N1 C21 -0.8(10) . . . . ?
C29 C25 N1 C21 177.7(6) . . . . ?
C24 C25 N1 Cu1 -174.3(5) . . . . ?
C29 C25 N1 Cu1 4.2(7) . . . . ?
C31 C32 N2 C29 0.6(10) . . . . ?
C31 C32 N2 Cu1 -171.8(5) . . . . ?
C28 C29 N2 C32 -0.6(10) . . . . ?
C25 C29 N2 C32 -179.7(6) . . . . ?
C28 C29 N2 Cu1 173.0(5) . . . . ?
C25 C29 N2 Cu1 -6.1(7) . . . . ?
O2 C1 O1 Cu1 5.2(13) . . . . ?
C2 C1 O1 Cu1 -176.9(7) . . . . ?
O4 C11 O3 Cu1 12.9(10) . . . . ?
C12 C11 O3 Cu1 -167.1(4) . . . . ?
C1 O1 Cu1 O5 2.9(7) . . . . ?
C1 O1 Cu1 N1 154.5(13) . . . . ?
C1 O1 Cu1 N2 175.7(7) . . . . ?
C1 O1 Cu1 O3 88.8(6) . . . . ?
C21 N1 Cu1 O1 -157.0(13) . . . . ?
C25 N1 Cu1 O1 15.7(17) . . . . ?
C21 N1 Cu1 O5 -5.2(6) . . . . ?
C25 N1 Cu1 O5 167.5(5) . . . . ?
C21 N1 Cu1 N2 -178.4(6) . . . . ?
C25 N1 Cu1 N2 -5.7(4) . . . . ?
C21 N1 Cu1 O3 -91.1(6) . . . . ?
C25 N1 Cu1 O3 81.6(4) . . . . ?
C32 N2 Cu1 O1 2.6(6) . . . . ?
C29 N2 Cu1 O1 -170.2(4) . . . . ?
C32 N2 Cu1 O5 133.3(13) . . . . ?
C29 N2 Cu1 O5 -39.5(15) . . . . ?
C32 N2 Cu1 N1 179.2(6) . . . . ?
C29 N2 Cu1 N1 6.5(4) . . . . ?
C32 N2 Cu1 O3 91.6(6) . . . . ?
C29 N2 Cu1 O3 -81.2(4) . . . . ?
C11 O3 Cu1 O1 -130.0(5) . . . . ?
C11 O3 Cu1 O5 -33.6(5) . . . . ?
C11 O3 Cu1 N1 58.5(6) . . . . ?
C11 O3 Cu1 N2 140.1(6) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.053
_database_code_depnum_ccdc_archive 'CCDC 993876'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rm135a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H54 N4 O4 Zn1'
_chemical_formula_sum            'C42 H54 N2 O4 Zn'
_chemical_formula_weight         716.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   12.0429(9)
_cell_length_b                   11.3433(5)
_cell_length_c                   14.8837(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.784(5)
_cell_angle_gamma                90.00
_cell_volume                     2009.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       blocks
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.8041
_exptl_absorpt_correction_T_max  0.8807
_exptl_absorpt_process_details   'North et al., 1968'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        0
_diffrn_reflns_number            1962
_diffrn_reflns_av_R_equivalents  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         24.97
_reflns_number_total             1865
_reflns_number_gt                1671
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0625P)²+1.3938P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1865
_refine_ls_number_parameters     126
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.0000 0.0000 0.0000 0.0362(2) Uani 1 4 d S . .
O1 O 0.13885(19) 0.0000 -0.07649(15) 0.0426(5) Uani 1 2 d S . .
O2 O -0.03623(19) 0.0000 -0.14502(15) 0.0458(6) Uani 1 2 d S . .
N1 N 0.0000 -0.1878(2) 0.0000 0.0404(6) Uani 1 2 d S . .
C1 C 0.0677(3) 0.0000 -0.1484(2) 0.0421(8) Uani 1 2 d S . .
C2 C 0.1086(3) 0.0000 -0.2400(3) 0.0560(10) Uani 1 2 d S . .
C3 C 0.1264(3) -0.1072(3) -0.2810(2) 0.0735(9) Uani 1 1 d . . .
C4 C 0.1659(3) -0.1032(4) -0.3646(2) 0.0979(14) Uani 1 1 d . . .
H4 H 0.1794 -0.1741 -0.3925 0.117 Uiso 1 1 calc R . .
C5 C 0.1855(4) 0.0000 -0.4075(3) 0.104(2) Uani 1 2 d S . .
C6 C 0.1005(4) -0.2245(4) -0.2379(3) 0.0994(13) Uani 1 1 d . . .
H6 H 0.0891 -0.2083 -0.1753 0.119 Uiso 1 1 calc R . .
C7 C -0.0056(5) -0.2775(6) -0.2866(6) 0.188(3) Uani 1 1 d . . .
H7A H -0.0202 -0.3505 -0.2580 0.282 Uiso 1 1 calc R . .
H7B H 0.0022 -0.2918 -0.3488 0.282 Uiso 1 1 calc R . .
H7C H -0.0669 -0.2241 -0.2841 0.282 Uiso 1 1 calc R . .
C8 C 0.1954(5) -0.3129(5) -0.2341(4) 0.150(2) Uani 1 1 d . . .
H8A H 0.2632 -0.2790 -0.2021 0.225 Uiso 1 1 calc R . .
H8B H 0.2063 -0.3330 -0.2948 0.225 Uiso 1 1 calc R . .
H8C H 0.1768 -0.3826 -0.2030 0.225 Uiso 1 1 calc R . .
C9 C 0.2268(5) 0.0000 -0.4996(4) 0.154(4) Uani 1 2 d S . .
H9 H 0.2268 0.0864 -0.4996 0.185 Uiso 0.50 1 calc PR . .
C10 C 0.3435(5) 0.0000 -0.4945(4) 0.139(3) Uani 1 2 d S . .
H10A H 0.3779 0.0000 -0.4319 0.209 Uiso 1 2 calc SR . .
H10B H 0.3665 0.0691 -0.5241 0.209 Uiso 0.50 1 calc PR . .
H10C H 0.3665 -0.0691 -0.5241 0.209 Uiso 0.50 1 calc PR . .
C11 C 0.1495(6) 0.0000 -0.5723(4) 0.193(6) Uani 1 2 d S . .
H11A H 0.0763 0.0000 -0.5542 0.289 Uiso 1 2 calc SR . .
H11B H 0.1579 -0.0691 -0.6079 0.289 Uiso 0.50 1 calc PR . .
H11C H 0.1579 0.0691 -0.6079 0.289 Uiso 0.50 1 calc PR . .
C21 C 0.0930(2) -0.2491(2) 0.0262(2) 0.0606(8) Uani 1 1 d . . .
H21 H 0.1594 -0.2080 0.0444 0.073 Uiso 1 1 calc R . .
C22 C 0.0963(2) -0.3707(2) 0.0278(2) 0.0612(8) Uani 1 1 d . . .
H22 H 0.1636 -0.4096 0.0477 0.073 Uiso 1 1 calc R . .
C23 C 0.0000 -0.4341(2) 0.0000 0.0387(7) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.130(2) 5 ?
Zn1 N1 2.130(2) . ?
Zn1 O2 2.136(2) 5 ?
Zn1 O2 2.136(2) . ?
Zn1 O1 2.162(2) 5 ?
Zn1 O1 2.162(2) . ?
Zn1 C1 2.469(3) . ?
Zn1 C1 2.469(3) 5 ?
O1 C1 1.265(4) . ?
O2 C1 1.260(4) . ?
N1 C21 1.325(3) 2 ?
N1 C21 1.325(3) . ?
C1 C2 1.518(5) . ?
C2 C3 1.392(4) . ?
C2 C3 1.392(4) 6 ?
C3 C4 1.400(4) . ?
C3 C6 1.529(6) . ?
C4 C5 1.371(5) . ?
C4 H4 0.9300 . ?
C5 C4 1.371(5) 6 ?
C5 C9 1.528(6) . ?
C6 C7 1.495(7) . ?
C6 C8 1.515(6) . ?
C6 H6 0.9800 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C11 1.316(8) . ?
C9 C10 1.395(8) . ?
C9 H9 0.9800 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C21 C22 1.381(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.374(3) . ?
C22 H22 0.9300 . ?
C23 C22 1.374(3) 2 ?
C23 C23 1.496(6) 5_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 N1 180.0 5 . ?
N1 Zn1 O2 90.0 5 5 ?
N1 Zn1 O2 90.0 . 5 ?
N1 Zn1 O2 90.0 5 . ?
N1 Zn1 O2 90.0 . . ?
O2 Zn1 O2 180.00(2) 5 . ?
N1 Zn1 O1 90.0 5 5 ?
N1 Zn1 O1 90.0 . 5 ?
O2 Zn1 O1 61.50(9) 5 5 ?
O2 Zn1 O1 118.50(9) . 5 ?
N1 Zn1 O1 90.0 5 . ?
N1 Zn1 O1 90.0 . . ?
O2 Zn1 O1 118.50(9) 5 . ?
O2 Zn1 O1 61.50(9) . . ?
O1 Zn1 O1 180.00(10) 5 . ?
N1 Zn1 C1 90.0 5 . ?
N1 Zn1 C1 90.0 . . ?
O2 Zn1 C1 149.31(10) 5 . ?
O2 Zn1 C1 30.69(10) . . ?
O1 Zn1 C1 149.19(10) 5 . ?
O1 Zn1 C1 30.81(10) . . ?
N1 Zn1 C1 90.0 5 5 ?
N1 Zn1 C1 90.0 . 5 ?
O2 Zn1 C1 30.69(10) 5 5 ?
O2 Zn1 C1 149.31(10) . 5 ?
O1 Zn1 C1 30.81(10) 5 5 ?
O1 Zn1 C1 149.19(10) . 5 ?
C1 Zn1 C1 180.00(15) . 5 ?
C1 O1 Zn1 88.11(19) . . ?
C1 O2 Zn1 89.42(19) . . ?
C21 N1 C21 116.7(3) 2 . ?
C21 N1 Zn1 121.67(14) 2 . ?
C21 N1 Zn1 121.67(14) . . ?
O2 C1 O1 121.0(3) . . ?
O2 C1 C2 119.8(3) . . ?
O1 C1 C2 119.3(3) . . ?
O2 C1 Zn1 59.89(17) . . ?
O1 C1 Zn1 61.07(17) . . ?
C2 C1 Zn1 179.7(3) . . ?
C3 C2 C3 121.8(4) . 6 ?
C3 C2 C1 119.10(19) . . ?
C3 C2 C1 119.10(19) 6 . ?
C2 C3 C4 117.2(4) . . ?
C2 C3 C6 121.4(3) . . ?
C4 C3 C6 121.3(3) . . ?
C5 C4 C3 123.2(4) . . ?
C5 C4 H4 118.4 . . ?
C3 C4 H4 118.4 . . ?
C4 C5 C4 117.3(4) . 6 ?
C4 C5 C9 121.4(2) . . ?
C4 C5 C9 121.4(2) 6 . ?
C7 C6 C8 109.6(4) . . ?
C7 C6 C3 111.2(4) . . ?
C8 C6 C3 113.0(4) . . ?
C7 C6 H6 107.6 . . ?
C8 C6 H6 107.6 . . ?
C3 C6 H6 107.6 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C9 C10 128.7(5) . . ?
C11 C9 C5 116.8(5) . . ?
C10 C9 C5 114.5(5) . . ?
C11 C9 H9 90.0 . . ?
C10 C9 H9 90.0 . . ?
C5 C9 H9 90.0 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C21 C22 123.5(2) . . ?
N1 C21 H21 118.3 . . ?
C22 C21 H21 118.3 . . ?
C23 C22 C21 119.7(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C22 116.9(3) . 2 ?
C22 C23 C23 121.53(15) . 5_545 ?
C22 C23 C23 121.53(15) 2 5_545 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Zn1 O1 C1 -90.0 5 . . . ?
N1 Zn1 O1 C1 90.0 . . . . ?
O2 Zn1 O1 C1 180.0 5 . . . ?
O2 Zn1 O1 C1 0.0 . . . . ?
O1 Zn1 O1 C1 -47(43) 5 . . . ?
C1 Zn1 O1 C1 180.0 5 . . . ?
N1 Zn1 O2 C1 90.0 5 . . . ?
N1 Zn1 O2 C1 -90.0 . . . . ?
O2 Zn1 O2 C1 96(100) 5 . . . ?
O1 Zn1 O2 C1 180.0 5 . . . ?
O1 Zn1 O2 C1 0.0 . . . . ?
C1 Zn1 O2 C1 180.0 5 . . . ?
N1 Zn1 N1 C21 0(17) 5 . . 2 ?
O2 Zn1 N1 C21 112.83(19) 5 . . 2 ?
O2 Zn1 N1 C21 -67.17(19) . . . 2 ?
O1 Zn1 N1 C21 51.33(19) 5 . . 2 ?
O1 Zn1 N1 C21 -128.67(19) . . . 2 ?
C1 Zn1 N1 C21 -97.86(19) . . . 2 ?
C1 Zn1 N1 C21 82.14(19) 5 . . 2 ?
N1 Zn1 N1 C21 0(100) 5 . . . ?
O2 Zn1 N1 C21 -67.17(19) 5 . . . ?
O2 Zn1 N1 C21 112.83(19) . . . . ?
O1 Zn1 N1 C21 -128.67(19) 5 . . . ?
O1 Zn1 N1 C21 51.33(19) . . . . ?
C1 Zn1 N1 C21 82.14(19) . . . . ?
C1 Zn1 N1 C21 -97.86(19) 5 . . . ?
Zn1 O2 C1 O1 0.0 . . . . ?
Zn1 O2 C1 C2 180.0 . . . . ?
Zn1 O1 C1 O2 0.0 . . . . ?
Zn1 O1 C1 C2 180.0 . . . . ?
N1 Zn1 C1 O2 -90.0 5 . . . ?
N1 Zn1 C1 O2 90.0 . . . . ?
O2 Zn1 C1 O2 180.0 5 . . . ?
O1 Zn1 C1 O2 0.0 5 . . . ?
O1 Zn1 C1 O2 180.0 . . . . ?
C1 Zn1 C1 O2 -58(100) 5 . . . ?
N1 Zn1 C1 O1 90.0 5 . . . ?
N1 Zn1 C1 O1 -90.0 . . . . ?
O2 Zn1 C1 O1 0.0 5 . . . ?
O2 Zn1 C1 O1 180.0 . . . . ?
O1 Zn1 C1 O1 180.0 5 . . . ?
C1 Zn1 C1 O1 122(100) 5 . . . ?
N1 Zn1 C1 C2 -90.00(5) 5 . . . ?
N1 Zn1 C1 C2 90.00(5) . . . . ?
O2 Zn1 C1 C2 180.00(5) 5 . . . ?
O2 Zn1 C1 C2 0.00(5) . . . . ?
O1 Zn1 C1 C2 0.00(5) 5 . . . ?
O1 Zn1 C1 C2 180.00(5) . . . . ?
C1 Zn1 C1 C2 -58(100) 5 . . . ?
O2 C1 C2 C3 -89.8(3) . . . . ?
O1 C1 C2 C3 90.2(3) . . . . ?
Zn1 C1 C2 C3 -89.8(4) . . . . ?
O2 C1 C2 C3 89.8(3) . . . 6 ?
O1 C1 C2 C3 -90.2(3) . . . 6 ?
Zn1 C1 C2 C3 89.8(4) . . . 6 ?
C3 C2 C3 C4 1.5(6) 6 . . . ?
C1 C2 C3 C4 -179.0(3) . . . . ?
C3 C2 C3 C6 -176.6(3) 6 . . . ?
C1 C2 C3 C6 2.9(6) . . . . ?
C2 C3 C4 C5 -1.1(6) . . . . ?
C6 C3 C4 C5 177.1(4) . . . . ?
C3 C4 C5 C4 0.6(8) . . . 6 ?
C3 C4 C5 C9 -179.0(5) . . . . ?
C2 C3 C6 C7 104.4(5) . . . . ?
C4 C3 C6 C7 -73.6(6) . . . . ?
C2 C3 C6 C8 -131.9(4) . . . . ?
C4 C3 C6 C8 50.1(5) . . . . ?
C4 C5 C9 C11 89.8(5) . . . . ?
C4 C5 C9 C11 -89.8(5) 6 . . . ?
C4 C5 C9 C10 -90.2(5) . . . . ?
C4 C5 C9 C10 90.2(5) 6 . . . ?
C21 N1 C21 C22 -0.5(3) 2 . . . ?
Zn1 N1 C21 C22 179.5(3) . . . . ?
N1 C21 C22 C23 1.0(5) . . . . ?
C21 C22 C23 C22 -0.5(2) . . . 2 ?
C21 C22 C23 C23 179.5(2) . . . 5_545 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.049
_database_code_depnum_ccdc_archive 'CCDC 993877'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_RK1-163

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H22 Mn N2 O4, C H4 O'
_chemical_formula_sum            'C23 H26 Mn N2 O5'
_chemical_formula_weight         465.40

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'
Mn Mn 0.3368 0.7283 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   13.211(8)
_cell_length_b                   11.690(7)
_cell_length_c                   14.445(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.835(11)
_cell_angle_gamma                90.00
_cell_volume                     2198(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3180
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      25.3

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             972
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8220
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16280
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3854
_reflns_number_gt                3391
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0398P)²+6.5272P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3854
_refine_ls_number_parameters     334
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0814
_refine_ls_wR_factor_ref         0.1625
_refine_ls_wR_factor_gt          0.1557
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_restrained_S_all      1.196
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4671(4) 0.7829(5) 0.6198(4) 0.0280(12) Uani 1 1 d . . .
C2 C 0.4698(4) 0.6644(4) 0.6200(4) 0.0255(12) Uani 1 1 d . . .
C3 C 0.3900(3) 0.6046(4) 0.5667(3) 0.0169(10) Uani 1 1 d . . .
C4 C 0.3107(4) 0.6681(4) 0.5168(4) 0.0252(12) Uani 1 1 d . . .
C5 C 0.3135(4) 0.7856(5) 0.5207(4) 0.0294(13) Uani 1 1 d . . .
C6 C 0.3888(4) 0.4763(4) 0.5661(3) 0.0192(10) Uani 1 1 d . . .
C7 C 0.4643(4) 0.4146(5) 0.6241(4) 0.0275(12) Uani 1 1 d . . .
C8 C 0.4620(4) 0.2975(5) 0.6233(4) 0.0268(12) Uani 1 1 d . . .
C9 C 0.3161(4) 0.2941(5) 0.5143(4) 0.0271(12) Uani 1 1 d . . .
C10 C 0.3143(4) 0.4121(4) 0.5094(4) 0.0260(12) Uani 1 1 d . . .
C11 C 0.2565(3) 0.0460(4) 0.6902(3) 0.0198(10) Uani 1 1 d . . .
C12 C 0.1770(3) 0.0523(4) 0.7528(3) 0.0215(11) Uani 1 1 d . . .
C13 C 0.1282(4) -0.0469(5) 0.7753(3) 0.0290(12) Uani 1 1 d . . .
C14 C 0.1603(5) -0.1618(5) 0.7421(5) 0.0519(18) Uani 1 1 d . . .
H14A H 0.1183 -0.2220 0.7638 0.078 Uiso 1 1 calc R . .
H14B H 0.2328 -0.1754 0.7678 0.078 Uiso 1 1 calc R . .
H14C H 0.1505 -0.1624 0.6734 0.078 Uiso 1 1 calc R . .
C15 C 0.0498(4) -0.0367(6) 0.8276(4) 0.0343(13) Uani 1 1 d . . .
C16 C 0.0191(4) 0.0673(5) 0.8585(3) 0.0317(13) Uani 1 1 d . . .
C17 C -0.0686(5) 0.0768(7) 0.9121(4) 0.0412(16) Uani 1 1 d . . .
C18 C 0.0711(4) 0.1640(5) 0.8375(4) 0.0322(13) Uani 1 1 d . . .
C19 C 0.1493(4) 0.1592(5) 0.7840(3) 0.0254(12) Uani 1 1 d . . .
C20 C 0.2015(4) 0.2664(5) 0.7596(4) 0.0399(15) Uani 1 1 d . . .
H20A H 0.2539 0.2469 0.7218 0.060 Uiso 1 1 calc R . .
H20B H 0.2340 0.3047 0.8174 0.060 Uiso 1 1 calc R . .
H20C H 0.1506 0.3176 0.7237 0.060 Uiso 1 1 calc R . .
C21 C 0.6352(4) 0.0195(4) 0.6346(3) 0.0218(11) Uani 1 1 d . . .
C22 C 0.7159(4) 0.0542(5) 0.7158(4) 0.0319(13) Uani 1 1 d . . .
H22A H 0.6840 0.0979 0.7611 0.048 Uiso 1 1 calc R . .
H22B H 0.7676 0.1015 0.6930 0.048 Uiso 1 1 calc R . .
H22C H 0.7487 -0.0144 0.7465 0.048 Uiso 1 1 calc R . .
C23 C -0.0371(6) 0.1239(11) 0.5676(7) 0.115(4) Uani 1 1 d D . .
H23A H -0.0247 0.0421 0.5791 0.172 Uiso 1 1 calc R . .
H23B H -0.0981 0.1341 0.5191 0.172 Uiso 1 1 calc R . .
H23C H -0.0482 0.1612 0.6258 0.172 Uiso 1 1 calc R . .
Mn1 Mn 0.38920(5) 0.04030(6) 0.57641(5) 0.0174(2) Uani 1 1 d . . .
N1 N 0.3900(3) 0.8433(3) 0.5718(3) 0.0233(9) Uani 1 1 d . . .
N2 N 0.3898(3) 0.2348(3) 0.5697(3) 0.0195(9) Uani 1 1 d . . .
O1 O 0.3378(3) 0.0375(3) 0.4303(2) 0.0279(8) Uani 1 1 d . . .
O2 O 0.5447(2) 0.0502(3) 0.6377(3) 0.0314(9) Uani 1 1 d . . .
O3 O 0.2275(2) 0.0467(3) 0.6024(2) 0.0281(8) Uani 1 1 d . . .
O4 O 0.3504(2) 0.0394(3) 0.7256(2) 0.0286(8) Uani 1 1 d . . .
O5 O 0.0465(5) 0.1721(6) 0.5378(5) 0.107(2) Uani 1 1 d D . .
H5A H 0.0813 0.1207 0.5176 0.161 Uiso 1 1 calc RD . .
H1 H 0.526(4) 0.822(4) 0.656(3) 0.024(13) Uiso 1 1 d . . .
H2 H 0.534(4) 0.628(5) 0.660(4) 0.048(17) Uiso 1 1 d . . .
H4 H 0.256(4) 0.637(5) 0.475(4) 0.034(15) Uiso 1 1 d . . .
H5 H 0.259(4) 0.830(5) 0.488(4) 0.033(15) Uiso 1 1 d . . .
H7 H 0.515(4) 0.450(5) 0.659(4) 0.030(15) Uiso 1 1 d . . .
H8 H 0.511(4) 0.254(5) 0.661(3) 0.028(14) Uiso 1 1 d . . .
H9 H 0.265(4) 0.250(5) 0.472(4) 0.043(17) Uiso 1 1 d . . .
H10 H 0.260(4) 0.454(4) 0.466(3) 0.025(13) Uiso 1 1 d . . .
H15 H 0.023(4) -0.104(5) 0.845(3) 0.026(14) Uiso 1 1 d . . .
H17A H -0.091(3) 0.000(4) 0.926(3) 0.014(12) Uiso 1 1 d . . .
H17B H -0.044(5) 0.132(6) 0.975(5) 0.07(2) Uiso 1 1 d . . .
H17C H -0.126(5) 0.112(6) 0.880(5) 0.06(2) Uiso 1 1 d . . .
H18 H 0.053(4) 0.238(5) 0.859(4) 0.036(16) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.331(6) . ?
C1 C2 1.386(7) . ?
C1 H1 0.97(5) . ?
C2 C3 1.384(7) . ?
C2 H2 1.03(6) . ?
C3 C4 1.382(7) . ?
C3 C6 1.499(6) . ?
C4 C5 1.375(7) . ?
C4 H4 0.93(5) . ?
C5 N1 1.330(6) . ?
C5 H5 0.95(5) . ?
C6 C10 1.388(7) . ?
C6 C7 1.390(7) . ?
C7 C8 1.369(8) . ?
C7 H7 0.87(5) . ?
C8 N2 1.340(6) . ?
C8 H8 0.92(5) . ?
C9 N2 1.342(6) . ?
C9 C10 1.381(7) . ?
C9 H9 0.98(6) . ?
C10 H10 1.00(5) . ?
C11 O4 1.260(5) . ?
C11 O3 1.261(5) . ?
C11 C12 1.500(6) . ?
C11 Mn1 2.600(5) . ?
C12 C13 1.392(7) . ?
C12 C19 1.398(7) . ?
C13 C15 1.387(7) . ?
C13 C14 1.510(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.379(8) . ?
C15 H15 0.92(5) . ?
C16 C18 1.384(8) . ?
C16 C17 1.504(7) . ?
C17 H17A 0.98(5) . ?
C17 H17B 1.11(7) . ?
C17 H17C 0.92(7) . ?
C18 C19 1.392(7) . ?
C18 H18 0.97(6) . ?
C19 C20 1.501(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 O1 1.252(6) 3_656 ?
C21 O2 1.255(6) . ?
C21 C22 1.500(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 O5 1.372(9) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
Mn1 O2 2.097(4) . ?
Mn1 O1 2.104(3) . ?
Mn1 O3 2.232(3) . ?
Mn1 N2 2.275(4) . ?
Mn1 O4 2.299(4) . ?
Mn1 N1 2.305(4) 1_545 ?
N1 Mn1 2.305(4) 1_565 ?
O1 C21 1.252(6) 3_656 ?
O5 H5A 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.3(5) . . ?
N1 C1 H1 120(3) . . ?
C2 C1 H1 117(3) . . ?
C3 C2 C1 119.1(5) . . ?
C3 C2 H2 125(3) . . ?
C1 C2 H2 115(3) . . ?
C4 C3 C2 117.2(5) . . ?
C4 C3 C6 121.8(4) . . ?
C2 C3 C6 121.0(4) . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 115(3) . . ?
C3 C4 H4 125(3) . . ?
N1 C5 C4 122.8(5) . . ?
N1 C5 H5 116(3) . . ?
C4 C5 H5 121(3) . . ?
C10 C6 C7 115.9(5) . . ?
C10 C6 C3 123.4(4) . . ?
C7 C6 C3 120.7(4) . . ?
C8 C7 C6 120.1(5) . . ?
C8 C7 H7 120(4) . . ?
C6 C7 H7 120(4) . . ?
N2 C8 C7 124.4(5) . . ?
N2 C8 H8 114(3) . . ?
C7 C8 H8 122(3) . . ?
N2 C9 C10 123.4(5) . . ?
N2 C9 H9 117(3) . . ?
C10 C9 H9 120(3) . . ?
C9 C10 C6 120.4(5) . . ?
C9 C10 H10 122(3) . . ?
C6 C10 H10 118(3) . . ?
O4 C11 O3 121.2(4) . . ?
O4 C11 C12 120.0(4) . . ?
O3 C11 C12 118.8(4) . . ?
O4 C11 Mn1 62.1(2) . . ?
O3 C11 Mn1 59.1(2) . . ?
C12 C11 Mn1 177.5(3) . . ?
C13 C12 C19 120.8(5) . . ?
C13 C12 C11 119.9(4) . . ?
C19 C12 C11 119.2(5) . . ?
C15 C13 C12 118.3(5) . . ?
C15 C13 C14 121.7(5) . . ?
C12 C13 C14 120.0(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C13 122.7(6) . . ?
C16 C15 H15 121(3) . . ?
C13 C15 H15 116(3) . . ?
C15 C16 C18 117.7(5) . . ?
C15 C16 C17 121.8(6) . . ?
C18 C16 C17 120.5(6) . . ?
C16 C17 H17A 109(3) . . ?
C16 C17 H17B 108(3) . . ?
H17A C17 H17B 115(4) . . ?
C16 C17 H17C 115(4) . . ?
H17A C17 H17C 105(5) . . ?
H17B C17 H17C 105(5) . . ?
C16 C18 C19 122.1(5) . . ?
C16 C18 H18 120(3) . . ?
C19 C18 H18 118(3) . . ?
C18 C19 C12 118.4(5) . . ?
C18 C19 C20 120.7(5) . . ?
C12 C19 C20 120.9(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C21 O2 125.0(4) 3_656 . ?
O1 C21 C22 118.3(4) 3_656 . ?
O2 C21 C22 116.7(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 H23A 109.5 . . ?
O5 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O5 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2 Mn1 O1 123.34(14) . . ?
O2 Mn1 O3 145.48(14) . . ?
O1 Mn1 O3 90.84(13) . . ?
O2 Mn1 N2 87.31(14) . . ?
O1 Mn1 N2 88.59(14) . . ?
O3 Mn1 N2 89.07(14) . . ?
O2 Mn1 O4 87.93(13) . . ?
O1 Mn1 O4 148.72(13) . . ?
O3 Mn1 O4 57.96(11) . . ?
N2 Mn1 O4 92.72(14) . . ?
O2 Mn1 N1 93.32(14) . 1_545 ?
O1 Mn1 N1 87.60(14) . 1_545 ?
O3 Mn1 N1 92.74(14) . 1_545 ?
N2 Mn1 N1 175.80(14) . 1_545 ?
O4 Mn1 N1 91.45(14) . 1_545 ?
O2 Mn1 C11 116.71(15) . . ?
O1 Mn1 C11 119.82(15) . . ?
O3 Mn1 C11 28.99(13) . . ?
N2 Mn1 C11 90.52(14) . . ?
O4 Mn1 C11 28.98(12) . . ?
N1 Mn1 C11 92.90(15) 1_545 . ?
C5 N1 C1 117.5(4) . . ?
C5 N1 Mn1 121.1(3) . 1_565 ?
C1 N1 Mn1 121.4(3) . 1_565 ?
C8 N2 C9 115.7(4) . . ?
C8 N2 Mn1 121.9(3) . . ?
C9 N2 Mn1 122.3(3) . . ?
C21 O1 Mn1 132.5(3) 3_656 . ?
C21 O2 Mn1 147.1(3) . . ?
C11 O3 Mn1 91.9(3) . . ?
C11 O4 Mn1 88.9(3) . . ?
C23 O5 H5A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 1.3(8) . . . . ?
C1 C2 C3 C4 -0.8(7) . . . . ?
C1 C2 C3 C6 -179.0(5) . . . . ?
C2 C3 C4 C5 0.5(8) . . . . ?
C6 C3 C4 C5 178.6(5) . . . . ?
C3 C4 C5 N1 -0.6(9) . . . . ?
C4 C3 C6 C10 6.2(7) . . . . ?
C2 C3 C6 C10 -175.7(5) . . . . ?
C4 C3 C6 C7 -173.5(5) . . . . ?
C2 C3 C6 C7 4.5(7) . . . . ?
C10 C6 C7 C8 -0.2(8) . . . . ?
C3 C6 C7 C8 179.6(5) . . . . ?
C6 C7 C8 N2 -0.5(9) . . . . ?
N2 C9 C10 C6 -2.6(8) . . . . ?
C7 C6 C10 C9 1.7(7) . . . . ?
C3 C6 C10 C9 -178.1(5) . . . . ?
O4 C11 C12 C13 -95.2(6) . . . . ?
O3 C11 C12 C13 84.5(6) . . . . ?
Mn1 C11 C12 C13 117(8) . . . . ?
O4 C11 C12 C19 88.0(6) . . . . ?
O3 C11 C12 C19 -92.4(6) . . . . ?
Mn1 C11 C12 C19 -60(8) . . . . ?
C19 C12 C13 C15 1.5(7) . . . . ?
C11 C12 C13 C15 -175.3(4) . . . . ?
C19 C12 C13 C14 -179.1(5) . . . . ?
C11 C12 C13 C14 4.1(7) . . . . ?
C12 C13 C15 C16 -0.6(8) . . . . ?
C14 C13 C15 C16 -179.9(5) . . . . ?
C13 C15 C16 C18 -1.4(8) . . . . ?
C13 C15 C16 C17 177.8(5) . . . . ?
C15 C16 C18 C19 2.5(8) . . . . ?
C17 C16 C18 C19 -176.7(5) . . . . ?
C16 C18 C19 C12 -1.6(8) . . . . ?
C16 C18 C19 C20 177.7(5) . . . . ?
C13 C12 C19 C18 -0.5(7) . . . . ?
C11 C12 C19 C18 176.3(4) . . . . ?
C13 C12 C19 C20 -179.8(5) . . . . ?
C11 C12 C19 C20 -3.0(7) . . . . ?
O4 C11 Mn1 O2 -7.4(3) . . . . ?
O3 C11 Mn1 O2 174.4(3) . . . . ?
C12 C11 Mn1 O2 142(8) . . . . ?
O4 C11 Mn1 O1 176.6(3) . . . . ?
O3 C11 Mn1 O1 -1.5(3) . . . . ?
C12 C11 Mn1 O1 -34(8) . . . . ?
O4 C11 Mn1 O3 178.2(5) . . . . ?
C12 C11 Mn1 O3 -33(8) . . . . ?
O4 C11 Mn1 N2 -94.7(3) . . . . ?
O3 C11 Mn1 N2 87.1(3) . . . . ?
C12 C11 Mn1 N2 54(8) . . . . ?
O3 C11 Mn1 O4 -178.2(5) . . . . ?
C12 C11 Mn1 O4 149(8) . . . . ?
O4 C11 Mn1 N1 87.8(3) . . . 1_545 ?
O3 C11 Mn1 N1 -90.4(3) . . . 1_545 ?
C12 C11 Mn1 N1 -123(8) . . . 1_545 ?
C4 C5 N1 C1 0.9(8) . . . . ?
C4 C5 N1 Mn1 -179.4(4) . . . 1_565 ?
C2 C1 N1 C5 -1.3(8) . . . . ?
C2 C1 N1 Mn1 179.0(4) . . . 1_565 ?
C7 C8 N2 C9 -0.2(8) . . . . ?
C7 C8 N2 Mn1 -178.0(4) . . . . ?
C10 C9 N2 C8 1.8(7) . . . . ?
C10 C9 N2 Mn1 179.5(4) . . . . ?
O2 Mn1 N2 C8 -19.5(4) . . . . ?
O1 Mn1 N2 C8 -143.0(4) . . . . ?
O3 Mn1 N2 C8 126.1(4) . . . . ?
O4 Mn1 N2 C8 68.3(4) . . . . ?
N1 Mn1 N2 C8 -118.2(19) 1_545 . . . ?
C11 Mn1 N2 C8 97.2(4) . . . . ?
O2 Mn1 N2 C9 162.8(4) . . . . ?
O1 Mn1 N2 C9 39.3(4) . . . . ?
O3 Mn1 N2 C9 -51.5(4) . . . . ?
O4 Mn1 N2 C9 -109.4(4) . . . . ?
N1 Mn1 N2 C9 64(2) 1_545 . . . ?
C11 Mn1 N2 C9 -80.5(4) . . . . ?
O2 Mn1 O1 C21 48.3(5) . . . 3_656 ?
O3 Mn1 O1 C21 -136.8(4) . . . 3_656 ?
N2 Mn1 O1 C21 134.1(4) . . . 3_656 ?
O4 Mn1 O1 C21 -133.0(4) . . . 3_656 ?
N1 Mn1 O1 C21 -44.1(4) 1_545 . . 3_656 ?
C11 Mn1 O1 C21 -136.1(4) . . . 3_656 ?
O1 C21 O2 Mn1 6.3(10) 3_656 . . . ?
C22 C21 O2 Mn1 -173.3(4) . . . . ?
O1 Mn1 O2 C21 -38.6(7) . . . . ?
O3 Mn1 O2 C21 150.4(6) . . . . ?
N2 Mn1 O2 C21 -125.2(6) . . . . ?
O4 Mn1 O2 C21 142.0(6) . . . . ?
N1 Mn1 O2 C21 50.7(6) 1_545 . . . ?
C11 Mn1 O2 C21 145.6(6) . . . . ?
O4 C11 O3 Mn1 -1.9(5) . . . . ?
C12 C11 O3 Mn1 178.5(4) . . . . ?
O2 Mn1 O3 C11 -8.9(4) . . . . ?
O1 Mn1 O3 C11 178.7(3) . . . . ?
N2 Mn1 O3 C11 -92.8(3) . . . . ?
O4 Mn1 O3 C11 1.0(3) . . . . ?
N1 Mn1 O3 C11 91.0(3) 1_545 . . . ?
O3 C11 O4 Mn1 1.8(5) . . . . ?
C12 C11 O4 Mn1 -178.5(4) . . . . ?
O2 Mn1 O4 C11 173.4(3) . . . . ?
O1 Mn1 O4 C11 -5.6(4) . . . . ?
O3 Mn1 O4 C11 -1.0(3) . . . . ?
N2 Mn1 O4 C11 86.2(3) . . . . ?
N1 Mn1 O4 C11 -93.4(3) 1_545 . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.077
_database_code_depnum_ccdc_archive 'CCDC 993878'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rm130

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H50 N4 O9 S1 Zn2'
_chemical_formula_sum            'C46 H50 N4 O9 S1 Zn2'
_chemical_formula_weight         965.70

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'
O O 0.0106 0.0060 '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'
Zn Zn 0.2839 1.4301 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   28.2040(18)
_cell_length_b                   11.4950(15)
_cell_length_c                   15.0420(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.001(5)
_cell_angle_gamma                90.00
_cell_volume                     4455.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       blocks
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2008
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.8424
_exptl_absorpt_correction_T_max  0.8908
_exptl_absorpt_process_details   'North et al., 1968'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4078
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3910
_reflns_number_gt                2996
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0414P)²+4.8898P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3910
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0882
_refine_ls_wR_factor_gt          0.0793
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.692646(11) 0.78438(2) 0.86951(2) 0.03345(11) Uani 1 1 d . . .
O1 O 0.67954(8) 0.7783(2) 0.69823(17) 0.0633(6) Uani 1 1 d . . .
O2 O 0.61975(7) 0.78659(17) 0.75445(13) 0.0467(5) Uani 1 1 d . . .
O3 O 0.66535(8) 0.78613(16) 0.97524(14) 0.0490(5) Uani 1 1 d . . .
O4 O 0.76937(8) 0.79237(17) 0.89943(18) 0.0617(6) Uani 1 1 d . . .
N1 N 0.69369(8) 0.59344(18) 0.87067(16) 0.0369(5) Uani 1 1 d . . .
N2 N 0.69412(8) 0.97479(18) 0.87422(15) 0.0365(5) Uani 1 1 d . . .
C1 C 0.65618(11) 0.5338(2) 0.8825(2) 0.0502(8) Uani 1 1 d . . .
H1 H 0.6293 0.5752 0.8887 0.060 Uiso 1 1 calc R . .
C2 C 0.65494(11) 0.4139(2) 0.8860(2) 0.0479(7) Uani 1 1 d . . .
H2 H 0.6279 0.3767 0.8950 0.057 Uiso 1 1 calc R . .
C3 C 0.69372(9) 0.3491(2) 0.87606(17) 0.0313(5) Uani 1 1 d . . .
C4 C 0.73231(11) 0.4115(2) 0.8621(2) 0.0438(7) Uani 1 1 d . . .
H4 H 0.7592 0.3725 0.8541 0.053 Uiso 1 1 calc R . .
C5 C 0.73060(11) 0.5310(2) 0.8600(2) 0.0433(7) Uani 1 1 d . . .
H5 H 0.7569 0.5705 0.8504 0.052 Uiso 1 1 calc R . .
C6 C 0.69411(9) 0.2195(2) 0.87742(17) 0.0324(5) Uani 1 1 d . . .
C7 C 0.65781(10) 0.1548(2) 0.8960(2) 0.0424(6) Uani 1 1 d . . .
H7 H 0.6326 0.1921 0.9106 0.051 Uiso 1 1 calc R . .
C8 C 0.65893(11) 1.0353(2) 0.8929(2) 0.0448(7) Uani 1 1 d . . .
H8 H 0.6336 0.9943 0.9046 0.054 Uiso 1 1 calc R . .
C9 C 0.72934(12) 1.0373(2) 0.8571(2) 0.0498(8) Uani 1 1 d . . .
H9 H 0.7545 0.9976 0.8440 0.060 Uiso 1 1 calc R . .
C10 C 0.73063(11) 0.1564(2) 0.8575(2) 0.0498(7) Uani 1 1 d . . .
H10 H 0.7560 0.1951 0.8444 0.060 Uiso 1 1 calc R . .
C11 C 0.63324(10) 0.7802(2) 0.6849(2) 0.0407(6) Uani 1 1 d . . .
C12 C 0.59079(10) 0.7752(3) 0.58370(19) 0.0408(6) Uani 1 1 d . . .
C13 C 0.57093(12) 0.6667(3) 0.5423(2) 0.0556(8) Uani 1 1 d . . .
C14 C 0.52932(13) 0.6647(4) 0.4518(3) 0.0702(10) Uani 1 1 d . . .
H14 H 0.5161 0.5932 0.4237 0.084 Uiso 1 1 calc R . .
C15 C 0.50701(13) 0.7643(4) 0.4026(2) 0.0709(11) Uani 1 1 d . . .
C16 C 0.52877(13) 0.8695(4) 0.4436(2) 0.0694(10) Uani 1 1 d . . .
H16 H 0.5150 0.9376 0.4095 0.083 Uiso 1 1 calc R . .
C17 C 0.57049(11) 0.8774(3) 0.5337(2) 0.0507(7) Uani 1 1 d . . .
C18 C 0.59393(16) 0.5564(3) 0.5940(3) 0.0882(13) Uani 1 1 d . . .
H18A H 0.5757 0.4913 0.5551 0.132 Uiso 1 1 calc R . .
H18B H 0.5911 0.5545 0.6554 0.132 Uiso 1 1 calc R . .
H18C H 0.6298 0.5525 0.6046 0.132 Uiso 1 1 calc R . .
C19 C 0.45946(14) 0.7581(5) 0.3066(3) 0.1053(18) Uani 1 1 d . . .
H19A H 0.4491 0.8354 0.2823 0.158 Uiso 1 1 calc R . .
H19B H 0.4316 0.7206 0.3167 0.158 Uiso 1 1 calc R . .
H19C H 0.4677 0.7144 0.2603 0.158 Uiso 1 1 calc R . .
C20 C 0.59393(15) 0.9922(3) 0.5763(3) 0.0752(11) Uani 1 1 d . . .
H20A H 0.5754 1.0537 0.5329 0.113 Uiso 1 1 calc R . .
H20B H 0.6297 0.9938 0.5855 0.113 Uiso 1 1 calc R . .
H20C H 0.5918 1.0027 0.6379 0.113 Uiso 1 1 calc R . .
C21 C 0.68527(10) 0.7409(2) 1.0573(2) 0.0367(6) Uani 1 1 d . . .
C22 C 0.65078(14) 0.7271(3) 1.1102(3) 0.0663(9) Uani 1 1 d . . .
H22A H 0.6167 0.7557 1.0704 0.099 Uiso 1 1 calc R . .
H22B H 0.6648 0.7703 1.1700 0.099 Uiso 1 1 calc R . .
H22C H 0.6487 0.6463 1.1243 0.099 Uiso 1 1 calc R . .
S1 S 0.51235(7) 0.6366(2) 0.73491(19) 0.0843(7) Uani 0.50 1 d P . .
C31 C 0.4801(3) 0.7281(9) 0.6556(5) 0.123(3) Uani 1 1 d . . .
O33 O 0.5286(2) 0.5463(6) 0.7762(7) 0.142(3) Uani 0.50 1 d P . .
H31B H 0.457(2) 0.781(4) 0.668(4) 0.116(18) Uiso 1 1 d . . .
H31C H 0.498(3) 0.805(7) 0.660(5) 0.20(4) Uiso 1 1 d . . .
H31A H 0.472(3) 0.700(6) 0.601(5) 0.17(3) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 2.025(2) . ?
Zn1 O3 2.0295(19) . ?
Zn1 O2 2.0805(19) . ?
Zn1 N2 2.190(2) . ?
Zn1 N1 2.195(2) . ?
Zn1 O1 2.450(2) . ?
Zn1 C11 2.596(3) . ?
O1 C11 1.238(3) . ?
O2 C11 1.253(3) . ?
O3 C21 1.243(3) . ?
O4 C21 1.237(3) 7_667 ?
N1 C5 1.327(3) . ?
N1 C1 1.332(3) . ?
N2 C8 1.333(3) . ?
N2 C9 1.333(3) . ?
C1 C2 1.381(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.380(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(3) . ?
C3 C6 1.490(3) . ?
C4 C5 1.375(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.383(4) . ?
C6 C10 1.389(4) . ?
C7 C8 1.375(4) 1_545 ?
C7 H7 0.9300 . ?
C8 C7 1.375(4) 1_565 ?
C8 H8 0.9300 . ?
C9 C10 1.369(4) 1_565 ?
C9 H9 0.9300 . ?
C10 C9 1.369(4) 1_545 ?
C10 H10 0.9300 . ?
C11 C12 1.507(4) . ?
C12 C17 1.387(4) . ?
C12 C13 1.405(4) . ?
C13 C14 1.389(4) . ?
C13 C18 1.491(5) . ?
C14 C15 1.370(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.383(6) . ?
C15 C19 1.521(5) . ?
C16 C17 1.390(4) . ?
C16 H16 0.9300 . ?
C17 C20 1.498(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.237(3) 7_667 ?
C21 C22 1.495(4) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
S1 S1 0.974(4) 2_656 ?
S1 O33 1.201(7) . ?
S1 O33 1.511(7) 2_656 ?
S1 C31 1.573(8) . ?
S1 C31 1.892(8) 2_656 ?
C31 S1 1.892(8) 2_656 ?
C31 H31B 0.97(5) . ?
C31 H31C 1.01(8) . ?
C31 H31A 0.82(7) . ?
O33 O33 1.481(13) 2_656 ?
O33 S1 1.511(7) 2_656 ?

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 O3 122.48(10) . . ?
O4 Zn1 O2 142.13(9) . . ?
O3 Zn1 O2 95.18(8) . . ?
O4 Zn1 N2 86.73(8) . . ?
O3 Zn1 N2 88.46(8) . . ?
O2 Zn1 N2 90.81(8) . . ?
O4 Zn1 N1 91.94(8) . . ?
O3 Zn1 N1 90.67(8) . . ?
O2 Zn1 N1 91.39(8) . . ?
N2 Zn1 N1 177.70(8) . . ?
O4 Zn1 O1 85.73(9) . . ?
O3 Zn1 O1 151.79(8) . . ?
O2 Zn1 O1 56.65(7) . . ?
N2 Zn1 O1 93.16(8) . . ?
N1 Zn1 O1 88.62(8) . . ?
O4 Zn1 C11 113.89(10) . . ?
O3 Zn1 C11 123.59(9) . . ?
O2 Zn1 C11 28.45(8) . . ?
N2 Zn1 C11 92.80(8) . . ?
N1 Zn1 C11 89.46(8) . . ?
O1 Zn1 C11 28.21(7) . . ?
C11 O1 Zn1 82.44(18) . . ?
C11 O2 Zn1 99.27(17) . . ?
C21 O3 Zn1 127.73(18) . . ?
C21 O4 Zn1 152.4(2) 7_667 . ?
C5 N1 C1 116.3(2) . . ?
C5 N1 Zn1 123.26(17) . . ?
C1 N1 Zn1 120.48(17) . . ?
C8 N2 C9 115.9(2) . . ?
C8 N2 Zn1 121.51(17) . . ?
C9 N2 Zn1 122.56(18) . . ?
N1 C1 C2 123.6(2) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 116.3(2) . . ?
C2 C3 C6 122.7(2) . . ?
C4 C3 C6 121.1(2) . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 124.0(2) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C7 C6 C10 115.9(2) . . ?
C7 C6 C3 122.6(2) . . ?
C10 C6 C3 121.5(2) . . ?
C8 C7 C6 120.1(2) 1_545 . ?
C8 C7 H7 119.9 1_545 . ?
C6 C7 H7 119.9 . . ?
N2 C8 C7 123.9(2) . 1_565 ?
N2 C8 H8 118.1 . . ?
C7 C8 H8 118.1 1_565 . ?
N2 C9 C10 123.9(3) . 1_565 ?
N2 C9 H9 118.0 . . ?
C10 C9 H9 118.0 1_565 . ?
C9 C10 C6 120.2(2) 1_545 . ?
C9 C10 H10 119.9 1_545 . ?
C6 C10 H10 119.9 . . ?
O1 C11 O2 121.6(3) . . ?
O1 C11 C12 121.1(3) . . ?
O2 C11 C12 117.3(2) . . ?
O1 C11 Zn1 69.35(16) . . ?
O2 C11 Zn1 52.28(13) . . ?
C12 C11 Zn1 169.5(2) . . ?
C17 C12 C13 120.6(3) . . ?
C17 C12 C11 119.9(3) . . ?
C13 C12 C11 119.4(3) . . ?
C14 C13 C12 118.4(3) . . ?
C14 C13 C18 120.8(3) . . ?
C12 C13 C18 120.9(3) . . ?
C15 C14 C13 122.3(4) . . ?
C15 C14 H14 118.8 . . ?
C13 C14 H14 118.8 . . ?
C14 C15 C16 117.8(3) . . ?
C14 C15 C19 120.5(4) . . ?
C16 C15 C19 121.6(4) . . ?
C15 C16 C17 122.6(4) . . ?
C15 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C12 C17 C16 118.2(3) . . ?
C12 C17 C20 120.1(3) . . ?
C16 C17 C20 121.7(3) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19A 109.5 . . ?
C15 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C15 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 O3 127.2(3) 7_667 . ?
O4 C21 C22 116.4(3) 7_667 . ?
O3 C21 C22 116.4(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
S1 S1 O33 87.4(4) 2_656 . ?
S1 S1 O33 52.5(3) 2_656 2_656 ?
O33 S1 O33 65.0(6) . 2_656 ?
S1 S1 C31 92.9(3) 2_656 . ?
O33 S1 C31 162.1(6) . . ?
O33 S1 C31 101.3(5) 2_656 . ?
S1 S1 C31 56.1(3) 2_656 2_656 ?
O33 S1 C31 98.4(6) . 2_656 ?
O33 S1 C31 106.7(4) 2_656 2_656 ?
C31 S1 C31 96.6(6) . 2_656 ?
S1 C31 S1 30.95(19) . 2_656 ?
S1 C31 H31B 120(3) . . ?
S1 C31 H31B 92(3) 2_656 . ?
S1 C31 H31C 115(4) . . ?
S1 C31 H31C 123(4) 2_656 . ?
H31B C31 H31C 78(5) . . ?
S1 C31 H31A 109(5) . . ?
S1 C31 H31A 122(5) 2_656 . ?
H31B C31 H31A 120(6) . . ?
H31C C31 H31A 110(7) . . ?
S1 O33 O33 67.7(4) . 2_656 ?
S1 O33 S1 40.1(3) . 2_656 ?
O33 O33 S1 47.3(3) 2_656 2_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Zn1 O1 C11 -176.51(17) . . . . ?
O3 Zn1 O1 C11 2.6(3) . . . . ?
O2 Zn1 O1 C11 -1.14(15) . . . . ?
N2 Zn1 O1 C11 -90.03(17) . . . . ?
N1 Zn1 O1 C11 91.44(17) . . . . ?
O4 Zn1 O2 C11 8.7(2) . . . . ?
O3 Zn1 O2 C11 -177.09(16) . . . . ?
N2 Zn1 O2 C11 94.38(17) . . . . ?
N1 Zn1 O2 C11 -86.29(17) . . . . ?
O1 Zn1 O2 C11 1.13(15) . . . . ?
O4 Zn1 O3 C21 -35.9(2) . . . . ?
O2 Zn1 O3 C21 148.3(2) . . . . ?
N2 Zn1 O3 C21 -121.0(2) . . . . ?
N1 Zn1 O3 C21 56.9(2) . . . . ?
O1 Zn1 O3 C21 145.2(2) . . . . ?
C11 Zn1 O3 C21 146.7(2) . . . . ?
O3 Zn1 O4 C21 51.4(5) . . . 7_667 ?
O2 Zn1 O4 C21 -135.5(4) . . . 7_667 ?
N2 Zn1 O4 C21 137.4(5) . . . 7_667 ?
N1 Zn1 O4 C21 -40.7(5) . . . 7_667 ?
O1 Zn1 O4 C21 -129.2(5) . . . 7_667 ?
C11 Zn1 O4 C21 -131.0(4) . . . 7_667 ?
O4 Zn1 N1 C5 -19.6(2) . . . . ?
O3 Zn1 N1 C5 -142.2(2) . . . . ?
O2 Zn1 N1 C5 122.6(2) . . . . ?
N2 Zn1 N1 C5 -74(2) . . . . ?
O1 Zn1 N1 C5 66.0(2) . . . . ?
C11 Zn1 N1 C5 94.2(2) . . . . ?
O4 Zn1 N1 C1 160.4(2) . . . . ?
O3 Zn1 N1 C1 37.9(2) . . . . ?
O2 Zn1 N1 C1 -57.3(2) . . . . ?
N2 Zn1 N1 C1 106(2) . . . . ?
O1 Zn1 N1 C1 -113.9(2) . . . . ?
C11 Zn1 N1 C1 -85.7(2) . . . . ?
O4 Zn1 N2 C8 -156.3(2) . . . . ?
O3 Zn1 N2 C8 -33.7(2) . . . . ?
O2 Zn1 N2 C8 61.5(2) . . . . ?
N1 Zn1 N2 C8 -101(2) . . . . ?
O1 Zn1 N2 C8 118.1(2) . . . . ?
C11 Zn1 N2 C8 89.9(2) . . . . ?
O4 Zn1 N2 C9 24.9(2) . . . . ?
O3 Zn1 N2 C9 147.5(2) . . . . ?
O2 Zn1 N2 C9 -117.3(2) . . . . ?
N1 Zn1 N2 C9 80(2) . . . . ?
O1 Zn1 N2 C9 -60.7(2) . . . . ?
C11 Zn1 N2 C9 -88.9(2) . . . . ?
C5 N1 C1 C2 1.4(4) . . . . ?
Zn1 N1 C1 C2 -178.6(2) . . . . ?
N1 C1 C2 C3 -0.6(5) . . . . ?
C1 C2 C3 C4 -0.5(4) . . . . ?
C1 C2 C3 C6 -178.9(3) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C6 C3 C4 C5 179.2(3) . . . . ?
C1 N1 C5 C4 -1.1(4) . . . . ?
Zn1 N1 C5 C4 178.9(2) . . . . ?
C3 C4 C5 N1 0.0(5) . . . . ?
C2 C3 C6 C7 -5.0(4) . . . . ?
C4 C3 C6 C7 176.7(2) . . . . ?
C2 C3 C6 C10 173.4(3) . . . . ?
C4 C3 C6 C10 -4.9(4) . . . . ?
C10 C6 C7 C8 -0.8(4) . . . 1_545 ?
C3 C6 C7 C8 177.7(2) . . . 1_545 ?
C9 N2 C8 C7 -0.6(4) . . . 1_565 ?
Zn1 N2 C8 C7 -179.5(2) . . . 1_565 ?
C8 N2 C9 C10 -0.3(4) . . . 1_565 ?
Zn1 N2 C9 C10 178.6(2) . . . 1_565 ?
C7 C6 C10 C9 0.0(4) . . . 1_545 ?
C3 C6 C10 C9 -178.5(3) . . . 1_545 ?
Zn1 O1 C11 O2 1.9(2) . . . . ?
Zn1 O1 C11 C12 -178.4(2) . . . . ?
Zn1 O2 C11 O1 -2.2(3) . . . . ?
Zn1 O2 C11 C12 178.0(2) . . . . ?
O4 Zn1 C11 O1 3.81(18) . . . . ?
O3 Zn1 C11 O1 -178.53(15) . . . . ?
O2 Zn1 C11 O1 178.0(3) . . . . ?
N2 Zn1 C11 O1 91.47(17) . . . . ?
N1 Zn1 C11 O1 -88.08(17) . . . . ?
O4 Zn1 C11 O2 -174.19(15) . . . . ?
O3 Zn1 C11 O2 3.47(19) . . . . ?
N2 Zn1 C11 O2 -86.53(17) . . . . ?
N1 Zn1 C11 O2 93.92(17) . . . . ?
O1 Zn1 C11 O2 -178.0(3) . . . . ?
O4 Zn1 C11 C12 176.2(10) . . . . ?
O3 Zn1 C11 C12 -6.1(11) . . . . ?
O2 Zn1 C11 C12 -9.6(10) . . . . ?
N2 Zn1 C11 C12 -96.1(11) . . . . ?
N1 Zn1 C11 C12 84.4(11) . . . . ?
O1 Zn1 C11 C12 172.4(11) . . . . ?
O1 C11 C12 C17 -91.6(3) . . . . ?
O2 C11 C12 C17 88.2(3) . . . . ?
Zn1 C11 C12 C17 96.7(11) . . . . ?
O1 C11 C12 C13 90.6(3) . . . . ?
O2 C11 C12 C13 -89.7(3) . . . . ?
Zn1 C11 C12 C13 -81.2(11) . . . . ?
C17 C12 C13 C14 -2.4(4) . . . . ?
C11 C12 C13 C14 175.5(3) . . . . ?
C17 C12 C13 C18 177.6(3) . . . . ?
C11 C12 C13 C18 -4.6(4) . . . . ?
C12 C13 C14 C15 -0.5(5) . . . . ?
C18 C13 C14 C15 179.5(3) . . . . ?
C13 C14 C15 C16 3.0(5) . . . . ?
C13 C14 C15 C19 -176.3(3) . . . . ?
C14 C15 C16 C17 -2.8(5) . . . . ?
C19 C15 C16 C17 176.4(3) . . . . ?
C13 C12 C17 C16 2.5(4) . . . . ?
C11 C12 C17 C16 -175.3(3) . . . . ?
C13 C12 C17 C20 -176.6(3) . . . . ?
C11 C12 C17 C20 5.5(4) . . . . ?
C15 C16 C17 C12 0.1(5) . . . . ?
C15 C16 C17 C20 179.3(3) . . . . ?
Zn1 O3 C21 O4 17.2(4) . . . 7_667 ?
Zn1 O3 C21 C22 -163.9(2) . . . . ?
O33 S1 C31 S1 90.6(16) . . . 2_656 ?
O33 S1 C31 S1 52.3(3) 2_656 . . 2_656 ?
C31 S1 C31 S1 -56.2(3) 2_656 . . 2_656 ?
S1 S1 O33 O33 49.4(6) 2_656 . . 2_656 ?
C31 S1 O33 O33 -42(2) . . . 2_656 ?
C31 S1 O33 O33 104.6(6) 2_656 . . 2_656 ?
O33 S1 O33 S1 -49.4(6) 2_656 . . 2_656 ?
C31 S1 O33 S1 -91.5(16) . . . 2_656 ?
C31 S1 O33 S1 55.2(3) 2_656 . . 2_656 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.055
_database_code_depnum_ccdc_archive 'CCDC 993879'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rk1-195

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H28 N2 O8 P2 Zn'
_chemical_formula_sum            'C34 H28 N2 O8 P2 Zn'
_chemical_formula_weight         719.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.74(12)
_cell_length_b                   28.36(13)
_cell_length_c                   10.39(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.66(8)
_cell_angle_gamma                90.00
_cell_volume                     6559(56)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5995
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      31.3

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2960
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23519
_diffrn_reflns_av_R_equivalents  0.1876
_diffrn_reflns_av_sigmaI/netI    0.1406
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5770
_reflns_number_gt                4708
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1295P)²+40.9902P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5770
_refine_ls_number_parameters     424
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.1326
_refine_ls_wR_factor_ref         0.3494
_refine_ls_wR_factor_gt          0.3206
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_restrained_S_all      1.308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1288(4) 0.2812(3) 0.7750(8) 0.024(2) Uani 1 1 d . . .
H1 H 0.1524 0.3088 0.7972 0.029 Uiso 1 1 calc R . .
C2 C 0.0675(4) 0.2839(3) 0.7798(8) 0.0180(19) Uani 1 1 d . . .
H2 H 0.0505 0.3122 0.8048 0.022 Uiso 1 1 calc R . .
C3 C 0.0326(4) 0.2441(3) 0.7470(8) 0.019(2) Uani 1 1 d . . .
C4 C 0.0599(4) 0.2041(3) 0.7098(8) 0.020(2) Uani 1 1 d . . .
H4 H 0.0371 0.1764 0.6846 0.024 Uiso 1 1 calc R . .
C5 C 0.1212(4) 0.2049(3) 0.7094(8) 0.0160(19) Uani 1 1 d U . .
H5 H 0.1393 0.1770 0.6850 0.019 Uiso 1 1 calc R . .
C6 C 0.3647(4) 0.2541(3) 0.6381(9) 0.024(2) Uani 1 1 d . . .
H6 H 0.3369 0.2615 0.5594 0.029 Uiso 1 1 calc R . .
C7 C 0.4243(4) 0.2547(3) 0.6359(9) 0.027(2) Uani 1 1 d . . .
H7 H 0.4369 0.2624 0.5568 0.033 Uiso 1 1 calc R . .
C8 C 0.4679(4) 0.2440(3) 0.7510(10) 0.032(3) Uani 1 1 d U . .
C9 C 0.4449(5) 0.2332(3) 0.8609(9) 0.029(2) Uani 1 1 d . . .
H9 H 0.4718 0.2254 0.9404 0.035 Uiso 1 1 calc R . .
C10 C 0.3838(4) 0.2334(3) 0.8585(8) 0.022(2) Uani 1 1 d . . .
H10 H 0.3702 0.2263 0.9370 0.027 Uiso 1 1 calc R . .
C11 C 0.1277(4) 0.1309(3) 0.9935(9) 0.021(2) Uani 1 1 d U . .
C12 C 0.0839(4) 0.1054(3) 0.9092(10) 0.028(2) Uani 1 1 d . . .
H12 H 0.0881 0.0977 0.8225 0.033 Uiso 1 1 calc R . .
C13 C 0.0333(5) 0.0915(3) 0.9570(10) 0.034(3) Uani 1 1 d . . .
H13 H 0.0025 0.0741 0.9016 0.041 Uiso 1 1 calc R . .
C14 C 0.0275(5) 0.1024(4) 1.0827(13) 0.045(3) Uani 1 1 d . . .
H14 H -0.0075 0.0930 1.1130 0.055 Uiso 1 1 calc R . .
C15 C 0.0728(5) 0.1273(4) 1.1659(11) 0.039(3) Uani 1 1 d U . .
H15 H 0.0690 0.1346 1.2530 0.047 Uiso 1 1 calc R . .
C16 C 0.1246(5) 0.1414(3) 1.1193(9) 0.031(2) Uani 1 1 d . . .
H16 H 0.1563 0.1579 1.1748 0.037 Uiso 1 1 calc R . .
C17 C 0.2988(4) 0.0938(3) 1.0303(9) 0.026(2) Uani 1 1 d . . .
C18 C 0.2833(5) 0.0510(4) 1.0815(10) 0.038(3) Uani 1 1 d . . .
H18 H 0.2576 0.0499 1.1430 0.046 Uiso 1 1 calc R . .
C19 C 0.3072(6) 0.0101(4) 1.0384(14) 0.056(4) Uani 1 1 d . . .
H19 H 0.2966 -0.0197 1.0689 0.067 Uiso 1 1 calc R . .
C20 C 0.3468(6) 0.0121(4) 0.9504(16) 0.063(4) Uani 1 1 d . . .
H20 H 0.3646 -0.0157 0.9242 0.076 Uiso 1 1 calc R . .
C21 C 0.3585(6) 0.0548(4) 0.9047(14) 0.059(4) Uani 1 1 d . . .
H21 H 0.3830 0.0561 0.8407 0.070 Uiso 1 1 calc R . .
C22 C 0.3375(4) 0.0964(3) 0.9441(10) 0.032(2) Uani 1 1 d . . .
H22 H 0.3491 0.1258 0.9135 0.038 Uiso 1 1 calc R . .
C23 C 0.3033(4) 0.4077(3) 0.4920(9) 0.025(2) Uani 1 1 d U . .
C24 C 0.3421(5) 0.4400(3) 0.5662(10) 0.031(2) Uani 1 1 d . . .
H24 H 0.3509 0.4379 0.6594 0.037 Uiso 1 1 calc R . .
C25 C 0.3679(5) 0.4750(4) 0.5038(12) 0.047(3) Uani 1 1 d . . .
H25 H 0.3947 0.4967 0.5550 0.056 Uiso 1 1 calc R . .
C26 C 0.3554(5) 0.4793(4) 0.3684(11) 0.042(3) Uani 1 1 d . . .
H26 H 0.3731 0.5036 0.3259 0.051 Uiso 1 1 calc R . .
C27 C 0.3155(4) 0.4463(4) 0.2957(10) 0.031(2) Uani 1 1 d . . .
H27 H 0.3060 0.4489 0.2026 0.037 Uiso 1 1 calc R . .
C28 C 0.2897(4) 0.4103(3) 0.3553(9) 0.029(2) Uani 1 1 d . . .
H28 H 0.2636 0.3880 0.3045 0.035 Uiso 1 1 calc R . .
C29 C 0.1317(4) 0.3694(3) 0.4894(9) 0.025(2) Uani 1 1 d . . .
C30 C 0.0744(4) 0.3695(4) 0.4059(10) 0.033(2) Uani 1 1 d . . .
H30 H 0.0684 0.3582 0.3181 0.039 Uiso 1 1 calc R . .
C31 C 0.0261(5) 0.3872(4) 0.4589(12) 0.045(3) Uani 1 1 d . . .
H31 H -0.0132 0.3868 0.4058 0.055 Uiso 1 1 calc R . .
C32 C 0.0338(5) 0.4047(4) 0.5831(11) 0.041(3) Uani 1 1 d . . .
H32 H 0.0008 0.4173 0.6150 0.050 Uiso 1 1 calc R . .
C33 C 0.0907(4) 0.4039(3) 0.6623(10) 0.025(2) Uani 1 1 d . . .
H33 H 0.0963 0.4161 0.7491 0.030 Uiso 1 1 calc R . .
C34 C 0.1408(4) 0.3854(3) 0.6171(8) 0.023(2) Uani 1 1 d . . .
H34 H 0.1794 0.3841 0.6731 0.028 Uiso 1 1 calc R . .
N1 N 0.1561(3) 0.2434(2) 0.7421(7) 0.0179(17) Uani 1 1 d . . .
N2 N 0.3427(4) 0.2434(2) 0.7477(7) 0.0213(17) Uani 1 1 d . . .
O1 O 0.2323(3) 0.3032(2) 0.6265(5) 0.0192(14) Uani 1 1 d . . .
O2 O 0.2626(3) 0.1858(2) 0.8804(6) 0.0213(14) Uani 1 1 d . . .
O3 O 0.2752(3) 0.2900(2) 0.9121(5) 0.0180(14) Uani 1 1 d . . .
O5 O 0.1756(3) 0.1440(2) 0.9331(6) 0.0246(15) Uani 1 1 d . . .
O6 O 0.2768(3) 0.1344(2) 1.0841(6) 0.0272(17) Uani 1 1 d . . .
O7 O 0.2335(3) 0.1950(2) 0.5944(6) 0.0213(14) Uani 1 1 d . . .
O8 O 0.2800(3) 0.3740(2) 0.5656(6) 0.0252(16) Uani 1 1 d . . .
O9 O 0.1777(3) 0.3513(2) 0.4324(6) 0.0248(15) Uani 1 1 d . . .
Zn01 Zn 0.25048(4) 0.24328(4) 0.75080(9) 0.0172(4) Uani 1 1 d . . .
P1 P 0.24021(10) 0.32926(8) 0.5095(2) 0.0196(6) Uani 1 1 d . . .
P3 P 0.23608(10) 0.17343(8) 0.9948(2) 0.0176(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.317(12) . ?
C1 C2 1.408(14) . ?
C1 H1 0.9500 . ?
C2 C3 1.382(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(13) . ?
C3 C3 1.50(2) 2_556 ?
C4 C5 1.394(14) . ?
C4 H4 0.9500 . ?
C5 N1 1.353(12) . ?
C5 H5 0.9500 . ?
C6 C7 1.359(16) . ?
C6 N2 1.367(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.424(13) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(16) . ?
C8 C8 1.46(2) 2_656 ?
C9 C10 1.385(15) . ?
C9 H9 0.9500 . ?
C10 N2 1.358(12) . ?
C10 H10 0.9500 . ?
C11 C16 1.356(14) . ?
C11 C12 1.389(13) . ?
C11 O5 1.411(12) . ?
C12 C13 1.397(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.374(17) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(16) . ?
C14 H14 0.9500 . ?
C15 C16 1.420(15) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.378(15) . ?
C17 C18 1.398(14) . ?
C17 O6 1.416(12) . ?
C18 C19 1.393(17) . ?
C18 H18 0.9500 . ?
C19 C20 1.407(19) . ?
C19 H19 0.9500 . ?
C20 C21 1.347(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.365(16) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.393(14) . ?
C23 C24 1.392(13) . ?
C23 O8 1.394(12) . ?
C24 C25 1.380(15) . ?
C24 H24 0.9500 . ?
C25 C26 1.382(17) . ?
C25 H25 0.9500 . ?
C26 C27 1.412(15) . ?
C26 H26 0.9500 . ?
C27 C28 1.384(14) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.378(14) . ?
C29 O9 1.400(13) . ?
C29 C30 1.412(14) . ?
C30 C31 1.415(15) . ?
C30 H30 0.9500 . ?
C31 C32 1.360(16) . ?
C31 H31 0.9500 . ?
C32 C33 1.385(15) . ?
C32 H32 0.9500 . ?
C33 C34 1.418(14) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
N1 Zn01 2.130(14) . ?
N2 Zn01 2.104(14) . ?
O1 P1 1.463(8) . ?
O1 Zn01 2.124(9) . ?
O2 P3 1.479(8) . ?
O2 Zn01 2.096(9) . ?
O3 P3 1.476(8) 7_557 ?
O3 Zn01 2.120(9) . ?
O5 P3 1.625(9) . ?
O6 P3 1.611(8) . ?
O7 P1 1.501(8) 7_556 ?
O7 Zn01 2.100(9) . ?
O8 P1 1.598(8) . ?
O9 P1 1.609(8) . ?
P1 O7 1.501(8) 7_556 ?
P3 O3 1.476(8) 7_557 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 125.0(8) . . ?
N1 C1 H1 117.5 . . ?
C2 C1 H1 117.5 . . ?
C3 C2 C1 118.1(8) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 118.0(9) . . ?
C2 C3 C3 120.9(6) . 2_556 ?
C4 C3 C3 121.1(6) . 2_556 ?
C3 C4 C5 119.6(8) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 123.1(8) . . ?
N1 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
C7 C6 N2 123.4(8) . . ?
C7 C6 H6 118.3 . . ?
N2 C6 H6 118.3 . . ?
C6 C7 C8 120.7(10) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C9 C8 C7 115.1(10) . . ?
C9 C8 C8 123.9(11) . 2_656 ?
C7 C8 C8 121.0(13) . 2_656 ?
C10 C9 C8 122.1(8) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
N2 C10 C9 122.1(9) . . ?
N2 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C16 C11 C12 123.4(10) . . ?
C16 C11 O5 124.4(8) . . ?
C12 C11 O5 112.1(9) . . ?
C11 C12 C13 117.4(10) . . ?
C11 C12 H12 121.3 . . ?
C13 C12 H12 121.3 . . ?
C14 C13 C12 121.2(10) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 120.1(11) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C16 119.4(11) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C11 C16 C15 118.4(9) . . ?
C11 C16 H16 120.8 . . ?
C15 C16 H16 120.8 . . ?
C22 C17 C18 122.4(10) . . ?
C22 C17 O6 122.4(9) . . ?
C18 C17 O6 114.9(10) . . ?
C17 C18 C19 117.2(12) . . ?
C17 C18 H18 121.4 . . ?
C19 C18 H18 121.4 . . ?
C18 C19 C20 121.1(11) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C21 C20 C19 117.6(12) . . ?
C21 C20 H20 121.2 . . ?
C19 C20 H20 121.2 . . ?
C20 C21 C22 124.4(14) . . ?
C20 C21 H21 117.8 . . ?
C22 C21 H21 117.8 . . ?
C21 C22 C17 117.1(11) . . ?
C21 C22 H22 121.4 . . ?
C17 C22 H22 121.4 . . ?
C28 C23 C24 121.0(9) . . ?
C28 C23 O8 124.4(8) . . ?
C24 C23 O8 114.6(8) . . ?
C25 C24 C23 119.7(10) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 121.4(10) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C25 C26 C27 117.6(10) . . ?
C25 C26 H26 121.2 . . ?
C27 C26 H26 121.2 . . ?
C28 C27 C26 122.3(10) . . ?
C28 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
C27 C28 C23 117.9(9) . . ?
C27 C28 H28 121.0 . . ?
C23 C28 H28 121.0 . . ?
C34 C29 O9 123.2(8) . . ?
C34 C29 C30 122.1(10) . . ?
O9 C29 C30 114.7(9) . . ?
C31 C30 C29 117.0(10) . . ?
C31 C30 H30 121.5 . . ?
C29 C30 H30 121.5 . . ?
C32 C31 C30 122.5(10) . . ?
C32 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
C31 C32 C33 118.9(10) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C32 C33 C34 121.7(10) . . ?
C32 C33 H33 119.2 . . ?
C34 C33 H33 119.2 . . ?
C29 C34 C33 117.8(9) . . ?
C29 C34 H34 121.1 . . ?
C33 C34 H34 121.1 . . ?
C1 N1 C5 116.1(8) . . ?
C1 N1 Zn01 120.9(6) . . ?
C5 N1 Zn01 122.9(6) . . ?
C10 N2 C6 116.6(9) . . ?
C10 N2 Zn01 120.2(7) . . ?
C6 N2 Zn01 123.2(6) . . ?
P1 O1 Zn01 150.2(4) . . ?
P3 O2 Zn01 132.7(4) . . ?
P3 O3 Zn01 154.7(4) 7_557 . ?
C11 O5 P3 128.9(6) . . ?
C17 O6 P3 122.7(6) . . ?
P1 O7 Zn01 144.8(4) 7_556 . ?
C23 O8 P1 126.4(6) . . ?
C29 O9 P1 126.3(6) . . ?
O2 Zn01 O7 88.3(4) . . ?
O2 Zn01 N2 90.5(3) . . ?
O7 Zn01 N2 91.0(3) . . ?
O2 Zn01 O3 89.9(4) . . ?
O7 Zn01 O3 175.2(2) . . ?
N2 Zn01 O3 84.6(3) . . ?
O2 Zn01 O1 175.4(2) . . ?
O7 Zn01 O1 93.9(4) . . ?
N2 Zn01 O1 93.5(3) . . ?
O3 Zn01 O1 88.2(4) . . ?
O2 Zn01 N1 91.7(3) . . ?
O7 Zn01 N1 86.7(3) . . ?
N2 Zn01 N1 176.8(3) . . ?
O3 Zn01 N1 97.8(3) . . ?
O1 Zn01 N1 84.4(3) . . ?
O1 P1 O7 119.9(5) . 7_556 ?
O1 P1 O8 104.6(4) . . ?
O7 P1 O8 110.3(4) 7_556 . ?
O1 P1 O9 111.4(4) . . ?
O7 P1 O9 105.1(5) 7_556 . ?
O8 P1 O9 104.6(5) . . ?
O3 P3 O2 120.8(4) 7_557 . ?
O3 P3 O6 105.1(5) 7_557 . ?
O2 P3 O6 110.2(5) . . ?
O3 P3 O5 112.0(4) 7_557 . ?
O2 P3 O5 104.8(4) . . ?
O6 P3 O5 102.5(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.4(13) . . . . ?
C1 C2 C3 C4 -0.8(12) . . . . ?
C1 C2 C3 C3 178.6(9) . . . 2_556 ?
C2 C3 C4 C5 1.5(12) . . . . ?
C3 C3 C4 C5 -177.9(9) 2_556 . . . ?
C3 C4 C5 N1 -1.1(13) . . . . ?
N2 C6 C7 C8 0.0(14) . . . . ?
C6 C7 C8 C9 0.1(13) . . . . ?
C6 C7 C8 C8 179.2(7) . . . 2_656 ?
C7 C8 C9 C10 -0.6(14) . . . . ?
C8 C8 C9 C10 -179.7(7) 2_656 . . . ?
C8 C9 C10 N2 1.2(15) . . . . ?
C16 C11 C12 C13 2.0(14) . . . . ?
O5 C11 C12 C13 -178.4(8) . . . . ?
C11 C12 C13 C14 -0.3(15) . . . . ?
C12 C13 C14 C15 -0.9(17) . . . . ?
C13 C14 C15 C16 0.5(17) . . . . ?
C12 C11 C16 C15 -2.5(15) . . . . ?
O5 C11 C16 C15 178.0(9) . . . . ?
C14 C15 C16 C11 1.2(16) . . . . ?
C22 C17 C18 C19 -2.1(14) . . . . ?
O6 C17 C18 C19 -175.8(9) . . . . ?
C17 C18 C19 C20 2.0(17) . . . . ?
C18 C19 C20 C21 -3(2) . . . . ?
C19 C20 C21 C22 4(2) . . . . ?
C20 C21 C22 C17 -4.2(18) . . . . ?
C18 C17 C22 C21 3.0(15) . . . . ?
O6 C17 C22 C21 176.3(9) . . . . ?
C28 C23 C24 C25 -0.2(16) . . . . ?
O8 C23 C24 C25 -180.0(10) . . . . ?
C23 C24 C25 C26 0.7(18) . . . . ?
C24 C25 C26 C27 -0.3(18) . . . . ?
C25 C26 C27 C28 -0.8(17) . . . . ?
C26 C27 C28 C23 1.3(16) . . . . ?
C24 C23 C28 C27 -0.8(15) . . . . ?
O8 C23 C28 C27 179.0(9) . . . . ?
C34 C29 C30 C31 0.4(15) . . . . ?
O9 C29 C30 C31 179.6(9) . . . . ?
C29 C30 C31 C32 1.9(17) . . . . ?
C30 C31 C32 C33 -2.0(18) . . . . ?
C31 C32 C33 C34 0.1(16) . . . . ?
O9 C29 C34 C33 178.6(8) . . . . ?
C30 C29 C34 C33 -2.2(14) . . . . ?
C32 C33 C34 C29 2.0(14) . . . . ?
C2 C1 N1 C5 0.8(12) . . . . ?
C2 C1 N1 Zn01 -176.1(7) . . . . ?
C4 C5 N1 C1 -0.1(12) . . . . ?
C4 C5 N1 Zn01 176.8(6) . . . . ?
C9 C10 N2 C6 -1.1(13) . . . . ?
C9 C10 N2 Zn01 -179.9(7) . . . . ?
C7 C6 N2 C10 0.5(13) . . . . ?
C7 C6 N2 Zn01 179.3(7) . . . . ?
C16 C11 O5 P3 0.0(13) . . . . ?
C12 C11 O5 P3 -179.5(6) . . . . ?
C22 C17 O6 P3 62.1(11) . . . . ?
C18 C17 O6 P3 -124.1(8) . . . . ?
C28 C23 O8 P1 7.2(14) . . . . ?
C24 C23 O8 P1 -173.0(7) . . . . ?
C34 C29 O9 P1 22.7(13) . . . . ?
C30 C29 O9 P1 -156.6(7) . . . . ?
P3 O2 Zn01 O7 -127.5(6) . . . . ?
P3 O2 Zn01 N2 141.6(5) . . . . ?
P3 O2 Zn01 O3 57.0(6) . . . . ?
P3 O2 Zn01 O1 -9(3) . . . . ?
P3 O2 Zn01 N1 -40.8(5) . . . . ?
P1 O7 Zn01 O2 -101.0(7) 7_556 . . . ?
P1 O7 Zn01 N2 -10.5(6) 7_556 . . . ?
P1 O7 Zn01 O3 -33(3) 7_556 . . . ?
P1 O7 Zn01 O1 83.0(7) 7_556 . . . ?
P1 O7 Zn01 N1 167.2(7) 7_556 . . . ?
C10 N2 Zn01 O2 -37.0(7) . . . . ?
C6 N2 Zn01 O2 144.3(7) . . . . ?
C10 N2 Zn01 O7 -125.2(7) . . . . ?
C6 N2 Zn01 O7 56.0(7) . . . . ?
C10 N2 Zn01 O3 52.9(7) . . . . ?
C6 N2 Zn01 O3 -125.9(7) . . . . ?
C10 N2 Zn01 O1 140.8(7) . . . . ?
C6 N2 Zn01 O1 -38.0(7) . . . . ?
C10 N2 Zn01 N1 -170(5) . . . . ?
C6 N2 Zn01 N1 12(6) . . . . ?
P3 O3 Zn01 O2 -109.8(9) 7_557 . . . ?
P3 O3 Zn01 O7 -178(55) 7_557 . . . ?
P3 O3 Zn01 N2 159.6(9) 7_557 . . . ?
P3 O3 Zn01 O1 65.9(8) 7_557 . . . ?
P3 O3 Zn01 N1 -18.2(9) 7_557 . . . ?
P1 O1 Zn01 O2 -165(2) . . . . ?
P1 O1 Zn01 O7 -47.0(8) . . . . ?
P1 O1 Zn01 N2 44.2(8) . . . . ?
P1 O1 Zn01 O3 128.7(8) . . . . ?
P1 O1 Zn01 N1 -133.3(8) . . . . ?
C1 N1 Zn01 O2 122.3(7) . . . . ?
C5 N1 Zn01 O2 -54.4(7) . . . . ?
C1 N1 Zn01 O7 -149.5(7) . . . . ?
C5 N1 Zn01 O7 33.8(7) . . . . ?
C1 N1 Zn01 N2 -105(5) . . . . ?
C5 N1 Zn01 N2 78(5) . . . . ?
C1 N1 Zn01 O3 32.2(7) . . . . ?
C5 N1 Zn01 O3 -144.5(6) . . . . ?
C1 N1 Zn01 O1 -55.2(7) . . . . ?
C5 N1 Zn01 O1 128.0(7) . . . . ?
Zn01 O1 P1 O7 14.0(9) . . . 7_556 ?
Zn01 O1 P1 O8 -110.4(8) . . . . ?
Zn01 O1 P1 O9 137.1(7) . . . . ?
C23 O8 P1 O1 175.0(7) . . . . ?
C23 O8 P1 O7 44.7(8) . . . 7_556 ?
C23 O8 P1 O9 -67.8(8) . . . . ?
C29 O9 P1 O1 35.6(8) . . . . ?
C29 O9 P1 O7 166.9(7) . . . 7_556 ?
C29 O9 P1 O8 -76.8(8) . . . . ?
Zn01 O2 P3 O3 -38.8(7) . . . 7_557 ?
Zn01 O2 P3 O6 -161.8(4) . . . . ?
Zn01 O2 P3 O5 88.6(6) . . . . ?
C17 O6 P3 O3 -178.1(7) . . . 7_557 ?
C17 O6 P3 O2 -46.4(8) . . . . ?
C17 O6 P3 O5 64.7(8) . . . . ?
C11 O5 P3 O3 -34.9(8) . . . 7_557 ?
C11 O5 P3 O2 -167.6(7) . . . . ?
C11 O5 P3 O6 77.3(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.327
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.190

_database_code_depnum_ccdc_archive 'CCDC 993880'
