# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Parthasarathi Dastidar'
_publ_contact_author_email       PARTHOD123@REDIFFMAIL.COM

_publ_section_title              
;
Zn(II) Metal-Organic-Frameworks (MOFs) Derived from a
Bis-pyridyl-bis-urea ligand: Effects of Crystallization Solvents on the
Structures and Anion Binding Properties
;
loop_
_publ_author_name
'Parthasarathi Dastidar'
'N. N. Adarsh'
'D. Krishna Kumar'

# Attachment 'an0261m_FINAL_L.cif'

data_an0261m
_database_code_depnum_ccdc_archive 'CCDC 679361'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H16 N6 O2'
_chemical_formula_weight         300.33

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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   P2(1)/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                   8.593(2)
_cell_length_b                   8.850(3)
_cell_length_c                   9.927(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.927(5)
_cell_angle_gamma                90.00
_cell_volume                     695.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GOLDEN-YELLOW
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             316
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9547
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  'BRUKER CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3931
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         26.99
_reflns_number_total             1495
_reflns_number_gt                1183
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER AXS SMART 3'
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'MERCURY 1.4'

_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)+(0.0607P)²+0.0521P] 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         1495
_refine_ls_number_parameters     132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1112
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
N1 N 1.02558(16) -0.21055(14) 0.62888(14) 0.0433(3) Uani 1 1 d . . .
C2 C 0.95846(18) -0.08489(16) 0.65753(16) 0.0388(4) Uani 1 1 d . . .
C3 C 0.81010(16) -0.01756(15) 0.56028(14) 0.0334(3) Uani 1 1 d . . .
C4 C 0.72839(19) -0.08823(17) 0.42614(16) 0.0397(4) Uani 1 1 d . . .
C5 C 0.8001(2) -0.21588(17) 0.39479(18) 0.0432(4) Uani 1 1 d . . .
C6 C 0.9465(2) -0.27308(17) 0.49734(18) 0.0444(4) Uani 1 1 d . . .
N7 N 0.75277(15) 0.11148(14) 0.60727(13) 0.0393(3) Uani 1 1 d . . .
C8 C 0.63087(18) 0.21102(15) 0.52065(15) 0.0352(3) Uani 1 1 d . . .
O9 O 0.56167(14) 0.20090(13) 0.38793(11) 0.0495(3) Uani 1 1 d . . .
N10 N 0.59639(17) 0.32198(14) 0.59827(15) 0.0422(4) Uani 1 1 d . . .
C11 C 0.46608(19) 0.43331(17) 0.52786(17) 0.0406(4) Uani 1 1 d . . .
H2 H 1.0198(19) -0.0379(17) 0.7541(18) 0.043(4) Uiso 1 1 d . . .
H4 H 0.6263(19) -0.0497(18) 0.3598(17) 0.044(4) Uiso 1 1 d . . .
H5 H 0.749(2) -0.2610(19) 0.3059(19) 0.048(5) Uiso 1 1 d . . .
H6 H 0.999(2) -0.3637(19) 0.4783(18) 0.049(4) Uiso 1 1 d . . .
H7 H 0.813(2) 0.142(2) 0.695(2) 0.050(5) Uiso 1 1 d . . .
H10 H 0.628(2) 0.3145(19) 0.687(2) 0.049(5) Uiso 1 1 d . . .
H11A H 0.3719(19) 0.3902(17) 0.4462(17) 0.040(4) Uiso 1 1 d . . .
H11B H 0.4205(19) 0.4697(18) 0.6016(17) 0.044(4) 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
N1 C2 1.333(2) . ?
N1 C6 1.335(2) . ?
C2 C3 1.3976(19) . ?
C2 H2 0.987(16) . ?
C3 C4 1.389(2) . ?
C3 N7 1.3941(19) . ?
C4 C5 1.379(2) . ?
C4 H4 0.932(15) . ?
C5 C6 1.371(2) . ?
C5 H5 0.910(18) . ?
C6 H6 0.975(17) . ?
N7 C8 1.3824(18) . ?
N7 H7 0.868(18) . ?
C8 O9 1.2195(17) . ?
C8 N10 1.3504(19) . ?
N10 C11 1.4503(19) . ?
N10 H10 0.816(18) . ?
C11 C11 1.513(3) 3_666 ?
C11 H11A 0.973(16) . ?
C11 H11B 1.008(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C6 117.19(13) . . ?
N1 C2 C3 124.21(14) . . ?
N1 C2 H2 116.5(9) . . ?
C3 C2 H2 119.3(9) . . ?
C4 C3 N7 125.25(13) . . ?
C4 C3 C2 117.05(13) . . ?
N7 C3 C2 117.66(12) . . ?
C5 C4 C3 118.81(14) . . ?
C5 C4 H4 121.3(10) . . ?
C3 C4 H4 119.9(10) . . ?
C6 C5 C4 119.77(15) . . ?
C6 C5 H5 120.9(11) . . ?
C4 C5 H5 119.3(11) . . ?
N1 C6 C5 122.93(15) . . ?
N1 C6 H6 115.6(10) . . ?
C5 C6 H6 121.4(10) . . ?
C8 N7 C3 126.50(12) . . ?
C8 N7 H7 116.0(12) . . ?
C3 N7 H7 116.3(12) . . ?
O9 C8 N10 123.15(13) . . ?
O9 C8 N7 123.90(13) . . ?
N10 C8 N7 112.95(13) . . ?
C8 N10 C11 121.26(13) . . ?
C8 N10 H10 120.1(12) . . ?
C11 N10 H10 116.5(12) . . ?
N10 C11 C11 111.78(16) . 3_666 ?
N10 C11 H11A 111.8(9) . . ?
C11 C11 H11A 108.4(9) 3_666 . ?
N10 C11 H11B 108.2(9) . . ?
C11 C11 H11B 109.3(9) 3_666 . ?
H11A C11 H11B 107.3(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 N1 0.868(18) 2.186(19) 3.0138(18) 159.2(16) 2_756
N10 H10 O9 0.816(18) 2.284(18) 3.011(2) 148.7(17) 4_566

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        26.99
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.035


# Attachment 'AN399l4m_FINAL_CP_2.cif'

data_kk399l4m
_database_code_depnum_ccdc_archive 'CCDC 679362'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H32 N6 O13 S Zn'
_chemical_formula_weight         613.91

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'
S S 0.1246 0.1234 '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                   7.6927(7)
_cell_length_b                   9.7564(9)
_cell_length_c                   17.2857(17)
_cell_angle_alpha                81.067(2)
_cell_angle_beta                 81.968(2)
_cell_angle_gamma                86.102(2)
_cell_volume                     1267.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       PLATE
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.6553
_exptl_absorpt_correction_T_max  0.9563
_exptl_absorpt_process_details   SADABS

_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_measurement_device_type  'BRUKER CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10614
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5430
_reflns_number_gt                4769
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER AXS SMART 3'
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXLTL'
_computing_publication_material  'MERCURY 1.4.1'

_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)+(0.0399P)²+1.3866P] 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         5430
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0944
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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 0.22210(4) 0.25532(3) 0.263813(17) 0.01057(9) Uani 1 1 d . . .
N1 N 0.2620(3) 0.3165(2) 0.13487(12) 0.0136(4) Uani 1 1 d . . .
C2 C 0.2224(3) 0.4465(3) 0.10124(15) 0.0148(5) Uani 1 1 d . . .
H2 H 0.1743 0.5125 0.1343 0.018 Uiso 1 1 calc R . .
C3 C 0.2491(3) 0.4884(3) 0.01974(15) 0.0132(5) Uani 1 1 d . . .
C4 C 0.3207(3) 0.3899(3) -0.02804(15) 0.0172(5) Uani 1 1 d . . .
H4 H 0.3400 0.4139 -0.0839 0.021 Uiso 1 1 calc R . .
C5 C 0.3627(4) 0.2576(3) 0.00712(16) 0.0181(6) Uani 1 1 d . . .
H5 H 0.4129 0.1896 -0.0243 0.022 Uiso 1 1 calc R . .
C6 C 0.3314(3) 0.2242(3) 0.08829(16) 0.0162(5) Uani 1 1 d . . .
H6 H 0.3603 0.1324 0.1118 0.019 Uiso 1 1 calc R . .
N7 N 0.2119(3) 0.6224(2) -0.01833(12) 0.0158(5) Uani 1 1 d . . .
H7 H 0.2234 0.6330 -0.0703 0.019 Uiso 1 1 calc R . .
C8 C 0.1597(3) 0.7386(3) 0.01545(15) 0.0147(5) Uani 1 1 d . . .
O9 O 0.1252(2) 0.73578(18) 0.08818(10) 0.0173(4) Uani 1 1 d . . .
N10 N 0.1505(3) 0.8563(2) -0.03508(13) 0.0181(5) Uani 1 1 d . . .
H10 H 0.1760 0.8534 -0.0861 0.022 Uiso 1 1 calc R . .
C11 C 0.0995(3) 0.9890(3) -0.00824(16) 0.0172(6) Uani 1 1 d . . .
H11A H 0.1468 1.0649 -0.0491 0.021 Uiso 1 1 calc R . .
H11B H 0.1515 0.9933 0.0405 0.021 Uiso 1 1 calc R . .
C12 C 0.5613(4) -0.4457(3) 0.50672(16) 0.0168(5) Uani 1 1 d . . .
H12A H 0.6438 -0.4902 0.5433 0.020 Uiso 1 1 calc R . .
H12B H 0.6315 -0.4108 0.4559 0.020 Uiso 1 1 calc R . .
N13 N 0.4662(3) -0.3294(2) 0.53927(13) 0.0161(5) Uani 1 1 d . . .
H13 H 0.4495 -0.3304 0.5908 0.019 Uiso 1 1 calc R . .
C14 C 0.4028(3) -0.2196(3) 0.49155(15) 0.0142(5) Uani 1 1 d . . .
O15 O 0.4125(2) -0.21615(19) 0.41974(10) 0.0176(4) Uani 1 1 d . . .
N16 N 0.3281(3) -0.1136(2) 0.53019(12) 0.0140(4) Uani 1 1 d . . .
H16 H 0.3288 -0.1261 0.5817 0.017 Uiso 1 1 calc R . .
C17 C 0.2507(3) 0.0121(3) 0.49768(15) 0.0123(5) Uani 1 1 d . . .
C18 C 0.1533(3) 0.0932(3) 0.55006(15) 0.0164(5) Uani 1 1 d . . .
H18 H 0.1387 0.0614 0.6053 0.020 Uiso 1 1 calc R . .
C19 C 0.0791(3) 0.2192(3) 0.52072(15) 0.0171(5) Uani 1 1 d . . .
H19 H 0.0135 0.2756 0.5556 0.020 Uiso 1 1 calc R . .
C20 C 0.1006(3) 0.2635(3) 0.44003(16) 0.0158(5) Uani 1 1 d . . .
H20 H 0.0486 0.3507 0.4202 0.019 Uiso 1 1 calc R . .
N21 N 0.1931(3) 0.1863(2) 0.38900(12) 0.0126(4) Uani 1 1 d . . .
C22 C 0.2664(3) 0.0634(3) 0.41748(15) 0.0132(5) Uani 1 1 d . . .
H22 H 0.3318 0.0091 0.3813 0.016 Uiso 1 1 calc R . .
O23 O 0.3568(3) 0.4291(2) 0.28003(13) 0.0198(4) Uani 1 1 d . . .
O24 O -0.0128(3) 0.3709(2) 0.27865(12) 0.0157(4) Uani 1 1 d . . .
O25 O 0.0932(3) 0.0778(2) 0.25229(11) 0.0154(4) Uani 1 1 d . . .
O26 O 0.4637(2) 0.13913(18) 0.25024(10) 0.0133(4) Uani 1 1 d . . .
S27 S 0.63982(8) 0.19627(6) 0.23539(3) 0.01114(14) Uani 1 1 d . . .
O28 O 0.6417(2) 0.32733(18) 0.18062(10) 0.0145(4) Uani 1 1 d . . .
O29 O 0.6954(2) 0.21998(18) 0.31037(10) 0.0147(4) Uani 1 1 d . . .
O30 O 0.7653(2) 0.09207(18) 0.20092(10) 0.0144(4) Uani 1 1 d . . .
O31 O 0.8896(3) 0.6229(2) 0.20808(13) 0.0308(5) Uani 1 1 d . . .
H31 H 0.9500 0.6635 0.1679 0.046 Uiso 1 1 calc R . .
C32 C 0.8308(4) 0.7191(3) 0.26097(18) 0.0281(7) Uani 1 1 d . . .
H32A H 0.9092 0.7981 0.2501 0.034 Uiso 1 1 calc R . .
H32B H 0.8374 0.6735 0.3159 0.034 Uiso 1 1 calc R . .
C33 C 0.6441(4) 0.7729(3) 0.25309(16) 0.0240(6) Uani 1 1 d . . .
H33A H 0.5669 0.6934 0.2616 0.029 Uiso 1 1 calc R . .
H33B H 0.6037 0.8316 0.2946 0.029 Uiso 1 1 calc R . .
O34 O 0.6286(3) 0.8519(2) 0.17774(12) 0.0236(4) Uani 1 1 d . . .
H34 H 0.6587 0.9332 0.1772 0.035 Uiso 1 1 calc R . .
O35 O 0.2726(3) 0.8636(2) 0.18971(12) 0.0200(4) Uani 1 1 d . . .
O36 O 0.2210(3) 0.6640(2) 0.32815(13) 0.0195(4) Uani 1 1 d . . .
H23A H 0.435(4) 0.437(3) 0.2521(19) 0.018(9) Uiso 1 1 d . . .
H23B H 0.311(5) 0.508(4) 0.295(2) 0.036(10) Uiso 1 1 d . . .
H24A H -0.099(5) 0.334(3) 0.2851(19) 0.020(9) Uiso 1 1 d . . .
H24B H -0.033(5) 0.446(4) 0.254(2) 0.045(12) Uiso 1 1 d . . .
H25A H 0.151(5) 0.018(4) 0.234(2) 0.030(10) Uiso 1 1 d . . .
H25B H 0.005(5) 0.088(4) 0.237(2) 0.035(11) Uiso 1 1 d . . .
H35A H 0.241(5) 0.820(4) 0.154(2) 0.049(12) Uiso 1 1 d . . .
H35B H 0.377(4) 0.871(3) 0.1790(16) 0.010(8) Uiso 1 1 d . . .
H36A H 0.276(5) 0.699(4) 0.358(2) 0.039(11) Uiso 1 1 d . . .
H36B H 0.227(4) 0.725(4) 0.288(2) 0.029(9) 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 O24 2.0707(19) . ?
Zn1 O25 2.1018(19) . ?
Zn1 O26 2.1137(17) . ?
Zn1 O23 2.120(2) . ?
Zn1 N21 2.149(2) . ?
Zn1 N1 2.200(2) . ?
N1 C6 1.336(3) . ?
N1 C2 1.344(3) . ?
C2 C3 1.395(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.399(4) . ?
C3 N7 1.399(3) . ?
C4 C5 1.376(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N7 C8 1.367(3) . ?
N7 H7 0.8800 . ?
C8 O9 1.244(3) . ?
C8 N10 1.334(3) . ?
N10 C11 1.454(3) . ?
N10 H10 0.8800 . ?
C11 C11 1.524(5) 2_575 ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N13 1.452(3) . ?
C12 C12 1.530(5) 2_646 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N13 C14 1.354(3) . ?
N13 H13 0.8800 . ?
C14 O15 1.228(3) . ?
C14 N16 1.368(3) . ?
N16 C17 1.398(3) . ?
N16 H16 0.8800 . ?
C17 C22 1.390(3) . ?
C17 C18 1.399(4) . ?
C18 C19 1.373(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(4) . ?
C19 H19 0.9500 . ?
C20 N21 1.345(3) . ?
C20 H20 0.9500 . ?
N21 C22 1.342(3) . ?
C22 H22 0.9500 . ?
O23 H23A 0.72(3) . ?
O23 H23B 0.89(4) . ?
O24 H24A 0.76(3) . ?
O24 H24B 0.81(4) . ?
O25 H25A 0.79(4) . ?
O25 H25B 0.76(4) . ?
O26 S27 1.4744(18) . ?
S27 O28 1.4678(18) . ?
S27 O29 1.4756(18) . ?
S27 O30 1.4881(18) . ?
O31 C32 1.420(4) . ?
O31 H31 0.8400 . ?
C32 C33 1.512(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 O34 1.422(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O34 H34 0.8400 . ?
O35 H35A 0.88(4) . ?
O35 H35B 0.80(3) . ?
O36 H36A 0.83(4) . ?
O36 H36B 0.84(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O24 Zn1 O25 92.18(9) . . ?
O24 Zn1 O26 178.94(7) . . ?
O25 Zn1 O26 88.65(8) . . ?
O24 Zn1 O23 89.14(9) . . ?
O25 Zn1 O23 177.36(8) . . ?
O26 Zn1 O23 90.00(8) . . ?
O24 Zn1 N21 89.20(8) . . ?
O25 Zn1 N21 87.78(8) . . ?
O26 Zn1 N21 90.18(7) . . ?
O23 Zn1 N21 89.95(8) . . ?
O24 Zn1 N1 93.72(8) . . ?
O25 Zn1 N1 91.11(8) . . ?
O26 Zn1 N1 86.92(7) . . ?
O23 Zn1 N1 91.09(8) . . ?
N21 Zn1 N1 176.92(8) . . ?
C6 N1 C2 118.6(2) . . ?
C6 N1 Zn1 119.78(17) . . ?
C2 N1 Zn1 121.64(17) . . ?
N1 C2 C3 122.7(2) . . ?
N1 C2 H2 118.6 . . ?
C3 C2 H2 118.6 . . ?
C2 C3 C4 117.8(2) . . ?
C2 C3 N7 125.1(2) . . ?
C4 C3 N7 117.0(2) . . ?
C5 C4 C3 118.9(2) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 119.7(2) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
N1 C6 C5 122.3(2) . . ?
N1 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C8 N7 C3 127.8(2) . . ?
C8 N7 H7 116.1 . . ?
C3 N7 H7 116.1 . . ?
O9 C8 N10 122.2(2) . . ?
O9 C8 N7 122.6(2) . . ?
N10 C8 N7 115.2(2) . . ?
O9 O9 C8 0(10) 1 . ?
C8 N10 C11 121.8(2) . . ?
C8 N10 H10 119.1 . . ?
C11 N10 H10 119.1 . . ?
N10 C11 C11 111.9(3) . 2_575 ?
N10 C11 H11A 109.2 . . ?
C11 C11 H11A 109.2 2_575 . ?
N10 C11 H11B 109.2 . . ?
C11 C11 H11B 109.2 2_575 . ?
H11A C11 H11B 107.9 . . ?
N13 C12 C12 112.4(3) . 2_646 ?
N13 C12 H12A 109.1 . . ?
C12 C12 H12A 109.1 2_646 . ?
N13 C12 H12B 109.1 . . ?
C12 C12 H12B 109.1 2_646 . ?
H12A C12 H12B 107.9 . . ?
C14 N13 C12 121.0(2) . . ?
C14 N13 H13 119.5 . . ?
C12 N13 H13 119.5 . . ?
O15 C14 N13 122.5(2) . . ?
O15 C14 N16 123.3(2) . . ?
N13 C14 N16 114.2(2) . . ?
C14 N16 C17 127.8(2) . . ?
C14 N16 H16 116.1 . . ?
C17 N16 H16 116.1 . . ?
C22 C17 N16 124.8(2) . . ?
C22 C17 C18 117.9(2) . . ?
N16 C17 C18 117.4(2) . . ?
C19 C18 C17 119.2(2) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 119.7(2) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
N21 C20 C19 121.7(2) . . ?
N21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C22 N21 C20 118.8(2) . . ?
C22 N21 Zn1 119.96(17) . . ?
C20 N21 Zn1 121.23(17) . . ?
N21 C22 C17 122.7(2) . . ?
N21 C22 H22 118.6 . . ?
C17 C22 H22 118.6 . . ?
Zn1 O23 H23A 110(3) . . ?
Zn1 O23 H23B 128(2) . . ?
H23A O23 H23B 114(3) . . ?
Zn1 O24 H24A 119(2) . . ?
Zn1 O24 H24B 124(3) . . ?
H24A O24 H24B 105(3) . . ?
Zn1 O25 H25A 117(3) . . ?
Zn1 O25 H25B 118(3) . . ?
H25A O25 H25B 111(4) . . ?
S27 O26 Zn1 125.87(10) . . ?
O28 S27 O26 111.17(10) . . ?
O28 S27 O29 109.36(10) . . ?
O26 S27 O29 110.05(10) . . ?
O28 S27 O30 109.70(10) . . ?
O26 S27 O30 108.03(10) . . ?
O29 S27 O30 108.47(10) . . ?
C32 O31 H31 109.5 . . ?
O31 C32 C33 111.6(3) . . ?
O31 C32 H32A 109.3 . . ?
C33 C32 H32A 109.3 . . ?
O31 C32 H32B 109.3 . . ?
C33 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
O34 C33 C32 112.3(2) . . ?
O34 C33 H33A 109.2 . . ?
C32 C33 H33A 109.2 . . ?
O34 C33 H33B 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C33 O34 H34 109.5 . . ?
H35A O35 H35B 106(3) . . ?
H36A O36 H36B 102(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O28 0.88 2.03 2.854(3) 154.5 2_665
N10 H10 O30 0.88 1.97 2.823(3) 162.7 2_665
N13 H13 O29 0.88 2.28 3.036(3) 144.0 2_656
N16 H16 O29 0.88 1.94 2.776(3) 158.8 2_656
O23 H23B O36 0.89(4) 1.77(4) 2.657(3) 178(3) 1
O24 H24A O29 0.76(3) 1.96(4) 2.713(3) 172(3) 1_455
O24 H24B O31 0.81(4) 1.88(4) 2.677(3) 171(4) 1_455
O25 H25A O35 0.79(4) 1.92(4) 2.708(3) 175(4) 1_545
O31 H31 O9 0.84 1.88 2.703(3) 167.8 1_655
O34 H34 O30 0.84 1.93 2.739(3) 162.8 1_565
O35 H35A O9 0.88(4) 1.85(4) 2.711(3) 167(4) 1
O35 H35B O34 0.80(4) 1.93(4) 2.715(3) 165(3) 1
O36 H36A O15 0.83(4) 1.91(4) 2.740(3) 176(4) 1_565
O36 H36B O35 0.84(4) 2.00(4) 2.841(3) 173(3) 1

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.082

# Attachment 'COMP_3_an362qrm_FINALCIF_R3.cif'

data_an362qrm
_database_code_depnum_ccdc_archive 'CCDC 679363'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H56 N12 O14 S Zn'
_chemical_formula_weight         978.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 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   P2(1)/n

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

_cell_length_a                   13.0983(12)
_cell_length_b                   13.9309(12)
_cell_length_c                   24.194(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.795(2)
_cell_angle_gamma                90.00
_cell_volume                     4399.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       NEEDLE
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2056
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8209
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_process_details   SADABS

_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_measurement_device_type  'BRUKER CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25302
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         27.00
_reflns_number_total             9563
_reflns_number_gt                6937
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER AXS SMART 3'
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXLTL'
_computing_publication_material  'MERCURY 1.4'

_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)+(0.0867P)²+3.3971P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9563
_refine_ls_number_parameters     577
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1818
_refine_ls_wR_factor_gt          0.1662
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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 0.76333(3) 0.24791(3) 0.996826(16) 0.01049(13) Uani 1 1 d . . .
N1 N 0.6096(2) 0.3138(2) 0.97639(12) 0.0131(7) Uani 1 1 d . . .
C2 C 0.5573(3) 0.3484(3) 1.01717(16) 0.0210(9) Uani 1 1 d . . .
H2 H 0.5891 0.3498 1.0530 0.025 Uiso 1 1 calc R . .
C3 C 0.4580(3) 0.3823(3) 1.00842(17) 0.0245(10) Uani 1 1 d . . .
H3 H 0.4252 0.4067 1.0380 0.029 Uiso 1 1 calc R . .
C4 C 0.4073(3) 0.3802(3) 0.95608(17) 0.0210(9) Uani 1 1 d . . .
H4 H 0.3396 0.4002 0.9498 0.025 Uiso 1 1 calc R . .
C5 C 0.4622(3) 0.3465(3) 0.91280(15) 0.0128(8) Uani 1 1 d . . .
C6 C 0.5624(3) 0.3154(3) 0.92535(15) 0.0130(8) Uani 1 1 d . . .
H6 H 0.5988 0.2943 0.8963 0.016 Uiso 1 1 calc R . .
N7 N 0.4206(2) 0.3398(2) 0.85757(13) 0.0162(7) Uani 1 1 d . . .
H7 H 0.4479 0.2995 0.8363 0.019 Uiso 1 1 calc R . .
C8 C 0.3394(3) 0.3931(3) 0.83512(16) 0.0170(8) Uani 1 1 d . . .
O9 O 0.2981(2) 0.4563(2) 0.86094(12) 0.0274(7) Uani 1 1 d . . .
N10 N 0.3091(2) 0.3712(2) 0.78223(13) 0.0204(8) Uani 1 1 d . . .
H10 H 0.3405 0.3281 0.7647 0.024 Uiso 1 1 calc R . .
C11 C 0.2214(3) 0.4225(3) 0.75524(18) 0.0264(10) Uani 1 1 d . . .
H11A H 0.2390 0.4897 0.7519 0.032 Uiso 1 1 calc R . .
H11B H 0.1644 0.4182 0.7783 0.032 Uiso 1 1 calc R . .
C12 C 0.1890(3) 0.3834(3) 0.69902(16) 0.0209(9) Uani 1 1 d . . .
H12A H 0.2432 0.3917 0.6744 0.025 Uiso 1 1 calc R . .
H12B H 0.1733 0.3155 0.7013 0.025 Uiso 1 1 calc R . .
N13 N 0.0984(3) 0.4370(3) 0.67869(14) 0.0258(9) Uani 1 1 d . . .
H13 H 0.0770 0.4819 0.6993 0.031 Uiso 1 1 calc R . .
C14 C 0.0466(3) 0.4204(3) 0.62987(16) 0.0164(8) Uani 1 1 d . . .
O15 O 0.0681(2) 0.35624(19) 0.59740(11) 0.0187(6) Uani 1 1 d . . .
N16 N -0.0331(2) 0.4830(2) 0.61828(13) 0.0160(7) Uani 1 1 d . . .
H16 H -0.0496 0.5188 0.6451 0.019 Uiso 1 1 calc R . .
C17 C -0.0903(3) 0.4944(3) 0.56734(15) 0.0125(8) Uani 1 1 d . . .
C18 C -0.1402(3) 0.5813(3) 0.55880(15) 0.0123(8) Uani 1 1 d . . .
H18 H -0.1312 0.6272 0.5867 0.015 Uiso 1 1 calc R . .
N19 N -0.2002(2) 0.6041(2) 0.51346(12) 0.0106(6) Uani 1 1 d . . .
C20 C -0.2120(3) 0.5369(3) 0.47339(15) 0.0125(8) Uani 1 1 d . . .
H20 H -0.2543 0.5503 0.4415 0.015 Uiso 1 1 calc R . .
C21 C -0.1634(3) 0.4486(3) 0.47789(16) 0.0138(8) Uani 1 1 d . . .
H21 H -0.1722 0.4046 0.4490 0.017 Uiso 1 1 calc R . .
C22 C -0.1023(3) 0.4261(3) 0.52493(15) 0.0126(8) Uani 1 1 d . . .
H22 H -0.0697 0.3669 0.5285 0.015 Uiso 1 1 calc R . .
N23 N 0.9166(2) 0.1838(2) 1.01893(12) 0.0121(7) Uani 1 1 d . . .
C24 C 0.9741(3) 0.1501(3) 0.97996(16) 0.0186(9) Uani 1 1 d . . .
H24 H 0.9466 0.1495 0.9433 0.022 Uiso 1 1 calc R . .
C25 C 1.0729(3) 0.1162(3) 0.99212(17) 0.0254(10) Uani 1 1 d . . .
H25 H 1.1099 0.0926 0.9639 0.030 Uiso 1 1 calc R . .
C26 C 1.1168(3) 0.1175(3) 1.04625(16) 0.0198(9) Uani 1 1 d . . .
H26 H 1.1833 0.0956 1.0550 0.024 Uiso 1 1 calc R . .
C27 C 1.0578(3) 0.1527(3) 1.08711(15) 0.0134(8) Uani 1 1 d . . .
C28 C 0.9583(3) 0.1820(3) 1.07191(15) 0.0128(8) Uani 1 1 d . . .
H28 H 0.9180 0.2016 1.0997 0.015 Uiso 1 1 calc R . .
N29 N 1.0921(2) 0.1627(2) 1.14325(12) 0.0151(7) Uani 1 1 d . . .
H29 H 1.0644 0.2074 1.1614 0.018 Uiso 1 1 calc R . .
C30 C 1.1658(3) 0.1080(3) 1.17221(16) 0.0137(8) Uani 1 1 d . . .
O31 O 1.2123(2) 0.0429(2) 1.15038(11) 0.0198(6) Uani 1 1 d . . .
N32 N 1.1818(2) 0.1321(2) 1.22636(13) 0.0184(7) Uani 1 1 d . . .
H32 H 1.1475 0.1790 1.2386 0.022 Uiso 1 1 calc R . .
C33 C 1.2545(3) 0.0822(3) 1.26446(16) 0.0195(9) Uani 1 1 d . . .
H33A H 1.2627 0.0170 1.2514 0.023 Uiso 1 1 calc R . .
H33B H 1.2274 0.0787 1.3005 0.023 Uiso 1 1 calc R . .
C34 C 1.3583(3) 0.1305(3) 1.27066(17) 0.0217(9) Uani 1 1 d . . .
H34A H 1.3814 0.1434 1.2343 0.026 Uiso 1 1 calc R . .
H34B H 1.3532 0.1912 1.2899 0.026 Uiso 1 1 calc R . .
N35 N 1.4315(3) 0.0685(3) 1.30182(14) 0.0224(8) Uani 1 1 d . . .
H35 H 1.4529 0.0190 1.2850 0.027 Uiso 1 1 calc R . .
C36 C 1.4682(3) 0.0822(3) 1.35461(16) 0.0171(8) Uani 1 1 d . . .
O37 O 1.4550(2) 0.15585(19) 1.38188(11) 0.0194(6) Uani 1 1 d . . .
N38 N 1.5259(2) 0.0065(2) 1.37623(13) 0.0154(7) Uani 1 1 d . . .
H38 H 1.5285 -0.0432 1.3553 0.018 Uiso 1 1 calc R . .
C39 C 1.5803(3) 0.0005(3) 1.42796(15) 0.0124(8) Uani 1 1 d . . .
C40 C 1.6197(3) -0.0891(3) 1.44290(15) 0.0140(8) Uani 1 1 d . . .
H40 H 1.6064 -0.1393 1.4180 0.017 Uiso 1 1 calc R . .
N41 N 1.6752(2) -0.1085(2) 1.49024(12) 0.0124(7) Uani 1 1 d . . .
C42 C 1.6954(3) -0.0358(3) 1.52594(16) 0.0144(8) Uani 1 1 d . . .
H42 H 1.7350 -0.0471 1.5590 0.017 Uiso 1 1 calc R . .
C43 C 1.6585(3) 0.0553(3) 1.51454(16) 0.0183(9) Uani 1 1 d . . .
H43 H 1.6729 0.1040 1.5403 0.022 Uiso 1 1 calc R . .
C44 C 1.6006(3) 0.0760(3) 1.46550(16) 0.0176(9) Uani 1 1 d . . .
H44 H 1.5760 0.1376 1.4578 0.021 Uiso 1 1 calc R . .
O45 O 0.7893(2) 0.25706(18) 0.91221(11) 0.0159(6) Uani 1 1 d . . .
O46 O 0.73641(19) 0.23754(18) 1.08103(10) 0.0135(6) Uani 1 1 d . . .
S47 S 0.48756(7) 0.16960(7) 0.74932(4) 0.0135(2) Uani 1 1 d . . .
O48 O 0.5397(2) 0.2514(2) 0.77761(12) 0.0324(8) Uani 1 1 d . . .
O49 O 0.3767(2) 0.1757(2) 0.75592(12) 0.0260(7) Uani 1 1 d . . .
O50 O 0.5046(2) 0.1698(2) 0.68980(11) 0.0209(6) Uani 1 1 d . . .
O51 O 0.5285(2) 0.0802(2) 0.77467(12) 0.0321(8) Uani 1 1 d . . .
O52 O 0.1697(3) 0.9442(3) 0.36230(14) 0.0449(10) Uani 1 1 d . . .
C53 C 0.0646(4) 0.9312(4) 0.3430(2) 0.0391(13) Uani 1 1 d . . .
H53A H 0.0506 0.9590 0.3064 0.047 Uiso 1 1 calc R . .
H53B H 0.0204 0.9614 0.3681 0.047 Uiso 1 1 calc R . .
C54 C 0.0466(4) 0.8221(3) 0.3411(2) 0.0349(11) Uani 1 1 d . . .
H54A H 0.0282 0.8003 0.3035 0.042 Uiso 1 1 calc R . .
H54B H -0.0067 0.8034 0.3645 0.042 Uiso 1 1 calc R . .
C55 C 0.1526(4) 0.7816(4) 0.3638(2) 0.0410(13) Uani 1 1 d . . .
H55A H 0.1563 0.7724 0.4036 0.049 Uiso 1 1 calc R . .
H55B H 0.1677 0.7214 0.3460 0.049 Uiso 1 1 calc R . .
C56 C 0.2211(4) 0.8583(4) 0.3484(2) 0.0450(14) Uani 1 1 d . . .
H56A H 0.2874 0.8533 0.3693 0.054 Uiso 1 1 calc R . .
H56B H 0.2305 0.8562 0.3091 0.054 Uiso 1 1 calc R . .
O57 O 0.1664(2) 0.0649(2) 0.86483(13) 0.0352(8) Uani 1 1 d . . .
C58 C 0.0662(4) 0.0388(3) 0.8423(2) 0.0345(12) Uani 1 1 d . . .
H58A H 0.0268 0.0134 0.8712 0.041 Uiso 1 1 calc R . .
H58B H 0.0702 -0.0100 0.8139 0.041 Uiso 1 1 calc R . .
C59 C 0.0162(4) 0.1276(4) 0.8177(2) 0.0347(12) Uani 1 1 d . . .
H59A H -0.0197 0.1625 0.8449 0.042 Uiso 1 1 calc R . .
H59B H -0.0313 0.1125 0.7860 0.042 Uiso 1 1 calc R . .
C60 C 0.1083(4) 0.1838(4) 0.8005(2) 0.0403(13) Uani 1 1 d . . .
H60A H 0.1294 0.1615 0.7653 0.048 Uiso 1 1 calc R . .
H60B H 0.0939 0.2521 0.7982 0.048 Uiso 1 1 calc R . .
C61 C 0.1884(4) 0.1613(4) 0.8478(2) 0.0368(12) Uani 1 1 d . . .
H61A H 0.2568 0.1652 0.8354 0.044 Uiso 1 1 calc R . .
H61B H 0.1834 0.2059 0.8782 0.044 Uiso 1 1 calc R . .
O62 O 0.7414(2) 0.1448(2) 0.82424(11) 0.0207(6) Uani 1 1 d . . .
O63 O 0.2576(2) 0.6411(2) 0.83557(11) 0.0217(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
Zn1 O46 2.101(3) . ?
Zn1 O45 2.107(3) . ?
Zn1 N41 2.169(3) 2_757 ?
Zn1 N19 2.174(3) 2_546 ?
Zn1 N23 2.221(3) . ?
Zn1 N1 2.231(3) . ?
N1 C6 1.334(5) . ?
N1 C2 1.337(5) . ?
C2 C3 1.384(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.380(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(5) . ?
C5 N7 1.403(5) . ?
C6 H6 0.9300 . ?
N7 C8 1.371(5) . ?
N7 H7 0.8600 . ?
C8 O9 1.230(5) . ?
C8 N10 1.343(5) . ?
N10 C11 1.459(5) . ?
N10 H10 0.8600 . ?
C11 C12 1.493(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N13 1.453(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N13 C14 1.332(5) . ?
N13 H13 0.8600 . ?
C14 O15 1.238(5) . ?
C14 N16 1.371(5) . ?
N16 C17 1.397(5) . ?
N16 H16 0.8600 . ?
C17 C18 1.383(5) . ?
C17 C22 1.399(5) . ?
C18 N19 1.334(5) . ?
C18 H18 0.9300 . ?
N19 C20 1.347(5) . ?
N19 Zn1 2.174(3) 2_556 ?
C20 C21 1.385(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.372(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N23 C24 1.340(5) . ?
N23 C28 1.351(5) . ?
C24 C25 1.386(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.386(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.394(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.385(5) . ?
C27 N29 1.402(5) . ?
C28 H28 0.9300 . ?
N29 C30 1.374(5) . ?
N29 H29 0.8600 . ?
C30 O31 1.235(4) . ?
C30 N32 1.352(5) . ?
N32 C33 1.447(5) . ?
N32 H32 0.8600 . ?
C33 C34 1.514(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N35 1.453(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
N35 C36 1.340(5) . ?
N35 H35 0.8600 . ?
C36 O37 1.239(5) . ?
C36 N38 1.375(5) . ?
N38 C39 1.391(5) . ?
N38 H38 0.8600 . ?
C39 C40 1.387(5) . ?
C39 C44 1.400(5) . ?
C40 N41 1.332(5) . ?
C40 H40 0.9300 . ?
N41 C42 1.344(5) . ?
N41 Zn1 2.169(3) 2_747 ?
C42 C43 1.377(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.384(5) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
S47 O48 1.468(3) 1 ?
S47 O48 1.468(3) . ?
S47 O51 1.469(3) . ?
S47 O50 1.476(3) . ?
S47 O49 1.476(3) . ?
S47 O49 1.476(3) 1 ?
O52 C56 1.426(6) . ?
O52 C53 1.428(6) . ?
C53 C54 1.538(7) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.555(7) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.463(7) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
O57 C58 1.426(6) . ?
O57 C61 1.441(6) . ?
C58 C59 1.499(6) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.525(7) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 C61 1.519(7) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O46 Zn1 O45 179.39(10) . . ?
O46 Zn1 N41 90.79(11) . 2_757 ?
O45 Zn1 N41 89.80(11) . 2_757 ?
O46 Zn1 N19 87.40(11) . 2_546 ?
O45 Zn1 N19 92.02(11) . 2_546 ?
N41 Zn1 N19 178.17(11) 2_757 2_546 ?
O46 Zn1 N23 87.73(10) . . ?
O45 Zn1 N23 92.43(11) . . ?
N41 Zn1 N23 91.11(11) 2_757 . ?
N19 Zn1 N23 89.09(11) 2_546 . ?
O46 Zn1 N1 91.23(10) . . ?
O45 Zn1 N1 88.61(11) . . ?
N41 Zn1 N1 88.26(11) 2_757 . ?
N19 Zn1 N1 91.51(11) 2_546 . ?
N23 Zn1 N1 178.78(11) . . ?
C6 N1 C2 116.8(3) . . ?
C6 N1 Zn1 123.5(2) . . ?
C2 N1 Zn1 119.6(2) . . ?
N1 C2 C3 122.9(4) . . ?
N1 C2 H2 118.6 . . ?
C3 C2 H2 118.6 . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 117.1(4) . . ?
C3 C4 H4 121.4 . . ?
C5 C4 H4 121.4 . . ?
C6 C5 C4 118.4(3) . . ?
C6 C5 N7 118.1(3) . . ?
C4 C5 N7 123.4(3) . . ?
N1 C6 C5 124.2(3) . . ?
N1 C6 H6 117.9 . . ?
C5 C6 H6 117.9 . . ?
C8 N7 C5 124.6(3) . . ?
C8 N7 H7 117.7 . . ?
C5 N7 H7 117.7 . . ?
O9 C8 N10 122.6(4) . . ?
O9 C8 N7 123.0(4) . . ?
N10 C8 N7 114.4(3) . . ?
C8 N10 C11 118.3(3) . . ?
C8 N10 H10 120.8 . . ?
C11 N10 H10 120.8 . . ?
N10 C11 C12 112.5(3) . . ?
N10 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
N10 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N13 C12 C11 106.4(3) . . ?
N13 C12 H12A 110.4 . . ?
C11 C12 H12A 110.4 . . ?
N13 C12 H12B 110.4 . . ?
C11 C12 H12B 110.4 . . ?
H12A C12 H12B 108.6 . . ?
C14 N13 C12 123.5(3) . . ?
C14 N13 H13 118.3 . . ?
C12 N13 H13 118.3 . . ?
O15 C14 N13 124.2(4) . . ?
O15 C14 N16 122.6(4) . . ?
N13 C14 N16 113.2(3) . . ?
C14 N16 C17 126.6(3) . . ?
C14 N16 H16 116.7 . . ?
C17 N16 H16 116.7 . . ?
C18 C17 N16 116.3(3) . . ?
C18 C17 C22 117.6(3) . . ?
N16 C17 C22 126.1(3) . . ?
N19 C18 C17 124.8(3) . . ?
N19 C18 H18 117.6 . . ?
C17 C18 H18 117.6 . . ?
C18 N19 C20 116.8(3) . . ?
C18 N19 Zn1 120.4(2) . 2_556 ?
C20 N19 Zn1 122.6(2) . 2_556 ?
N19 C20 C21 122.4(3) . . ?
N19 C20 H20 118.8 . . ?
C21 C20 H20 118.8 . . ?
C22 C21 C20 120.1(4) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C17 118.3(3) . . ?
C21 C22 H22 120.8 . . ?
C17 C22 H22 120.8 . . ?
C24 N23 C28 117.1(3) . . ?
C24 N23 Zn1 121.4(2) . . ?
C28 N23 Zn1 121.4(2) . . ?
N23 C24 C25 122.7(4) . . ?
N23 C24 H24 118.7 . . ?
C25 C24 H24 118.7 . . ?
C26 C25 C24 120.2(4) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C27 117.6(4) . . ?
C25 C26 H26 121.2 . . ?
C27 C26 H26 121.2 . . ?
C28 C27 C26 118.7(3) . . ?
C28 C27 N29 116.5(3) . . ?
C26 C27 N29 124.7(3) . . ?
N23 C28 C27 123.6(3) . . ?
N23 C28 H28 118.2 . . ?
C27 C28 H28 118.2 . . ?
C30 N29 C27 126.5(3) . . ?
C30 N29 H29 116.8 . . ?
C27 N29 H29 116.8 . . ?
O31 C30 N32 123.7(3) . . ?
O31 C30 N29 122.6(3) . . ?
N32 C30 N29 113.7(3) . . ?
C30 N32 C33 122.6(3) . . ?
C30 N32 H32 118.7 . . ?
C33 N32 H32 118.7 . . ?
N32 C33 C34 112.8(3) . . ?
N32 C33 H33A 109.0 . . ?
C34 C33 H33A 109.0 . . ?
N32 C33 H33B 109.0 . . ?
C34 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
N35 C34 C33 109.5(3) . . ?
N35 C34 H34A 109.8 . . ?
C33 C34 H34A 109.8 . . ?
N35 C34 H34B 109.8 . . ?
C33 C34 H34B 109.8 . . ?
H34A C34 H34B 108.2 . . ?
C36 N35 C34 125.3(4) . . ?
C36 N35 H35 117.3 . . ?
C34 N35 H35 117.3 . . ?
O37 C36 N35 124.8(4) . . ?
O37 C36 N38 121.9(4) . . ?
N35 C36 N38 113.3(4) . . ?
C36 N38 C39 127.7(3) . . ?
C36 N38 H38 116.1 . . ?
C39 N38 H38 116.1 . . ?
C40 C39 N38 116.1(3) . . ?
C40 C39 C44 117.4(3) . . ?
N38 C39 C44 126.5(3) . . ?
N41 C40 C39 124.8(4) . . ?
N41 C40 H40 117.6 . . ?
C39 C40 H40 117.6 . . ?
C40 N41 C42 117.6(3) . . ?
C40 N41 Zn1 118.7(3) . 2_747 ?
C42 N41 Zn1 123.5(2) . 2_747 ?
N41 C42 C43 121.3(4) . . ?
N41 C42 H42 119.3 . . ?
C43 C42 H42 119.3 . . ?
C42 C43 C44 121.4(4) . . ?
C42 C43 H43 119.3 . . ?
C44 C43 H43 119.3 . . ?
C43 C44 C39 117.4(4) . . ?
C43 C44 H44 121.3 . . ?
C39 C44 H44 121.3 . . ?
O48 S47 O51 108.9(2) 1 . ?
O48 S47 O51 108.9(2) . . ?
O48 S47 O50 110.57(17) 1 . ?
O48 S47 O50 110.57(17) . . ?
O51 S47 O50 109.21(17) . . ?
O48 S47 O49 109.15(18) 1 . ?
O48 S47 O49 109.15(18) . . ?
O51 S47 O49 109.36(18) . . ?
O50 S47 O49 109.64(17) . . ?
O48 S47 O49 109.15(18) 1 1 ?
O48 S47 O49 109.15(18) . 1 ?
O51 S47 O49 109.36(18) . 1 ?
O50 S47 O49 109.64(17) . 1 ?
C56 O52 C53 106.1(4) . . ?
O52 C53 C54 106.1(4) . . ?
O52 C53 H53A 110.5 . . ?
C54 C53 H53A 110.5 . . ?
O52 C53 H53B 110.5 . . ?
C54 C53 H53B 110.5 . . ?
H53A C53 H53B 108.7 . . ?
C53 C54 C55 102.6(4) . . ?
C53 C54 H54A 111.2 . . ?
C55 C54 H54A 111.2 . . ?
C53 C54 H54B 111.2 . . ?
C55 C54 H54B 111.2 . . ?
H54A C54 H54B 109.2 . . ?
C56 C55 C54 101.2(4) . . ?
C56 C55 H55A 111.5 . . ?
C54 C55 H55A 111.5 . . ?
C56 C55 H55B 111.5 . . ?
C54 C55 H55B 111.5 . . ?
H55A C55 H55B 109.4 . . ?
O52 C56 C55 104.0(4) . . ?
O52 C56 H56A 111.0 . . ?
C55 C56 H56A 111.0 . . ?
O52 C56 H56B 111.0 . . ?
C55 C56 H56B 111.0 . . ?
H56A C56 H56B 109.0 . . ?
C58 O57 C61 109.1(3) . . ?
O57 C58 C59 107.4(4) . . ?
O57 C58 H58A 110.2 . . ?
C59 C58 H58A 110.2 . . ?
O57 C58 H58B 110.2 . . ?
C59 C58 H58B 110.2 . . ?
H58A C58 H58B 108.5 . . ?
C58 C59 C60 101.7(4) . . ?
C58 C59 H59A 111.4 . . ?
C60 C59 H59A 111.4 . . ?
C58 C59 H59B 111.4 . . ?
C60 C59 H59B 111.4 . . ?
H59A C59 H59B 109.3 . . ?
C61 C60 C59 101.6(4) . . ?
C61 C60 H60A 111.4 . . ?
C59 C60 H60A 111.4 . . ?
C61 C60 H60B 111.4 . . ?
C59 C60 H60B 111.4 . . ?
H60A C60 H60B 109.3 . . ?
O57 C61 C60 105.4(4) . . ?
O57 C61 H61A 110.7 . . ?
C60 C61 H61A 110.7 . . ?
O57 C61 H61B 110.7 . . ?
C60 C61 H61B 110.7 . . ?
H61A C61 H61B 108.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N38 H38 O50 0.86 2.10 2.938(4) 164.8 3_757
N35 H35 O51 0.86 2.03 2.856(5) 161.2 3_757
N32 H32 O48 0.86 2.01 2.832(4) 159.4 4_666
N29 H29 O50 0.86 2.03 2.872(4) 167.7 4_666
N16 H16 O51 0.86 2.12 2.919(4) 154.6 2_556
N13 H13 O51 0.86 2.08 2.886(5) 155.5 2_556
N10 H10 O49 0.86 2.19 2.950(5) 147.3 1
N7 H7 O48 0.86 2.05 2.864(4) 157.9 1

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.122

# Attachment 'COMP_4_an362q1m_FINACIF_R3.cif'

data_an362q1m
_database_code_depnum_ccdc_archive 'CCDC 679364'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H52 N12 O14 S Zn'
_chemical_formula_weight         950.31

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   13.1959(16)
_cell_length_b                   13.9981(17)
_cell_length_c                   23.607(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.712(2)
_cell_angle_gamma                90.00
_cell_volume                     4345.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       PLATE
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1992
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7555
_exptl_absorpt_correction_T_max  0.9729
_exptl_absorpt_process_details   SADABS

_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_measurement_device_type  'BRUKER CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25460
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         28.32
_reflns_number_total             9920
_reflns_number_gt                6792
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER AXS SMART 3'
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXLTL'
_computing_publication_material  'MERCURY 1.4.1'

_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)+(0.1000P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9920
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0880
_refine_ls_wR_factor_ref         0.2359
_refine_ls_wR_factor_gt          0.2163
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_restrained_S_all      1.310
_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 0.75929(4) 0.25170(4) 0.99647(2) 0.01220(17) Uani 1 1 d . . .
N1 N 0.6082(3) 0.3194(3) 0.97770(17) 0.0166(9) Uani 1 1 d . . .
C2 C 0.5612(4) 0.3566(4) 1.0211(2) 0.0311(14) Uani 1 1 d . . .
H2 H 0.5964 0.3601 1.0569 0.037 Uiso 1 1 calc R . .
C3 C 0.4627(4) 0.3896(5) 1.0142(3) 0.0430(17) Uani 1 1 d . . .
H3 H 0.4326 0.4151 1.0451 0.052 Uiso 1 1 calc R . .
C4 C 0.4083(4) 0.3850(4) 0.9617(2) 0.0311(14) Uani 1 1 d . . .
H4 H 0.3412 0.4059 0.9568 0.037 Uiso 1 1 calc R . .
C5 C 0.4569(4) 0.3484(3) 0.9169(2) 0.0190(11) Uani 1 1 d . . .
C6 C 0.5576(3) 0.3175(3) 0.9273(2) 0.0156(10) Uani 1 1 d . . .
H6 H 0.5906 0.2942 0.8968 0.019 Uiso 1 1 calc R . .
N7 N 0.4121(3) 0.3365(3) 0.86141(19) 0.0276(11) Uani 1 1 d . . .
H7 H 0.4418 0.2992 0.8390 0.033 Uiso 1 1 calc R . .
C8 C 0.3238(5) 0.3805(5) 0.8406(3) 0.0414(16) Uani 1 1 d . . .
O9 O 0.2823(3) 0.4452(3) 0.86564(17) 0.0459(12) Uani 1 1 d . . .
N10 N 0.3018(7) 0.3646(7) 0.7865(4) 0.023(2) Uiso 0.47 1 d P . .
N10' N 0.2745(8) 0.3272(7) 0.7923(4) 0.038(3) Uiso 0.53 1 d P . .
C11 C 0.2031(9) 0.4079(9) 0.7613(5) 0.028(3) Uiso 0.51 1 d P . .
C11' C 0.1775(12) 0.3625(12) 0.7610(7) 0.058(4) Uiso 0.49 1 d P . .
C12 C 0.1896(5) 0.3817(6) 0.7021(3) 0.062(2) Uani 1 1 d . . .
N13 N 0.1047(4) 0.4417(4) 0.6793(2) 0.0447(15) Uani 1 1 d . . .
H13 H 0.0907 0.4922 0.6979 0.054 Uiso 1 1 calc R . .
C14 C 0.0489(4) 0.4224(4) 0.6318(2) 0.0262(13) Uani 1 1 d . . .
O15 O 0.0626(3) 0.3526(2) 0.60110(17) 0.0288(9) Uani 1 1 d . . .
N16 N -0.0278(3) 0.4872(3) 0.61902(18) 0.0236(10) Uani 1 1 d . . .
H16 H -0.0402 0.5261 0.6458 0.028 Uiso 1 1 calc R . .
C17 C -0.0876(3) 0.4978(3) 0.5686(2) 0.0163(10) Uani 1 1 d . . .
C18 C -0.1343(3) 0.5857(3) 0.5597(2) 0.0153(10) Uani 1 1 d . . .
H18 H -0.1220 0.6322 0.5875 0.018 Uiso 1 1 calc R . .
N19 N -0.1962(3) 0.6083(3) 0.51364(17) 0.0139(8) Uani 1 1 d . . .
C20 C -0.2119(3) 0.5413(3) 0.4730(2) 0.0143(10) Uani 1 1 d . . .
H20 H -0.2547 0.5547 0.4408 0.017 Uiso 1 1 calc R . .
C21 C -0.1655(4) 0.4527(3) 0.4783(2) 0.0206(11) Uani 1 1 d . . .
H21 H -0.1771 0.4080 0.4493 0.025 Uiso 1 1 calc R . .
C22 C -0.1035(4) 0.4298(3) 0.5250(2) 0.0184(11) Uani 1 1 d . . .
H22 H -0.0721 0.3703 0.5282 0.022 Uiso 1 1 calc R . .
N23 N 0.9093(3) 0.1846(2) 1.01765(17) 0.0142(8) Uani 1 1 d . . .
C24 C 0.9651(4) 0.1494(4) 0.9774(2) 0.0215(11) Uani 1 1 d . . .
H24 H 0.9383 0.1507 0.9397 0.026 Uiso 1 1 calc R . .
C25 C 1.0609(4) 0.1115(4) 0.9901(2) 0.0301(13) Uani 1 1 d . . .
H25 H 1.0963 0.0858 0.9612 0.036 Uiso 1 1 calc R . .
C26 C 1.1042(4) 0.1115(4) 1.0452(2) 0.0285(13) Uani 1 1 d . . .
H26 H 1.1693 0.0874 1.0539 0.034 Uiso 1 1 calc R . .
C27 C 1.0483(4) 0.1484(3) 1.0876(2) 0.0175(10) Uani 1 1 d . . .
C28 C 0.9507(3) 0.1817(3) 1.0713(2) 0.0158(10) Uani 1 1 d . . .
H28 H 0.9116 0.2035 1.0997 0.019 Uiso 1 1 calc R . .
N29 N 1.0822(3) 0.1582(3) 1.14448(18) 0.0255(10) Uani 1 1 d . . .
H29 H 1.0521 0.2006 1.1634 0.031 Uiso 1 1 calc R . .
C30 C 1.1591(4) 0.1074(3) 1.1739(2) 0.0218(11) Uani 1 1 d . . .
O31 O 1.2080(3) 0.0453(2) 1.15108(15) 0.0270(9) Uani 1 1 d . . .
N32 N 1.1743(3) 0.1332(3) 1.22896(18) 0.0249(10) Uani 1 1 d . . .
H32 H 1.1390 0.1791 1.2415 0.030 Uiso 1 1 calc R . .
C33 C 1.2487(4) 0.0852(3) 1.2675(2) 0.0212(11) Uani 1 1 d . . .
H33A H 1.2517 0.0184 1.2569 0.025 Uiso 1 1 calc R . .
H33B H 1.2267 0.0882 1.3057 0.025 Uiso 1 1 calc R . .
C34 C 1.3554(4) 0.1281(3) 1.2680(2) 0.0192(11) Uani 1 1 d . . .
H34A H 1.3737 0.1353 1.2292 0.023 Uiso 1 1 calc R . .
H34B H 1.3561 0.1908 1.2854 0.023 Uiso 1 1 calc R . .
N35 N 1.4288(3) 0.0671(3) 1.29926(17) 0.0187(9) Uani 1 1 d . . .
H35 H 1.4502 0.0177 1.2821 0.022 Uiso 1 1 calc R . .
C36 C 1.4656(3) 0.0822(3) 1.3529(2) 0.0143(10) Uani 1 1 d . . .
O37 O 1.4523(2) 0.1563(2) 1.38080(14) 0.0181(7) Uani 1 1 d . . .
N38 N 1.5228(3) 0.0071(3) 1.37586(16) 0.0159(9) Uani 1 1 d . . .
H38 H 1.5245 -0.0428 1.3547 0.019 Uiso 1 1 calc R . .
C39 C 1.5776(3) 0.0012(3) 1.4281(2) 0.0135(10) Uani 1 1 d . . .
C40 C 1.6206(3) -0.0877(3) 1.4426(2) 0.0144(10) Uani 1 1 d . . .
H40 H 1.6086 -0.1374 1.4168 0.017 Uiso 1 1 calc R . .
N41 N 1.6769(3) -0.1069(3) 1.49027(16) 0.0131(8) Uani 1 1 d . . .
C42 C 1.6936(3) -0.0348(3) 1.5276(2) 0.0163(10) Uani 1 1 d . . .
H42 H 1.7330 -0.0458 1.5615 0.020 Uiso 1 1 calc R . .
C43 C 1.6537(4) 0.0553(3) 1.5169(2) 0.0179(11) Uani 1 1 d . . .
H43 H 1.6667 0.1034 1.5436 0.022 Uiso 1 1 calc R . .
C44 C 1.5957(3) 0.0750(3) 1.4678(2) 0.0149(10) Uani 1 1 d . . .
H44 H 1.5690 0.1357 1.4608 0.018 Uiso 1 1 calc R . .
O45 O 0.7826(2) 0.2606(2) 0.90894(14) 0.0162(7) Uani 1 1 d . . .
O46 O 0.7323(2) 0.2405(2) 1.08376(14) 0.0166(7) Uani 1 1 d . . .
S47 S 0.48261(9) 0.16930(9) 0.74986(5) 0.0189(3) Uani 1 1 d . . .
O48 O 0.5193(3) 0.2597(3) 0.77533(17) 0.0324(10) Uani 1 1 d . . .
O49 O 0.3748(3) 0.1557(3) 0.76086(16) 0.0354(10) Uani 1 1 d . . .
O50 O 0.4934(3) 0.1695(2) 0.68871(14) 0.0235(8) Uani 1 1 d . . .
O51 O 0.5439(3) 0.0902(3) 0.77636(16) 0.0366(10) Uani 1 1 d . . .
O60 O 0.7444(3) 0.1397(2) 0.82115(14) 0.0248(8) Uani 1 1 d . . .
C57 C 0.0986(6) 0.0676(6) 0.8270(3) 0.069(3) Uani 1 1 d . . .
C58 C 0.0435(7) 0.0162(7) 0.7730(4) 0.099(3) Uani 1 1 d . . .
H58A H 0.0648 0.0450 0.7391 0.148 Uiso 1 1 calc R . .
H58B H -0.0288 0.0228 0.7737 0.148 Uiso 1 1 calc R . .
H58C H 0.0610 -0.0504 0.7737 0.148 Uiso 1 1 calc R . .
C59 C 0.1204(11) 0.1753(10) 0.8225(6) 0.080(4) Uiso 0.67 1 d P . .
C59' C 0.0453(18) 0.1594(16) 0.8299(10) 0.053(6) Uiso 0.33 1 d P . .
O56 O 0.1402(5) 0.0205(4) 0.8638(2) 0.084(2) Uani 1 1 d . . .
O52 O 0.1325(4) 0.9688(3) 0.36466(18) 0.0489(12) Uani 1 1 d . . .
C53 C 0.1384(5) 0.8893(4) 0.3467(2) 0.0369(15) Uani 1 1 d . . .
C54 C 0.2390(6) 0.8459(5) 0.3358(3) 0.060(2) Uani 1 1 d . . .
H54A H 0.2921 0.8917 0.3446 0.089 Uiso 1 1 calc R . .
H54B H 0.2384 0.8278 0.2966 0.089 Uiso 1 1 calc R . .
H54C H 0.2509 0.7905 0.3593 0.089 Uiso 1 1 calc R . .
C55 C 0.0463(6) 0.8245(5) 0.3371(3) 0.060(2) Uani 1 1 d . . .
H55A H 0.0530 0.7717 0.3631 0.090 Uiso 1 1 calc R . .
H55B H 0.0417 0.8009 0.2988 0.090 Uiso 1 1 calc R . .
H55C H -0.0141 0.8599 0.3433 0.090 Uiso 1 1 calc R . .
O61 O 0.2652(3) 0.6310(3) 0.83251(15) 0.0276(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O45 2.118(3) . ?
Zn1 O46 2.126(3) . ?
Zn1 N41 2.163(4) 2_757 ?
Zn1 N19 2.179(4) 2_546 ?
Zn1 N23 2.211(4) . ?
Zn1 N1 2.219(4) . ?
N1 C6 1.316(6) . ?
N1 C2 1.345(6) . ?
C2 C3 1.377(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.399(6) . ?
C5 N7 1.402(6) . ?
C6 H6 0.9300 . ?
N7 C8 1.373(7) . ?
N7 H7 0.8600 . ?
C8 O9 1.233(7) . ?
C8 N10 1.306(11) . ?
C8 N10' 1.468(12) . ?
N10 N10' 0.656(12) . ?
N10 C11 1.513(14) . ?
N10 C11' 1.701(19) . ?
N10' C11' 1.508(18) . ?
N10' C11 1.608(15) . ?
C11 C11' 0.719(17) . ?
C11 C12 1.442(13) . ?
C11' C12 1.439(17) . ?
C12 N13 1.467(7) . ?
N13 C14 1.318(7) . ?
N13 H13 0.8600 . ?
C14 O15 1.239(6) . ?
C14 N16 1.375(6) . ?
N16 C17 1.381(6) . ?
N16 H16 0.8600 . ?
C17 C18 1.385(6) . ?
C17 C22 1.403(7) . ?
C18 N19 1.343(6) . ?
C18 H18 0.9300 . ?
N19 C20 1.345(6) . ?
N19 Zn1 2.179(4) 2_556 ?
C20 C21 1.384(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.357(7) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N23 C28 1.337(6) . ?
N23 C24 1.343(6) . ?
C24 C25 1.381(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.378(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.390(7) . ?
C26 H26 0.9300 . ?
C27 N29 1.387(6) . ?
C27 C28 1.394(6) . ?
C28 H28 0.9300 . ?
N29 C30 1.379(6) . ?
N29 H29 0.8600 . ?
C30 O31 1.233(6) . ?
C30 N32 1.347(6) . ?
N32 C33 1.448(6) . ?
N32 H32 0.8600 . ?
C33 C34 1.529(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N35 1.447(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
N35 C36 1.336(6) . ?
N35 H35 0.8600 . ?
C36 O37 1.248(5) . ?
C36 N38 1.378(5) . ?
N38 C39 1.380(6) . ?
N38 H38 0.8600 . ?
C39 C40 1.398(6) . ?
C39 C44 1.402(6) . ?
C40 N41 1.323(6) . ?
C40 H40 0.9300 . ?
N41 C42 1.347(6) . ?
N41 Zn1 2.163(4) 2_747 ?
C42 C43 1.381(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.363(6) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
S47 O50 1.462(3) . ?
S47 O48 1.466(3) 1 ?
S47 O48 1.466(3) . ?
S47 O49 1.479(4) . ?
S47 O51 1.480(4) . ?
C57 O56 1.189(8) . ?
C57 C59' 1.47(2) . ?
C57 C59 1.539(15) . ?
C57 C58 1.587(12) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 C59' 1.04(2) . ?
O52 C53 1.197(7) . ?
C53 C54 1.501(9) . ?
C53 C55 1.519(8) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O45 Zn1 O46 178.46(11) . . ?
O45 Zn1 N41 90.06(13) . 2_757 ?
O46 Zn1 N41 91.22(13) . 2_757 ?
O45 Zn1 N19 91.86(13) . 2_546 ?
O46 Zn1 N19 86.88(13) . 2_546 ?
N41 Zn1 N19 177.94(14) 2_757 2_546 ?
O45 Zn1 N23 92.66(14) . . ?
O46 Zn1 N23 88.15(14) . . ?
N41 Zn1 N23 91.45(14) 2_757 . ?
N19 Zn1 N23 87.72(13) 2_546 . ?
O45 Zn1 N1 88.88(14) . . ?
O46 Zn1 N1 90.31(13) . . ?
N41 Zn1 N1 88.34(14) 2_757 . ?
N19 Zn1 N1 92.44(14) 2_546 . ?
N23 Zn1 N1 178.44(14) . . ?
C6 N1 C2 117.8(4) . . ?
C6 N1 Zn1 123.5(3) . . ?
C2 N1 Zn1 118.4(3) . . ?
N1 C2 C3 121.9(5) . . ?
N1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C2 C3 C4 120.5(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 117.6(5) . . ?
C5 C4 H4 121.2 . . ?
C3 C4 H4 121.2 . . ?
C4 C5 C6 118.4(5) . . ?
C4 C5 N7 125.0(5) . . ?
C6 C5 N7 116.6(4) . . ?
N1 C6 C5 123.8(4) . . ?
N1 C6 H6 118.1 . . ?
C5 C6 H6 118.1 . . ?
C8 N7 C5 124.2(4) . . ?
C8 N7 H7 117.9 . . ?
C5 N7 H7 117.9 . . ?
O9 C8 N10 121.5(6) . . ?
O9 C8 N7 123.7(6) . . ?
N10 C8 N7 112.8(6) . . ?
O9 C8 N10' 124.0(6) . . ?
N7 C8 N10' 111.0(6) . . ?
C8 N10 C11 115.5(8) . . ?
C8 N10 C11' 118.6(9) . . ?
C8 N10' C11' 121.2(10) . . ?
C8 N10' C11 101.7(8) . . ?
C11' C11 C12 75.3(18) . . ?
C11' C11 N10 92.2(19) . . ?
C12 C11 N10 108.2(8) . . ?
C12 C11 N10' 106.5(8) . . ?
C11 C11' C12 75.8(18) . . ?
C12 C11' N10' 112.2(11) . . ?
C12 C11' N10 99.0(10) . . ?
C11' C12 N13 108.6(8) . . ?
C11 C12 N13 103.9(6) . . ?
C14 N13 C12 123.5(5) . . ?
C14 N13 H13 118.3 . . ?
C12 N13 H13 118.3 . . ?
O15 C14 N13 124.2(5) . . ?
O15 C14 N16 122.2(5) . . ?
N13 C14 N16 113.7(5) . . ?
C14 N16 C17 128.2(5) . . ?
C14 N16 H16 115.9 . . ?
C17 N16 H16 115.9 . . ?
N16 C17 C18 116.2(4) . . ?
N16 C17 C22 126.8(4) . . ?
C18 C17 C22 117.0(5) . . ?
N19 C18 C17 124.4(4) . . ?
N19 C18 H18 117.8 . . ?
C17 C18 H18 117.8 . . ?
C18 N19 C20 117.4(4) . . ?
C18 N19 Zn1 120.5(3) . 2_556 ?
C20 N19 Zn1 122.0(3) . 2_556 ?
N19 C20 C21 121.3(4) . . ?
N19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 121.1(5) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C17 118.6(4) . . ?
C21 C22 H22 120.7 . . ?
C17 C22 H22 120.7 . . ?
C28 N23 C24 117.0(4) . . ?
C28 N23 Zn1 121.0(3) . . ?
C24 N23 Zn1 121.9(3) . . ?
N23 C24 C25 122.2(5) . . ?
N23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C26 C25 C24 120.4(5) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 118.4(5) . . ?
C25 C26 H26 120.8 . . ?
C27 C26 H26 120.8 . . ?
N29 C27 C26 125.8(4) . . ?
N29 C27 C28 116.9(4) . . ?
C26 C27 C28 117.3(5) . . ?
N23 C28 C27 124.6(5) . . ?
N23 C28 H28 117.7 . . ?
C27 C28 H28 117.7 . . ?
C30 N29 C27 127.1(4) . . ?
C30 N29 H29 116.5 . . ?
C27 N29 H29 116.5 . . ?
O31 C30 N32 124.7(5) . . ?
O31 C30 N29 122.1(5) . . ?
N32 C30 N29 113.1(4) . . ?
C30 N32 C33 121.4(4) . . ?
C30 N32 H32 119.3 . . ?
C33 N32 H32 119.3 . . ?
N32 C33 C34 113.5(4) . . ?
N32 C33 H33A 108.9 . . ?
C34 C33 H33A 108.9 . . ?
N32 C33 H33B 108.9 . . ?
C34 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
N35 C34 C33 110.4(4) . . ?
N35 C34 H34A 109.6 . . ?
C33 C34 H34A 109.6 . . ?
N35 C34 H34B 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C36 N35 C34 124.5(4) . . ?
C36 N35 H35 117.7 . . ?
C34 N35 H35 117.7 . . ?
O37 C36 N35 125.1(4) . . ?
O37 C36 N38 121.5(4) . . ?
N35 C36 N38 113.4(4) . . ?
C36 N38 C39 128.8(4) . . ?
C36 N38 H38 115.6 . . ?
C39 N38 H38 115.6 . . ?
N38 C39 C40 116.4(4) . . ?
N38 C39 C44 126.9(4) . . ?
C40 C39 C44 116.6(4) . . ?
N41 C40 C39 125.3(4) . . ?
N41 C40 H40 117.4 . . ?
C39 C40 H40 117.4 . . ?
C40 N41 C42 117.0(4) . . ?
C40 N41 Zn1 119.6(3) . 2_747 ?
C42 N41 Zn1 123.4(3) . 2_747 ?
N41 C42 C43 121.7(4) . . ?
N41 C42 H42 119.2 . . ?
C43 C42 H42 119.2 . . ?
C44 C43 C42 121.3(4) . . ?
C44 C43 H43 119.4 . . ?
C42 C43 H43 119.4 . . ?
C43 C44 C39 118.1(4) . . ?
C43 C44 H44 120.9 . . ?
C39 C44 H44 120.9 . . ?
O50 S47 O48 110.3(2) . 1 ?
O50 S47 O48 110.3(2) . . ?
O50 S47 O49 110.3(2) . . ?
O48 S47 O49 109.2(2) 1 . ?
O48 S47 O49 109.2(2) . . ?
O50 S47 O51 108.9(2) . . ?
O48 S47 O51 108.8(2) 1 . ?
O48 S47 O51 108.8(2) . . ?
O49 S47 O51 109.3(2) . . ?
O56 C57 C59' 130.2(12) . . ?
O56 C57 C59 121.1(10) . . ?
O56 C57 C58 119.3(8) . . ?
C59' C57 C58 104.1(11) . . ?
C59 C57 C58 117.7(8) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C59' C59 C57 66.1(15) . . ?
C59 C59' C57 73.3(16) . . ?
O52 C53 C54 121.5(6) . . ?
O52 C53 C55 122.2(6) . . ?
C54 C53 C55 116.2(6) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O48 0.86 1.97 2.786(6) 158.9 1
N13 H13 O51 0.86 2.36 3.099(6) 143.7 2_556
N13 H13 O49 0.86 2.51 3.314(7) 154.9 2_556
N16 H16 O51 0.86 2.05 2.882(6) 163.0 2_556
N29 H29 O50 0.86 2.08 2.912(5) 161.9 4_666
N32 H32 O48 0.86 2.02 2.828(5) 156.4 4_666
N35 H35 O51 0.86 2.05 2.876(5) 160.1 3_757
N38 H38 O50 0.86 2.05 2.903(5) 169.9 3_757

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.916
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.137

# Attachment 'COMP_5_an416em_CIF_FINAL_R4.cif'

data_an416em
_database_code_depnum_ccdc_archive 'CCDC 679365'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H56 N12 O16 S Zn'
_chemical_formula_weight         1010.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 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   P2(1)/n

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

_cell_length_a                   13.3717(9)
_cell_length_b                   13.6950(9)
_cell_length_c                   24.4168(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.4120(10)
_cell_angle_gamma                90.00
_cell_volume                     4443.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       NEEDLE
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2120
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7716
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_process_details   SADABS

_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_measurement_device_type  'BRUKER SMART CCD AREA DETECTOR'
_diffrn_measurement_method       PHI-OMEGA
_diffrn_detector_area_resol_mean 0.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37697
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         28.28
_reflns_number_total             10497
_reflns_number_gt                8562
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER AXS SMART 3'
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXLTL'
_computing_publication_material  'MERCURY 1.4'

_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)+(0.1000P)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_number_reflns         10497
_refine_ls_number_parameters     627
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.1626
_refine_ls_wR_factor_gt          0.1523
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_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 0.75810(2) 0.246922(19) 0.997663(11) 0.01026(10) Uani 1 1 d . . .
N1 N 0.60600(16) 0.31409(15) 0.97643(9) 0.0130(4) Uani 1 1 d . . .
C2 C 0.5600(2) 0.3526(2) 1.01726(11) 0.0180(6) Uani 1 1 d . . .
H2 H 0.5962 0.3594 1.0518 0.022 Uiso 1 1 calc R . .
C3 C 0.4607(2) 0.3827(2) 1.01010(11) 0.0214(6) Uani 1 1 d . . .
H3 H 0.4315 0.4094 1.0395 0.026 Uiso 1 1 calc R . .
C4 C 0.4050(2) 0.3733(2) 0.95971(11) 0.0200(6) Uani 1 1 d . . .
H4 H 0.3375 0.3913 0.9548 0.024 Uiso 1 1 calc R . .
C5 C 0.4526(2) 0.33573(19) 0.91578(10) 0.0144(5) Uani 1 1 d . . .
C6 C 0.55315(19) 0.30836(18) 0.92630(10) 0.0121(5) Uani 1 1 d . . .
H6 H 0.5855 0.2849 0.8972 0.014 Uiso 1 1 calc R . .
N7 N 0.40505(16) 0.32200(16) 0.86226(9) 0.0161(5) Uani 1 1 d . . .
H7 H 0.4328 0.2828 0.8410 0.019 Uiso 1 1 calc R . .
C8 C 0.31675(19) 0.36716(19) 0.84147(11) 0.0155(5) Uani 1 1 d . . .
O9 O 0.27527(15) 0.43072(14) 0.86670(8) 0.0237(5) Uani 1 1 d . . .
N10 N 0.27968(16) 0.33718(16) 0.79071(9) 0.0174(5) Uani 1 1 d . . .
H10 H 0.3082 0.2909 0.7744 0.021 Uiso 1 1 calc R . .
C11 C 0.1901(2) 0.3852(2) 0.76428(11) 0.0220(6) Uani 1 1 d . . .
H11A H 0.2014 0.4552 0.7642 0.026 Uiso 1 1 calc R . .
H11B H 0.1343 0.3725 0.7854 0.026 Uiso 1 1 calc R . .
C12 C 0.1631(2) 0.3509(2) 0.70617(11) 0.0204(6) Uani 1 1 d . . .
H12A H 0.2214 0.3537 0.6859 0.024 Uiso 1 1 calc R . .
H12B H 0.1390 0.2840 0.7059 0.024 Uiso 1 1 calc R . .
N13 N 0.08422(17) 0.41578(17) 0.68135(9) 0.0199(5) Uani 1 1 d . . .
H13 H 0.0666 0.4642 0.7005 0.024 Uiso 1 1 calc R . .
C14 C 0.03776(18) 0.40403(18) 0.63038(11) 0.0137(5) Uani 1 1 d . . .
O15 O 0.06067(14) 0.34142(13) 0.59740(8) 0.0172(4) Uani 1 1 d . . .
N16 N -0.03853(16) 0.46964(16) 0.61728(9) 0.0159(5) Uani 1 1 d . . .
H16 H -0.0548 0.5057 0.6438 0.019 Uiso 1 1 calc R . .
C17 C -0.09261(18) 0.48444(18) 0.56597(10) 0.0116(5) Uani 1 1 d . . .
C18 C -0.13968(18) 0.57447(19) 0.55732(10) 0.0132(5) Uani 1 1 d . . .
H18 H -0.1304 0.6202 0.5856 0.016 Uiso 1 1 calc R . .
N19 N -0.19711(15) 0.60013(15) 0.51145(9) 0.0124(4) Uani 1 1 d . . .
C20 C -0.21056(18) 0.53364(18) 0.47093(10) 0.0128(5) Uani 1 1 d . . .
H20 H -0.2514 0.5492 0.4388 0.015 Uiso 1 1 calc R . .
C21 C -0.1654(2) 0.44223(19) 0.47550(11) 0.0159(5) Uani 1 1 d . . .
H21 H -0.1755 0.3981 0.4464 0.019 Uiso 1 1 calc R . .
C22 C -0.10521(19) 0.41660(19) 0.52330(10) 0.0140(5) Uani 1 1 d . . .
H22 H -0.0742 0.3558 0.5268 0.017 Uiso 1 1 calc R . .
N23 N 0.91069(16) 0.18173(15) 1.02246(9) 0.0126(4) Uani 1 1 d . . .
C24 C 0.9684(2) 0.1500(2) 0.98451(11) 0.0214(6) Uani 1 1 d . . .
H24 H 0.9417 0.1498 0.9477 0.026 Uiso 1 1 calc R . .
C25 C 1.0656(2) 0.1178(2) 0.99800(12) 0.0280(7) Uani 1 1 d . . .
H25 H 1.1027 0.0955 0.9705 0.034 Uiso 1 1 calc R . .
C26 C 1.1084(2) 0.1184(2) 1.05225(12) 0.0223(6) Uani 1 1 d . . .
H26 H 1.1741 0.0970 1.0618 0.027 Uiso 1 1 calc R . .
C27 C 1.05024(19) 0.15188(18) 1.09202(11) 0.0137(5) Uani 1 1 d . . .
C28 C 0.95140(18) 0.18012(18) 1.07502(11) 0.0129(5) Uani 1 1 d . . .
H28 H 0.9113 0.1990 1.1019 0.015 Uiso 1 1 calc R . .
N29 N 1.08279(16) 0.16342(16) 1.14815(9) 0.0171(5) Uani 1 1 d . . .
H29 H 1.0528 0.2072 1.1656 0.021 Uiso 1 1 calc R . .
C30 C 1.15858(19) 0.11110(19) 1.17824(11) 0.0158(5) Uani 1 1 d . . .
O31 O 1.20794(14) 0.04790(14) 1.15711(8) 0.0200(4) Uani 1 1 d . . .
N32 N 1.17342(16) 0.13729(17) 1.23167(9) 0.0185(5) Uani 1 1 d . . .
H32 H 1.1392 0.1847 1.2432 0.022 Uiso 1 1 calc R . .
C33 C 1.24659(19) 0.0865(2) 1.27009(11) 0.0182(6) Uani 1 1 d . . .
H33A H 1.2522 0.0195 1.2579 0.022 Uiso 1 1 calc R . .
H33B H 1.2223 0.0852 1.3061 0.022 Uiso 1 1 calc R . .
C34 C 1.3501(2) 0.1331(2) 1.27546(12) 0.0204(6) Uani 1 1 d . . .
H34A H 1.3700 0.1456 1.2391 0.024 Uiso 1 1 calc R . .
H34B H 1.3482 0.1950 1.2946 0.024 Uiso 1 1 calc R . .
N35 N 1.42278(17) 0.06894(18) 1.30569(9) 0.0205(5) Uani 1 1 d . . .
H35 H 1.4443 0.0199 1.2884 0.025 Uiso 1 1 calc R . .
C36 C 1.45867(18) 0.08078(19) 1.35862(11) 0.0141(5) Uani 1 1 d . . .
O37 O 1.44100(14) 0.15223(14) 1.38706(8) 0.0193(4) Uani 1 1 d . . .
N38 N 1.51863(16) 0.00491(16) 1.37924(9) 0.0152(5) Uani 1 1 d . . .
H38 H 1.5210 -0.0452 1.3582 0.018 Uiso 1 1 calc R . .
C39 C 1.57614(18) -0.00003(18) 1.43049(10) 0.0124(5) Uani 1 1 d . . .
C40 C 1.61932(18) -0.09046(18) 1.44411(10) 0.0120(5) Uani 1 1 d . . .
H40 H 1.6053 -0.1415 1.4193 0.014 Uiso 1 1 calc R . .
N41 N 1.67934(15) -0.10888(15) 1.49017(8) 0.0124(4) Uani 1 1 d . . .
C42 C 1.69901(19) -0.03468(19) 1.52639(10) 0.0141(5) Uani 1 1 d . . .
H42 H 1.7409 -0.0455 1.5588 0.017 Uiso 1 1 calc R . .
C43 C 1.6580(2) 0.0563(2) 1.51595(11) 0.0196(6) Uani 1 1 d . . .
H43 H 1.6725 0.1059 1.5416 0.024 Uiso 1 1 calc R . .
C44 C 1.5956(2) 0.07589(19) 1.46822(11) 0.0176(6) Uani 1 1 d . . .
H44 H 1.5676 0.1375 1.4615 0.021 Uiso 1 1 calc R . .
O45 O 0.78038(16) 0.25344(15) 0.91399(9) 0.0157(4) Uani 1 1 d . . .
H45A H 0.760(3) 0.225(3) 0.8890(14) 0.020(9) Uiso 1 1 d . . .
H45B H 0.825(3) 0.282(3) 0.9074(14) 0.022(9) Uiso 1 1 d . . .
O46 O 0.73514(15) 0.23840(14) 1.08178(8) 0.0125(4) Uani 1 1 d . . .
H46A H 0.744(3) 0.278(3) 1.1017(15) 0.028(10) Uiso 1 1 d . . .
H46B H 0.682(3) 0.211(3) 1.0873(15) 0.034(10) Uiso 1 1 d . . .
S47 S 0.48040(5) 0.16202(5) 0.75038(2) 0.01312(15) Uani 1 1 d . . .
O48 O 0.52524(16) 0.24760(14) 0.78065(8) 0.0236(5) Uani 1 1 d . . .
O49 O 0.37157(14) 0.15888(14) 0.75477(8) 0.0192(4) Uani 1 1 d . . .
O50 O 0.49832(14) 0.16682(13) 0.69178(7) 0.0171(4) Uani 1 1 d . . .
O51 O 0.52891(14) 0.07207(14) 0.77500(8) 0.0218(4) Uani 1 1 d . . .
O52 O 0.16795(17) 0.93547(17) 0.36581(9) 0.0332(5) Uani 1 1 d . . .
C53 C 0.0739(3) 0.9519(3) 0.33082(14) 0.0370(8) Uani 1 1 d . . .
H53A H 0.0881 0.9634 0.2933 0.044 Uiso 1 1 calc R . .
H53B H 0.0412 1.0097 0.3433 0.044 Uiso 1 1 calc R . .
C54 C 0.0044(2) 0.8660(2) 0.33199(15) 0.0339(8) Uani 1 1 d . . .
H54A H -0.0162 0.8589 0.3686 0.041 Uiso 1 1 calc R . .
H54B H -0.0553 0.8767 0.3064 0.041 Uiso 1 1 calc R . .
O55 O 0.05424(18) 0.77823(18) 0.31719(10) 0.0373(6) Uani 1 1 d . . .
C56 C 0.1446(3) 0.7652(3) 0.35354(15) 0.0396(9) Uani 1 1 d . . .
H56A H 0.1776 0.7053 0.3443 0.048 Uiso 1 1 calc R . .
H56B H 0.1285 0.7597 0.3912 0.048 Uiso 1 1 calc R . .
C57 C 0.2132(3) 0.8496(3) 0.34882(13) 0.0352(8) Uani 1 1 d . . .
H57A H 0.2763 0.8384 0.3717 0.042 Uiso 1 1 calc R . .
H57B H 0.2275 0.8564 0.3109 0.042 Uiso 1 1 calc R . .
O58 O 0.17520(18) 0.12632(19) 0.86684(11) 0.0424(6) Uani 1 1 d . . .
C59 C 0.0836(3) 0.1791(2) 0.85116(16) 0.0397(9) Uani 1 1 d . . .
H59A H 0.0909 0.2190 0.8190 0.048 Uiso 1 1 calc R . .
H59B H 0.0692 0.2219 0.8810 0.048 Uiso 1 1 calc R . .
C60 C -0.0015(2) 0.1081(3) 0.83834(15) 0.0377(8) Uani 1 1 d . . .
H60A H -0.0105 0.0706 0.8711 0.045 Uiso 1 1 calc R . .
H60B H -0.0632 0.1438 0.8276 0.045 Uiso 1 1 calc R . .
O61 O 0.01793(19) 0.0435(2) 0.79512(10) 0.0457(7) Uani 1 1 d . . .
C62 C 0.1088(3) -0.0065(3) 0.81012(15) 0.0392(8) Uani 1 1 d . . .
H62A H 0.1234 -0.0485 0.7800 0.047 Uiso 1 1 calc R . .
H62B H 0.1019 -0.0474 0.8419 0.047 Uiso 1 1 calc R . .
C63 C 0.1953(3) 0.0647(3) 0.82380(16) 0.0427(9) Uani 1 1 d . . .
H63A H 0.2569 0.0287 0.8344 0.051 Uiso 1 1 calc R . .
H63B H 0.2046 0.1034 0.7915 0.051 Uiso 1 1 calc R . .
O64 O 0.73127(18) 0.14062(16) 0.82569(9) 0.0197(4) Uani 1 1 d . . .
H64A H 0.749(2) 0.084(3) 0.8265(14) 0.028(10) Uiso 1 1 d . . .
H64B H 0.684(3) 0.142(3) 0.8138(18) 0.047(15) Uiso 1 1 d . . .
O65 O 0.25121(17) 0.62464(17) 0.84209(9) 0.0216(5) Uani 1 1 d . . .
H65A H 0.256(2) 0.569(3) 0.8499(13) 0.020(9) Uiso 1 1 d . . .
H65B H 0.215(3) 0.636(3) 0.8183(16) 0.028(11) 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 O45 2.099(2) . ?
Zn1 O46 2.1135(19) . ?
Zn1 N41 2.152(2) 2_757 ?
Zn1 N19 2.171(2) 2_546 ?
Zn1 N1 2.240(2) . ?
Zn1 N23 2.247(2) . ?
N1 C2 1.337(3) . ?
N1 C6 1.346(3) . ?
C2 C3 1.383(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.405(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(3) . ?
C5 N7 1.401(3) . ?
C6 H6 0.9300 . ?
N7 C8 1.379(3) . ?
N7 H7 0.8600 . ?
C8 O9 1.233(3) 1 ?
C8 O9 1.233(3) . ?
C8 N10 1.347(3) . ?
N10 C11 1.452(3) . ?
N10 H10 0.8600 . ?
C11 C12 1.500(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N13 1.458(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N13 C14 1.337(3) . ?
N13 H13 0.8600 . ?
C14 O15 1.238(3) . ?
C14 N16 1.370(3) . ?
N16 C17 1.390(3) . ?
N16 H16 0.8600 . ?
C17 C18 1.390(3) . ?
C17 C22 1.392(3) . ?
C18 N19 1.332(3) . ?
C18 H18 0.9300 . ?
N19 C20 1.342(3) . ?
N19 Zn1 2.172(2) 2_556 ?
C20 C21 1.389(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.387(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N23 C28 1.337(3) . ?
N23 C24 1.343(3) . ?
C24 C25 1.377(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.383(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.388(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.395(3) . ?
C27 N29 1.400(3) . ?
C28 H28 0.9300 . ?
N29 C30 1.384(3) . ?
N29 H29 0.8600 . ?
C30 O31 1.236(3) . ?
C30 N32 1.346(3) . ?
N32 C33 1.455(3) . ?
N32 H32 0.8600 . ?
C33 C34 1.516(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N35 1.449(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
N35 C36 1.337(3) . ?
N35 H35 0.8600 . ?
C36 O37 1.238(3) . ?
C36 N38 1.373(3) . ?
N38 C39 1.396(3) . ?
N38 H38 0.8600 . ?
C39 C40 1.391(3) . ?
C39 C44 1.394(4) . ?
C40 N41 1.331(3) . ?
C40 H40 0.9300 . ?
N41 C42 1.353(3) . ?
N41 Zn1 2.152(2) 2_747 ?
C42 C43 1.374(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.381(4) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
O45 H45A 0.75(3) . ?
O45 H45B 0.75(4) . ?
O46 H46A 0.73(4) . ?
O46 H46B 0.83(4) . ?
S47 O49 1.4717(19) 1 ?
S47 O49 1.4717(19) . ?
S47 O48 1.4766(19) . ?
S47 O48 1.4766(19) 1 ?
S47 O50 1.4783(18) . ?
S47 O51 1.4875(19) 1 ?
S47 O51 1.4875(19) . ?
O52 C57 1.407(4) . ?
O52 C53 1.457(4) . ?
C53 C54 1.502(5) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 O55 1.439(4) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
O55 C56 1.428(4) . ?
C56 C57 1.489(5) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
O58 C63 1.397(4) . ?
O58 C59 1.437(4) . ?
C59 C60 1.503(5) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 O61 1.423(4) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
O61 C62 1.407(4) . ?
C62 C63 1.522(5) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
O64 H64A 0.81(4) . ?
O64 H64B 0.66(4) . ?
O65 H65A 0.78(3) . ?
O65 H65B 0.73(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O45 Zn1 O46 179.25(8) . . ?
O45 Zn1 N41 90.01(8) . 2_757 ?
O46 Zn1 N41 90.74(8) . 2_757 ?
O45 Zn1 N19 91.84(8) . 2_546 ?
O46 Zn1 N19 87.41(8) . 2_546 ?
N41 Zn1 N19 177.85(7) 2_757 2_546 ?
O45 Zn1 N1 88.92(8) . . ?
O46 Zn1 N1 91.20(8) . . ?
N41 Zn1 N1 89.09(8) 2_757 . ?
N19 Zn1 N1 92.04(8) 2_546 . ?
O45 Zn1 N23 93.20(8) . . ?
O46 Zn1 N23 86.69(8) . . ?
N41 Zn1 N23 90.01(8) 2_757 . ?
N19 Zn1 N23 88.80(8) 2_546 . ?
N1 Zn1 N23 177.69(7) . . ?
C2 N1 C6 117.6(2) . . ?
C2 N1 Zn1 118.11(17) . . ?
C6 N1 Zn1 123.89(17) . . ?
N1 C2 C3 122.6(2) . . ?
N1 C2 H2 118.7 . . ?
C3 C2 H2 118.7 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 118.2(2) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 120.9 . . ?
C6 C5 N7 117.7(2) . . ?
C6 C5 C4 118.0(2) . . ?
N7 C5 C4 124.4(2) . . ?
N1 C6 C5 123.4(2) . . ?
N1 C6 H6 118.3 . . ?
C5 C6 H6 118.3 . . ?
C8 N7 C5 124.3(2) . . ?
C8 N7 H7 117.8 . . ?
C5 N7 H7 117.8 . . ?
O9 C8 N10 122.4(2) 1 . ?
O9 C8 N10 122.4(2) . . ?
O9 C8 N7 123.2(2) 1 . ?
O9 C8 N7 123.2(2) . . ?
N10 C8 N7 114.5(2) . . ?
C8 N10 C11 118.1(2) . . ?
C8 N10 H10 120.9 . . ?
C11 N10 H10 120.9 . . ?
N10 C11 C12 112.2(2) . . ?
N10 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
N10 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N13 C12 C11 106.8(2) . . ?
N13 C12 H12A 110.4 . . ?
C11 C12 H12A 110.4 . . ?
N13 C12 H12B 110.4 . . ?
C11 C12 H12B 110.4 . . ?
H12A C12 H12B 108.6 . . ?
C14 N13 C12 123.5(2) . . ?
C14 N13 H13 118.2 . . ?
C12 N13 H13 118.2 . . ?
O15 C14 N13 124.5(2) . . ?
O15 C14 N16 122.3(2) . . ?
N13 C14 N16 113.2(2) . . ?
C14 N16 C17 127.2(2) . . ?
C14 N16 H16 116.4 . . ?
C17 N16 H16 116.4 . . ?
N16 C17 C18 116.6(2) . . ?
N16 C17 C22 125.8(2) . . ?
C18 C17 C22 117.6(2) . . ?
N19 C18 C17 124.8(2) . . ?
N19 C18 H18 117.6 . . ?
C17 C18 H18 117.6 . . ?
C18 N19 C20 117.3(2) . . ?
C18 N19 Zn1 120.32(17) . 2_556 ?
C20 N19 Zn1 122.33(16) . 2_556 ?
N19 C20 C21 122.1(2) . . ?
N19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C22 C21 C20 120.1(2) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C17 118.1(2) . . ?
C21 C22 H22 120.9 . . ?
C17 C22 H22 120.9 . . ?
C28 N23 C24 116.9(2) . . ?
C28 N23 Zn1 121.68(17) . . ?
C24 N23 Zn1 121.15(17) . . ?
N23 C24 C25 122.6(3) . . ?
N23 C24 H24 118.7 . . ?
C25 C24 H24 118.7 . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C27 117.9(2) . . ?
C25 C26 H26 121.1 . . ?
C27 C26 H26 121.1 . . ?
C26 C27 C28 118.0(2) . . ?
C26 C27 N29 125.8(2) . . ?
C28 C27 N29 116.1(2) . . ?
N23 C28 C27 124.1(2) . . ?
N23 C28 H28 117.9 . . ?
C27 C28 H28 117.9 . . ?
C30 N29 C27 126.2(2) . . ?
C30 N29 H29 116.9 . . ?
C27 N29 H29 116.9 . . ?
O31 C30 N32 124.3(2) . . ?
O31 C30 N29 122.3(2) . . ?
N32 C30 N29 113.4(2) . . ?
C30 N32 C33 120.9(2) . . ?
C30 N32 H32 119.6 . . ?
C33 N32 H32 119.6 . . ?
N32 C33 C34 113.3(2) . . ?
N32 C33 H33A 108.9 . . ?
C34 C33 H33A 108.9 . . ?
N32 C33 H33B 108.9 . . ?
C34 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
N35 C34 C33 110.1(2) . . ?
N35 C34 H34A 109.7 . . ?
C33 C34 H34A 109.7 . . ?
N35 C34 H34B 109.7 . . ?
C33 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
C36 N35 C34 124.5(2) . . ?
C36 N35 H35 117.7 . . ?
C34 N35 H35 117.7 . . ?
O37 C36 N35 124.6(2) . . ?
O37 C36 N38 122.2(2) . . ?
N35 C36 N38 113.2(2) . . ?
C36 N38 C39 127.3(2) . . ?
C36 N38 H38 116.3 . . ?
C39 N38 H38 116.3 . . ?
C40 C39 C44 117.7(2) . . ?
C40 C39 N38 115.5(2) . . ?
C44 C39 N38 126.9(2) . . ?
N41 C40 C39 124.5(2) . . ?
N41 C40 H40 117.8 . . ?
C39 C40 H40 117.8 . . ?
C40 N41 C42 117.7(2) . . ?
C40 N41 Zn1 118.62(17) . 2_747 ?
C42 N41 Zn1 123.67(16) . 2_747 ?
N41 C42 C43 121.0(2) . . ?
N41 C42 H42 119.5 . . ?
C43 C42 H42 119.5 . . ?
C42 C43 C44 121.6(3) . . ?
C42 C43 H43 119.2 . . ?
C44 C43 H43 119.2 . . ?
C43 C44 C39 117.6(2) . . ?
C43 C44 H44 121.2 . . ?
C39 C44 H44 121.2 . . ?
Zn1 O45 H45A 134(3) . . ?
Zn1 O45 H45B 116(3) . . ?
H45A O45 H45B 109(4) . . ?
Zn1 O46 H46A 125(3) . . ?
Zn1 O46 H46B 114(3) . . ?
H46A O46 H46B 108(4) . . ?
O49 S47 O48 109.65(12) 1 . ?
O49 S47 O48 109.65(12) . . ?
O49 S47 O48 109.65(12) 1 1 ?
O49 S47 O48 109.65(12) . 1 ?
O49 S47 O50 109.89(11) 1 . ?
O49 S47 O50 109.89(11) . . ?
O48 S47 O50 110.39(11) . . ?
O48 S47 O50 110.39(11) 1 . ?
O49 S47 O51 109.67(11) 1 1 ?
O49 S47 O51 109.67(11) . 1 ?
O48 S47 O51 108.71(12) . 1 ?
O48 S47 O51 108.71(12) 1 1 ?
O50 S47 O51 108.51(11) . 1 ?
O49 S47 O51 109.67(11) 1 . ?
O49 S47 O51 109.67(11) . . ?
O48 S47 O51 108.71(12) . . ?
O48 S47 O51 108.71(12) 1 . ?
O50 S47 O51 108.51(11) . . ?
C57 O52 C53 109.2(2) . . ?
O52 C53 C54 111.3(3) . . ?
O52 C53 H53A 109.4 . . ?
C54 C53 H53A 109.4 . . ?
O52 C53 H53B 109.4 . . ?
C54 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
O55 C54 C53 110.2(3) . . ?
O55 C54 H54A 109.6 . . ?
C53 C54 H54A 109.6 . . ?
O55 C54 H54B 109.6 . . ?
C53 C54 H54B 109.6 . . ?
H54A C54 H54B 108.1 . . ?
C56 O55 C54 109.4(3) . . ?
O55 C56 C57 109.9(3) . . ?
O55 C56 H56A 109.7 . . ?
C57 C56 H56A 109.7 . . ?
O55 C56 H56B 109.7 . . ?
C57 C56 H56B 109.7 . . ?
H56A C56 H56B 108.2 . . ?
O52 C57 C56 109.7(3) . . ?
O52 C57 H57A 109.7 . . ?
C56 C57 H57A 109.7 . . ?
O52 C57 H57B 109.7 . . ?
C56 C57 H57B 109.7 . . ?
H57A C57 H57B 108.2 . . ?
C63 O58 C59 109.5(3) . . ?
O58 C59 C60 109.4(3) . . ?
O58 C59 H59A 109.8 . . ?
C60 C59 H59A 109.8 . . ?
O58 C59 H59B 109.8 . . ?
C60 C59 H59B 109.8 . . ?
H59A C59 H59B 108.2 . . ?
O61 C60 C59 111.1(3) . . ?
O61 C60 H60A 109.4 . . ?
C59 C60 H60A 109.4 . . ?
O61 C60 H60B 109.4 . . ?
C59 C60 H60B 109.4 . . ?
H60A C60 H60B 108.0 . . ?
C62 O61 C60 109.5(3) . . ?
O61 C62 C63 111.0(3) . . ?
O61 C62 H62A 109.4 . . ?
C63 C62 H62A 109.4 . . ?
O61 C62 H62B 109.4 . . ?
C63 C62 H62B 109.4 . . ?
H62A C62 H62B 108.0 . . ?
O58 C63 C62 110.3(3) . . ?
O58 C63 H63A 109.6 . . ?
C62 C63 H63A 109.6 . . ?
O58 C63 H63B 109.6 . . ?
C62 C63 H63B 109.6 . . ?
H63A C63 H63B 108.1 . . ?
H64A O64 H64B 108(4) . . ?
H65A O65 H65B 115(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O48 0.86 2.08 2.882(3) 154.5 1
N10 H10 O49 0.86 2.08 2.913(3) 164.2 1
N13 H13 O51 0.86 2.08 2.892(3) 156.5 2_556
N16 H16 O51 0.86 2.17 2.971(3) 153.9 2_556
N29 H29 O50 0.86 2.01 2.843(3) 164.6 4_666
N32 H32 O48 0.86 2.08 2.893(3) 157.5 4_666
N35 H35 O51 0.86 2.06 2.883(3) 160.6 3_757
N38 H38 O50 0.86 2.06 2.916(3) 170.6 3_757
O45 H45A O64 0.75(3) 1.93(4) 2.674(3) 170(4) 1
O45 H45B O37 0.75(4) 1.91(4) 2.651(3) 176(4) 4_565
O46 H46A O65 0.73(4) 1.90(4) 2.633(3) 171(4) 3_667
O64 H64A O31 0.81(4) 1.93(4) 2.725(3) 169(3) 3_757
O64 H64B O51 0.66(4) 2.39(4) 2.998(3) 154(5) 1
O64 H64B O48 0.66(4) 2.62(4) 3.205(3) 148(5) 1
O65 H65A O9 0.78(3) 1.95(3) 2.734(3) 176(3) 1
O65 H65B O49 0.73(4) 2.04(4) 2.764(3) 172(4) 2_556
O46 H46B O15 0.83(4) 1.82(4) 2.642(3) 176(4) 4_666

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.103


