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

data_added_by_encifer
#==========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_address     
;
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       majf247@yahoo.com
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_phone       +86-431-85098620
_publ_requested_journal          CrystEngComm

#=========================================================== 

data_Compound-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 Co2 N10 O12'
_chemical_formula_sum            'C32 H32 Co2 N10 O12'
_chemical_formula_weight         866.54

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'
Co Co 0.3494 0.9721 '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 1 2/c 1'
_symmetry_space_group_name_hall  '-C 2yc'


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                   36.0605(19)
_cell_length_b                   5.2677(2)
_cell_length_c                   19.4061(10)
_cell_angle_alpha                90
_cell_angle_beta                 113.793(7)
_cell_angle_gamma                90
_cell_volume                     3373.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6265
_cell_measurement_theta_min      3.1083
_cell_measurement_theta_max      29.1370

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1776
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7915
_exptl_absorpt_correction_T_max  0.8564
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;

_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10896
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         27.10
_reflns_number_total             3681
_reflns_number_gt                3284
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_cell_refinement       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_data_reduction        
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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)+(0.0320P)²+4.6537P] 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         3681
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0772
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.873574(7) 0.84470(5) 0.820270(13) 0.01830(9) Uani 1 1 d . . .
C1 C 0.87982(5) 0.5701(4) 1.04345(10) 0.0179(4) Uani 1 1 d . . .
C2 C 0.87231(6) 0.6654(4) 1.10330(10) 0.0194(4) Uani 1 1 d . . .
H2 H 0.8552 0.8043 1.0961 0.023 Uiso 1 1 calc R . .
C3 C 0.89032(6) 0.5536(4) 1.17397(10) 0.0195(4) Uani 1 1 d . . .
C4 C 0.91536(6) 0.3445(4) 1.18397(11) 0.0213(4) Uani 1 1 d . . .
H4 H 0.9270 0.2666 1.2309 0.026 Uiso 1 1 calc R . .
C5 C 0.92313(6) 0.2510(4) 1.12421(11) 0.0202(4) Uani 1 1 d . . .
C6 C 0.90563(6) 0.3627(4) 1.05400(10) 0.0202(4) Uani 1 1 d . . .
H6 H 0.9110 0.3004 1.0141 0.024 Uiso 1 1 calc R . .
C7 C 0.86250(6) 0.7077(4) 0.96874(10) 0.0187(4) Uani 1 1 d . . .
C8 C 0.88562(5) 0.6650(4) 1.24176(10) 0.0180(4) Uani 1 1 d . . .
C9 C 0.96055(6) -0.0692(4) 1.08975(12) 0.0260(4) Uani 1 1 d . . .
H9A H 0.9392 -0.0454 1.0400 0.031 Uiso 1 1 calc R . .
H9B H 0.9641 -0.2502 1.0994 0.031 Uiso 1 1 calc R . .
C10 C 1.03749(6) 0.2943(4) 1.07377(12) 0.0266(4) Uani 1 1 d . . .
H10 H 1.0476 0.4331 1.0572 0.032 Uiso 1 1 calc R . .
C11 C 1.03571(6) -0.0452(4) 1.12821(11) 0.0241(4) Uani 1 1 d . . .
H11 H 1.0427 -0.1931 1.1568 0.029 Uiso 1 1 calc R . .
C12 C 0.79396(6) 0.8930(4) 0.68337(12) 0.0289(5) Uani 1 1 d . . .
H12 H 0.8032 1.0442 0.6711 0.035 Uiso 1 1 calc R . .
C13 C 0.75531(7) 0.5708(4) 0.67782(13) 0.0343(5) Uani 1 1 d . . .
H13 H 0.7337 0.4573 0.6624 0.041 Uiso 1 1 calc R . .
C14 C 0.79026(6) 0.5532(4) 0.74011(13) 0.0326(5) Uani 1 1 d . . .
H14 H 0.7967 0.4230 0.7754 0.039 Uiso 1 1 calc R . .
C15 C 0.72850(7) 0.8845(5) 0.56977(12) 0.0361(5) Uani 1 1 d . . .
H15A H 0.7211 1.0570 0.5765 0.043 Uiso 1 1 calc R A 1
H15B H 0.7042 0.7813 0.5538 0.043 Uiso 1 1 calc R A 1
C16 C 0.7447(2) 0.8818(15) 0.5084(3) 0.038(2) Uani 0.432(11) 1 d P . 1
H16A H 0.7244 0.9539 0.4627 0.046 Uiso 0.432(11) 1 calc PR . 1
H16B H 0.7686 0.9882 0.5239 0.046 Uiso 0.432(11) 1 calc PR . 1
C16' C 0.72983(14) 0.7372(13) 0.5031(2) 0.0353(17) Uani 0.568(11) 1 d P . 2
H16C H 0.7247 0.5592 0.5085 0.042 Uiso 0.568(11) 1 calc PR . 2
H16D H 0.7085 0.7986 0.4570 0.042 Uiso 0.568(11) 1 calc PR . 2
N1 N 0.99797(5) 0.0388(3) 1.09169(9) 0.0227(3) Uani 1 1 d . . .
N2 N 0.99847(5) 0.2608(4) 1.05588(10) 0.0294(4) Uani 1 1 d . . .
N3 N 1.06181(5) 0.1097(3) 1.11836(9) 0.0239(4) Uani 1 1 d . . .
N4 N 0.81474(5) 0.7560(3) 0.74350(9) 0.0253(4) Uani 1 1 d . . .
N5 N 0.75810(5) 0.7884(3) 0.64216(9) 0.0276(4) Uani 1 1 d . . .
O1 O 0.87545(4) 0.6417(2) 0.91947(7) 0.0233(3) Uani 1 1 d . . .
O2 O 0.83787(5) 0.8815(3) 0.96128(8) 0.0315(4) Uani 1 1 d . . .
O3 O 0.87779(4) 0.8981(3) 1.23900(7) 0.0231(3) Uani 1 1 d . . .
O4 O 0.89207(4) 0.5231(3) 1.29749(7) 0.0236(3) Uani 1 1 d . . .
O5 O 0.94926(4) 0.0448(3) 1.14344(8) 0.0280(3) Uani 1 1 d . . .
O1W O 0.85214(5) 1.1470(3) 0.86153(9) 0.0297(4) Uani 1 1 d . . .
H1A H 0.8463(8) 1.099(5) 0.8970(16) 0.045 Uiso 1 1 d . . .
H1B H 0.8640(9) 1.272(6) 0.8725(16) 0.045 Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1W 2.0673(15) . ?
Co1 N4 2.0949(17) . ?
Co1 O3 2.1308(13) 6_575 ?
Co1 O4 2.1523(14) 6_565 ?
Co1 N3 2.1602(17) 5_767 ?
Co1 O1 2.1791(13) . ?
C1 C2 1.389(2) . ?
C1 C6 1.395(3) . ?
C1 C7 1.513(3) . ?
C2 C3 1.390(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(3) . ?
C3 C8 1.511(2) . ?
C4 C5 1.388(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(3) . ?
C5 O5 1.387(2) . ?
C6 H6 0.9300 . ?
C7 O2 1.242(2) . ?
C7 O1 1.270(2) . ?
C8 O3 1.256(2) . ?
C8 O4 1.257(2) . ?
C9 O5 1.398(2) . ?
C9 N1 1.451(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.318(3) . ?
C10 N3 1.360(3) . ?
C10 H10 0.9300 . ?
C11 N3 1.317(3) . ?
C11 N1 1.331(2) . ?
C11 H11 0.9300 . ?
C12 N4 1.318(3) . ?
C12 N5 1.334(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.352(3) . ?
C13 N5 1.364(3) . ?
C13 H13 0.9300 . ?
C14 N4 1.370(3) . ?
C14 H14 0.9300 . ?
C15 N5 1.469(3) . ?
C15 C16 1.523(7) . ?
C15 C16' 1.526(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C16 1.511(14) 7_666 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16' C16' 1.514(10) 7_666 ?
C16' H16C 0.9700 . ?
C16' H16D 0.9700 . ?
N1 N2 1.364(2) . ?
N3 Co1 2.1602(16) 5_767 ?
O3 Co1 2.1308(13) 6_576 ?
O4 Co1 2.1523(14) 6_566 ?
O1W H1A 0.83(3) . ?
O1W H1B 0.77(3) . ?

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
O1W Co1 N4 91.01(7) . . ?
O1W Co1 O3 86.92(6) . 6_575 ?
N4 Co1 O3 88.26(6) . 6_575 ?
O1W Co1 O4 165.53(6) . 6_565 ?
N4 Co1 O4 87.82(6) . 6_565 ?
O3 Co1 O4 107.46(5) 6_575 6_565 ?
O1W Co1 N3 100.92(7) . 5_767 ?
N4 Co1 N3 167.04(7) . 5_767 ?
O3 Co1 N3 87.37(6) 6_575 5_767 ?
O4 Co1 N3 81.87(6) 6_565 5_767 ?
O1W Co1 O1 85.36(6) . . ?
N4 Co1 O1 100.40(6) . . ?
O3 Co1 O1 168.48(5) 6_575 . ?
O4 Co1 O1 80.67(5) 6_565 . ?
N3 Co1 O1 85.71(6) 5_767 . ?
C2 C1 C6 120.26(17) . . ?
C2 C1 C7 118.94(17) . . ?
C6 C1 C7 120.60(16) . . ?
C3 C2 C1 120.06(17) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.55(16) . . ?
C2 C3 C8 121.50(17) . . ?
C4 C3 C8 118.81(16) . . ?
C3 C4 C5 120.27(17) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 O5 126.14(17) . . ?
C6 C5 C4 120.46(18) . . ?
O5 C5 C4 113.41(16) . . ?
C5 C6 C1 119.38(17) . . ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 . . ?
O2 C7 O1 125.22(17) . . ?
O2 C7 C1 117.65(16) . . ?
O1 C7 C1 117.08(16) . . ?
O3 C8 O4 125.33(17) . . ?
O3 C8 C3 116.41(16) . . ?
O4 C8 C3 118.12(16) . . ?
O5 C9 N1 111.07(17) . . ?
O5 C9 H9A 109.4 . . ?
N1 C9 H9A 109.4 . . ?
O5 C9 H9B 109.4 . . ?
N1 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 N3 114.67(18) . . ?
N2 C10 H10 122.7 . . ?
N3 C10 H10 122.7 . . ?
N3 C11 N1 110.72(18) . . ?
N3 C11 H11 124.6 . . ?
N1 C11 H11 124.6 . . ?
N4 C12 N5 111.83(19) . . ?
N4 C12 H12 124.1 . . ?
N5 C12 H12 124.1 . . ?
C14 C13 N5 106.15(19) . . ?
C14 C13 H13 126.9 . . ?
N5 C13 H13 126.9 . . ?
C13 C14 N4 109.85(19) . . ?
C13 C14 H14 125.1 . . ?
N4 C14 H14 125.1 . . ?
N5 C15 C16 112.6(3) . . ?
N5 C15 C16' 112.1(2) . . ?
C16 C15 C16' 34.8(3) . . ?
N5 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
C16' C15 H15A 134.0 . . ?
N5 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C16' C15 H15B 77.1 . . ?
H15A C15 H15B 107.8 . . ?
C16 C16 C15 112.8(8) 7_666 . ?
C16 C16 H16A 109.0 7_666 . ?
C15 C16 H16A 109.0 . . ?
C16 C16 H16B 109.0 7_666 . ?
C15 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C16' C16' C15 112.5(6) 7_666 . ?
C16' C16' H16C 109.1 7_666 . ?
C15 C16' H16C 109.1 . . ?
C16' C16' H16D 109.1 7_666 . ?
C15 C16' H16D 109.1 . . ?
H16C C16' H16D 107.8 . . ?
C11 N1 N2 109.59(16) . . ?
C11 N1 C9 128.61(18) . . ?
N2 N1 C9 121.76(16) . . ?
C10 N2 N1 102.29(17) . . ?
C11 N3 C10 102.74(16) . . ?
C11 N3 Co1 131.60(14) . 5_767 ?
C10 N3 Co1 123.11(13) . 5_767 ?
C12 N4 C14 105.02(17) . . ?
C12 N4 Co1 123.94(14) . . ?
C14 N4 Co1 130.98(14) . . ?
C12 N5 C13 107.15(18) . . ?
C12 N5 C15 125.81(19) . . ?
C13 N5 C15 126.95(19) . . ?
C7 O1 Co1 129.85(12) . . ?
C8 O3 Co1 132.22(12) . 6_576 ?
C8 O4 Co1 138.33(13) . 6_566 ?
C5 O5 C9 120.44(16) . . ?
Co1 O1W H1A 110.1(19) . . ?
Co1 O1W H1B 121(2) . . ?
H1A O1W H1B 109(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
C6 C1 C2 C3 -0.4(3) . . . . ?
C7 C1 C2 C3 -175.24(17) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
C1 C2 C3 C8 174.90(17) . . . . ?
C2 C3 C4 C5 1.5(3) . . . . ?
C8 C3 C4 C5 -174.39(17) . . . . ?
C3 C4 C5 C6 -0.9(3) . . . . ?
C3 C4 C5 O5 178.85(17) . . . . ?
O5 C5 C6 C1 179.97(18) . . . . ?
C4 C5 C6 C1 -0.3(3) . . . . ?
C2 C1 C6 C5 1.0(3) . . . . ?
C7 C1 C6 C5 175.75(17) . . . . ?
C2 C1 C7 O2 -9.2(3) . . . . ?
C6 C1 C7 O2 175.92(18) . . . . ?
C2 C1 C7 O1 168.39(17) . . . . ?
C6 C1 C7 O1 -6.4(3) . . . . ?
C2 C3 C8 O3 -24.2(3) . . . . ?
C4 C3 C8 O3 151.55(18) . . . . ?
C2 C3 C8 O4 159.79(18) . . . . ?
C4 C3 C8 O4 -24.4(3) . . . . ?
N5 C13 C14 N4 -0.2(3) . . . . ?
N5 C15 C16 C16 61.2(9) . . . 7_666 ?
C16' C15 C16 C16 -35.4(6) . . . 7_666 ?
N5 C15 C16' C16' -63.1(7) . . . 7_666 ?
C16 C15 C16' C16' 35.2(5) . . . 7_666 ?
N3 C11 N1 N2 -0.4(2) . . . . ?
N3 C11 N1 C9 -177.71(18) . . . . ?
O5 C9 N1 C11 95.1(2) . . . . ?
O5 C9 N1 N2 -82.0(2) . . . . ?
N3 C10 N2 N1 0.0(2) . . . . ?
C11 N1 N2 C10 0.2(2) . . . . ?
C9 N1 N2 C10 177.78(18) . . . . ?
N1 C11 N3 C10 0.3(2) . . . . ?
N1 C11 N3 Co1 162.07(14) . . . 5_767 ?
N2 C10 N3 C11 -0.2(2) . . . . ?
N2 C10 N3 Co1 -163.96(14) . . . 5_767 ?
N5 C12 N4 C14 -0.4(2) . . . . ?
N5 C12 N4 Co1 177.08(13) . . . . ?
C13 C14 N4 C12 0.4(3) . . . . ?
C13 C14 N4 Co1 -176.85(15) . . . . ?
O1W Co1 N4 C12 72.00(17) . . . . ?
O3 Co1 N4 C12 -14.89(17) 6_575 . . . ?
O4 Co1 N4 C12 -122.43(17) 6_565 . . . ?
N3 Co1 N4 C12 -85.2(3) 5_767 . . . ?
O1 Co1 N4 C12 157.47(17) . . . . ?
O1W Co1 N4 C14 -111.24(19) . . . . ?
O3 Co1 N4 C14 161.88(19) 6_575 . . . ?
O4 Co1 N4 C14 54.33(19) 6_565 . . . ?
N3 Co1 N4 C14 91.5(3) 5_767 . . . ?
O1 Co1 N4 C14 -25.8(2) . . . . ?
N4 C12 N5 C13 0.3(3) . . . . ?
N4 C12 N5 C15 -176.55(19) . . . . ?
C14 C13 N5 C12 0.0(3) . . . . ?
C14 C13 N5 C15 176.8(2) . . . . ?
C16 C15 N5 C12 63.2(5) . . . . ?
C16' C15 N5 C12 101.0(4) . . . . ?
C16 C15 N5 C13 -113.0(4) . . . . ?
C16' C15 N5 C13 -75.2(4) . . . . ?
O2 C7 O1 Co1 17.0(3) . . . . ?
C1 C7 O1 Co1 -160.43(12) . . . . ?
O1W Co1 O1 C7 7.31(17) . . . . ?
N4 Co1 O1 C7 -82.87(17) . . . . ?
O3 Co1 O1 C7 55.4(3) 6_575 . . . ?
O4 Co1 O1 C7 -168.90(17) 6_565 . . . ?
N3 Co1 O1 C7 108.65(17) 5_767 . . . ?
O4 C8 O3 Co1 2.2(3) . . . 6_576 ?
C3 C8 O3 Co1 -173.50(12) . . . 6_576 ?
O3 C8 O4 Co1 133.56(18) . . . 6_566 ?
C3 C8 O4 Co1 -50.8(3) . . . 6_566 ?
C6 C5 O5 C9 0.5(3) . . . . ?
C4 C5 O5 C9 -179.15(17) . . . . ?
N1 C9 O5 C5 93.0(2) . . . . ?

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
O1W H1B O4 0.77(3) 2.34(3) 2.842(2) 124(3) 6_575

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 978487'
data_added_by_encifer
#==========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_address     
;
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       majf247@yahoo.com
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_phone       +86-431-85098620
_publ_requested_journal          CrystEngComm

#=========================END

data_Compound-2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 Mn2 N10 O12'
_chemical_formula_sum            'C32 H32 Mn2 N10 O12'
_chemical_formula_weight         858.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'C 1 2/c 1'
_symmetry_space_group_name_hall  '-C 2yc'

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                   36.364(2)
_cell_length_b                   5.3141(3)
_cell_length_c                   19.5932(11)
_cell_angle_alpha                90
_cell_angle_beta                 113.105(9)
_cell_angle_gamma                90
_cell_volume                     3482.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3827
_cell_measurement_theta_min      3.0555
_cell_measurement_theta_max      29.1103

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8118
_exptl_absorpt_correction_T_max  0.8555
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;

_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11666
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         27.10
_reflns_number_total             3792
_reflns_number_gt                2925
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_cell_refinement       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_data_reduction        
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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)+(0.0409P)²+0.2881P] 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         3792
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.127037(9) 1.15804(6) 0.677639(17) 0.02242(11) Uani 1 1 d . . .
C1 C 0.10889(6) 0.5548(4) 0.82303(11) 0.0233(5) Uani 1 1 d . . .
C2 C 0.12676(6) 0.6655(4) 0.89265(12) 0.0228(5) Uani 1 1 d . . .
H2 H 0.1435 0.8036 0.8991 0.027 Uiso 1 1 calc R . .
C3 C 0.11979(6) 0.5715(4) 0.95241(11) 0.0229(5) Uani 1 1 d . . .
C4 C 0.09416(6) 0.3661(4) 0.94272(12) 0.0238(5) Uani 1 1 d . . .
H4 H 0.0888 0.3048 0.9824 0.029 Uiso 1 1 calc R . .
C5 C 0.07680(6) 0.2550(4) 0.87334(12) 0.0240(5) Uani 1 1 d . . .
C6 C 0.08415(6) 0.3478(4) 0.81409(12) 0.0253(5) Uani 1 1 d . . .
H6 H 0.0725 0.2711 0.7679 0.030 Uiso 1 1 calc R . .
C7 C 0.11380(6) 0.6656(4) 0.75633(12) 0.0227(5) Uani 1 1 d . . .
C8 C 0.13720(6) 0.7059(4) 1.02627(12) 0.0234(5) Uani 1 1 d . . .
C9 C 0.04042(7) -0.0648(4) 0.90947(14) 0.0309(5) Uani 1 1 d . . .
H9A H 0.0616 -0.0404 0.9580 0.037 Uiso 1 1 calc R . .
H9B H 0.0372 -0.2443 0.9000 0.037 Uiso 1 1 calc R . .
C10 C -0.03528(7) 0.2900(4) 0.92881(13) 0.0327(5) Uani 1 1 d . . .
H10 H -0.0452 0.4272 0.9458 0.039 Uiso 1 1 calc R . .
C11 C -0.03361(7) -0.0459(4) 0.87493(13) 0.0310(5) Uani 1 1 d . . .
H11 H -0.0404 -0.1932 0.8471 0.037 Uiso 1 1 calc R . .
C12 C 0.20735(7) 1.1184(4) 0.81770(13) 0.0337(6) Uani 1 1 d . . .
H12 H 0.1979 0.9675 0.8287 0.040 Uiso 1 1 calc R . .
C13 C 0.24593(7) 1.4371(5) 0.82570(14) 0.0379(6) Uani 1 1 d . . .
H13 H 0.2673 1.5494 0.8418 0.046 Uiso 1 1 calc R . .
C14 C 0.21206(7) 1.4572(5) 0.76425(14) 0.0375(6) Uani 1 1 d . . .
H14 H 0.2063 1.5883 0.7302 0.045 Uiso 1 1 calc R . .
C15 C 0.27160(7) 1.1198(5) 0.93042(14) 0.0420(6) Uani 1 1 d . . .
H15A H 0.2983 1.1337 0.9311 0.050 Uiso 1 1 calc R A 1
H15B H 0.2661 0.9428 0.9341 0.050 Uiso 1 1 calc R A 1
C16 C 0.26997(18) 1.2581(17) 0.9969(3) 0.042(2) Uani 0.594(13) 1 d P . 1
H16A H 0.2903 1.1892 1.0417 0.050 Uiso 0.594(13) 1 calc PR . 1
H16B H 0.2764 1.4338 0.9938 0.050 Uiso 0.594(13) 1 calc PR . 1
C16' C 0.2550(3) 1.116(2) 0.9906(4) 0.040(3) Uani 0.406(13) 1 d P . 2
H16C H 0.2745 1.0398 1.0350 0.048 Uiso 0.406(13) 1 calc PR . 2
H16D H 0.2310 1.0138 0.9742 0.048 Uiso 0.406(13) 1 calc PR . 2
N1 N 0.00344(5) 0.0399(3) 0.90903(10) 0.0275(4) Uani 1 1 d . . .
N2 N 0.00286(6) 0.2602(4) 0.94451(11) 0.0349(5) Uani 1 1 d . . .
N3 N -0.05959(5) 0.1058(3) 0.88577(10) 0.0297(4) Uani 1 1 d . . .
N4 N 0.18739(5) 1.2574(4) 0.75905(10) 0.0315(4) Uani 1 1 d . . .
N5 N 0.24266(6) 1.2193(4) 0.85954(11) 0.0323(4) Uani 1 1 d . . .
O1 O 0.10667(4) 0.5272(3) 0.70052(8) 0.0281(3) Uani 1 1 d . . .
O2 O 0.12308(5) 0.8944(3) 0.75962(8) 0.0301(4) Uani 1 1 d . . .
O3 O 0.16172(5) 0.8766(3) 1.03277(9) 0.0373(4) Uani 1 1 d . . .
O4 O 0.12477(5) 0.6410(3) 1.07582(8) 0.0284(4) Uani 1 1 d . . .
O5 O 0.05110(5) 0.0499(3) 0.85559(9) 0.0337(4) Uani 1 1 d . . .
O1W O 0.14991(6) 0.8481(3) 0.63375(10) 0.0344(4) Uani 1 1 d . . .
H1A H 0.1383(9) 0.722(6) 0.6186(17) 0.052 Uiso 1 1 d . . .
H1B H 0.1545(8) 0.901(5) 0.5980(17) 0.052 Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1W 2.1693(16) . ?
Mn1 O2 2.1783(14) . ?
Mn1 O1 2.2041(15) 1_565 ?
Mn1 N4 2.2119(19) . ?
Mn1 O4 2.2357(14) 6_575 ?
Mn1 N3 2.2902(18) 2_566 ?
C1 C6 1.388(3) . ?
C1 C2 1.391(3) . ?
C1 C7 1.507(3) . ?
C2 C3 1.385(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.399(3) . ?
C3 C8 1.512(3) . ?
C4 C5 1.386(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(3) . ?
C5 O5 1.388(3) . ?
C6 H6 0.9300 . ?
C7 O2 1.257(2) . ?
C7 O1 1.257(2) . ?
C8 O3 1.243(3) . ?
C8 O4 1.269(2) . ?
C9 O5 1.400(3) . ?
C9 N1 1.452(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.307(3) . ?
C10 N3 1.366(3) . ?
C10 H10 0.9300 . ?
C11 N3 1.321(3) . ?
C11 N1 1.328(3) . ?
C11 H11 0.9300 . ?
C12 N4 1.318(3) . ?
C12 N5 1.335(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.347(3) . ?
C13 N5 1.362(3) . ?
C13 H13 0.9300 . ?
C14 N4 1.368(3) . ?
C14 H14 0.9300 . ?
C15 N5 1.473(3) . ?
C15 C16' 1.520(9) . ?
C15 C16 1.517(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C16 1.507(13) 7_577 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16' C16' 1.547(18) 7_577 ?
C16' H16C 0.9700 . ?
C16' H16D 0.9700 . ?
N1 N2 1.366(3) . ?
N3 Mn1 2.2902(18) 2_546 ?
O1 Mn1 2.2041(15) 1_545 ?
O4 Mn1 2.2357(14) 6_576 ?
O1W H1A 0.79(3) . ?
O1W H1B 0.83(3) . ?

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
O1W Mn1 O2 87.17(6) . . ?
O1W Mn1 O1 165.50(6) . 1_565 ?
O2 Mn1 O1 107.31(5) . 1_565 ?
O1W Mn1 N4 92.34(7) . . ?
O2 Mn1 N4 87.46(7) . . ?
O1 Mn1 N4 87.62(7) 1_565 . ?
O1W Mn1 O4 83.96(6) . 6_575 ?
O2 Mn1 O4 167.24(6) . 6_575 ?
O1 Mn1 O4 81.87(5) 1_565 6_575 ?
N4 Mn1 O4 102.02(7) . 6_575 ?
O1W Mn1 N3 100.86(7) . 2_566 ?
O2 Mn1 N3 87.44(6) . 2_566 ?
O1 Mn1 N3 81.05(6) 1_565 2_566 ?
N4 Mn1 N3 165.59(7) . 2_566 ?
O4 Mn1 N3 85.25(6) 6_575 2_566 ?
C6 C1 C2 119.31(18) . . ?
C6 C1 C7 119.46(18) . . ?
C2 C1 C7 121.11(18) . . ?
C3 C2 C1 120.43(19) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 119.99(19) . . ?
C2 C3 C8 119.47(19) . . ?
C4 C3 C8 120.32(18) . . ?
C5 C4 C3 119.24(19) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 120.55(19) . . ?
C6 C5 O5 113.78(18) . . ?
C4 C5 O5 125.67(18) . . ?
C5 C6 C1 120.46(19) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O2 C7 O1 124.76(18) . . ?
O2 C7 C1 117.02(18) . . ?
O1 C7 C1 118.14(18) . . ?
O3 C8 O4 125.22(19) . . ?
O3 C8 C3 117.19(18) . . ?
O4 C8 C3 117.56(18) . . ?
O5 C9 N1 111.04(18) . . ?
O5 C9 H9A 109.4 . . ?
N1 C9 H9A 109.4 . . ?
O5 C9 H9B 109.4 . . ?
N1 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 N3 115.4(2) . . ?
N2 C10 H10 122.3 . . ?
N3 C10 H10 122.3 . . ?
N3 C11 N1 111.0(2) . . ?
N3 C11 H11 124.5 . . ?
N1 C11 H11 124.5 . . ?
N4 C12 N5 112.2(2) . . ?
N4 C12 H12 123.9 . . ?
N5 C12 H12 123.9 . . ?
C14 C13 N5 106.2(2) . . ?
C14 C13 H13 126.9 . . ?
N5 C13 H13 126.9 . . ?
C13 C14 N4 110.4(2) . . ?
C13 C14 H14 124.8 . . ?
N4 C14 H14 124.8 . . ?
N5 C15 C16' 112.4(3) . . ?
N5 C15 C16 112.4(3) . . ?
C16' C15 C16 34.8(3) . . ?
N5 C15 H15A 109.1 . . ?
C16' C15 H15A 133.6 . . ?
C16 C15 H15A 109.1 . . ?
N5 C15 H15B 109.1 . . ?
C16' C15 H15B 77.0 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C16 C16 C15 113.9(8) 7_577 . ?
C16 C16 H16A 108.8 7_577 . ?
C15 C16 H16A 108.8 . . ?
C16 C16 H16B 108.8 7_577 . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C15 C16' C16' 112.1(11) . 7_577 ?
C15 C16' H16C 109.2 . . ?
C16' C16' H16C 109.2 7_577 . ?
C15 C16' H16D 109.2 . . ?
C16' C16' H16D 109.2 7_577 . ?
H16C C16' H16D 107.9 . . ?
C11 N1 N2 109.56(17) . . ?
C11 N1 C9 128.77(19) . . ?
N2 N1 C9 121.64(18) . . ?
C10 N2 N1 102.20(18) . . ?
C11 N3 C10 101.91(19) . . ?
C11 N3 Mn1 131.91(16) . 2_546 ?
C10 N3 Mn1 122.95(15) . 2_546 ?
C12 N4 C14 104.45(19) . . ?
C12 N4 Mn1 123.08(15) . . ?
C14 N4 Mn1 132.46(15) . . ?
C12 N5 C13 106.8(2) . . ?
C12 N5 C15 126.4(2) . . ?
C13 N5 C15 126.7(2) . . ?
C7 O1 Mn1 136.58(14) . 1_545 ?
C7 O2 Mn1 132.72(13) . . ?
C8 O4 Mn1 130.78(13) . 6_576 ?
C5 O5 C9 120.78(17) . . ?
Mn1 O1W H1A 124(2) . . ?
Mn1 O1W H1B 108.4(19) . . ?
H1A O1W H1B 103(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
C6 C1 C2 C3 -0.4(3) . . . . ?
C7 C1 C2 C3 175.63(19) . . . . ?
C1 C2 C3 C4 -0.9(3) . . . . ?
C1 C2 C3 C8 -175.72(18) . . . . ?
C2 C3 C4 C5 1.6(3) . . . . ?
C8 C3 C4 C5 176.37(19) . . . . ?
C3 C4 C5 C6 -1.0(3) . . . . ?
C3 C4 C5 O5 179.54(19) . . . . ?
C4 C5 C6 C1 -0.4(3) . . . . ?
O5 C5 C6 C1 179.17(18) . . . . ?
C2 C1 C6 C5 1.1(3) . . . . ?
C7 C1 C6 C5 -175.04(19) . . . . ?
C6 C1 C7 O2 154.1(2) . . . . ?
C2 C1 C7 O2 -22.0(3) . . . . ?
C6 C1 C7 O1 -22.9(3) . . . . ?
C2 C1 C7 O1 161.11(19) . . . . ?
C2 C3 C8 O3 -9.7(3) . . . . ?
C4 C3 C8 O3 175.55(19) . . . . ?
C2 C3 C8 O4 168.26(19) . . . . ?
C4 C3 C8 O4 -6.5(3) . . . . ?
N5 C13 C14 N4 0.5(3) . . . . ?
N5 C15 C16 C16 60.7(9) . . . 7_577 ?
C16' C15 C16 C16 -36.7(7) . . . 7_577 ?
N5 C15 C16' C16' -62.4(12) . . . 7_577 ?
C16 C15 C16' C16' 35.0(8) . . . 7_577 ?
N3 C11 N1 N2 -0.2(3) . . . . ?
N3 C11 N1 C9 -178.0(2) . . . . ?
O5 C9 N1 C11 95.7(3) . . . . ?
O5 C9 N1 N2 -81.8(3) . . . . ?
N3 C10 N2 N1 0.0(3) . . . . ?
C11 N1 N2 C10 0.1(2) . . . . ?
C9 N1 N2 C10 178.1(2) . . . . ?
N1 C11 N3 C10 0.2(3) . . . . ?
N1 C11 N3 Mn1 159.64(15) . . . 2_546 ?
N2 C10 N3 C11 -0.1(3) . . . . ?
N2 C10 N3 Mn1 -161.97(16) . . . 2_546 ?
N5 C12 N4 C14 0.6(3) . . . . ?
N5 C12 N4 Mn1 -178.55(15) . . . . ?
C13 C14 N4 C12 -0.7(3) . . . . ?
C13 C14 N4 Mn1 178.36(17) . . . . ?
O1W Mn1 N4 C12 -71.36(19) . . . . ?
O2 Mn1 N4 C12 15.70(19) . . . . ?
O1 Mn1 N4 C12 123.15(19) 1_565 . . . ?
O4 Mn1 N4 C12 -155.68(18) 6_575 . . . ?
N3 Mn1 N4 C12 85.1(3) 2_566 . . . ?
O1W Mn1 N4 C14 109.8(2) . . . . ?
O2 Mn1 N4 C14 -163.2(2) . . . . ?
O1 Mn1 N4 C14 -55.7(2) 1_565 . . . ?
O4 Mn1 N4 C14 25.5(2) 6_575 . . . ?
N3 Mn1 N4 C14 -93.8(3) 2_566 . . . ?
N4 C12 N5 C13 -0.3(3) . . . . ?
N4 C12 N5 C15 177.1(2) . . . . ?
C14 C13 N5 C12 -0.1(3) . . . . ?
C14 C13 N5 C15 -177.5(2) . . . . ?
C16' C15 N5 C12 -63.3(6) . . . . ?
C16 C15 N5 C12 -101.1(4) . . . . ?
C16' C15 N5 C13 113.6(6) . . . . ?
C16 C15 N5 C13 75.8(5) . . . . ?
O2 C7 O1 Mn1 128.6(2) . . . 1_545 ?
C1 C7 O1 Mn1 -54.7(3) . . . 1_545 ?
O1 C7 O2 Mn1 5.1(3) . . . . ?
C1 C7 O2 Mn1 -171.59(14) . . . . ?
O1W Mn1 O2 C7 -37.18(19) . . . . ?
O1 Mn1 O2 C7 143.64(19) 1_565 . . . ?
N4 Mn1 O2 C7 -129.6(2) . . . . ?
O4 Mn1 O2 C7 8.7(4) 6_575 . . . ?
N3 Mn1 O2 C7 63.84(19) 2_566 . . . ?
O3 C8 O4 Mn1 17.3(3) . . . 6_576 ?
C3 C8 O4 Mn1 -160.43(13) . . . 6_576 ?
C6 C5 O5 C9 -179.53(19) . . . . ?
C4 C5 O5 C9 0.0(3) . . . . ?
N1 C9 O5 C5 93.4(2) . . . . ?

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
O1W H1A O1 0.79(3) 2.53(3) 2.951(2) 115(3) .
O1W H1B O3 0.83(3) 1.83(3) 2.628(2) 159(3) 6_575

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.062
_database_code_depnum_ccdc_archive 'CCDC 978488'
data_added_by_encifer
#==========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_address     
;
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       majf247@yahoo.com
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_phone       +86-431-85098620
_publ_requested_journal          CrystEngComm

#=========================END

data_Compound-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H38 Mn2 N12 O10'
_chemical_formula_sum            'C36 H38 Mn2 N12 O10'
_chemical_formula_weight         908.66

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

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

_cell_length_a                   8.9623(13)
_cell_length_b                   10.1747(11)
_cell_length_c                   12.1422(10)
_cell_angle_alpha                100.966(9)
_cell_angle_beta                 110.157(11)
_cell_angle_gamma                103.494(11)
_cell_volume                     965.28(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2955
_cell_measurement_theta_min      3.0939
_cell_measurement_theta_max      29.1451

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             468
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8109
_exptl_absorpt_correction_T_max  0.8679
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;

_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6871
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.10
_reflns_number_total             4130
_reflns_number_gt                3404
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_cell_refinement       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_data_reduction        
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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)+(0.0328P)²+0.0340P] 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         4130
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.16203(4) 0.36217(3) 0.01972(3) 0.02578(11) Uani 1 1 d . . .
C1 C 0.3820(2) 0.06533(19) 0.10827(17) 0.0247(4) Uani 1 1 d . . .
C2 C 0.2789(2) -0.06948(19) 0.08628(17) 0.0259(4) Uani 1 1 d . . .
H2 H 0.1628 -0.0904 0.0533 0.031 Uiso 1 1 calc R . .
C3 C 0.3489(2) -0.17397(18) 0.11350(17) 0.0236(4) Uani 1 1 d . . .
C4 C 0.5214(2) -0.14156(19) 0.16517(17) 0.0253(4) Uani 1 1 d . . .
H4 H 0.5686 -0.2122 0.1795 0.030 Uiso 1 1 calc R . .
C5 C 0.6239(2) -0.0037(2) 0.19551(17) 0.0246(4) Uani 1 1 d . . .
C6 C 0.5559(2) 0.09970(19) 0.16543(18) 0.0264(4) Uani 1 1 d . . .
H6 H 0.6254 0.1914 0.1831 0.032 Uiso 1 1 calc R . .
C7 C 0.3046(2) 0.1742(2) 0.07096(18) 0.0269(4) Uani 1 1 d . . .
C8 C 0.2374(2) -0.32066(19) 0.09051(17) 0.0250(4) Uani 1 1 d . . .
C9 C 0.8936(3) 0.1511(2) 0.34093(19) 0.0368(5) Uani 1 1 d . . .
H9A H 0.9849 0.1401 0.4063 0.044 Uiso 1 1 calc R . .
H9B H 0.8269 0.1909 0.3771 0.044 Uiso 1 1 calc R . .
C10 C 1.0436(3) 0.4356(2) 0.2464(2) 0.0403(5) Uani 1 1 d . . .
H10 H 1.0670 0.5300 0.2474 0.048 Uiso 1 1 calc R . .
C11 C 1.0273(3) 0.2240(2) 0.2019(2) 0.0359(5) Uani 1 1 d . . .
H11 H 1.0342 0.1368 0.1680 0.043 Uiso 1 1 calc R . .
C12 C 0.0871(3) 0.2500(2) -0.2667(2) 0.0414(6) Uani 1 1 d . . .
H12 H -0.0005 0.1731 -0.2753 0.050 Uiso 1 1 calc R . .
C13 C 0.2934(3) 0.4350(2) -0.18595(19) 0.0307(5) Uani 1 1 d . . .
H13 H 0.3810 0.5153 -0.1303 0.037 Uiso 1 1 calc R . .
C14 C 0.3374(3) 0.4585(3) -0.3757(2) 0.0470(6) Uani 1 1 d . . .
H14A H 0.3825 0.5602 -0.3378 0.056 Uiso 1 1 calc R . .
H14B H 0.2551 0.4400 -0.4584 0.056 Uiso 1 1 calc R . .
C15 C 0.4779(3) 0.4038(3) -0.3821(2) 0.0486(6) Uani 1 1 d . . .
H15A H 0.5422 0.4641 -0.4142 0.058 Uiso 1 1 calc R . .
H15B H 0.5524 0.4126 -0.2992 0.058 Uiso 1 1 calc R . .
C16 C 0.4250(4) 0.2533(3) -0.4590(2) 0.0588(7) Uani 1 1 d . . .
H16A H 0.3544 0.2440 -0.5431 0.071 Uiso 1 1 calc R . .
H16B H 0.3589 0.1920 -0.4288 0.071 Uiso 1 1 calc R . .
C17 C 0.5755(4) 0.2057(3) -0.4571(3) 0.0716(9) Uani 1 1 d . . .
H17A H 0.6381 0.2655 -0.4905 0.086 Uiso 1 1 calc R . .
H17B H 0.6487 0.2213 -0.3722 0.086 Uiso 1 1 calc R . .
C18 C 0.5340(4) 0.0526(3) -0.5273(3) 0.0763(10) Uani 1 1 d . . .
H18A H 0.4527 0.0342 -0.6103 0.092 Uiso 1 1 calc R . .
H18B H 0.6352 0.0390 -0.5327 0.092 Uiso 1 1 calc R . .
N1 N 0.9624(2) 0.24761(17) 0.28288(15) 0.0299(4) Uani 1 1 d . . .
N2 N 0.9717(3) 0.38551(19) 0.31369(18) 0.0430(5) Uani 1 1 d . . .
N3 N 1.0815(2) 0.34124(18) 0.17546(16) 0.0343(4) Uani 1 1 d . . .
N4 N 0.1902(2) 0.34660(17) -0.15709(15) 0.0311(4) Uani 1 1 d . . .
N5 N 0.1196(3) 0.2724(2) -0.36012(18) 0.0467(5) Uani 1 1 d . . .
N6 N 0.2543(2) 0.39305(19) -0.30547(16) 0.0360(4) Uani 1 1 d . . .
O1 O 0.39402(17) 0.30249(14) 0.11182(13) 0.0348(3) Uani 1 1 d . . .
O2 O 0.15144(17) 0.13519(14) 0.00094(13) 0.0321(3) Uani 1 1 d . . .
O3 O 0.09352(17) -0.33576(14) 0.08777(13) 0.0342(3) Uani 1 1 d . . .
O4 O 0.29839(17) -0.41943(13) 0.07976(13) 0.0328(3) Uani 1 1 d . . .
O5 O 0.79402(17) 0.01929(14) 0.25638(14) 0.0348(3) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 2.1131(13) 1_565 ?
Mn1 O3 2.1308(14) 2 ?
Mn1 N4 2.2271(17) . ?
Mn1 O2 2.2533(13) . ?
Mn1 N3 2.2727(17) 1_455 ?
Mn1 O1 2.2775(14) . ?
Mn1 C7 2.5932(19) . ?
C1 C2 1.380(3) . ?
C1 C6 1.394(3) . ?
C1 C7 1.498(3) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(3) . ?
C3 C8 1.503(2) . ?
C4 C5 1.384(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(3) . ?
C5 O5 1.384(2) . ?
C6 H6 0.9300 . ?
C7 O2 1.256(2) . ?
C7 O1 1.259(2) . ?
C8 O3 1.250(2) . ?
C8 O4 1.258(2) . ?
C9 O5 1.391(2) . ?
C9 N1 1.457(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.309(3) . ?
C10 N3 1.348(3) . ?
C10 H10 0.9300 . ?
C11 N1 1.316(3) . ?
C11 N3 1.321(2) . ?
C11 H11 0.9300 . ?
C12 N5 1.311(3) . ?
C12 N4 1.350(3) . ?
C12 H12 0.9300 . ?
C13 N4 1.320(2) . ?
C13 N6 1.325(3) . ?
C13 H13 0.9300 . ?
C14 N6 1.465(3) . ?
C14 C15 1.510(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.501(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.530(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.516(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C18 1.483(5) 2_654 ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
N1 N2 1.356(2) . ?
N3 Mn1 2.2727(17) 1_655 ?
N5 N6 1.361(3) . ?
O3 Mn1 2.1308(14) 2 ?
O4 Mn1 2.1132(13) 1_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
O4 Mn1 O3 107.70(5) 1_565 2 ?
O4 Mn1 N4 89.08(6) 1_565 . ?
O3 Mn1 N4 84.34(6) 2 . ?
O4 Mn1 O2 151.14(5) 1_565 . ?
O3 Mn1 O2 100.95(5) 2 . ?
N4 Mn1 O2 90.42(6) . . ?
O4 Mn1 N3 101.13(6) 1_565 1_455 ?
O3 Mn1 N3 86.50(6) 2 1_455 ?
N4 Mn1 N3 167.99(6) . 1_455 ?
O2 Mn1 N3 83.70(6) . 1_455 ?
O4 Mn1 O1 93.33(5) 1_565 . ?
O3 Mn1 O1 158.92(5) 2 . ?
N4 Mn1 O1 94.99(6) . . ?
O2 Mn1 O1 57.97(5) . . ?
N3 Mn1 O1 90.77(6) 1_455 . ?
O4 Mn1 C7 122.36(6) 1_565 . ?
O3 Mn1 C7 129.90(6) 2 . ?
N4 Mn1 C7 94.19(6) . . ?
O2 Mn1 C7 28.97(5) . . ?
N3 Mn1 C7 85.74(6) 1_455 . ?
O1 Mn1 C7 29.03(5) . . ?
C2 C1 C6 120.20(17) . . ?
C2 C1 C7 119.26(17) . . ?
C6 C1 C7 120.54(17) . . ?
C1 C2 C3 119.89(18) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 119.86(17) . . ?
C4 C3 C8 119.98(16) . . ?
C2 C3 C8 120.13(17) . . ?
C3 C4 C5 119.86(17) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.60(18) . . ?
C6 C5 O5 124.37(17) . . ?
C4 C5 O5 115.03(16) . . ?
C5 C6 C1 119.31(17) . . ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 . . ?
O2 C7 O1 121.63(17) . . ?
O2 C7 C1 119.11(17) . . ?
O1 C7 C1 119.25(18) . . ?
O2 C7 Mn1 60.33(9) . . ?
O1 C7 Mn1 61.43(10) . . ?
C1 C7 Mn1 175.51(14) . . ?
O3 C8 O4 124.52(17) . . ?
O3 C8 C3 118.27(17) . . ?
O4 C8 C3 117.16(17) . . ?
O5 C9 N1 111.20(17) . . ?
O5 C9 H9A 109.4 . . ?
N1 C9 H9A 109.4 . . ?
O5 C9 H9B 109.4 . . ?
N1 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 N3 115.43(19) . . ?
N2 C10 H10 122.3 . . ?
N3 C10 H10 122.3 . . ?
N1 C11 N3 110.67(18) . . ?
N1 C11 H11 124.7 . . ?
N3 C11 H11 124.7 . . ?
N5 C12 N4 115.1(2) . . ?
N5 C12 H12 122.5 . . ?
N4 C12 H12 122.5 . . ?
N4 C13 N6 110.28(19) . . ?
N4 C13 H13 124.9 . . ?
N6 C13 H13 124.9 . . ?
N6 C14 C15 112.43(18) . . ?
N6 C14 H14A 109.1 . . ?
C15 C14 H14A 109.1 . . ?
N6 C14 H14B 109.1 . . ?
C15 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
C16 C15 C14 115.8(2) . . ?
C16 C15 H15A 108.3 . . ?
C14 C15 H15A 108.3 . . ?
C16 C15 H15B 108.3 . . ?
C14 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
C15 C16 C17 112.2(2) . . ?
C15 C16 H16A 109.2 . . ?
C17 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
C17 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C18 C17 C16 115.8(3) . . ?
C18 C17 H17A 108.3 . . ?
C16 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
C16 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C18 C18 C17 114.7(3) 2_654 . ?
C18 C18 H18A 108.6 2_654 . ?
C17 C18 H18A 108.6 . . ?
C18 C18 H18B 108.6 2_654 . ?
C17 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C11 N1 N2 109.96(16) . . ?
C11 N1 C9 129.48(18) . . ?
N2 N1 C9 120.52(18) . . ?
C10 N2 N1 101.86(17) . . ?
C11 N3 C10 102.08(17) . . ?
C11 N3 Mn1 127.43(14) . 1_655 ?
C10 N3 Mn1 129.24(14) . 1_655 ?
C13 N4 C12 102.70(17) . . ?
C13 N4 Mn1 130.15(14) . . ?
C12 N4 Mn1 126.64(14) . . ?
C12 N5 N6 102.07(18) . . ?
C13 N6 N5 109.87(17) . . ?
C13 N6 C14 128.35(19) . . ?
N5 N6 C14 121.77(18) . . ?
C7 O1 Mn1 89.53(12) . . ?
C7 O2 Mn1 90.70(11) . . ?
C8 O3 Mn1 146.78(14) . 2 ?
C8 O4 Mn1 125.54(13) . 1_545 ?
C5 O5 C9 118.09(16) . . ?

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
C6 C1 C2 C3 -4.4(3) . . . . ?
C7 C1 C2 C3 176.06(17) . . . . ?
C1 C2 C3 C4 1.6(3) . . . . ?
C1 C2 C3 C8 179.61(17) . . . . ?
C2 C3 C4 C5 3.3(3) . . . . ?
C8 C3 C4 C5 -174.73(17) . . . . ?
C3 C4 C5 C6 -5.4(3) . . . . ?
C3 C4 C5 O5 174.61(17) . . . . ?
C4 C5 C6 C1 2.5(3) . . . . ?
O5 C5 C6 C1 -177.49(17) . . . . ?
C2 C1 C6 C5 2.4(3) . . . . ?
C7 C1 C6 C5 -178.09(17) . . . . ?
C2 C1 C7 O2 -13.0(3) . . . . ?
C6 C1 C7 O2 167.49(18) . . . . ?
C2 C1 C7 O1 166.01(18) . . . . ?
C6 C1 C7 O1 -13.5(3) . . . . ?
C2 C1 C7 Mn1 68.5(19) . . . . ?
C6 C1 C7 Mn1 -111.0(18) . . . . ?
O4 Mn1 C7 O2 -174.84(10) 1_565 . . . ?
O3 Mn1 C7 O2 2.84(14) 2 . . . ?
N4 Mn1 C7 O2 -83.28(12) . . . . ?
N3 Mn1 C7 O2 84.68(12) 1_455 . . . ?
O1 Mn1 C7 O2 -176.01(19) . . . . ?
O4 Mn1 C7 O1 1.18(14) 1_565 . . . ?
O3 Mn1 C7 O1 178.85(10) 2 . . . ?
N4 Mn1 C7 O1 92.74(12) . . . . ?
O2 Mn1 C7 O1 176.01(19) . . . . ?
N3 Mn1 C7 O1 -99.31(12) 1_455 . . . ?
O4 Mn1 C7 C1 101.2(18) 1_565 . . . ?
O3 Mn1 C7 C1 -81.1(19) 2 . . . ?
N4 Mn1 C7 C1 -167.3(18) . . . . ?
O2 Mn1 C7 C1 -84.0(18) . . . . ?
N3 Mn1 C7 C1 0.7(18) 1_455 . . . ?
O1 Mn1 C7 C1 100.0(19) . . . . ?
C4 C3 C8 O3 154.07(18) . . . . ?
C2 C3 C8 O3 -24.0(3) . . . . ?
C4 C3 C8 O4 -23.4(3) . . . . ?
C2 C3 C8 O4 158.54(17) . . . . ?
N6 C14 C15 C16 69.8(3) . . . . ?
C14 C15 C16 C17 -178.2(2) . . . . ?
C15 C16 C17 C18 177.1(2) . . . . ?
C16 C17 C18 C18 -68.8(5) . . . 2_654 ?
N3 C11 N1 N2 0.0(2) . . . . ?
N3 C11 N1 C9 -177.67(18) . . . . ?
O5 C9 N1 C11 -42.5(3) . . . . ?
O5 C9 N1 N2 140.02(19) . . . . ?
N3 C10 N2 N1 -0.2(3) . . . . ?
C11 N1 N2 C10 0.1(2) . . . . ?
C9 N1 N2 C10 178.02(18) . . . . ?
N1 C11 N3 C10 -0.1(2) . . . . ?
N1 C11 N3 Mn1 -168.15(13) . . . 1_655 ?
N2 C10 N3 C11 0.2(3) . . . . ?
N2 C10 N3 Mn1 167.94(15) . . . 1_655 ?
N6 C13 N4 C12 -0.2(2) . . . . ?
N6 C13 N4 Mn1 -172.34(13) . . . . ?
N5 C12 N4 C13 0.1(3) . . . . ?
N5 C12 N4 Mn1 172.59(15) . . . . ?
O4 Mn1 N4 C13 16.16(17) 1_565 . . . ?
O3 Mn1 N4 C13 124.05(17) 2 . . . ?
O2 Mn1 N4 C13 -134.98(17) . . . . ?
N3 Mn1 N4 C13 164.5(2) 1_455 . . . ?
O1 Mn1 N4 C13 -77.10(17) . . . . ?
C7 Mn1 N4 C13 -106.22(17) . . . . ?
O4 Mn1 N4 C12 -154.21(17) 1_565 . . . ?
O3 Mn1 N4 C12 -46.32(17) 2 . . . ?
O2 Mn1 N4 C12 54.65(17) . . . . ?
N3 Mn1 N4 C12 -5.8(4) 1_455 . . . ?
O1 Mn1 N4 C12 112.52(17) . . . . ?
C7 Mn1 N4 C12 83.40(17) . . . . ?
N4 C12 N5 N6 0.1(3) . . . . ?
N4 C13 N6 N5 0.3(2) . . . . ?
N4 C13 N6 C14 -178.94(19) . . . . ?
C12 N5 N6 C13 -0.2(2) . . . . ?
C12 N5 N6 C14 179.1(2) . . . . ?
C15 C14 N6 C13 89.1(3) . . . . ?
C15 C14 N6 N5 -90.1(3) . . . . ?
O2 C7 O1 Mn1 4.07(19) . . . . ?
C1 C7 O1 Mn1 -174.93(16) . . . . ?
O4 Mn1 O1 C7 -179.01(12) 1_565 . . . ?
O3 Mn1 O1 C7 -2.4(2) 2 . . . ?
N4 Mn1 O1 C7 -89.64(12) . . . . ?
O2 Mn1 O1 C7 -2.28(11) . . . . ?
N3 Mn1 O1 C7 79.80(12) 1_455 . . . ?
O1 C7 O2 Mn1 -4.1(2) . . . . ?
C1 C7 O2 Mn1 174.89(15) . . . . ?
O4 Mn1 O2 C7 9.06(18) 1_565 . . . ?
O3 Mn1 O2 C7 -177.78(11) 2 . . . ?
N4 Mn1 O2 C7 97.90(12) . . . . ?
N3 Mn1 O2 C7 -92.59(12) 1_455 . . . ?
O1 Mn1 O2 C7 2.28(11) . . . . ?
O4 C8 O3 Mn1 -97.5(3) . . . 2 ?
C3 C8 O3 Mn1 85.2(3) . . . 2 ?
O3 C8 O4 Mn1 13.0(3) . . . 1_545 ?
C3 C8 O4 Mn1 -169.69(12) . . . 1_545 ?
C6 C5 O5 C9 31.7(3) . . . . ?
C4 C5 O5 C9 -148.32(17) . . . . ?
N1 C9 O5 C5 -91.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.054
_database_code_depnum_ccdc_archive 'CCDC 978489'
data_added_by_encifer
#==========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_address     
;
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       majf247@yahoo.com
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_phone       +86-431-85098620
_publ_requested_journal          CrystEngComm

#=========================END

data_Compound-4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 N10 Ni2 O12, 4H2O'
_chemical_formula_sum            'C32 H40 N10 Ni2 O16'
_chemical_formula_weight         938.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

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

_cell_length_a                   9.2436(5)
_cell_length_b                   11.0384(5)
_cell_length_c                   22.7044(9)
_cell_angle_alpha                91.226(4)
_cell_angle_beta                 91.585(4)
_cell_angle_gamma                113.366(5)
_cell_volume                     2124.51(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5343
_cell_measurement_theta_min      3.0135
_cell_measurement_theta_max      29.1851

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             972
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7606
_exptl_absorpt_correction_T_max  0.7944
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;

_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15201
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.10
_reflns_number_total             9124
_reflns_number_gt                6630
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_cell_refinement       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_data_reduction        
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.
H atoms of O1W, O2W and O3W were refined isotropically with 
distance restraints of O---H = 0.85+-0.01 Å. 
The distances of H1A...H1B, H2A...H2B and H3A...H3B were restrained to 1.44+-0.01 Å
;

_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)+(0.1013P)²+1.2355P] 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         9124
_refine_ls_number_parameters     590
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1915
_refine_ls_wR_factor_gt          0.1687
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.006
_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
Ni1 Ni 0.64983(6) 0.80520(5) 0.76005(2) 0.03488(17) Uani 1 1 d . . .
Ni2 Ni 0.0000 0.0000 0.5000 0.03040(19) Uani 1 2 d S . .
Ni3 Ni 0.5000 0.0000 1.0000 0.02956(19) Uani 1 2 d S . .
C1 C 0.5667(5) 0.5490(4) 0.62653(18) 0.0331(9) Uani 1 1 d . . .
C2 C 0.4161(5) 0.4503(4) 0.61682(18) 0.0322(9) Uani 1 1 d . . .
H2 H 0.3345 0.4482 0.6404 0.039 Uiso 1 1 calc R . .
C3 C 0.3879(4) 0.3554(4) 0.57218(18) 0.0307(8) Uani 1 1 d . . .
C4 C 0.5095(5) 0.3584(4) 0.53684(19) 0.0331(9) Uani 1 1 d . . .
H4 H 0.4908 0.2952 0.5066 0.040 Uiso 1 1 calc R . .
C5 C 0.6587(4) 0.4562(4) 0.54711(19) 0.0334(9) Uani 1 1 d . . .
C6 C 0.6871(5) 0.5515(4) 0.59189(18) 0.0337(9) Uani 1 1 d . . .
H6 H 0.7878 0.6171 0.5984 0.040 Uiso 1 1 calc R . .
C7 C 0.5951(5) 0.6511(4) 0.67478(19) 0.0367(9) Uani 1 1 d . . .
C8 C 0.2246(5) 0.2457(4) 0.5635(2) 0.0349(9) Uani 1 1 d . . .
C9 C 0.7737(5) 0.3901(4) 0.4640(2) 0.0388(10) Uani 1 1 d . . .
H9A H 0.8569 0.4371 0.4377 0.047 Uiso 1 1 calc R . .
H9B H 0.6735 0.3737 0.4438 0.047 Uiso 1 1 calc R . .
C10 C 0.7072(5) 0.0652(4) 0.4948(3) 0.0515(13) Uani 1 1 d . . .
H10 H 0.6442 -0.0219 0.5027 0.062 Uiso 1 1 calc R . .
C11 C 0.9059(5) 0.2355(4) 0.48091(19) 0.0353(9) Uani 1 1 d . . .
H11 H 1.0092 0.2954 0.4766 0.042 Uiso 1 1 calc R . .
C12 C 0.4831(5) 0.5499(4) 0.88479(18) 0.0317(8) Uani 1 1 d . . .
C13 C 0.5309(4) 0.4465(4) 0.89029(18) 0.0309(8) Uani 1 1 d . . .
H13 H 0.6111 0.4426 0.8674 0.037 Uiso 1 1 calc R . .
C14 C 0.4587(4) 0.3483(4) 0.93010(18) 0.0301(8) Uani 1 1 d . . .
C15 C 0.3382(4) 0.3539(4) 0.96363(18) 0.0321(9) Uani 1 1 d . . .
H15 H 0.2915 0.2898 0.9910 0.039 Uiso 1 1 calc R . .
C16 C 0.2880(4) 0.4545(4) 0.95626(19) 0.0334(9) Uani 1 1 d . . .
C17 C 0.3598(5) 0.5530(4) 0.91706(19) 0.0349(9) Uani 1 1 d . . .
H17 H 0.3252 0.6208 0.9124 0.042 Uiso 1 1 calc R . .
C18 C 0.5599(5) 0.6565(4) 0.84253(19) 0.0354(9) Uani 1 1 d . . .
C19 C 0.5037(5) 0.2320(4) 0.9344(2) 0.0338(9) Uani 1 1 d . . .
C20 C 0.1019(5) 0.3895(4) 1.0347(2) 0.0415(10) Uani 1 1 d . . .
H20A H 0.0625 0.4375 1.0617 0.050 Uiso 1 1 calc R . .
H20B H 0.1854 0.3733 1.0553 0.050 Uiso 1 1 calc R . .
C21 C -0.1413(6) 0.0638(5) 1.0008(3) 0.073(2) Uani 1 1 d . . .
H21 H -0.1613 -0.0248 0.9938 0.088 Uiso 1 1 calc R . .
C22 C -0.1779(5) 0.2341(4) 1.0130(2) 0.0446(11) Uani 1 1 d . . .
H22 H -0.2238 0.2950 1.0173 0.054 Uiso 1 1 calc R . .
C23 C 0.9180(6) 1.0681(5) 0.7829(2) 0.0530(12) Uani 1 1 d . . .
H23 H 0.8779 1.1064 0.7541 0.064 Uiso 1 1 calc R . .
C24 C 1.0725(9) 1.0451(7) 0.8504(3) 0.112(3) Uani 1 1 d . . .
H24 H 1.1571 1.0599 0.8768 0.135 Uiso 1 1 calc R . .
C25 C 0.9449(10) 0.9316(7) 0.8401(3) 0.118(4) Uani 1 1 d . . .
H25 H 0.9254 0.8545 0.8602 0.141 Uiso 1 1 calc R . .
C26 C 1.1613(6) 1.2706(5) 0.8075(3) 0.0581(14) Uani 1 1 d . . .
H26A H 1.2309 1.2987 0.8424 0.070 Uiso 1 1 calc R . .
H26B H 1.1017 1.3257 0.8056 0.070 Uiso 1 1 calc R . .
C27 C 1.2595(6) 1.2932(6) 0.7545(3) 0.0624(14) Uani 1 1 d . B .
H27A H 1.3246 1.3869 0.7534 0.075 Uiso 1 1 calc R . .
H27B H 1.1894 1.2696 0.7197 0.075 Uiso 1 1 calc R . .
C28 C 1.3652(9) 1.2195(9) 0.7507(3) 0.097(2) Uani 1 1 d . . .
H28A H 1.4539 1.2674 0.7776 0.116 Uiso 1 1 calc R A 1
H28B H 1.3075 1.1359 0.7687 0.116 Uiso 1 1 calc R A 1
C29 C 1.429(3) 1.188(3) 0.7034(11) 0.112(13) Uani 0.310(17) 1 d P B 1
H29A H 1.5336 1.2571 0.6994 0.134 Uiso 0.310(17) 1 calc PR B 1
H29B H 1.3662 1.1890 0.6687 0.134 Uiso 0.310(17) 1 calc PR B 1
C29' C 1.3031(13) 1.1056(10) 0.7171(5) 0.077(4) Uani 0.690(17) 1 d P B 2
H29C H 1.2573 1.1205 0.6804 0.092 Uiso 0.690(17) 1 calc PR B 2
H29D H 1.2211 1.0381 0.7379 0.092 Uiso 0.690(17) 1 calc PR B 2
C30 C 1.4770(9) 0.9817(7) 0.7418(3) 0.079(2) Uani 1 1 d . B .
H30 H 1.4354 0.9649 0.7790 0.095 Uiso 1 1 calc R . .
C31 C 1.6035(11) 0.9804(7) 0.6663(3) 0.097(2) Uani 1 1 d . B .
H31 H 1.6686 0.9621 0.6402 0.116 Uiso 1 1 calc R . .
C32 C 1.5255(13) 1.0577(9) 0.6554(4) 0.123(4) Uani 1 1 d . B .
H32 H 1.5270 1.1023 0.6210 0.148 Uiso 1 1 calc R . .
N1 N 0.7815(4) 0.2649(3) 0.47739(16) 0.0331(7) Uani 1 1 d . . .
N2 N 0.6501(4) 0.1545(4) 0.4861(2) 0.0558(12) Uani 1 1 d . . .
N3 N 0.8643(4) 0.1098(3) 0.49131(16) 0.0338(8) Uani 1 1 d . . .
N4 N -0.0243(4) 0.2645(3) 1.01778(17) 0.0358(8) Uani 1 1 d . . .
N5 N 0.0012(5) 0.1535(4) 1.0107(3) 0.0734(16) Uani 1 1 d . . .
N6 N -0.2568(4) 0.1084(3) 1.00149(17) 0.0369(8) Uani 1 1 d . . .
N7 N 0.8484(5) 0.9444(4) 0.79678(18) 0.0489(10) Uani 1 1 d . . .
N8 N 1.0511(5) 1.1334(4) 0.81379(19) 0.0539(11) Uani 1 1 d . . .
N9 N 1.4444(11) 1.0586(7) 0.7037(3) 0.124(3) Uani 1 1 d . . .
N10 N 1.5732(5) 0.9327(4) 0.72144(18) 0.0476(9) Uani 1 1 d . . .
O1 O 0.7298(3) 0.7405(3) 0.68528(14) 0.0445(8) Uani 1 1 d . . .
O2 O 0.4817(3) 0.6447(3) 0.70678(14) 0.0436(8) Uani 1 1 d . . .
O3 O 0.1253(4) 0.2394(3) 0.60088(15) 0.0516(9) Uani 1 1 d . . .
O4 O 0.2026(3) 0.1681(3) 0.51944(14) 0.0377(7) Uani 1 1 d . . .
O5 O 0.7894(3) 0.4698(3) 0.51513(14) 0.0420(7) Uani 1 1 d . . .
O6 O 0.5128(4) 0.7486(3) 0.83612(13) 0.0407(7) Uani 1 1 d . . .
O7 O 0.6693(4) 0.6526(3) 0.81213(14) 0.0435(7) Uani 1 1 d . . .
O8 O 0.5750(5) 0.2082(3) 0.89314(16) 0.0590(10) Uani 1 1 d . . .
O9 O 0.4625(3) 0.1651(3) 0.97954(14) 0.0374(7) Uani 1 1 d . . .
O10 O 0.1647(3) 0.4681(3) 0.98595(15) 0.0444(8) Uani 1 1 d . . .
O1W O -0.0587(4) -0.0182(3) 0.58858(14) 0.0443(7) Uani 1 1 d D . .
H1B H -0.024(6) 0.060(2) 0.603(2) 0.066 Uiso 1 1 d D . .
H1A H -0.016(5) -0.067(4) 0.603(2) 0.066 Uiso 1 1 d D . .
O2W O 0.5032(5) 0.0474(3) 1.08977(15) 0.0548(9) Uani 1 1 d D . .
H2A H 0.471(6) 0.106(4) 1.101(2) 0.082 Uiso 1 1 d D . .
H2B H 0.462(6) -0.026(3) 1.106(2) 0.082 Uiso 1 1 d D . .
O3W O 1.0452(6) 0.8258(6) 0.6595(3) 0.0966(16) Uani 1 1 d D . .
O4W O 0.1797(7) 0.6483(7) 0.6932(5) 0.173(4) Uani 1 1 d . . .
O5W O 0.8224(15) 1.3244(11) 0.8108(10) 0.229(11) Uani 0.50 1 d P . .
O6W O -0.0080(9) 0.4073(8) 0.6445(4) 0.077(3) Uani 0.50 1 d P . .
O7W O 0.195(2) 0.732(2) 0.8111(14) 0.288(15) Uani 0.50 1 d P . .
O8W O -0.0597(12) 0.5849(10) 0.8180(6) 0.111(4) Uani 0.50 1 d P . .
H3A H 0.959(5) 0.802(9) 0.677(4) 0.166 Uiso 1 1 d D . .
H3B H 1.114(7) 0.803(10) 0.676(4) 0.166 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N7 2.012(4) . ?
Ni1 N10 2.015(4) 1_455 ?
Ni1 O1 2.091(3) . ?
Ni1 O6 2.125(3) . ?
Ni1 O7 2.140(3) . ?
Ni1 O2 2.153(3) . ?
Ni1 C7 2.454(4) . ?
Ni1 C18 2.455(4) . ?
Ni2 N3 2.070(3) 2_656 ?
Ni2 N3 2.070(3) 1_455 ?
Ni2 O4 2.075(3) 2_556 ?
Ni2 O4 2.075(3) . ?
Ni2 O1W 2.091(3) 2_556 ?
Ni2 O1W 2.091(3) . ?
Ni3 O9 2.046(3) 2_657 ?
Ni3 O9 2.046(3) . ?
Ni3 N6 2.085(3) 2_557 ?
Ni3 N6 2.085(3) 1_655 ?
Ni3 O2W 2.090(3) 2_657 ?
Ni3 O2W 2.090(3) . ?
C1 C6 1.372(6) . ?
C1 C2 1.394(5) . ?
C1 C7 1.495(6) . ?
C2 C3 1.384(5) . ?
C3 C4 1.390(6) . ?
C3 C8 1.519(5) . ?
C4 C5 1.382(5) . ?
C5 O5 1.386(5) . ?
C5 C6 1.389(6) . ?
C7 O1 1.257(5) . ?
C7 O2 1.272(5) . ?
C8 O3 1.250(5) . ?
C8 O4 1.260(5) . ?
C9 O5 1.409(5) . ?
C9 N1 1.450(5) . ?
C10 N2 1.305(6) . ?
C10 N3 1.341(5) . ?
C11 N3 1.313(5) . ?
C11 N1 1.314(5) . ?
C12 C17 1.383(6) . ?
C12 C13 1.386(5) . ?
C12 C18 1.494(6) . ?
C13 C14 1.393(5) . ?
C14 C15 1.387(5) . ?
C14 C19 1.502(5) . ?
C15 C16 1.375(5) . ?
C16 C17 1.384(6) . ?
C16 O10 1.396(5) . ?
C18 O7 1.254(5) . ?
C18 O6 1.264(5) . ?
C19 O8 1.242(5) . ?
C19 O9 1.253(5) . ?
C20 O10 1.411(5) . ?
C20 N4 1.445(5) . ?
C21 N5 1.306(6) . ?
C21 N6 1.342(5) . ?
C22 N6 1.303(5) . ?
C22 N4 1.324(5) . ?
C23 N7 1.308(6) . ?
C23 N8 1.324(6) . ?
C24 C25 1.347(8) . ?
C24 N8 1.363(8) . ?
C25 N7 1.357(8) . ?
C26 N8 1.465(6) . ?
C26 C27 1.492(8) . ?
C27 C28 1.503(9) . ?
C28 C29 1.34(2) . ?
C28 C29' 1.362(11) . ?
C29 N9 1.49(2) . ?
C29' N9 1.618(12) . ?
C30 N10 1.300(7) . ?
C30 N9 1.334(8) . ?
C31 C32 1.341(11) . ?
C31 N10 1.361(7) . ?
C32 N9 1.347(11) . ?
N1 N2 1.360(5) . ?
N3 Ni2 2.070(3) 1_655 ?
N4 N5 1.344(5) . ?
N6 Ni3 2.085(3) 1_455 ?
N10 Ni1 2.015(4) 1_655 ?

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
N7 Ni1 N10 95.61(17) . 1_455 ?
N7 Ni1 O1 103.04(15) . . ?
N10 Ni1 O1 98.61(15) 1_455 . ?
N7 Ni1 O6 99.71(15) . . ?
N10 Ni1 O6 103.84(14) 1_455 . ?
O1 Ni1 O6 146.10(11) . . ?
N7 Ni1 O7 93.05(15) . . ?
N10 Ni1 O7 164.09(15) 1_455 . ?
O1 Ni1 O7 92.39(12) . . ?
O6 Ni1 O7 61.43(11) . . ?
N7 Ni1 O2 164.64(15) . . ?
N10 Ni1 O2 90.27(15) 1_455 . ?
O1 Ni1 O2 61.96(11) . . ?
O6 Ni1 O2 92.61(12) . . ?
O7 Ni1 O2 84.77(13) . . ?
N7 Ni1 C7 133.64(16) . . ?
N10 Ni1 C7 96.48(15) 1_455 . ?
O1 Ni1 C7 30.82(12) . . ?
O6 Ni1 C7 120.26(13) . . ?
O7 Ni1 C7 87.08(13) . . ?
O2 Ni1 C7 31.19(12) . . ?
N7 Ni1 C18 100.42(15) . . ?
N10 Ni1 C18 133.89(16) 1_455 . ?
O1 Ni1 C18 118.94(13) . . ?
O6 Ni1 C18 30.99(12) . . ?
O7 Ni1 C18 30.71(12) . . ?
O2 Ni1 C18 85.44(13) . . ?
C7 Ni1 C18 102.67(14) . . ?
N3 Ni2 N3 180.000(1) 2_656 1_455 ?
N3 Ni2 O4 91.90(12) 2_656 2_556 ?
N3 Ni2 O4 88.10(12) 1_455 2_556 ?
N3 Ni2 O4 88.10(12) 2_656 . ?
N3 Ni2 O4 91.90(12) 1_455 . ?
O4 Ni2 O4 180.00(17) 2_556 . ?
N3 Ni2 O1W 87.15(13) 2_656 2_556 ?
N3 Ni2 O1W 92.85(13) 1_455 2_556 ?
O4 Ni2 O1W 91.70(12) 2_556 2_556 ?
O4 Ni2 O1W 88.30(12) . 2_556 ?
N3 Ni2 O1W 92.85(13) 2_656 . ?
N3 Ni2 O1W 87.15(13) 1_455 . ?
O4 Ni2 O1W 88.30(12) 2_556 . ?
O4 Ni2 O1W 91.70(12) . . ?
O1W Ni2 O1W 180.000(1) 2_556 . ?
O9 Ni3 O9 180.00(17) 2_657 . ?
O9 Ni3 N6 90.47(12) 2_657 2_557 ?
O9 Ni3 N6 89.53(12) . 2_557 ?
O9 Ni3 N6 89.53(12) 2_657 1_655 ?
O9 Ni3 N6 90.47(12) . 1_655 ?
N6 Ni3 N6 180.000(2) 2_557 1_655 ?
O9 Ni3 O2W 90.10(13) 2_657 2_657 ?
O9 Ni3 O2W 89.90(13) . 2_657 ?
N6 Ni3 O2W 88.65(15) 2_557 2_657 ?
N6 Ni3 O2W 91.35(15) 1_655 2_657 ?
O9 Ni3 O2W 89.90(13) 2_657 . ?
O9 Ni3 O2W 90.10(13) . . ?
N6 Ni3 O2W 91.35(15) 2_557 . ?
N6 Ni3 O2W 88.65(15) 1_655 . ?
O2W Ni3 O2W 180.000(2) 2_657 . ?
C6 C1 C2 119.8(4) . . ?
C6 C1 C7 120.7(3) . . ?
C2 C1 C7 119.4(4) . . ?
C3 C2 C1 120.1(4) . . ?
C2 C3 C4 120.1(4) . . ?
C2 C3 C8 119.5(3) . . ?
C4 C3 C8 120.4(3) . . ?
C5 C4 C3 119.3(4) . . ?
C4 C5 O5 124.9(4) . . ?
C4 C5 C6 120.6(4) . . ?
O5 C5 C6 114.5(3) . . ?
C1 C6 C5 120.0(4) . . ?
O1 C7 O2 119.6(4) . . ?
O1 C7 C1 121.2(4) . . ?
O2 C7 C1 119.2(4) . . ?
O1 C7 Ni1 58.5(2) . . ?
O2 C7 Ni1 61.3(2) . . ?
C1 C7 Ni1 174.5(3) . . ?
O3 C8 O4 126.0(4) . . ?
O3 C8 C3 117.3(4) . . ?
O4 C8 C3 116.7(4) . . ?
O5 C9 N1 112.2(4) . . ?
N2 C10 N3 114.3(4) . . ?
N3 C11 N1 110.6(3) . . ?
C17 C12 C13 120.1(4) . . ?
C17 C12 C18 119.3(4) . . ?
C13 C12 C18 120.5(4) . . ?
C12 C13 C14 119.8(4) . . ?
C15 C14 C13 119.8(3) . . ?
C15 C14 C19 119.6(3) . . ?
C13 C14 C19 120.4(3) . . ?
C16 C15 C14 119.8(4) . . ?
C15 C16 C17 120.7(4) . . ?
C15 C16 O10 125.0(4) . . ?
C17 C16 O10 114.3(3) . . ?
C12 C17 C16 119.7(4) . . ?
O7 C18 O6 119.8(4) . . ?
O7 C18 C12 119.6(4) . . ?
O6 C18 C12 120.6(4) . . ?
O7 C18 Ni1 60.6(2) . . ?
O6 C18 Ni1 59.9(2) . . ?
C12 C18 Ni1 169.6(3) . . ?
O8 C19 O9 125.4(4) . . ?
O8 C19 C14 118.2(4) . . ?
O9 C19 C14 116.4(4) . . ?
O10 C20 N4 112.7(4) . . ?
N5 C21 N6 115.4(4) . . ?
N6 C22 N4 111.5(4) . . ?
N7 C23 N8 113.3(5) . . ?
C25 C24 N8 105.2(5) . . ?
C24 C25 N7 111.3(6) . . ?
N8 C26 C27 114.5(4) . . ?
C26 C27 C28 116.5(6) . . ?
C29 C28 C29' 53.4(14) . . ?
C29 C28 C27 129.7(11) . . ?
C29' C28 C27 114.1(7) . . ?
C28 C29 N9 116.4(13) . . ?
C28 C29' N9 107.8(8) . . ?
N10 C30 N9 112.9(7) . . ?
C32 C31 N10 109.7(7) . . ?
C31 C32 N9 107.1(7) . . ?
C11 N1 N2 109.1(3) . . ?
C11 N1 C9 128.7(3) . . ?
N2 N1 C9 122.2(3) . . ?
C10 N2 N1 102.8(3) . . ?
C11 N3 C10 103.2(3) . . ?
C11 N3 Ni2 130.2(3) . 1_655 ?
C10 N3 Ni2 126.6(3) . 1_655 ?
C22 N4 N5 108.8(3) . . ?
C22 N4 C20 129.0(3) . . ?
N5 N4 C20 121.8(4) . . ?
C21 N5 N4 102.4(4) . . ?
C22 N6 C21 101.8(4) . . ?
C22 N6 Ni3 128.8(3) . 1_455 ?
C21 N6 Ni3 128.5(3) . 1_455 ?
C23 N7 C25 103.5(4) . . ?
C23 N7 Ni1 127.9(4) . . ?
C25 N7 Ni1 128.5(4) . . ?
C23 N8 C24 106.5(4) . . ?
C23 N8 C26 127.4(5) . . ?
C24 N8 C26 125.9(5) . . ?
C30 N9 C32 105.8(6) . . ?
C30 N9 C29 139.1(12) . . ?
C32 N9 C29 104.6(9) . . ?
C30 N9 C29' 119.1(8) . . ?
C32 N9 C29' 133.8(7) . . ?
C29 N9 C29' 45.8(9) . . ?
C30 N10 C31 104.5(5) . . ?
C30 N10 Ni1 128.1(4) . 1_655 ?
C31 N10 Ni1 127.3(4) . 1_655 ?
C7 O1 Ni1 90.7(2) . . ?
C7 O2 Ni1 87.5(2) . . ?
C8 O4 Ni2 125.6(3) . . ?
C5 O5 C9 120.5(3) . . ?
C18 O6 Ni1 89.1(2) . . ?
C18 O7 Ni1 88.7(2) . . ?
C19 O9 Ni3 127.4(3) . . ?
C16 O10 C20 119.7(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
O1W H1B O3 0.849(10) 1.91(3) 2.676(4) 149(5) .
O3W H3A O1 0.853(10) 1.96(3) 2.770(5) 157(8) .
O1W H1A O3W 0.848(10) 1.98(2) 2.797(6) 160(5) 1_445
O2W H2A O6 0.851(10) 2.08(4) 2.835(4) 147(6) 2_667
O2W H2B O8 0.847(10) 1.90(3) 2.660(4) 148(5) 2_657
O3W H3B O4W 0.854(10) 2.07(6) 2.813(8) 146(10) 1_655

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.096
_database_code_depnum_ccdc_archive 'CCDC 978490'
data_added_by_encifer
#==========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_address     
;
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       majf247@yahoo.com
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_phone       +86-431-85098620
_publ_requested_journal          CrystEngComm

#=========================END

data_Compound-5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 Cu2 N10 O11,2H2O'
_chemical_formula_sum            'C32 H34 Cu2 N10 O13'
_chemical_formula_weight         893.77

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'
Cu Cu 0.3201 1.2651 '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'
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   'P 21/c '
_symmetry_space_group_name_hall  '-P 2ybc'

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                   11.5342(8)
_cell_length_b                   20.5261(12)
_cell_length_c                   19.3153(13)
_cell_angle_alpha                90
_cell_angle_beta                 126.053(5)
_cell_angle_gamma                90
_cell_volume                     3697.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2467
_cell_measurement_theta_min      3.2442
_cell_measurement_theta_max      29.1813

_exptl_crystal_description       rhomb
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1832
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7246
_exptl_absorpt_correction_T_max  0.7485
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;

_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14790
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         26.37
_reflns_number_total             7400
_reflns_number_gt                4550
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_cell_refinement       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_data_reduction        
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.
H atoms of O1W, O2W and O3W were refined isotropically with 
distance restraints of O---H = 0.85+-0.01 Å. 
The distances of H1A...H1B, H2A...H2B and H3A...H3B were restrained to 1.44+-0.01 Å
;

_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)+(0.0357P)²+0.1363P] 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         7400
_refine_ls_number_parameters     542
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1244
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.49412(5) 0.83720(2) 0.75623(4) 0.02929(17) Uani 1 1 d . . .
Cu2 Cu 0.04598(5) 1.19085(2) 0.30106(3) 0.02748(16) Uani 1 1 d . . .
O1 O 0.3738(3) 0.75923(13) 0.71787(19) 0.0321(8) Uani 1 1 d . . .
O2 O 0.5849(3) 0.71082(15) 0.7972(2) 0.0494(10) Uani 1 1 d . . .
O3 O 0.5828(3) 0.46232(15) 0.7783(2) 0.0456(10) Uani 1 1 d . . .
O4 O 0.3723(3) 0.41220(13) 0.70333(19) 0.0306(8) Uani 1 1 d . . .
O5 O 0.0244(3) 0.58608(14) 0.51647(19) 0.0371(8) Uani 1 1 d . . .
O6 O 0.1472(3) 1.10758(13) 0.32417(18) 0.0288(7) Uani 1 1 d . . .
O7 O -0.0694(3) 1.06244(14) 0.2477(2) 0.0457(10) Uani 1 1 d . . .
O8 O -0.0821(3) 0.83827(14) 0.12850(19) 0.0362(8) Uani 1 1 d . . .
O9 O 0.0704(3) 0.76985(13) 0.23500(18) 0.0286(7) Uani 1 1 d . . .
O10 O 0.4842(3) 0.91997(13) 0.44824(19) 0.0330(8) Uani 1 1 d . . .
N1 N -0.0217(3) 0.67291(17) 0.4218(2) 0.0290(9) Uani 1 1 d . . .
N2 N 0.0741(4) 0.72314(19) 0.4479(3) 0.0402(10) Uani 1 1 d . . .
N3 N -0.0188(3) 0.69411(17) 0.3119(2) 0.0311(9) Uani 1 1 d . . .
N4 N 0.4917(3) 0.84363(17) 0.5421(2) 0.0292(9) Uani 1 1 d . . .
N5 N 0.3726(4) 0.80592(19) 0.5098(3) 0.0434(11) Uani 1 1 d . . .
N6 N 0.4721(4) 0.83302(17) 0.6469(2) 0.0304(9) Uani 1 1 d . . .
N7 N 0.4861(4) 0.84455(18) 0.8543(2) 0.0343(10) Uani 1 1 d . . .
N8 N 0.5192(5) 0.8777(2) 0.9718(3) 0.0516(12) Uani 1 1 d . . .
N9 N 0.0336(4) 1.17481(17) 0.3981(2) 0.0340(10) Uani 1 1 d . . .
N10 N -0.0304(4) 1.12572(19) 0.4716(3) 0.0421(11) Uani 1 1 d . . .
C1 C 0.3766(4) 0.64541(19) 0.7031(3) 0.0265(10) Uani 1 1 d . . .
C2 C 0.4457(4) 0.5864(2) 0.7342(3) 0.0303(11) Uani 1 1 d . . .
H2 H 0.5414 0.5853 0.7812 0.036 Uiso 1 1 calc R . .
C3 C 0.3730(4) 0.5283(2) 0.6955(3) 0.0292(11) Uani 1 1 d . . .
C4 C 0.2311(4) 0.5308(2) 0.6237(3) 0.0304(11) Uani 1 1 d . . .
H4 H 0.1810 0.4923 0.5982 0.036 Uiso 1 1 calc R . .
C5 C 0.1637(4) 0.5903(2) 0.5900(3) 0.0273(10) Uani 1 1 d . . .
C6 C 0.2354(4) 0.6473(2) 0.6302(3) 0.0287(11) Uani 1 1 d . . .
H6 H 0.1893 0.6872 0.6087 0.034 Uiso 1 1 calc R . .
C7 C 0.4534(5) 0.7086(2) 0.7435(3) 0.0320(11) Uani 1 1 d . . .
C8 C 0.4490(4) 0.4642(2) 0.7290(3) 0.0306(11) Uani 1 1 d . . .
C9 C -0.0535(4) 0.6438(2) 0.4772(3) 0.0315(11) Uani 1 1 d . . .
H9A H -0.0314 0.6749 0.5213 0.038 Uiso 1 1 calc R . .
H9B H -0.1552 0.6342 0.4439 0.038 Uiso 1 1 calc R . .
C10 C 0.0701(5) 0.7339(2) 0.3801(3) 0.0386(12) Uani 1 1 d . . .
H10 H 0.1242 0.7665 0.3782 0.046 Uiso 1 1 calc R . .
C11 C -0.0744(5) 0.6565(2) 0.3413(3) 0.0354(12) Uani 1 1 d . . .
H11 H -0.1406 0.6233 0.3104 0.043 Uiso 1 1 calc R . .
C12 C 0.1327(4) 0.99367(19) 0.3022(3) 0.0253(10) Uani 1 1 d . . .
C13 C 0.0542(4) 0.94259(19) 0.2471(3) 0.0269(10) Uani 1 1 d . . .
H13 H -0.0413 0.9490 0.2015 0.032 Uiso 1 1 calc R . .
C14 C 0.1166(4) 0.8818(2) 0.2594(3) 0.0251(10) Uani 1 1 d . . .
C15 C 0.2588(4) 0.87227(19) 0.3278(3) 0.0261(10) Uani 1 1 d . . .
H15 H 0.3004 0.8313 0.3376 0.031 Uiso 1 1 calc R . .
C16 C 0.3383(4) 0.9237(2) 0.3812(3) 0.0253(10) Uani 1 1 d . . .
C17 C 0.2755(4) 0.9837(2) 0.3694(3) 0.0269(10) Uani 1 1 d . . .
H17 H 0.3291 1.0177 0.4068 0.032 Uiso 1 1 calc R . .
C18 C 0.0620(4) 1.0586(2) 0.2892(3) 0.0295(11) Uani 1 1 d . . .
C19 C 0.0266(4) 0.8261(2) 0.2010(3) 0.0257(10) Uani 1 1 d . . .
C20 C 0.5405(4) 0.8600(2) 0.4906(3) 0.0298(11) Uani 1 1 d . . .
H20A H 0.6444 0.8623 0.5269 0.036 Uiso 1 1 calc R . .
H20B H 0.5117 0.8260 0.4485 0.036 Uiso 1 1 calc R . .
C21 C 0.3666(5) 0.8007(2) 0.5748(3) 0.0430(13) Uani 1 1 d . . .
H21 H 0.2958 0.7767 0.5723 0.052 Uiso 1 1 calc R . .
C22 C 0.5478(4) 0.8593(2) 0.6224(3) 0.0319(11) Uani 1 1 d . . .
H22 H 0.6288 0.8851 0.6568 0.038 Uiso 1 1 calc R . .
C23 C 0.5677(5) 0.8791(3) 0.9251(4) 0.0477(14) Uani 1 1 d . . .
H23 H 0.6494 0.9016 0.9400 0.057 Uiso 1 1 calc R . .
C24 C 0.3993(6) 0.8397(3) 0.9293(4) 0.0614(16) Uani 1 1 d . . .
H24 H 0.3415 0.8301 0.9469 0.074 Uiso 1 1 calc R . .
C25 C 0.3802(6) 0.8186(2) 0.8580(4) 0.0507(14) Uani 1 1 d . . .
H25 H 0.3073 0.7911 0.8175 0.061 Uiso 1 1 calc R . .
C26 C 0.5776(7) 0.9165(3) 1.0518(4) 0.072(2) Uani 1 1 d . . .
C27 C 0.4917(10) 0.9780(4) 1.0302(5) 0.090(5) Uani 0.89(2) 1 d P . 1
C27' C 0.624(6) 0.999(3) 1.030(4) 0.07(2) Uani 0.11(2) 1 d PU . 2
C28 C -0.0615(5) 1.1359(2) 0.3947(3) 0.0396(13) Uani 1 1 d . . .
H28 H -0.1403 1.1179 0.3445 0.048 Uiso 1 1 calc R . .
C29 C 0.0936(6) 1.1585(3) 0.5292(4) 0.0538(15) Uani 1 1 d . . .
H29 H 0.1423 1.1598 0.5883 0.065 Uiso 1 1 calc R . .
C30 C 0.1312(5) 1.1887(2) 0.4832(3) 0.0436(13) Uani 1 1 d . . .
H30 H 0.2115 1.2151 0.5059 0.052 Uiso 1 1 calc R . .
C31 C -0.1017(6) 1.0787(3) 0.4919(4) 0.0569(16) Uani 1 1 d . . .
H31A H -0.1970 1.0698 0.4407 0.068 Uiso 1 1 calc R . .
H31B H -0.1117 1.0974 0.5342 0.068 Uiso 1 1 calc R . .
C32 C -0.0187(7) 1.0157(3) 0.5260(4) 0.0679(18) Uani 1 1 d . . .
H32A H 0.0693 1.0242 0.5821 0.082 Uiso 1 1 calc R . .
H32B H -0.0745 0.9852 0.5336 0.082 Uiso 1 1 calc R . .
O1W O 0.2609(3) 1.25010(15) 0.3781(3) 0.0438(9) Uani 1 1 d D . .
H1A H 0.224(6) 1.272(3) 0.394(3) 0.066 Uiso 1 1 d D . .
H1B H 0.278(5) 1.273(3) 0.344(3) 0.066 Uiso 1 1 d D . .
O2W O 0.7590(5) 0.6731(2) 0.7482(3) 0.0733(13) Uani 1 1 d D . .
H2A H 0.693(7) 0.689(3) 0.754(5) 0.110 Uiso 1 1 d D . .
H2B H 0.764(7) 0.635(3) 0.748(5) 0.110 Uiso 1 1 d D . .
O3W O 0.7567(4) 0.53543(19) 0.7469(3) 0.0631(12) Uani 1 1 d D . .
H3A H 0.706(6) 0.520(3) 0.762(4) 0.095 Uiso 1 1 d D . .
H3B H 0.805(6) 0.506(3) 0.742(4) 0.095 Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.956(3) . ?
Cu1 N7 1.957(4) . ?
Cu1 N6 1.976(4) . ?
Cu1 O4 1.984(3) 2_656 ?
Cu2 O9 1.954(3) 2 ?
Cu2 O6 1.967(3) . ?
Cu2 N9 1.989(4) . ?
Cu2 N3 2.015(4) 2 ?
Cu2 O1W 2.344(3) . ?
O1 C7 1.278(5) . ?
O2 C7 1.236(5) . ?
O3 C8 1.249(5) . ?
O4 C8 1.285(5) . ?
O4 Cu1 1.984(3) 2_646 ?
O5 C5 1.386(4) . ?
O5 C9 1.408(5) . ?
O6 C18 1.285(5) . ?
O7 C18 1.231(5) . ?
O8 C19 1.236(5) . ?
O9 C19 1.277(5) . ?
O9 Cu2 1.954(3) 2_545 ?
O10 C16 1.396(4) . ?
O10 C20 1.407(5) . ?
N1 C11 1.336(6) . ?
N1 N2 1.372(5) . ?
N1 C9 1.450(6) . ?
N2 C10 1.301(6) . ?
N3 C11 1.326(6) . ?
N3 C10 1.365(6) . ?
N3 Cu2 2.015(4) 2_545 ?
N4 C22 1.321(6) . ?
N4 N5 1.367(5) . ?
N4 C20 1.442(6) . ?
N5 C21 1.301(6) . ?
N6 C22 1.328(6) . ?
N6 C21 1.366(5) . ?
N7 C23 1.320(6) . ?
N7 C25 1.371(6) . ?
N8 C23 1.312(7) . ?
N8 C24 1.364(7) . ?
N8 C26 1.501(7) . ?
N9 C28 1.328(6) . ?
N9 C30 1.369(6) . ?
N10 C28 1.322(6) . ?
N10 C29 1.365(6) . ?
N10 C31 1.463(6) . ?
C1 C2 1.379(5) . ?
C1 C6 1.392(5) . ?
C1 C7 1.504(6) . ?
C2 C3 1.394(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(5) . ?
C3 C8 1.500(6) . ?
C4 C5 1.388(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.378(5) . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.385(5) . ?
C12 C17 1.386(5) . ?
C12 C18 1.504(6) . ?
C13 C14 1.389(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(5) . ?
C14 C19 1.510(6) . ?
C15 C16 1.381(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.379(5) . ?
C17 H17 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.332(8) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.503(9) . ?
C26 C27' 1.90(6) . ?
C27 C27 1.574(18) 3_677 ?
C28 H28 0.9300 . ?
C29 C30 1.346(7) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.510(7) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C32 1.455(12) 3_576 ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
O1W H1A 0.80(5) . ?
O1W H1B 0.92(5) . ?
O2W H2A 0.91(6) . ?
O2W H2B 0.79(6) . ?
O3W H3A 0.86(6) . ?
O3W H3B 0.87(6) . ?

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 N7 90.14(14) . . ?
O1 Cu1 N6 86.76(14) . . ?
N7 Cu1 N6 171.62(15) . . ?
O1 Cu1 O4 175.83(12) . 2_656 ?
N7 Cu1 O4 91.56(14) . 2_656 ?
N6 Cu1 O4 92.06(14) . 2_656 ?
O9 Cu2 O6 173.52(12) 2 . ?
O9 Cu2 N9 93.32(14) 2 . ?
O6 Cu2 N9 90.26(14) . . ?
O9 Cu2 N3 87.15(13) 2 2 ?
O6 Cu2 N3 88.15(14) . 2 ?
N9 Cu2 N3 166.99(15) . 2 ?
O9 Cu2 O1W 92.51(11) 2 . ?
O6 Cu2 O1W 92.41(11) . . ?
N9 Cu2 O1W 97.08(16) . . ?
N3 Cu2 O1W 95.89(15) 2 . ?
C7 O1 Cu1 109.3(3) . . ?
C8 O4 Cu1 107.1(2) . 2_646 ?
C5 O5 C9 119.1(3) . . ?
C18 O6 Cu2 113.1(2) . . ?
C19 O9 Cu2 125.9(2) . 2_545 ?
C16 O10 C20 118.6(3) . . ?
C11 N1 N2 109.5(4) . . ?
C11 N1 C9 127.9(4) . . ?
N2 N1 C9 122.5(4) . . ?
C10 N2 N1 102.3(4) . . ?
C11 N3 C10 102.3(4) . . ?
C11 N3 Cu2 129.6(3) . 2_545 ?
C10 N3 Cu2 127.9(3) . 2_545 ?
C22 N4 N5 109.8(4) . . ?
C22 N4 C20 129.3(4) . . ?
N5 N4 C20 120.9(4) . . ?
C21 N5 N4 102.5(4) . . ?
C22 N6 C21 102.3(4) . . ?
C22 N6 Cu1 131.7(3) . . ?
C21 N6 Cu1 126.0(3) . . ?
C23 N7 C25 105.6(5) . . ?
C23 N7 Cu1 129.2(4) . . ?
C25 N7 Cu1 124.8(3) . . ?
C23 N8 C24 106.8(5) . . ?
C23 N8 C26 125.6(5) . . ?
C24 N8 C26 127.3(6) . . ?
C28 N9 C30 104.8(4) . . ?
C28 N9 Cu2 124.7(3) . . ?
C30 N9 Cu2 129.3(3) . . ?
C28 N10 C29 107.4(5) . . ?
C28 N10 C31 125.5(5) . . ?
C29 N10 C31 126.3(5) . . ?
C2 C1 C6 119.8(4) . . ?
C2 C1 C7 121.3(4) . . ?
C6 C1 C7 118.8(4) . . ?
C1 C2 C3 120.5(4) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 C2 119.2(4) . . ?
C4 C3 C8 120.5(4) . . ?
C2 C3 C8 120.3(4) . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 O5 125.5(3) . . ?
C6 C5 C4 119.9(4) . . ?
O5 C5 C4 114.6(3) . . ?
C5 C6 C1 120.2(4) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
O2 C7 O1 122.9(4) . . ?
O2 C7 C1 121.6(4) . . ?
O1 C7 C1 115.5(4) . . ?
O3 C8 O4 122.0(4) . . ?
O3 C8 C3 120.2(4) . . ?
O4 C8 C3 117.9(3) . . ?
O5 C9 N1 112.7(4) . . ?
O5 C9 H9A 109.1 . . ?
N1 C9 H9A 109.1 . . ?
O5 C9 H9B 109.1 . . ?
N1 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 N3 115.5(4) . . ?
N2 C10 H10 122.2 . . ?
N3 C10 H10 122.2 . . ?
N3 C11 N1 110.3(4) . . ?
N3 C11 H11 124.9 . . ?
N1 C11 H11 124.9 . . ?
C13 C12 C17 119.1(4) . . ?
C13 C12 C18 119.8(3) . . ?
C17 C12 C18 121.0(4) . . ?
C12 C13 C14 120.6(4) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 119.6(4) . . ?
C15 C14 C19 120.8(4) . . ?
C13 C14 C19 119.5(3) . . ?
C16 C15 C14 119.8(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 O10 115.6(3) . . ?
C15 C16 O10 124.0(4) . . ?
C16 C17 C12 120.4(4) . . ?
C16 C17 H17 119.8 . . ?
C12 C17 H17 119.8 . . ?
O7 C18 O6 124.0(4) . . ?
O7 C18 C12 120.3(4) . . ?
O6 C18 C12 115.7(3) . . ?
O8 C19 O9 126.6(4) . . ?
O8 C19 C14 119.1(4) . . ?
O9 C19 C14 114.2(4) . . ?
O10 C20 N4 111.8(3) . . ?
O10 C20 H20A 109.3 . . ?
N4 C20 H20A 109.3 . . ?
O10 C20 H20B 109.3 . . ?
N4 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
N5 C21 N6 114.9(4) . . ?
N5 C21 H21 122.5 . . ?
N6 C21 H21 122.5 . . ?
N4 C22 N6 110.4(4) . . ?
N4 C22 H22 124.8 . . ?
N6 C22 H22 124.8 . . ?
N8 C23 N7 111.5(5) . . ?
N8 C23 H23 124.2 . . ?
N7 C23 H23 124.2 . . ?
C25 C24 N8 107.5(5) . . ?
C25 C24 H24 126.3 . . ?
N8 C24 H24 126.3 . . ?
C24 C25 N7 108.5(5) . . ?
C24 C25 H25 125.8 . . ?
N7 C25 H25 125.8 . . ?
N8 C26 C27 109.6(5) . . ?
N8 C26 C27' 105.0(18) . . ?
C27 C26 C27' 54.3(18) . . ?
C26 C27 C27 109.9(9) . 3_677 ?
N10 C28 N9 111.7(4) . . ?
N10 C28 H28 124.1 . . ?
N9 C28 H28 124.1 . . ?
C30 C29 N10 106.2(5) . . ?
C30 C29 H29 126.9 . . ?
N10 C29 H29 126.9 . . ?
C29 C30 N9 109.9(5) . . ?
C29 C30 H30 125.1 . . ?
N9 C30 H30 125.1 . . ?
N10 C31 C32 111.7(4) . . ?
N10 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
N10 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
C32 C32 C31 116.7(7) 3_576 . ?
C32 C32 H32A 108.1 3_576 . ?
C31 C32 H32A 108.1 . . ?
C32 C32 H32B 108.1 3_576 . ?
C31 C32 H32B 108.1 . . ?
H32A C32 H32B 107.3 . . ?
Cu2 O1W H1A 86(4) . . ?
Cu2 O1W H1B 114(3) . . ?
H1A O1W H1B 113(4) . . ?
H2A O2W H2B 116(6) . . ?
H3A O3W H3B 113(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
N7 Cu1 O1 C7 -97.3(3) . . . . ?
N6 Cu1 O1 C7 90.5(3) . . . . ?
O4 Cu1 O1 C7 17(2) 2_656 . . . ?
O9 Cu2 O6 C18 -39.3(13) 2 . . . ?
N9 Cu2 O6 C18 84.2(3) . . . . ?
N3 Cu2 O6 C18 -82.9(3) 2 . . . ?
O1W Cu2 O6 C18 -178.7(3) . . . . ?
C11 N1 N2 C10 0.9(5) . . . . ?
C9 N1 N2 C10 180.0(4) . . . . ?
C22 N4 N5 C21 -1.0(5) . . . . ?
C20 N4 N5 C21 178.2(4) . . . . ?
O1 Cu1 N6 C22 -160.9(4) . . . . ?
N7 Cu1 N6 C22 130.6(10) . . . . ?
O4 Cu1 N6 C22 15.1(4) 2_656 . . . ?
O1 Cu1 N6 C21 20.1(4) . . . . ?
N7 Cu1 N6 C21 -48.4(12) . . . . ?
O4 Cu1 N6 C21 -163.9(4) 2_656 . . . ?
O1 Cu1 N7 C23 164.1(4) . . . . ?
N6 Cu1 N7 C23 -127.6(9) . . . . ?
O4 Cu1 N7 C23 -12.1(4) 2_656 . . . ?
O1 Cu1 N7 C25 -23.3(4) . . . . ?
N6 Cu1 N7 C25 45.0(12) . . . . ?
O4 Cu1 N7 C25 160.5(4) 2_656 . . . ?
O9 Cu2 N9 C28 95.2(4) 2 . . . ?
O6 Cu2 N9 C28 -79.4(4) . . . . ?
N3 Cu2 N9 C28 3.5(9) 2 . . . ?
O1W Cu2 N9 C28 -171.8(3) . . . . ?
O9 Cu2 N9 C30 -99.3(4) 2 . . . ?
O6 Cu2 N9 C30 86.1(4) . . . . ?
N3 Cu2 N9 C30 169.0(5) 2 . . . ?
O1W Cu2 N9 C30 -6.4(4) . . . . ?
C6 C1 C2 C3 -3.1(7) . . . . ?
C7 C1 C2 C3 -179.5(4) . . . . ?
C1 C2 C3 C4 1.8(7) . . . . ?
C1 C2 C3 C8 179.4(4) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C8 C3 C4 C5 -176.2(4) . . . . ?
C9 O5 C5 C6 0.8(7) . . . . ?
C9 O5 C5 C4 179.9(4) . . . . ?
C3 C4 C5 C6 -3.3(7) . . . . ?
C3 C4 C5 O5 177.5(4) . . . . ?
O5 C5 C6 C1 -178.9(5) . . . . ?
C4 C5 C6 C1 2.1(7) . . . . ?
C2 C1 C6 C5 1.1(7) . . . . ?
C7 C1 C6 C5 177.7(4) . . . . ?
Cu1 O1 C7 O2 12.5(6) . . . . ?
Cu1 O1 C7 C1 -166.9(3) . . . . ?
C2 C1 C7 O2 10.8(7) . . . . ?
C6 C1 C7 O2 -165.7(5) . . . . ?
C2 C1 C7 O1 -169.8(4) . . . . ?
C6 C1 C7 O1 13.7(7) . . . . ?
Cu1 O4 C8 O3 -7.2(6) 2_646 . . . ?
Cu1 O4 C8 C3 170.8(3) 2_646 . . . ?
C4 C3 C8 O3 161.8(5) . . . . ?
C2 C3 C8 O3 -15.7(7) . . . . ?
C4 C3 C8 O4 -16.3(7) . . . . ?
C2 C3 C8 O4 166.2(4) . . . . ?
C5 O5 C9 N1 82.7(5) . . . . ?
C11 N1 C9 O5 81.0(5) . . . . ?
N2 N1 C9 O5 -97.9(5) . . . . ?
N1 N2 C10 N3 -1.0(5) . . . . ?
C11 N3 C10 N2 0.7(6) . . . . ?
Cu2 N3 C10 N2 -175.7(3) 2_545 . . . ?
C10 N3 C11 N1 0.0(5) . . . . ?
Cu2 N3 C11 N1 176.3(3) 2_545 . . . ?
N2 N1 C11 N3 -0.6(5) . . . . ?
C9 N1 C11 N3 -179.6(4) . . . . ?
C17 C12 C13 C14 0.8(7) . . . . ?
C18 C12 C13 C14 -178.4(4) . . . . ?
C12 C13 C14 C15 0.4(7) . . . . ?
C12 C13 C14 C19 177.0(4) . . . . ?
C13 C14 C15 C16 -2.3(7) . . . . ?
C19 C14 C15 C16 -178.8(4) . . . . ?
C14 C15 C16 C17 3.1(7) . . . . ?
C14 C15 C16 O10 -175.7(4) . . . . ?
C20 O10 C16 C17 150.4(4) . . . . ?
C20 O10 C16 C15 -30.7(6) . . . . ?
C15 C16 C17 C12 -1.9(7) . . . . ?
O10 C16 C17 C12 177.0(4) . . . . ?
C13 C12 C17 C16 0.0(7) . . . . ?
C18 C12 C17 C16 179.2(4) . . . . ?
Cu2 O6 C18 O7 -2.3(6) . . . . ?
Cu2 O6 C18 C12 178.2(3) . . . . ?
C13 C12 C18 O7 20.9(7) . . . . ?
C17 C12 C18 O7 -158.3(5) . . . . ?
C13 C12 C18 O6 -159.6(4) . . . . ?
C17 C12 C18 O6 21.2(6) . . . . ?
Cu2 O9 C19 O8 -19.9(7) 2_545 . . . ?
Cu2 O9 C19 C14 157.1(3) 2_545 . . . ?
C15 C14 C19 O8 -159.1(4) . . . . ?
C13 C14 C19 O8 24.4(6) . . . . ?
C15 C14 C19 O9 23.7(6) . . . . ?
C13 C14 C19 O9 -152.9(4) . . . . ?
C16 O10 C20 N4 -70.5(5) . . . . ?
C22 N4 C20 O10 -87.9(5) . . . . ?
N5 N4 C20 O10 93.1(4) . . . . ?
N4 N5 C21 N6 0.9(6) . . . . ?
C22 N6 C21 N5 -0.5(6) . . . . ?
Cu1 N6 C21 N5 178.7(3) . . . . ?
N5 N4 C22 N6 0.7(5) . . . . ?
C20 N4 C22 N6 -178.3(4) . . . . ?
C21 N6 C22 N4 -0.2(5) . . . . ?
Cu1 N6 C22 N4 -179.3(3) . . . . ?
C24 N8 C23 N7 0.4(6) . . . . ?
C26 N8 C23 N7 -173.9(5) . . . . ?
C25 N7 C23 N8 -1.2(6) . . . . ?
Cu1 N7 C23 N8 172.5(3) . . . . ?
C23 N8 C24 C25 0.6(7) . . . . ?
C26 N8 C24 C25 174.8(5) . . . . ?
N8 C24 C25 N7 -1.3(7) . . . . ?
C23 N7 C25 C24 1.5(6) . . . . ?
Cu1 N7 C25 C24 -172.5(4) . . . . ?
C23 N8 C26 C27 95.4(7) . . . . ?
C24 N8 C26 C27 -77.7(8) . . . . ?
C23 N8 C26 C27' 39(2) . . . . ?
C24 N8 C26 C27' -134.6(19) . . . . ?
N8 C26 C27 C27 -63.5(10) . . . 3_677 ?
C27' C26 C27 C27 31(2) . . . 3_677 ?
C29 N10 C28 N9 -1.3(6) . . . . ?
C31 N10 C28 N9 -171.4(4) . . . . ?
C30 N9 C28 N10 1.0(5) . . . . ?
Cu2 N9 C28 N10 169.4(3) . . . . ?
C28 N10 C29 C30 1.1(6) . . . . ?
C31 N10 C29 C30 171.1(5) . . . . ?
N10 C29 C30 N9 -0.6(6) . . . . ?
C28 N9 C30 C29 -0.2(5) . . . . ?
Cu2 N9 C30 C29 -167.9(4) . . . . ?
C28 N10 C31 C32 97.1(6) . . . . ?
C29 N10 C31 C32 -71.1(7) . . . . ?
N10 C31 C32 C32 -53.1(9) . . . 3_576 ?

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
O1W H1A O8 0.80(5) 1.97(5) 2.689(4) 150(5) 2
O1W H1B O2W 0.92(5) 1.92(5) 2.798(6) 159(5) 3_676
O3W H3B O7 0.87(6) 1.97(6) 2.832(5) 172(6) 4_676
O2W H2A O2 0.91(6) 1.90(7) 2.786(6) 164(7) .
O2W H2B O3W 0.79(6) 2.04(7) 2.826(6) 174(7) .
O3W H3A O3 0.86(6) 2.01(6) 2.842(5) 164(6) .

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.089
_database_code_depnum_ccdc_archive 'CCDC 978491'
data_added_by_encifer
#==========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_address     
;
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       majf247@yahoo.com
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_phone       +86-431-85098620
_publ_requested_journal          CrystEngComm

#=========================END

data_Compound-6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H38 Cu2 N12 O10, 4H2O'
_chemical_formula_sum            'C36 H46 Cu2 N12 O14'
_chemical_formula_weight         997.93

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           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_hall  '-P 2ybc'

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                   13.5928(9)
_cell_length_b                   8.7066(5)
_cell_length_c                   18.2172(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.900(6)
_cell_angle_gamma                90
_cell_volume                     2148.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1884
_cell_measurement_theta_min      3.0409
_cell_measurement_theta_max      29.0627

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7396
_exptl_absorpt_correction_T_max  0.7833
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;

_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8925
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.10
_reflns_number_total             4620
_reflns_number_gt                3082
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_cell_refinement       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_data_reduction        
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.
For  c15, c15',c16 and c16' atoms, SIMU restraints were used to make them 
behave similar anisotropic displacement parameters. 
The distance of H14A...H15B was restrained to 1.9+-0.01 Å
The distances of c15...c16 and c15'...c16' were restrained to 1.3+-0.01 Å
;

_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)+(0.0429P)²+0.3255P] 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         4620
_refine_ls_number_parameters     321
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1170
_refine_ls_wR_factor_gt          0.1000
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002

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 0.16511(3) 0.61121(5) 0.71430(2) 0.02801(15) Uani 1 1 d . . .
C1 C 0.2001(3) 0.5038(4) 0.49736(18) 0.0277(8) Uani 1 1 d . . .
C2 C 0.2037(3) 0.5971(4) 0.43593(18) 0.0274(8) Uani 1 1 d . . .
H2 H 0.1961 0.7027 0.4406 0.033 Uiso 1 1 calc R . .
C3 C 0.2183(2) 0.5353(4) 0.36815(18) 0.0257(8) Uani 1 1 d . . .
C5 C 0.2273(2) 0.2847(4) 0.42223(19) 0.0263(8) Uani 1 1 d . . .
C4 C 0.2313(2) 0.3775(4) 0.36149(18) 0.0283(8) Uani 1 1 d . . .
H4 H 0.2427 0.3350 0.3161 0.034 Uiso 1 1 calc R . .
C6 C 0.2126(2) 0.3466(4) 0.49066(19) 0.0275(8) Uani 1 1 d . . .
H6 H 0.2111 0.2831 0.5316 0.033 Uiso 1 1 calc R . .
C7 C 0.1842(3) 0.5790(4) 0.57013(19) 0.0306(8) Uani 1 1 d . . .
C8 C 0.2165(3) 0.6327(4) 0.29961(19) 0.0304(8) Uani 1 1 d . . .
C9 C 0.1445(3) 0.0504(4) 0.4114(2) 0.0329(9) Uani 1 1 d . . .
H9A H 0.1199 0.0567 0.4598 0.039 Uiso 1 1 calc R . .
H9B H 0.1537 -0.0572 0.4001 0.039 Uiso 1 1 calc R . .
C10 C 0.0103(3) 0.1907(4) 0.2549(2) 0.0331(9) Uani 1 1 d . . .
H10 H -0.0031 0.2035 0.2043 0.040 Uiso 1 1 calc R . .
C11 C 0.0027(3) 0.2185(4) 0.3685(2) 0.0317(8) Uani 1 1 d . . .
H11 H -0.0138 0.2510 0.4145 0.038 Uiso 1 1 calc R . .
C12 C 0.3320(4) 0.3852(5) 0.7012(3) 0.0604(13) Uani 1 1 d . B .
H12 H 0.2948 0.3260 0.6666 0.072 Uiso 1 1 calc R . .
C13 C 0.3720(3) 0.5572(5) 0.7768(3) 0.0530(12) Uani 1 1 d . . .
H13 H 0.3715 0.6428 0.8073 0.064 Uiso 1 1 calc R . .
C14 C 0.5449(4) 0.4725(7) 0.8162(4) 0.098(2) Uani 1 1 d . . .
H14A H 0.5668 0.5785 0.8200 0.118 Uiso 1 1 calc R A 1
H14B H 0.5930 0.4151 0.7910 0.118 Uiso 1 1 calc RD A 1
C15 C 0.5392(15) 0.4016(15) 0.8995(12) 0.106(4) Uani 0.519(10) 1 d PDU B 1
H15A H 0.6015 0.4180 0.9286 0.127 Uiso 0.519(10) 1 calc PR B 1
H15B H 0.4876 0.4530 0.9239 0.127 Uiso 0.519(10) 1 calc PR B 1
C16 C 0.5197(11) 0.2498(15) 0.8941(10) 0.106(4) Uani 0.481(10) 1 d PDU B 1
H16A H 0.5721 0.1931 0.8733 0.127 Uiso 0.481(10) 1 calc PR B 1
H16B H 0.4571 0.2288 0.8663 0.127 Uiso 0.481(10) 1 calc PR B 1
C15' C 0.5587(9) 0.3352(14) 0.8681(8) 0.090(3) Uani 0.519(10) 1 d PDU B 2
H15C H 0.5484 0.2403 0.8407 0.107 Uiso 0.519(10) 1 calc PRD B 2
H15D H 0.6252 0.3346 0.8921 0.107 Uiso 0.519(10) 1 calc PR B 2
C16' C 0.4908(11) 0.348(2) 0.9199(8) 0.093(3) Uani 0.481(10) 1 d PDU B 2
H16C H 0.4247 0.3318 0.8967 0.111 Uiso 0.481(10) 1 calc PR B 2
H16D H 0.4939 0.4495 0.9415 0.111 Uiso 0.481(10) 1 calc PR B 2
C17 C 0.5159(8) 0.2162(13) 0.9853(6) 0.165(4) Uani 1 1 d . . .
H17A H 0.5776 0.2364 1.0145 0.198 Uiso 1 1 calc R B 1
H17B H 0.4607 0.2644 1.0067 0.198 Uiso 1 1 calc R B 1
C18 C 0.4997(6) 0.0519(13) 0.9657(4) 0.142(4) Uani 1 1 d . . .
H18A H 0.5511 0.0182 0.9355 0.170 Uiso 1 1 calc R . .
H18B H 0.4368 0.0413 0.9367 0.170 Uiso 1 1 calc R . .
N1 N 0.0723(2) 0.1164(3) 0.35724(15) 0.0281(7) Uani 1 1 d . . .
N2 N 0.0787(2) 0.0974(3) 0.28312(15) 0.0315(7) Uani 1 1 d . . .
N3 N -0.0396(2) 0.2673(3) 0.30486(16) 0.0292(7) Uani 1 1 d . . .
N4 N 0.2964(2) 0.5121(3) 0.73208(17) 0.0366(8) Uani 1 1 d . . .
N5 N 0.4231(3) 0.3528(5) 0.7240(2) 0.0720(12) Uani 1 1 d . . .
N6 N 0.4481(3) 0.4655(4) 0.7729(2) 0.0600(11) Uani 1 1 d . B .
O1 O 0.14653(18) 0.4965(3) 0.61898(13) 0.0348(6) Uani 1 1 d . . .
O2 O 0.2073(2) 0.7148(3) 0.58005(14) 0.0444(7) Uani 1 1 d . . .
O3 O 0.19147(18) 0.7737(3) 0.30660(13) 0.0314(6) Uani 1 1 d . . .
O4 O 0.2369(2) 0.5755(3) 0.24146(14) 0.0525(8) Uani 1 1 d . . .
O5 O 0.23609(17) 0.1270(2) 0.41262(13) 0.0317(6) Uani 1 1 d . . .
O1W O 0.0150(3) 0.2224(5) 0.5669(2) 0.0707(11) Uani 1 1 d . . .
H1B H 0.040(5) 0.306(7) 0.569(4) 0.106 Uiso 1 1 d . . .
H1A H 0.065(5) 0.167(7) 0.580(3) 0.106 Uiso 1 1 d . . .
O2W O 0.8206(3) 0.5308(4) 0.8968(2) 0.0711(11) Uani 1 1 d . . .
H2A H 0.807(5) 0.526(7) 0.850(3) 0.107 Uiso 1 1 d . . .
H2B H 0.819(4) 0.446(7) 0.919(3) 0.107 Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 1.964(2) 4_576 ?
Cu1 N4 1.984(3) . ?
Cu1 O1 2.001(2) . ?
Cu1 N3 2.012(3) 3_566 ?
C1 C6 1.386(5) . ?
C1 C2 1.387(5) . ?
C1 C7 1.511(5) . ?
C2 C3 1.377(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.392(4) . ?
C3 C8 1.508(5) . ?
C5 C4 1.375(5) . ?
C5 C6 1.388(5) . ?
C5 O5 1.390(4) . ?
C4 H4 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.232(4) . ?
C7 O1 1.284(4) . ?
C8 O4 1.224(4) . ?
C8 O3 1.283(4) . ?
C9 O5 1.411(4) . ?
C9 N1 1.450(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.306(4) . ?
C10 N3 1.357(4) . ?
C10 H10 0.9300 . ?
C11 N3 1.319(4) . ?
C11 N1 1.326(4) . ?
C11 H11 0.9300 . ?
C12 N5 1.303(6) . ?
C12 N4 1.348(5) . ?
C12 H12 0.9300 . ?
C13 N6 1.314(5) . ?
C13 N4 1.316(5) . ?
C13 H13 0.9300 . ?
C14 N6 1.476(6) . ?
C14 C15' 1.525(10) . ?
C14 C15 1.65(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.350(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.69(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C15' C16' 1.380(9) . ?
C15' H15C 0.9700 . ?
C15' H15D 0.9700 . ?
C16' C17 1.666(18) . ?
C16' H16C 0.9700 . ?
C16' H16D 0.9700 . ?
C17 C18 1.487(12) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C18 1.542(16) 3_657 ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
N1 N2 1.370(4) . ?
N3 Cu1 2.012(3) 3_566 ?
N5 N6 1.350(5) . ?
O3 Cu1 1.964(2) 4_575 ?
O1W H1B 0.81(6) . ?
O1W H1A 0.85(6) . ?
O2W H2A 0.86(6) . ?
O2W H2B 0.84(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cu1 N4 89.22(12) 4_576 . ?
O3 Cu1 O1 176.60(10) 4_576 . ?
N4 Cu1 O1 88.25(12) . . ?
O3 Cu1 N3 88.30(11) 4_576 3_566 ?
N4 Cu1 N3 173.98(12) . 3_566 ?
O1 Cu1 N3 93.99(11) . 3_566 ?
C6 C1 C2 119.6(3) . . ?
C6 C1 C7 122.2(3) . . ?
C2 C1 C7 118.1(3) . . ?
C3 C2 C1 120.8(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 C8 122.0(3) . . ?
C4 C3 C8 118.5(3) . . ?
C4 C5 C6 120.9(3) . . ?
C4 C5 O5 118.0(3) . . ?
C6 C5 O5 121.1(3) . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C1 C6 C5 119.4(3) . . ?
C1 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
O2 C7 O1 123.2(3) . . ?
O2 C7 C1 119.4(3) . . ?
O1 C7 C1 117.4(3) . . ?
O4 C8 O3 123.9(3) . . ?
O4 C8 C3 119.9(3) . . ?
O3 C8 C3 116.2(3) . . ?
O5 C9 N1 111.6(3) . . ?
O5 C9 H9A 109.3 . . ?
N1 C9 H9A 109.3 . . ?
O5 C9 H9B 109.3 . . ?
N1 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 N3 114.9(3) . . ?
N2 C10 H10 122.5 . . ?
N3 C10 H10 122.5 . . ?
N3 C11 N1 110.1(3) . . ?
N3 C11 H11 125.0 . . ?
N1 C11 H11 125.0 . . ?
N5 C12 N4 114.2(4) . . ?
N5 C12 H12 122.9 . . ?
N4 C12 H12 122.9 . . ?
N6 C13 N4 111.2(4) . . ?
N6 C13 H13 124.4 . . ?
N4 C13 H13 124.4 . . ?
N6 C14 C15' 110.8(6) . . ?
N6 C14 C15 111.6(7) . . ?
C15' C14 C15 31.6(6) . . ?
N6 C14 H14A 109.3 . . ?
C15' C14 H14A 133.0 . . ?
C15 C14 H14A 109.3 . . ?
N6 C14 H14B 109.3 . . ?
C15' C14 H14B 80.6 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C14 108.9(15) . . ?
C16 C15 H15A 109.9 . . ?
C14 C15 H15A 109.9 . . ?
C16 C15 H15B 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
C15 C16 C17 96.9(15) . . ?
C15 C16 H16A 112.4 . . ?
C17 C16 H16A 112.4 . . ?
C15 C16 H16B 112.4 . . ?
C17 C16 H16B 112.4 . . ?
H16A C16 H16B 109.9 . . ?
C16' C15' C14 108.0(12) . . ?
C16' C15' H15C 110.1 . . ?
C14 C15' H15C 110.1 . . ?
C16' C15' H15D 110.1 . . ?
C14 C15' H15D 110.1 . . ?
H15C C15' H15D 108.4 . . ?
C15' C16' C17 109.1(11) . . ?
C15' C16' H16C 109.9 . . ?
C17 C16' H16C 109.9 . . ?
C15' C16' H16D 109.9 . . ?
C17 C16' H16D 109.9 . . ?
H16C C16' H16D 108.3 . . ?
C18 C17 C16' 118.1(10) . . ?
C18 C17 C16 86.9(8) . . ?
C16' C17 C16 36.9(6) . . ?
C18 C17 H17A 114.2 . . ?
C16' C17 H17A 112.5 . . ?
C16 C17 H17A 114.2 . . ?
C18 C17 H17B 114.2 . . ?
C16' C17 H17B 82.7 . . ?
C16 C17 H17B 114.2 . . ?
H17A C17 H17B 111.3 . . ?
C17 C18 C18 112.2(10) . 3_657 ?
C17 C18 H18A 109.2 . . ?
C18 C18 H18A 109.2 3_657 . ?
C17 C18 H18B 109.2 . . ?
C18 C18 H18B 109.2 3_657 . ?
H18A C18 H18B 107.9 . . ?
C11 N1 N2 109.8(3) . . ?
C11 N1 C9 127.6(3) . . ?
N2 N1 C9 121.7(3) . . ?
C10 N2 N1 102.1(3) . . ?
C11 N3 C10 103.0(3) . . ?
C11 N3 Cu1 128.4(2) . 3_566 ?
C10 N3 Cu1 127.4(2) . 3_566 ?
C13 N4 C12 102.4(4) . . ?
C13 N4 Cu1 127.9(3) . . ?
C12 N4 Cu1 129.6(3) . . ?
C12 N5 N6 103.4(4) . . ?
C13 N6 N5 108.8(4) . . ?
C13 N6 C14 128.0(5) . . ?
N5 N6 C14 123.1(4) . . ?
C7 O1 Cu1 107.1(2) . . ?
C8 O3 Cu1 115.7(2) . 4_575 ?
C5 O5 C9 112.6(2) . . ?
H1B O1W H1A 100(6) . . ?
H2A O2W H2B 115(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.8(5) . . . . ?
C7 C1 C2 C3 179.8(3) . . . . ?
C1 C2 C3 C4 -1.1(5) . . . . ?
C1 C2 C3 C8 176.3(3) . . . . ?
C6 C5 C4 C3 -1.4(5) . . . . ?
O5 C5 C4 C3 177.1(3) . . . . ?
C2 C3 C4 C5 1.4(5) . . . . ?
C8 C3 C4 C5 -176.0(3) . . . . ?
C2 C1 C6 C5 -0.8(5) . . . . ?
C7 C1 C6 C5 -179.7(3) . . . . ?
C4 C5 C6 C1 1.1(5) . . . . ?
O5 C5 C6 C1 -177.3(3) . . . . ?
C6 C1 C7 O2 154.7(3) . . . . ?
C2 C1 C7 O2 -24.2(5) . . . . ?
C6 C1 C7 O1 -25.3(5) . . . . ?
C2 C1 C7 O1 155.7(3) . . . . ?
C2 C3 C8 O4 174.7(3) . . . . ?
C4 C3 C8 O4 -8.0(5) . . . . ?
C2 C3 C8 O3 -6.2(5) . . . . ?
C4 C3 C8 O3 171.1(3) . . . . ?
N6 C14 C15 C16 65.9(16) . . . . ?
C15' C14 C15 C16 -29.1(12) . . . . ?
C14 C15 C16 C17 -178.6(10) . . . . ?
N6 C14 C15' C16' -66.3(14) . . . . ?
C15 C14 C15' C16' 31.3(12) . . . . ?
C14 C15' C16' C17 -170.7(10) . . . . ?
C15' C16' C17 C18 -68.8(17) . . . . ?
C15' C16' C17 C16 -33.2(11) . . . . ?
C15 C16 C17 C18 -177.5(13) . . . . ?
C15 C16 C17 C16' 33.5(10) . . . . ?
C16' C17 C18 C18 -165.5(9) . . . 3_657 ?
C16 C17 C18 C18 174.0(9) . . . 3_657 ?
N3 C11 N1 N2 1.2(4) . . . . ?
N3 C11 N1 C9 171.1(3) . . . . ?
O5 C9 N1 C11 -97.4(4) . . . . ?
O5 C9 N1 N2 71.4(4) . . . . ?
N3 C10 N2 N1 -0.2(4) . . . . ?
C11 N1 N2 C10 -0.6(4) . . . . ?
C9 N1 N2 C10 -171.2(3) . . . . ?
N1 C11 N3 C10 -1.3(4) . . . . ?
N1 C11 N3 Cu1 167.0(2) . . . 3_566 ?
N2 C10 N3 C11 0.9(4) . . . . ?
N2 C10 N3 Cu1 -167.5(2) . . . 3_566 ?
N6 C13 N4 C12 0.6(5) . . . . ?
N6 C13 N4 Cu1 -178.2(3) . . . . ?
N5 C12 N4 C13 -0.4(5) . . . . ?
N5 C12 N4 Cu1 178.4(3) . . . . ?
O3 Cu1 N4 C13 -17.9(4) 4_576 . . . ?
O1 Cu1 N4 C13 159.8(4) . . . . ?
N3 Cu1 N4 C13 47.8(13) 3_566 . . . ?
O3 Cu1 N4 C12 163.6(4) 4_576 . . . ?
O1 Cu1 N4 C12 -18.7(4) . . . . ?
N3 Cu1 N4 C12 -130.7(11) 3_566 . . . ?
N4 C12 N5 N6 0.1(6) . . . . ?
N4 C13 N6 N5 -0.6(5) . . . . ?
N4 C13 N6 C14 -177.2(4) . . . . ?
C12 N5 N6 C13 0.3(5) . . . . ?
C12 N5 N6 C14 177.1(4) . . . . ?
C15' C14 N6 C13 112.3(8) . . . . ?
C15 C14 N6 C13 78.3(8) . . . . ?
C15' C14 N6 N5 -63.9(9) . . . . ?
C15 C14 N6 N5 -97.8(8) . . . . ?
O2 C7 O1 Cu1 -13.2(4) . . . . ?
C1 C7 O1 Cu1 166.8(2) . . . . ?
O3 Cu1 O1 C7 -45.5(17) 4_576 . . . ?
N4 Cu1 O1 C7 -87.6(2) . . . . ?
N3 Cu1 O1 C7 86.8(2) 3_566 . . . ?
O4 C8 O3 Cu1 10.1(5) . . . 4_575 ?
C3 C8 O3 Cu1 -168.9(2) . . . 4_575 ?
C4 C5 O5 C9 -102.8(4) . . . . ?
C6 C5 O5 C9 75.7(4) . . . . ?
N1 C9 O5 C5 53.8(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
O1W H1B O1 0.81(6) 2.33(6) 3.082(4) 156(6) .
O1W H1A O2W 0.85(6) 1.97(6) 2.821(5) 175(6) 2_646
O2W H2A O4 0.86(6) 1.93(6) 2.734(4) 155(6) 3_666
O2W H2B O2 0.84(6) 2.05(6) 2.814(4) 151(6) 2_646

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 978492'
data_added_by_encifer
#==========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_address     
;
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       majf247@yahoo.com
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_phone       +86-431-85098620
_publ_requested_journal          CrystEngComm

#=========================END

data_Compound-7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H28 N10 O10 Zn2, 4H2O'
_chemical_formula_sum            'C32 H36 N10 O14 Zn2'
_chemical_formula_weight         915.45

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

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

_cell_length_a                   9.7409(14)
_cell_length_b                   10.3056(16)
_cell_length_c                   11.2358(18)
_cell_angle_alpha                116.914(16)
_cell_angle_beta                 96.328(13)
_cell_angle_gamma                109.365(14)
_cell_volume                     902.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1540
_cell_measurement_theta_min      3.5150
_cell_measurement_theta_max      29.1139

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             470
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6928
_exptl_absorpt_correction_T_max  0.7651
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;

_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6394
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3658
_reflns_number_gt                2633
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_cell_refinement       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_data_reduction        
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.
H atoms of O1W and O2W  were refined isotropically with 
distance restraints of O---H = 0.85+-0.01 Å. 
The distances of H1A...H1B and H2A...H2B were restrained to 1.44+-0.01 Å
;

_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)+(0.0204P)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         3658
_refine_ls_number_parameters     274
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.39928(5) 0.39226(5) 0.24603(5) 0.02952(15) Uani 1 1 d . . .
C1 C 0.3416(4) 0.8041(4) 0.3437(4) 0.0248(9) Uani 1 1 d . . .
C2 C 0.3653(4) 0.8997(4) 0.2845(4) 0.0262(9) Uani 1 1 d . . .
H2 H 0.4086 0.8773 0.2121 0.031 Uiso 1 1 calc R . .
C3 C 0.3256(4) 1.0267(4) 0.3315(4) 0.0267(9) Uani 1 1 d . . .
C4 C 0.2602(4) 1.0603(4) 0.4389(4) 0.0287(9) Uani 1 1 d . . .
H4 H 0.2320 1.1450 0.4703 0.034 Uiso 1 1 calc R . .
C5 C 0.2371(4) 0.9669(4) 0.4993(4) 0.0270(9) Uani 1 1 d . . .
C6 C 0.2763(4) 0.8388(4) 0.4519(4) 0.0277(9) Uani 1 1 d . . .
H6 H 0.2591 0.7760 0.4923 0.033 Uiso 1 1 calc R . .
C7 C 0.3850(4) 0.6657(4) 0.2894(4) 0.0288(9) Uani 1 1 d . . .
C8 C 0.3525(4) 1.1276(5) 0.2664(4) 0.0303(9) Uani 1 1 d . . .
C9 C 0.1707(5) 1.1441(5) 0.6836(4) 0.0360(10) Uani 1 1 d . . .
H9A H 0.0779 1.1432 0.6411 0.043 Uiso 1 1 calc R . .
H9B H 0.2578 1.2263 0.6855 0.043 Uiso 1 1 calc R . .
C10 C 0.1156(5) 1.1691(5) 0.9907(5) 0.0399(11) Uani 1 1 d . . .
H10 H 0.0586 1.1449 1.0451 0.048 Uiso 1 1 calc R . .
C11 C 0.3000(5) 1.2720(5) 0.9342(5) 0.0342(10) Uani 1 1 d . . .
H11 H 0.3963 1.3318 0.9357 0.041 Uiso 1 1 calc R . .
C12 C 0.6787(5) 0.4055(5) 0.1585(5) 0.0416(11) Uani 1 1 d . . .
H12 H 0.6234 0.3556 0.0648 0.050 Uiso 1 1 calc R . .
C13 C 0.8656(5) 0.5145(5) 0.3448(5) 0.0436(11) Uani 1 1 d . . .
H13 H 0.9620 0.5551 0.4059 0.052 Uiso 1 1 calc R . .
C14 C 0.7372(5) 0.5118(5) 0.3794(5) 0.0426(11) Uani 1 1 d . . .
H14 H 0.7304 0.5508 0.4700 0.051 Uiso 1 1 calc R . .
C15 C 0.9253(5) 0.4162(5) 0.1136(5) 0.0441(12) Uani 1 1 d . . .
H15A H 0.8775 0.3036 0.0392 0.053 Uiso 1 1 calc R . .
H15B H 1.0227 0.4379 0.1689 0.053 Uiso 1 1 calc R . .
C16 C 0.9526(5) 0.5199(5) 0.0496(4) 0.0408(11) Uani 1 1 d . . .
H16A H 1.0058 0.6326 0.1237 0.049 Uiso 1 1 calc R . .
H16B H 0.8551 0.5027 -0.0016 0.049 Uiso 1 1 calc R . .
N1 N 0.1786(4) 1.1778(4) 0.8228(4) 0.0310(8) Uani 1 1 d . . .
N2 N 0.0549(4) 1.1072(4) 0.8561(4) 0.0412(9) Uani 1 1 d . . .
N3 N 0.2655(4) 1.2699(4) 1.0449(3) 0.0296(8) Uani 1 1 d . . .
N4 N 0.6187(4) 0.4437(4) 0.2623(4) 0.0332(8) Uani 1 1 d . . .
N5 N 0.8270(4) 0.4465(4) 0.2036(4) 0.0362(9) Uani 1 1 d . . .
O1 O 0.3548(3) 0.5788(3) 0.3444(3) 0.0346(7) Uani 1 1 d . . .
O2 O 0.4448(3) 0.6402(3) 0.1946(3) 0.0386(7) Uani 1 1 d . . .
O3 O 0.4005(4) 1.0884(3) 0.1639(3) 0.0495(9) Uani 1 1 d . . .
O4 O 0.3272(3) 1.2528(3) 0.3225(3) 0.0328(7) Uani 1 1 d . . .
O5 O 0.1711(3) 0.9915(3) 0.6053(3) 0.0411(8) Uani 1 1 d . . .
O1W O 0.3219(5) 0.9480(5) -0.1310(4) 0.0815(12) Uani 1 1 d D . .
H2A H 0.9032(15) 0.213(6) 0.268(7) 0.122 Uiso 1 1 d D . .
H1A H 0.398(4) 0.930(7) -0.150(5) 0.122 Uiso 1 1 d D . .
O2W O 1.0006(5) 0.2567(5) 0.2846(5) 0.0836(12) Uani 1 1 d D . .
H2B H 1.044(5) 0.201(6) 0.295(7) 0.125 Uiso 1 1 d D . .
H1B H 0.317(6) 0.968(8) -0.050(3) 0.125 Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.960(2) . ?
Zn1 O4 1.969(2) 1_545 ?
Zn1 N4 1.990(3) . ?
Zn1 N3 2.019(3) 1_544 ?
C1 C6 1.392(4) . ?
C1 C2 1.394(4) . ?
C1 C7 1.501(5) . ?
C2 C3 1.377(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(4) . ?
C3 C8 1.496(5) . ?
C4 C5 1.385(4) . ?
C4 H4 0.9300 . ?
C5 O5 1.378(4) . ?
C5 C6 1.383(5) . ?
C6 H6 0.9300 . ?
C7 O2 1.236(4) . ?
C7 O1 1.279(4) . ?
C8 O3 1.237(4) . ?
C8 O4 1.278(4) . ?
C9 O5 1.414(4) . ?
C9 N1 1.427(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.313(5) . ?
C10 N3 1.344(5) . ?
C10 H10 0.9300 . ?
C11 N1 1.311(5) . ?
C11 N3 1.331(4) . ?
C11 H11 0.9300 . ?
C12 N4 1.320(4) . ?
C12 N5 1.328(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.345(5) . ?
C13 N5 1.356(5) . ?
C13 H13 0.9300 . ?
C14 N4 1.359(5) . ?
C14 H14 0.9300 . ?
C15 N5 1.470(4) . ?
C15 C16 1.510(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C16 1.525(7) 2_765 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
N1 N2 1.373(4) . ?
N3 Zn1 2.019(3) 1_566 ?
O4 Zn1 1.969(2) 1_565 ?
O1W H1A 0.850(10) . ?
O1W H1B 0.851(10) . ?
O2W H2A 0.859(10) . ?
O2W H2B 0.857(10) . ?

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 Zn1 O4 107.63(9) . 1_545 ?
O1 Zn1 N4 115.33(12) . . ?
O4 Zn1 N4 108.47(11) 1_545 . ?
O1 Zn1 N3 105.52(12) . 1_544 ?
O4 Zn1 N3 106.98(12) 1_545 1_544 ?
N4 Zn1 N3 112.52(13) . 1_544 ?
C6 C1 C2 118.8(3) . . ?
C6 C1 C7 121.4(3) . . ?
C2 C1 C7 119.8(3) . . ?
C3 C2 C1 121.1(3) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 C8 120.1(3) . . ?
C4 C3 C8 120.1(3) . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
O5 C5 C4 123.1(3) . . ?
O5 C5 C6 116.3(3) . . ?
C4 C5 C6 120.6(3) . . ?
C5 C6 C1 120.0(3) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
O2 C7 O1 123.8(3) . . ?
O2 C7 C1 119.5(3) . . ?
O1 C7 C1 116.7(3) . . ?
O3 C8 O4 123.5(3) . . ?
O3 C8 C3 119.0(3) . . ?
O4 C8 C3 117.5(3) . . ?
O5 C9 N1 108.0(3) . . ?
O5 C9 H9A 110.1 . . ?
N1 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
N1 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 N3 115.6(3) . . ?
N2 C10 H10 122.2 . . ?
N3 C10 H10 122.2 . . ?
N1 C11 N3 110.3(3) . . ?
N1 C11 H11 124.9 . . ?
N3 C11 H11 124.9 . . ?
N4 C12 N5 112.1(4) . . ?
N4 C12 H12 123.9 . . ?
N5 C12 H12 123.9 . . ?
C14 C13 N5 106.6(4) . . ?
C14 C13 H13 126.7 . . ?
N5 C13 H13 126.7 . . ?
C13 C14 N4 110.0(4) . . ?
C13 C14 H14 125.0 . . ?
N4 C14 H14 125.0 . . ?
N5 C15 C16 112.0(3) . . ?
N5 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
N5 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 C16 111.2(4) . 2_765 ?
C15 C16 H16A 109.4 . . ?
C16 C16 H16A 109.4 2_765 . ?
C15 C16 H16B 109.4 . . ?
C16 C16 H16B 109.4 2_765 . ?
H16A C16 H16B 108.0 . . ?
C11 N1 N2 110.3(3) . . ?
C11 N1 C9 127.0(3) . . ?
N2 N1 C9 122.6(4) . . ?
C10 N2 N1 101.3(3) . . ?
C11 N3 C10 102.5(4) . . ?
C11 N3 Zn1 129.6(3) . 1_566 ?
C10 N3 Zn1 127.9(3) . 1_566 ?
C12 N4 C14 104.7(3) . . ?
C12 N4 Zn1 126.9(3) . . ?
C14 N4 Zn1 128.2(3) . . ?
C12 N5 C13 106.7(3) . . ?
C12 N5 C15 125.3(4) . . ?
C13 N5 C15 128.0(4) . . ?
C7 O1 Zn1 110.4(2) . . ?
C8 O4 Zn1 112.8(2) . 1_565 ?
C5 O5 C9 117.5(2) . . ?
H1A O1W H1B 115.3(19) . . ?
H2A O2W H2B 113.5(18) . . ?

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
C6 C1 C2 C3 0.1(6) . . . . ?
C7 C1 C2 C3 179.5(4) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
C1 C2 C3 C8 179.9(4) . . . . ?
C2 C3 C4 C5 0.8(6) . . . . ?
C8 C3 C4 C5 -179.4(4) . . . . ?
C3 C4 C5 O5 -179.2(3) . . . . ?
C3 C4 C5 C6 -1.1(6) . . . . ?
O5 C5 C6 C1 179.1(3) . . . . ?
C4 C5 C6 C1 0.9(6) . . . . ?
C2 C1 C6 C5 -0.4(6) . . . . ?
C7 C1 C6 C5 -179.8(4) . . . . ?
C6 C1 C7 O2 -178.9(4) . . . . ?
C2 C1 C7 O2 1.7(6) . . . . ?
C6 C1 C7 O1 2.1(6) . . . . ?
C2 C1 C7 O1 -177.3(3) . . . . ?
C2 C3 C8 O3 5.0(6) . . . . ?
C4 C3 C8 O3 -174.7(4) . . . . ?
C2 C3 C8 O4 -173.5(4) . . . . ?
C4 C3 C8 O4 6.7(6) . . . . ?
N5 C13 C14 N4 -0.2(5) . . . . ?
N5 C15 C16 C16 -176.8(4) . . . 2_765 ?
N3 C11 N1 N2 0.0(4) . . . . ?
N3 C11 N1 C9 -177.8(3) . . . . ?
O5 C9 N1 C11 101.1(4) . . . . ?
O5 C9 N1 N2 -76.4(4) . . . . ?
N3 C10 N2 N1 -0.8(4) . . . . ?
C11 N1 N2 C10 0.4(4) . . . . ?
C9 N1 N2 C10 178.4(3) . . . . ?
N1 C11 N3 C10 -0.5(4) . . . . ?
N1 C11 N3 Zn1 -178.3(2) . . . 1_566 ?
N2 C10 N3 C11 0.8(4) . . . . ?
N2 C10 N3 Zn1 178.7(2) . . . 1_566 ?
N5 C12 N4 C14 -0.5(4) . . . . ?
N5 C12 N4 Zn1 -175.1(2) . . . . ?
C13 C14 N4 C12 0.4(4) . . . . ?
C13 C14 N4 Zn1 175.0(3) . . . . ?
O1 Zn1 N4 C12 -121.6(3) . . . . ?
O4 Zn1 N4 C12 117.7(3) 1_545 . . . ?
N3 Zn1 N4 C12 -0.5(3) 1_544 . . . ?
O1 Zn1 N4 C14 65.0(3) . . . . ?
O4 Zn1 N4 C14 -55.7(3) 1_545 . . . ?
N3 Zn1 N4 C14 -173.9(3) 1_544 . . . ?
N4 C12 N5 C13 0.4(5) . . . . ?
N4 C12 N5 C15 178.3(3) . . . . ?
C14 C13 N5 C12 -0.1(4) . . . . ?
C14 C13 N5 C15 -177.9(3) . . . . ?
C16 C15 N5 C12 70.1(5) . . . . ?
C16 C15 N5 C13 -112.5(5) . . . . ?
O2 C7 O1 Zn1 -5.1(5) . . . . ?
C1 C7 O1 Zn1 173.9(3) . . . . ?
O4 Zn1 O1 C7 -173.4(2) 1_545 . . . ?
N4 Zn1 O1 C7 65.3(3) . . . . ?
N3 Zn1 O1 C7 -59.5(3) 1_544 . . . ?
O3 C8 O4 Zn1 -8.0(5) . . . 1_565 ?
C3 C8 O4 Zn1 170.5(3) . . . 1_565 ?
C4 C5 O5 C9 -19.9(5) . . . . ?
C6 C5 O5 C9 161.9(4) . . . . ?
N1 C9 O5 C5 -149.0(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
O1W H1B O3 0.851(10) 2.04(3) 2.832(5) 154(6) .
O2W H2A O1W 0.859(10) 2.11(3) 2.901(6) 152(6) 2_665
O1W H1A O3 0.850(10) 2.048(15) 2.890(4) 171(5) 2_675

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.088
_database_code_depnum_ccdc_archive 'CCDC 978493'
data_added_by_encifer
#==========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_address     
;
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       majf247@yahoo.com
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_phone       +86-431-85098620
_publ_requested_journal          CrystEngComm

#=========================END

data_Compound-8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H28 N10 O10 Zn2, H2O'
_chemical_formula_sum            'C32 H30 N10 O11 Zn2'
_chemical_formula_weight         861.40

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'
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 1 2/c 1'
_symmetry_space_group_name_hall  '-C 2yc'

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                   18.5740(10)
_cell_length_b                   11.8625(6)
_cell_length_c                   16.8934(8)
_cell_angle_alpha                90
_cell_angle_beta                 112.071(6)
_cell_angle_gamma                90
_cell_volume                     3449.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1828
_cell_measurement_theta_min      2.6775
_cell_measurement_theta_max      29.1116

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    1.468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6840
_exptl_absorpt_correction_T_max  0.7288
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;

_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6850
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         27.10
_reflns_number_total             3706
_reflns_number_gt                2596
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_cell_refinement       
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_data_reduction        
'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.
For O1W atom, anisotropic displacement ellipsoids were rather 
elongated which led us to use the ISOR restraint.
;

_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)+(0.0402P)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         3706
_refine_ls_number_parameters     249
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.1058
_refine_ls_wR_factor_gt          0.0909
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.28677(2) 0.23064(4) 0.70386(2) 0.03054(15) Uani 1 1 d . . .
C1 C 0.05790(19) 0.3151(3) 0.5707(2) 0.0285(8) Uani 1 1 d . . .
C2 C 0.0154(2) 0.3302(3) 0.4836(2) 0.0319(8) Uani 1 1 d . . .
H2 H 0.0416 0.3410 0.4468 0.038 Uiso 1 1 calc R . .
C3 C -0.0650(2) 0.3295(3) 0.45106(19) 0.0316(8) Uani 1 1 d . . .
C4 C -0.1043(2) 0.3181(3) 0.5062(2) 0.0319(8) Uani 1 1 d . . .
H4 H -0.1583 0.3182 0.4851 0.038 Uiso 1 1 calc R . .
C5 C -0.06221(19) 0.3066(3) 0.5929(2) 0.0287(8) Uani 1 1 d . . .
C6 C 0.01807(19) 0.3039(3) 0.6250(2) 0.0315(8) Uani 1 1 d . . .
H6 H 0.0454 0.2945 0.6833 0.038 Uiso 1 1 calc R . .
C7 C 0.1439(2) 0.2993(3) 0.6010(2) 0.0327(8) Uani 1 1 d . . .
C8 C -0.1076(2) 0.3291(3) 0.3556(2) 0.0343(8) Uani 1 1 d . . .
C9 C -0.1760(2) 0.2928(3) 0.6305(2) 0.0347(9) Uani 1 1 d . . .
H9A H -0.1897 0.2578 0.6748 0.042 Uiso 1 1 calc R . .
H9B H -0.2008 0.2505 0.5781 0.042 Uiso 1 1 calc R . .
C10 C -0.2506(2) 0.5579(4) 0.5567(2) 0.0443(10) Uani 1 1 d . . .
H10 H -0.2758 0.6107 0.5147 0.053 Uiso 1 1 calc R . .
C11 C -0.1899(2) 0.4876(3) 0.6767(2) 0.0405(10) Uani 1 1 d . . .
H11 H -0.1635 0.4768 0.7350 0.049 Uiso 1 1 calc R . .
C12 C 0.4126(2) 0.3389(3) 0.6606(2) 0.0355(9) Uani 1 1 d . . .
H12 H 0.4360 0.2699 0.6593 0.043 Uiso 1 1 calc R . .
C13 C 0.3895(3) 0.5182(4) 0.6528(3) 0.0558(12) Uani 1 1 d . . .
H13 H 0.3929 0.5955 0.6453 0.067 Uiso 1 1 calc R . .
C14 C 0.3370(2) 0.4646(3) 0.6764(3) 0.0487(10) Uani 1 1 d . . .
H14 H 0.2970 0.4994 0.6877 0.058 Uiso 1 1 calc R . .
C15 C 0.4990(2) 0.4571(4) 0.6099(2) 0.0468(10) Uani 1 1 d . . .
H15A H 0.5302 0.3894 0.6176 0.056 Uiso 1 1 calc R . .
H15B H 0.5325 0.5168 0.6430 0.056 Uiso 1 1 calc R . .
C16 C 0.4678(2) 0.4896(3) 0.5168(2) 0.0424(10) Uani 1 1 d . . .
H16A H 0.4367 0.5574 0.5091 0.051 Uiso 1 1 calc R . .
H16B H 0.4342 0.4299 0.4836 0.051 Uiso 1 1 calc R . .
N1 N -0.20376(17) 0.4076(3) 0.61801(17) 0.0339(7) Uani 1 1 d . . .
N2 N -0.2430(2) 0.4523(3) 0.53938(18) 0.0473(9) Uani 1 1 d . . .
N3 N -0.21873(17) 0.5842(3) 0.64088(17) 0.0371(8) Uani 1 1 d . . .
N4 N 0.35115(17) 0.3515(3) 0.68121(17) 0.0339(7) Uani 1 1 d . . .
N5 N 0.43696(18) 0.4369(3) 0.64209(18) 0.0376(7) Uani 1 1 d . . .
O1 O 0.18118(13) 0.2878(2) 0.68284(14) 0.0390(6) Uani 1 1 d . . .
O2 O 0.17578(15) 0.2915(2) 0.54956(15) 0.0485(7) Uani 1 1 d . . .
O3 O -0.07110(15) 0.3442(3) 0.30870(15) 0.0508(8) Uani 1 1 d . . .
O4 O -0.18002(14) 0.3057(2) 0.32759(14) 0.0427(7) Uani 1 1 d . . .
O5 O -0.09467(14) 0.2893(2) 0.65400(14) 0.0354(6) Uani 1 1 d . . .
O1W O 0.0000 0.486(3) 0.2500 0.68(2) Uani 1 2 d SU . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.977(2) . ?
Zn1 O4 1.992(2) 8_556 ?
Zn1 N4 1.994(3) . ?
Zn1 N3 2.020(3) 3_545 ?
C1 C6 1.384(4) . ?
C1 C2 1.395(4) . ?
C1 C7 1.495(5) . ?
C2 C3 1.385(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(5) . ?
C3 C8 1.505(4) . ?
C4 C5 1.383(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(4) . ?
C5 O5 1.392(4) . ?
C6 H6 0.9300 . ?
C7 O2 1.225(4) . ?
C7 O1 1.300(4) . ?
C8 O3 1.235(4) . ?
C8 O4 1.277(4) . ?
C9 O5 1.411(4) . ?
C9 N1 1.442(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.306(5) . ?
C10 N3 1.356(4) . ?
C10 H10 0.9300 . ?
C11 N3 1.312(4) . ?
C11 N1 1.326(4) . ?
C11 H11 0.9300 . ?
C12 N4 1.321(4) . ?
C12 N5 1.327(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.345(6) . ?
C13 N5 1.364(5) . ?
C13 H13 0.9300 . ?
C14 N4 1.365(5) . ?
C14 H14 0.9300 . ?
C15 N5 1.468(5) . ?
C15 C16 1.508(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C16 1.524(7) 5_666 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
N1 N2 1.360(4) . ?
N3 Zn1 2.020(3) 3_455 ?
O4 Zn1 1.992(2) 8_455 ?

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 Zn1 O4 99.08(10) . 8_556 ?
O1 Zn1 N4 110.18(12) . . ?
O4 Zn1 N4 112.67(11) 8_556 . ?
O1 Zn1 N3 110.49(11) . 3_545 ?
O4 Zn1 N3 107.52(12) 8_556 3_545 ?
N4 Zn1 N3 115.64(12) . 3_545 ?
C6 C1 C2 118.7(3) . . ?
C6 C1 C7 122.0(3) . . ?
C2 C1 C7 119.0(3) . . ?
C3 C2 C1 121.0(3) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 C8 118.7(3) . . ?
C4 C3 C8 121.4(3) . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 O5 114.2(3) . . ?
C4 C5 O5 124.7(3) . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O2 C7 O1 122.7(3) . . ?
O2 C7 C1 120.4(3) . . ?
O1 C7 C1 116.8(3) . . ?
O3 C8 O4 123.3(3) . . ?
O3 C8 C3 119.5(3) . . ?
O4 C8 C3 117.0(3) . . ?
O5 C9 N1 110.8(3) . . ?
O5 C9 H9A 109.5 . . ?
N1 C9 H9A 109.5 . . ?
O5 C9 H9B 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N2 C10 N3 114.4(3) . . ?
N2 C10 H10 122.8 . . ?
N3 C10 H10 122.8 . . ?
N3 C11 N1 110.5(3) . . ?
N3 C11 H11 124.8 . . ?
N1 C11 H11 124.8 . . ?
N4 C12 N5 111.6(3) . . ?
N4 C12 H12 124.2 . . ?
N5 C12 H12 124.2 . . ?
C14 C13 N5 106.4(4) . . ?
C14 C13 H13 126.8 . . ?
N5 C13 H13 126.8 . . ?
C13 C14 N4 109.7(4) . . ?
C13 C14 H14 125.1 . . ?
N4 C14 H14 125.1 . . ?
N5 C15 C16 112.4(3) . . ?
N5 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
N5 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 C16 112.4(4) . 5_666 ?
C15 C16 H16A 109.1 . . ?
C16 C16 H16A 109.1 5_666 . ?
C15 C16 H16B 109.1 . . ?
C16 C16 H16B 109.1 5_666 . ?
H16A C16 H16B 107.9 . . ?
C11 N1 N2 109.5(3) . . ?
C11 N1 C9 127.4(3) . . ?
N2 N1 C9 122.8(3) . . ?
C10 N2 N1 102.7(3) . . ?
C11 N3 C10 103.0(3) . . ?
C11 N3 Zn1 125.3(2) . 3_455 ?
C10 N3 Zn1 131.7(3) . 3_455 ?
C12 N4 C14 105.2(3) . . ?
C12 N4 Zn1 127.5(3) . . ?
C14 N4 Zn1 127.0(3) . . ?
C12 N5 C13 107.1(3) . . ?
C12 N5 C15 128.0(3) . . ?
C13 N5 C15 124.8(3) . . ?
C7 O1 Zn1 108.8(2) . . ?
C8 O4 Zn1 107.7(2) . 8_455 ?
C5 O5 C9 120.2(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
C6 C1 C2 C3 -2.6(5) . . . . ?
C7 C1 C2 C3 170.9(3) . . . . ?
C1 C2 C3 C4 2.6(5) . . . . ?
C1 C2 C3 C8 -171.2(3) . . . . ?
C2 C3 C4 C5 -0.6(5) . . . . ?
C8 C3 C4 C5 173.0(3) . . . . ?
C3 C4 C5 C6 -1.4(5) . . . . ?
C3 C4 C5 O5 -176.8(3) . . . . ?
C4 C5 C6 C1 1.4(5) . . . . ?
O5 C5 C6 C1 177.3(3) . . . . ?
C2 C1 C6 C5 0.6(5) . . . . ?
C7 C1 C6 C5 -172.7(3) . . . . ?
C6 C1 C7 O2 168.0(4) . . . . ?
C2 C1 C7 O2 -5.3(5) . . . . ?
C6 C1 C7 O1 -8.0(5) . . . . ?
C2 C1 C7 O1 178.7(3) . . . . ?
C2 C3 C8 O3 -9.3(5) . . . . ?
C4 C3 C8 O3 176.9(4) . . . . ?
C2 C3 C8 O4 166.3(3) . . . . ?
C4 C3 C8 O4 -7.4(5) . . . . ?
N5 C13 C14 N4 0.5(5) . . . . ?
N5 C15 C16 C16 -179.9(4) . . . 5_666 ?
N3 C11 N1 N2 0.5(4) . . . . ?
N3 C11 N1 C9 174.2(3) . . . . ?
O5 C9 N1 C11 -66.9(5) . . . . ?
O5 C9 N1 N2 106.1(4) . . . . ?
N3 C10 N2 N1 0.3(5) . . . . ?
C11 N1 N2 C10 -0.5(4) . . . . ?
C9 N1 N2 C10 -174.5(3) . . . . ?
N1 C11 N3 C10 -0.3(4) . . . . ?
N1 C11 N3 Zn1 179.5(2) . . . 3_455 ?
N2 C10 N3 C11 0.0(5) . . . . ?
N2 C10 N3 Zn1 -179.7(3) . . . 3_455 ?
N5 C12 N4 C14 -0.9(4) . . . . ?
N5 C12 N4 Zn1 173.9(2) . . . . ?
C13 C14 N4 C12 0.2(5) . . . . ?
C13 C14 N4 Zn1 -174.6(3) . . . . ?
O1 Zn1 N4 C12 -155.7(3) . . . . ?
O4 Zn1 N4 C12 94.7(3) 8_556 . . . ?
N3 Zn1 N4 C12 -29.6(3) 3_545 . . . ?
O1 Zn1 N4 C14 18.1(3) . . . . ?
O4 Zn1 N4 C14 -91.6(3) 8_556 . . . ?
N3 Zn1 N4 C14 144.2(3) 3_545 . . . ?
N4 C12 N5 C13 1.2(4) . . . . ?
N4 C12 N5 C15 -174.6(3) . . . . ?
C14 C13 N5 C12 -1.0(5) . . . . ?
C14 C13 N5 C15 175.0(4) . . . . ?
C16 C15 N5 C12 106.3(4) . . . . ?
C16 C15 N5 C13 -68.8(5) . . . . ?
O2 C7 O1 Zn1 -10.1(4) . . . . ?
C1 C7 O1 Zn1 165.9(2) . . . . ?
O4 Zn1 O1 C7 -169.6(2) 8_556 . . . ?
N4 Zn1 O1 C7 72.1(2) . . . . ?
N3 Zn1 O1 C7 -56.9(3) 3_545 . . . ?
O3 C8 O4 Zn1 11.1(5) . . . 8_455 ?
C3 C8 O4 Zn1 -164.4(2) . . . 8_455 ?
C6 C5 O5 C9 178.3(3) . . . . ?
C4 C5 O5 C9 -6.0(5) . . . . ?
N1 C9 O5 C5 -76.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.081

#=========================END
_database_code_depnum_ccdc_archive 'CCDC 978494'
