# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

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

data_a
_database_code_depnum_ccdc_archive 'CCDC 1437785'
_audit_update_record             
;
2016-01-15 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H42 Cu2 N20 O13'
_chemical_formula_weight         1041.94

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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   I2/a

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

_cell_length_a                   8.2134(16)
_cell_length_b                   16.974(3)
_cell_length_c                   19.396(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.13(3)
_cell_angle_gamma                90.00
_cell_volume                     2653.2(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2033
_cell_measurement_theta_min      2.1400
_cell_measurement_theta_max      27.8247

_exptl_crystal_description       Prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8449
_exptl_absorpt_correction_T_max  0.8449
_exptl_absorpt_process_details   ?

_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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8801
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_sigmaI/netI    0.1304
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2329
_reflns_number_gt                1114
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
ISOR 0.01 0.02 O3 
DELU 0.001 0.001 O3
;

_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)+(0.1253P)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         2329
_refine_ls_number_parameters     175
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1526
_refine_ls_R_factor_gt           0.0788
_refine_ls_wR_factor_ref         0.2485
_refine_ls_wR_factor_gt          0.2186
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4401(6) 0.0659(3) 0.1264(2) 0.0485(14) Uani 1 1 d . . .
C2 C 0.3217(6) 0.1055(3) 0.1675(3) 0.0586(16) Uani 1 1 d . . .
H2A H 0.2338 0.1316 0.1349 0.070 Uiso 1 1 calc R . .
H2B H 0.2713 0.0657 0.1924 0.070 Uiso 1 1 calc R . .
C3 C 0.5034(6) 0.1497(3) 0.2802(2) 0.0552(15) Uani 1 1 d . . .
H3 H 0.5220 0.1024 0.3045 0.066 Uiso 1 1 calc R . .
C4 C 0.5705(6) 0.2239(3) 0.3001(3) 0.0565(15) Uani 1 1 d . . .
C5 C 0.6919(6) 0.2467(3) 0.3655(2) 0.0667(17) Uani 1 1 d . . .
H5A H 0.7435 0.1996 0.3881 0.080 Uiso 1 1 calc R . .
H5B H 0.7784 0.2793 0.3526 0.080 Uiso 1 1 calc R . .
C6 C 0.5175(6) 0.2587(3) 0.4591(3) 0.0629(17) Uani 1 1 d . . .
H6 H 0.4928 0.2058 0.4647 0.075 Uiso 1 1 calc R . .
C7 C 0.4687(6) 0.3218(3) 0.4929(2) 0.0525(15) Uani 1 1 d . . .
H7 H 0.4022 0.3190 0.5265 0.063 Uiso 1 1 calc R . .
C8 C 0.6168(5) 0.3689(3) 0.4235(2) 0.0457(14) Uani 1 1 d . . .
H8 H 0.6741 0.4031 0.3993 0.055 Uiso 1 1 calc R . .
Cu1 Cu 0.5000 0.5000 0.5000 0.0427(2) Uani 1 2 d S . .
N1 N 0.5305(4) 0.3906(2) 0.47072(18) 0.0410(11) Uani 1 1 d . . .
N2 N 0.6108(4) 0.2903(2) 0.4152(2) 0.0505(12) Uani 1 1 d . . .
N3 N 0.4064(5) 0.1632(3) 0.2178(2) 0.0552(13) Uani 1 1 d . . .
N4 N 0.4122(5) 0.2391(3) 0.1985(2) 0.0646(14) Uani 1 1 d . . .
N5 N 0.5105(5) 0.2752(3) 0.2490(2) 0.0668(15) Uani 1 1 d . . .
O1 O 0.5898(4) 0.0684(2) 0.14833(18) 0.0619(11) Uani 1 1 d . . .
O2 O 0.3683(4) 0.0358(2) 0.06799(15) 0.0484(9) Uani 1 1 d . . .
O3 O 0.170(2) 0.5098(11) 0.1089(9) 0.097(5) Uani 0.25 1 d PGU . .
H3A H 0.1567 0.5556 0.0910 0.146 Uiso 0.25 1 d PG . .
H3B H 0.2579 0.5085 0.1400 0.146 Uiso 0.25 1 d PG . .
O4 O 0.3758(9) 0.5640(4) 0.7627(4) 0.064(2) Uani 0.50 1 d P . .
H4A H 0.3254 0.5835 0.7953 0.097 Uiso 0.50 1 d PR . .
H4B H 0.4379 0.6024 0.7529 0.097 Uiso 0.50 1 d PR . .
O5 O 0.6705(10) 0.8587(5) 0.4197(4) 0.097(3) Uani 0.50 1 d PG . .
H5C H 0.6680 0.8852 0.4567 0.145 Uiso 0.50 1 d PG . .
H5D H 0.6151 0.8165 0.4204 0.145 Uiso 0.50 1 d PG . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.222(5) . ?
C1 O2 1.279(5) . ?
C1 C2 1.527(7) . ?
C2 N3 1.460(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.334(6) . ?
C3 C4 1.398(7) . ?
C3 H3 0.9300 . ?
C4 N5 1.341(6) . ?
C4 C5 1.504(6) . ?
C5 N2 1.472(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N2 1.362(7) . ?
C6 C7 1.356(7) . ?
C6 H6 0.9300 . ?
C7 N1 1.374(6) . ?
C7 H7 0.9300 . ?
C8 N1 1.314(6) . ?
C8 N2 1.344(6) . ?
C8 H8 0.9300 . ?
Cu1 O2 1.957(3) 4 ?
Cu1 O2 1.957(3) 8 ?
Cu1 N1 1.972(4) 5_666 ?
Cu1 N1 1.972(4) . ?
N3 N4 1.346(6) . ?
N4 N5 1.297(6) . ?
O2 Cu1 1.957(3) 4_545 ?
O3 H3A 0.8503 . ?
O3 H3B 0.8498 . ?
O4 H4A 0.8856 . ?
O4 H4B 0.8718 . ?
O5 H5C 0.8501 . ?
O5 H5D 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 125.7(5) . . ?
O1 C1 C2 120.2(4) . . ?
O2 C1 C2 114.0(4) . . ?
N3 C2 C1 112.0(4) . . ?
N3 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N3 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N3 C3 C4 103.3(4) . . ?
N3 C3 H3 128.3 . . ?
C4 C3 H3 128.3 . . ?
N5 C4 C3 108.2(4) . . ?
N5 C4 C5 122.9(5) . . ?
C3 C4 C5 128.9(5) . . ?
N2 C5 C4 111.8(4) . . ?
N2 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
N2 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
N2 C6 C7 104.2(5) . . ?
N2 C6 H6 127.9 . . ?
C7 C6 H6 127.9 . . ?
C6 C7 N1 111.1(5) . . ?
C6 C7 H7 124.5 . . ?
N1 C7 H7 124.5 . . ?
N1 C8 N2 110.5(4) . . ?
N1 C8 H8 124.7 . . ?
N2 C8 H8 124.7 . . ?
O2 Cu1 O2 180 4 8 ?
O2 Cu1 N1 91.09(15) 4 5_666 ?
O2 Cu1 N1 88.91(15) 8 5_666 ?
O2 Cu1 N1 88.91(15) 4 . ?
O2 Cu1 N1 91.09(15) 8 . ?
N1 Cu1 N1 180 5_666 . ?
C8 N1 C7 105.1(4) . . ?
C8 N1 Cu1 125.4(3) . . ?
C7 N1 Cu1 129.4(3) . . ?
C8 N2 C6 109.1(4) . . ?
C8 N2 C5 124.5(4) . . ?
C6 N2 C5 126.4(4) . . ?
C3 N3 N4 111.7(4) . . ?
C3 N3 C2 127.9(4) . . ?
N4 N3 C2 119.6(4) . . ?
N5 N4 N3 107.0(4) . . ?
N4 N5 C4 109.7(4) . . ?
C1 O2 Cu1 120.1(3) . 4_545 ?
H3A O3 H3B 109.5 . . ?
H4A O4 H4B 104.5 . . ?
H5C O5 H5D 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N3 18.1(6) . . . . ?
O2 C1 C2 N3 -158.2(4) . . . . ?
N3 C3 C4 N5 -0.3(6) . . . . ?
N3 C3 C4 C5 -179.0(5) . . . . ?
N5 C4 C5 N2 75.7(6) . . . . ?
C3 C4 C5 N2 -105.8(6) . . . . ?
N2 C6 C7 N1 -0.2(5) . . . . ?
N2 C8 N1 C7 0.3(4) . . . . ?
N2 C8 N1 Cu1 -179.1(3) . . . . ?
C6 C7 N1 C8 0.0(5) . . . . ?
C6 C7 N1 Cu1 179.4(3) . . . . ?
O2 Cu1 N1 C8 1.5(3) 4 . . . ?
O2 Cu1 N1 C8 -178.5(3) 8 . . . ?
N1 Cu1 N1 C8 153(100) 5_666 . . . ?
O2 Cu1 N1 C7 -177.8(3) 4 . . . ?
O2 Cu1 N1 C7 2.2(3) 8 . . . ?
N1 Cu1 N1 C7 -27(100) 5_666 . . . ?
N1 C8 N2 C6 -0.5(5) . . . . ?
N1 C8 N2 C5 178.9(4) . . . . ?
C7 C6 N2 C8 0.4(5) . . . . ?
C7 C6 N2 C5 -178.9(4) . . . . ?
C4 C5 N2 C8 -101.3(5) . . . . ?
C4 C5 N2 C6 77.9(6) . . . . ?
C4 C3 N3 N4 0.9(5) . . . . ?
C4 C3 N3 C2 171.1(5) . . . . ?
C1 C2 N3 C3 -77.2(6) . . . . ?
C1 C2 N3 N4 92.2(5) . . . . ?
C3 N3 N4 N5 -1.2(6) . . . . ?
C2 N3 N4 N5 -172.3(4) . . . . ?
N3 N4 N5 C4 1.0(6) . . . . ?
C3 C4 N5 N4 -0.4(6) . . . . ?
C5 C4 N5 N4 178.4(5) . . . . ?
O1 C1 O2 Cu1 -7.4(6) . . . 4_545 ?
C2 C1 O2 Cu1 168.6(3) . . . 4_545 ?

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
O4 H4A O3 0.89 2.23 2.747(19) 116.7 2_556
O4 H4B N5 0.87 2.12 2.907(8) 149.7 5_666
O5 H5C O5 0.85 2.55 3.136(16) 127.4 2_656
O5 H5D N4 0.85 2.62 3.039(9) 111.3 4

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.121
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1437786'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H16 Co N10 O4'
_chemical_formula_weight         471.32

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'
Cl Cl 0.1484 0.1585 '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   P2(1)/c

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

_cell_length_a                   4.8427(10)
_cell_length_b                   9.4938(19)
_cell_length_c                   20.097(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.37(3)
_cell_angle_gamma                90.00
_cell_volume                     923.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2439
_cell_measurement_theta_min      2.1451
_cell_measurement_theta_max      30.8683

_exptl_crystal_description       Prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             482
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8279
_exptl_absorpt_correction_T_max  0.8279
_exptl_absorpt_process_details   ?

_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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6033
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1628
_reflns_number_gt                1406
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0858P)²+0.6757P] 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         1628
_refine_ls_number_parameters     142
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1544
_refine_ls_wR_factor_gt          0.1466
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7391(9) 0.0759(4) 0.2521(2) 0.0329(10) Uani 1 1 d . . .
H1 H 0.7104 0.1724 0.2557 0.039 Uiso 1 1 calc R . .
C2 C 0.9172(8) -0.0033(4) 0.28868(17) 0.0167(8) Uani 1 1 d . . .
C3 C 0.3985(11) 0.0106(5) 0.1532(2) 0.0417(12) Uani 1 1 d . . .
H3A H 0.3447 -0.0789 0.1333 0.050 Uiso 1 1 calc R . .
H3B H 0.2353 0.0534 0.1710 0.050 Uiso 1 1 calc R . .
C4 C 0.4362(9) 0.2365(5) 0.0897(2) 0.0350(10) Uani 1 1 d . . .
H4 H 0.2968 0.2832 0.1113 0.042 Uiso 1 1 calc R . .
C5 C 0.7183(10) 0.0731(5) 0.0610(3) 0.0459(12) Uani 1 1 d . . .
H5 H 0.8132 -0.0116 0.0579 0.055 Uiso 1 1 calc R . .
C6 C 0.7606(10) 0.1918(5) 0.0258(2) 0.0402(11) Uani 1 1 d . . .
H6 H 0.8922 0.2019 -0.0063 0.048 Uiso 1 1 calc R . .
C7 C 1.1101(9) 0.0395(5) 0.3425(2) 0.0334(10) Uani 1 1 d . . .
H7A H 1.1954 0.1277 0.3301 0.040 Uiso 1 1 calc R . .
H7B H 1.2554 -0.0306 0.3469 0.040 Uiso 1 1 calc R . .
C8 C 0.9840(8) 0.0585(4) 0.4099(2) 0.0265(9) Uani 1 1 d . . .
Co1 Co 0.5000 0.0000 0.5000 0.0262(3) Uani 1 2 d S . .
N1 N 0.5078(7) 0.1026(4) 0.10213(17) 0.0339(9) Uani 1 1 d . . .
N2 N 0.5832(7) 0.2946(4) 0.04407(16) 0.0299(8) Uani 1 1 d . . .
N3 N 0.6093(10) -0.0141(4) 0.2085(2) 0.0477(11) Uani 1 1 d . . .
N4 N 0.7128(10) -0.1450(4) 0.2208(2) 0.0501(11) Uani 1 1 d . . .
N5 N 0.9024(9) -0.1368(4) 0.2698(2) 0.0500(11) Uani 1 1 d . . .
O1 O 1.1497(5) 0.0936(3) 0.45592(13) 0.0326(7) Uani 1 1 d . . .
O2 O 0.7272(6) 0.0429(3) 0.41367(14) 0.0332(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.341(6) . ?
C1 N3 1.358(6) . ?
C1 H1 0.9300 . ?
C2 N5 1.325(5) . ?
C2 C7 1.458(6) . ?
C3 N1 1.464(6) . ?
C3 N3 1.497(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N2 1.307(5) . ?
C4 N1 1.338(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.351(7) . ?
C5 N1 1.367(6) . ?
C5 H5 0.9300 . ?
C6 N2 1.361(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.519(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O1 1.244(5) . ?
C8 O2 1.258(5) . ?
Co1 O1 2.080(3) 3_756 ?
Co1 O1 2.080(3) 1_455 ?
Co1 O2 2.132(3) 3_656 ?
Co1 O2 2.132(3) . ?
Co1 N2 2.172(3) 2_645 ?
Co1 N2 2.172(3) 4_566 ?
N2 Co1 2.172(3) 2_655 ?
N3 N4 1.359(6) . ?
N4 N5 1.321(5) . ?
O1 Co1 2.080(3) 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
C2 C1 N3 105.7(4) . . ?
C2 C1 H1 127.1 . . ?
N3 C1 H1 127.1 . . ?
N5 C2 C1 110.7(4) . . ?
N5 C2 C7 120.3(4) . . ?
C1 C2 C7 129.0(4) . . ?
N1 C3 N3 111.1(4) . . ?
N1 C3 H3A 109.4 . . ?
N3 C3 H3A 109.4 . . ?
N1 C3 H3B 109.4 . . ?
N3 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N2 C4 N1 112.8(4) . . ?
N2 C4 H4 123.6 . . ?
N1 C4 H4 123.6 . . ?
C6 C5 N1 106.2(4) . . ?
C6 C5 H5 126.9 . . ?
N1 C5 H5 126.9 . . ?
C5 C6 N2 110.2(4) . . ?
C5 C6 H6 124.9 . . ?
N2 C6 H6 124.9 . . ?
C2 C7 C8 115.2(3) . . ?
C2 C7 H7A 108.5 . . ?
C8 C7 H7A 108.5 . . ?
C2 C7 H7B 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
O1 C8 O2 126.5(4) . . ?
O1 C8 C7 115.1(3) . . ?
O2 C8 C7 118.3(4) . . ?
O1 Co1 O1 180 3_756 1_455 ?
O1 Co1 O2 90.64(11) 3_756 3_656 ?
O1 Co1 O2 89.36(11) 1_455 3_656 ?
O1 Co1 O2 89.36(11) 3_756 . ?
O1 Co1 O2 90.64(11) 1_455 . ?
O2 Co1 O2 180 3_656 . ?
O1 Co1 N2 85.65(12) 3_756 2_645 ?
O1 Co1 N2 94.35(12) 1_455 2_645 ?
O2 Co1 N2 93.86(12) 3_656 2_645 ?
O2 Co1 N2 86.14(12) . 2_645 ?
O1 Co1 N2 94.35(12) 3_756 4_566 ?
O1 Co1 N2 85.65(12) 1_455 4_566 ?
O2 Co1 N2 86.14(12) 3_656 4_566 ?
O2 Co1 N2 93.86(12) . 4_566 ?
N2 Co1 N2 180 2_645 4_566 ?
C4 N1 C5 106.0(4) . . ?
C4 N1 C3 126.8(4) . . ?
C5 N1 C3 127.0(4) . . ?
C4 N2 C6 104.8(4) . . ?
C4 N2 Co1 124.6(3) . 2_655 ?
C6 N2 Co1 130.0(3) . 2_655 ?
C1 N3 N4 107.5(4) . . ?
C1 N3 C3 131.6(4) . . ?
N4 N3 C3 120.9(4) . . ?
N5 N4 N3 108.8(4) . . ?
N4 N5 C2 107.3(4) . . ?
C8 O1 Co1 133.7(3) . 1_655 ?
C8 O2 Co1 128.1(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
N3 C1 C2 N5 -0.1(5) . . . . ?
N3 C1 C2 C7 179.7(4) . . . . ?
N1 C5 C6 N2 0.2(6) . . . . ?
N5 C2 C7 C8 -100.0(5) . . . . ?
C1 C2 C7 C8 80.3(5) . . . . ?
C2 C7 C8 O1 179.3(4) . . . . ?
C2 C7 C8 O2 -3.2(6) . . . . ?
N2 C4 N1 C5 0.1(5) . . . . ?
N2 C4 N1 C3 175.5(4) . . . . ?
C6 C5 N1 C4 -0.2(5) . . . . ?
C6 C5 N1 C3 -175.6(4) . . . . ?
N3 C3 N1 C4 -108.3(5) . . . . ?
N3 C3 N1 C5 66.1(6) . . . . ?
N1 C4 N2 C6 0.0(5) . . . . ?
N1 C4 N2 Co1 171.6(3) . . . 2_655 ?
C5 C6 N2 C4 -0.2(5) . . . . ?
C5 C6 N2 Co1 -171.2(3) . . . 2_655 ?
C2 C1 N3 N4 0.4(5) . . . . ?
C2 C1 N3 C3 -177.1(5) . . . . ?
N1 C3 N3 C1 61.5(7) . . . . ?
N1 C3 N3 N4 -115.7(5) . . . . ?
C1 N3 N4 N5 -0.6(6) . . . . ?
C3 N3 N4 N5 177.2(4) . . . . ?
N3 N4 N5 C2 0.5(6) . . . . ?
C1 C2 N5 N4 -0.3(5) . . . . ?
C7 C2 N5 N4 180.0(4) . . . . ?
O2 C8 O1 Co1 121.5(4) . . . 1_655 ?
C7 C8 O1 Co1 -61.2(5) . . . 1_655 ?
O1 C8 O2 Co1 -23.0(6) . . . . ?
C7 C8 O2 Co1 159.8(3) . . . . ?
O1 Co1 O2 C8 -26.0(4) 3_756 . . . ?
O1 Co1 O2 C8 154.0(4) 1_455 . . . ?
O2 Co1 O2 C8 131(100) 3_656 . . . ?
N2 Co1 O2 C8 -111.7(4) 2_645 . . . ?
N2 Co1 O2 C8 68.3(4) 4_566 . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.089
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1437787'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H16 Mn N10 O4'
_chemical_formula_weight         467.33

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

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

_cell_length_a                   4.9140(10)
_cell_length_b                   9.3923(19)
_cell_length_c                   20.417(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.66(3)
_cell_angle_gamma                90.00
_cell_volume                     941.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    288(2)
_cell_measurement_reflns_used    2486
_cell_measurement_theta_min      1.9970
_cell_measurement_theta_max      27.8406

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             478
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8641
_exptl_absorpt_correction_T_max  0.8641
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      288(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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7614
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.84
_reflns_number_total             2219
_reflns_number_gt                1784
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0391P)²+0.3753P] 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         2219
_refine_ls_number_parameters     142
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0960(6) 0.0008(4) 0.34344(14) 0.0473(8) Uani 1 1 d . . .
H1A H 1.1524 -0.0900 0.3621 0.057 Uiso 1 1 calc R . .
H1B H 1.2552 0.0462 0.3263 0.057 Uiso 1 1 calc R . .
C2 C 0.8887(5) -0.0237(3) 0.28868(13) 0.0356(6) Uani 1 1 d . . .
C3 C 0.7615(6) 0.0695(3) 0.24654(13) 0.0378(6) Uani 1 1 d . . .
H3 H 0.7919 0.1671 0.2439 0.045 Uiso 1 1 calc R . .
C4 C 0.3938(5) 0.0381(3) 0.15727(12) 0.0363(6) Uani 1 1 d . . .
H4A H 0.3073 0.1258 0.1703 0.044 Uiso 1 1 calc R . .
H4B H 0.2525 -0.0336 0.1517 0.044 Uiso 1 1 calc R . .
C5 C 0.5213(5) 0.0620(3) 0.09148(12) 0.0311(6) Uani 1 1 d . . .
C6 C 0.7366(6) 0.1787(3) 0.46988(15) 0.0485(8) Uani 1 1 d . . .
H6 H 0.6059 0.1879 0.5011 0.058 Uiso 1 1 calc R . .
C7 C 1.0602(6) 0.2258(3) 0.40763(13) 0.0420(7) Uani 1 1 d . . .
H7 H 1.1982 0.2733 0.3869 0.050 Uiso 1 1 calc R . .
C8 C 0.7804(7) 0.0598(4) 0.43457(17) 0.0555(9) Uani 1 1 d . . .
H8 H 0.6872 -0.0261 0.4368 0.067 Uiso 1 1 calc R . .
Mn1 Mn 1.0000 0.0000 0.0000 0.03379(19) Uani 1 2 d S . .
N1 N 0.5850(4) -0.0069(2) 0.20992(10) 0.0306(5) Uani 1 1 d . . .
N2 N 0.6003(6) -0.1435(3) 0.22701(13) 0.0559(8) Uani 1 1 d . . .
N3 N 0.7863(6) -0.1532(3) 0.27554(13) 0.0576(8) Uani 1 1 d . . .
N4 N 0.9882(5) 0.0908(3) 0.39500(11) 0.0389(6) Uani 1 1 d . . .
N5 N 0.9126(4) 0.2835(3) 0.45286(11) 0.0382(6) Uani 1 1 d . . .
O1 O 0.7726(3) 0.0455(2) 0.08829(9) 0.0422(5) Uani 1 1 d . . .
O2 O 0.3579(3) 0.1012(2) 0.04619(9) 0.0414(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N4 1.468(3) . ?
C1 C2 1.495(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.338(4) . ?
C2 C3 1.359(4) . ?
C3 N1 1.329(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.457(3) . ?
C4 C5 1.525(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O1 1.249(3) . ?
C5 O2 1.252(3) . ?
C6 C8 1.353(4) . ?
C6 N5 1.366(4) . ?
C6 H6 0.9300 . ?
C7 N5 1.317(3) . ?
C7 N4 1.338(4) . ?
C7 H7 0.9300 . ?
C8 N4 1.363(4) . ?
C8 H8 0.9300 . ?
Mn1 O2 2.1753(19) 1_655 ?
Mn1 O2 2.1753(19) 3_655 ?
Mn1 O1 2.2061(19) . ?
Mn1 O1 2.2061(19) 3_755 ?
Mn1 N5 2.282(2) 4_565 ?
Mn1 N5 2.282(2) 2_745 ?
N1 N2 1.331(3) . ?
N2 N3 1.320(3) . ?
N5 Mn1 2.282(2) 2_755 ?
O2 Mn1 2.1753(19) 1_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
N4 C1 C2 111.6(2) . . ?
N4 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N4 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C3 107.5(2) . . ?
N3 C2 C1 121.8(3) . . ?
C3 C2 C1 130.6(3) . . ?
N1 C3 C2 106.1(2) . . ?
N1 C3 H3 127.0 . . ?
C2 C3 H3 127.0 . . ?
N1 C4 C5 114.5(2) . . ?
N1 C4 H4A 108.6 . . ?
C5 C4 H4A 108.6 . . ?
N1 C4 H4B 108.6 . . ?
C5 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
O1 C5 O2 126.9(2) . . ?
O1 C5 C4 118.4(2) . . ?
O2 C5 C4 114.7(2) . . ?
C8 C6 N5 110.0(3) . . ?
C8 C6 H6 125.0 . . ?
N5 C6 H6 125.0 . . ?
N5 C7 N4 112.1(3) . . ?
N5 C7 H7 124.0 . . ?
N4 C7 H7 124.0 . . ?
C6 C8 N4 106.4(3) . . ?
C6 C8 H8 126.8 . . ?
N4 C8 H8 126.8 . . ?
O2 Mn1 O2 180 1_655 3_655 ?
O2 Mn1 O1 89.49(7) 1_655 . ?
O2 Mn1 O1 90.51(7) 3_655 . ?
O2 Mn1 O1 90.51(7) 1_655 3_755 ?
O2 Mn1 O1 89.49(7) 3_655 3_755 ?
O1 Mn1 O1 180 . 3_755 ?
O2 Mn1 N5 85.76(8) 1_655 4_565 ?
O2 Mn1 N5 94.24(8) 3_655 4_565 ?
O1 Mn1 N5 94.56(8) . 4_565 ?
O1 Mn1 N5 85.44(8) 3_755 4_565 ?
O2 Mn1 N5 94.24(8) 1_655 2_745 ?
O2 Mn1 N5 85.76(8) 3_655 2_745 ?
O1 Mn1 N5 85.44(8) . 2_745 ?
O1 Mn1 N5 94.56(8) 3_755 2_745 ?
N5 Mn1 N5 180 4_565 2_745 ?
C3 N1 N2 110.2(2) . . ?
C3 N1 C4 129.8(2) . . ?
N2 N1 C4 120.0(2) . . ?
N3 N2 N1 107.0(2) . . ?
N2 N3 C2 109.2(2) . . ?
C7 N4 C8 106.7(3) . . ?
C7 N4 C1 125.6(3) . . ?
C8 N4 C1 127.4(3) . . ?
C7 N5 C6 104.9(2) . . ?
C7 N5 Mn1 124.3(2) . 2_755 ?
C6 N5 Mn1 130.07(19) . 2_755 ?
C5 O1 Mn1 127.30(17) . . ?
C5 O2 Mn1 132.06(18) . 1_455 ?

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
N4 C1 C2 N3 -114.5(3) . . . . ?
N4 C1 C2 C3 62.3(4) . . . . ?
N3 C2 C3 N1 0.6(3) . . . . ?
C1 C2 C3 N1 -176.5(3) . . . . ?
N1 C4 C5 O1 -1.8(4) . . . . ?
N1 C4 C5 O2 -179.7(2) . . . . ?
N5 C6 C8 N4 0.2(4) . . . . ?
C2 C3 N1 N2 -0.8(3) . . . . ?
C2 C3 N1 C4 179.6(2) . . . . ?
C5 C4 N1 C3 78.9(3) . . . . ?
C5 C4 N1 N2 -100.6(3) . . . . ?
C3 N1 N2 N3 0.7(3) . . . . ?
C4 N1 N2 N3 -179.6(2) . . . . ?
N1 N2 N3 C2 -0.3(4) . . . . ?
C3 C2 N3 N2 -0.2(4) . . . . ?
C1 C2 N3 N2 177.3(3) . . . . ?
N5 C7 N4 C8 0.1(3) . . . . ?
N5 C7 N4 C1 174.4(2) . . . . ?
C6 C8 N4 C7 -0.2(4) . . . . ?
C6 C8 N4 C1 -174.4(3) . . . . ?
C2 C1 N4 C7 -108.5(3) . . . . ?
C2 C1 N4 C8 64.6(4) . . . . ?
N4 C7 N5 C6 0.0(3) . . . . ?
N4 C7 N5 Mn1 171.25(17) . . . 2_755 ?
C8 C6 N5 C7 -0.1(4) . . . . ?
C8 C6 N5 Mn1 -170.7(2) . . . 2_755 ?
O2 C5 O1 Mn1 -24.7(4) . . . . ?
C4 C5 O1 Mn1 157.69(19) . . . . ?
O2 Mn1 O1 C5 153.1(2) 1_655 . . . ?
O2 Mn1 O1 C5 -26.9(2) 3_655 . . . ?
O1 Mn1 O1 C5 -80(100) 3_755 . . . ?
N5 Mn1 O1 C5 67.4(2) 4_565 . . . ?
N5 Mn1 O1 C5 -112.6(2) 2_745 . . . ?
O1 C5 O2 Mn1 120.6(3) . . . 1_455 ?
C4 C5 O2 Mn1 -61.7(3) . . . 1_455 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.84
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.057
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1437788'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H16 Cd N10 O4'
_chemical_formula_weight         524.79

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   4.9534(10)
_cell_length_b                   9.1796(18)
_cell_length_c                   20.865(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.90(3)
_cell_angle_gamma                90.00
_cell_volume                     946.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2654
_cell_measurement_theta_min      2.2185
_cell_measurement_theta_max      30.7796

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             524
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7947
_exptl_absorpt_correction_T_max  0.7947
_exptl_absorpt_process_details   ?

_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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6072
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1656
_reflns_number_gt                1422
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0258P)²+0.5072P] 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         1656
_refine_ls_number_parameters     142
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0706
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2835(9) 0.4530(5) 0.4303(2) 0.0566(12) Uani 1 1 d . . .
H1 H 0.1928 0.5416 0.4313 0.068 Uiso 1 1 calc R . .
C2 C 0.2411(8) 0.3341(5) 0.46625(19) 0.0524(11) Uani 1 1 d . . .
H2 H 0.1138 0.3278 0.4969 0.063 Uiso 1 1 calc R . .
C3 C 0.5553(8) 0.2790(5) 0.40641(18) 0.0448(10) Uani 1 1 d . . .
H3 H 0.6892 0.2279 0.3868 0.054 Uiso 1 1 calc R . .
C4 C 0.5923(8) 0.5055(5) 0.34129(19) 0.0525(11) Uani 1 1 d . . .
H4A H 0.7513 0.4587 0.3260 0.063 Uiso 1 1 calc R . .
H4B H 0.6465 0.5999 0.3586 0.063 Uiso 1 1 calc R . .
C5 C 0.0377(7) 0.4290(4) 0.09235(17) 0.0337(8) Uani 1 1 d . . .
C6 C -0.0968(7) 0.4576(4) 0.15444(17) 0.0398(10) Uani 1 1 d . . .
H6A H -0.2351 0.5314 0.1464 0.048 Uiso 1 1 calc R . .
H6B H -0.1859 0.3691 0.1670 0.048 Uiso 1 1 calc R . .
C7 C 0.3857(8) 0.5263(4) 0.28604(17) 0.0377(9) Uani 1 1 d . . .
C8 C 0.2627(8) 0.4297(4) 0.24466(19) 0.0422(9) Uani 1 1 d . . .
H8 H 0.2951 0.3301 0.2428 0.051 Uiso 1 1 calc R . .
Cd1 Cd 0.5000 0.0000 0.5000 0.03780(15) Uani 1 2 d S . .
N1 N 0.4869(6) 0.4168(4) 0.39220(14) 0.0413(8) Uani 1 1 d . . .
N2 N 0.4119(6) 0.2242(4) 0.45122(15) 0.0422(8) Uani 1 1 d . . .
N3 N 0.0871(6) 0.5053(3) 0.20748(13) 0.0335(7) Uani 1 1 d . . .
N4 N 0.2824(8) 0.6580(4) 0.27171(18) 0.0649(11) Uani 1 1 d . . .
N5 N 0.0965(8) 0.6453(4) 0.22323(18) 0.0638(11) Uani 1 1 d . . .
O1 O -0.1172(5) 0.3846(3) 0.04640(12) 0.0475(7) Uani 1 1 d . . .
O2 O 0.2846(5) 0.4489(3) 0.09198(12) 0.0499(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.349(6) . ?
C1 N1 1.366(5) . ?
C1 H1 0.9300 . ?
C2 N2 1.366(5) . ?
C2 H2 0.9300 . ?
C3 N2 1.312(5) . ?
C3 N1 1.337(5) . ?
C3 H3 0.9300 . ?
C4 N1 1.463(5) . ?
C4 C7 1.501(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O2 1.237(4) . ?
C5 O1 1.254(4) . ?
C5 C6 1.519(5) . ?
C6 N3 1.452(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N4 1.339(5) . ?
C7 C8 1.353(5) . ?
C8 N3 1.322(5) . ?
C8 H8 0.9300 . ?
Cd1 O2 2.306(2) 4_566 ?
Cd1 O2 2.306(2) 2_645 ?
Cd1 O1 2.325(3) 4_666 ?
Cd1 O1 2.325(3) 2_545 ?
Cd1 N2 2.324(3) 3_656 ?
Cd1 N2 2.324(3) . ?
N3 N5 1.326(4) . ?
N4 N5 1.326(5) . ?
O1 Cd1 2.325(3) 2 ?
O2 Cd1 2.306(2) 2_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
C2 C1 N1 106.0(4) . . ?
C2 C1 H1 127.0 . . ?
N1 C1 H1 127.0 . . ?
C1 C2 N2 110.3(4) . . ?
C1 C2 H2 124.8 . . ?
N2 C2 H2 124.8 . . ?
N2 C3 N1 112.3(3) . . ?
N2 C3 H3 123.9 . . ?
N1 C3 H3 123.9 . . ?
N1 C4 C7 111.7(3) . . ?
N1 C4 H4A 109.3 . . ?
C7 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C7 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
O2 C5 O1 126.6(3) . . ?
O2 C5 C6 118.1(3) . . ?
O1 C5 C6 115.3(3) . . ?
N3 C6 C5 114.4(3) . . ?
N3 C6 H6A 108.7 . . ?
C5 C6 H6A 108.7 . . ?
N3 C6 H6B 108.7 . . ?
C5 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
N4 C7 C8 107.5(3) . . ?
N4 C7 C4 121.1(4) . . ?
C8 C7 C4 131.3(4) . . ?
N3 C8 C7 106.3(3) . . ?
N3 C8 H8 126.9 . . ?
C7 C8 H8 126.9 . . ?
O2 Cd1 O2 180 4_566 2_645 ?
O2 Cd1 O1 88.35(9) 4_566 4_666 ?
O2 Cd1 O1 91.65(9) 2_645 4_666 ?
O2 Cd1 O1 91.65(9) 4_566 2_545 ?
O2 Cd1 O1 88.35(9) 2_645 2_545 ?
O1 Cd1 O1 180 4_666 2_545 ?
O2 Cd1 N2 84.23(11) 4_566 3_656 ?
O2 Cd1 N2 95.77(11) 2_645 3_656 ?
O1 Cd1 N2 95.61(10) 4_666 3_656 ?
O1 Cd1 N2 84.39(10) 2_545 3_656 ?
O2 Cd1 N2 95.77(11) 4_566 . ?
O2 Cd1 N2 84.23(11) 2_645 . ?
O1 Cd1 N2 84.39(10) 4_666 . ?
O1 Cd1 N2 95.61(10) 2_545 . ?
N2 Cd1 N2 180 3_656 . ?
C3 N1 C1 106.7(3) . . ?
C3 N1 C4 126.2(4) . . ?
C1 N1 C4 126.9(4) . . ?
C3 N2 C2 104.7(3) . . ?
C3 N2 Cd1 123.8(3) . . ?
C2 N2 Cd1 130.8(3) . . ?
C8 N3 N5 110.6(3) . . ?
C8 N3 C6 130.0(3) . . ?
N5 N3 C6 119.4(3) . . ?
N5 N4 C7 109.0(3) . . ?
N3 N5 N4 106.6(3) . . ?
C5 O1 Cd1 127.5(2) . 2 ?
C5 O2 Cd1 123.3(2) . 2_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -0.4(5) . . . . ?
O2 C5 C6 N3 -0.4(5) . . . . ?
O1 C5 C6 N3 178.5(3) . . . . ?
N1 C4 C7 N4 114.0(5) . . . . ?
N1 C4 C7 C8 -63.2(6) . . . . ?
N4 C7 C8 N3 -0.9(5) . . . . ?
C4 C7 C8 N3 176.7(4) . . . . ?
N2 C3 N1 C1 -0.4(5) . . . . ?
N2 C3 N1 C4 -175.1(3) . . . . ?
C2 C1 N1 C3 0.5(5) . . . . ?
C2 C1 N1 C4 175.1(4) . . . . ?
C7 C4 N1 C3 107.2(4) . . . . ?
C7 C4 N1 C1 -66.4(6) . . . . ?
N1 C3 N2 C2 0.2(5) . . . . ?
N1 C3 N2 Cd1 -171.7(2) . . . . ?
C1 C2 N2 C3 0.1(5) . . . . ?
C1 C2 N2 Cd1 171.2(3) . . . . ?
O2 Cd1 N2 C3 157.3(3) 4_566 . . . ?
O2 Cd1 N2 C3 -22.7(3) 2_645 . . . ?
O1 Cd1 N2 C3 69.5(3) 4_666 . . . ?
O1 Cd1 N2 C3 -110.5(3) 2_545 . . . ?
N2 Cd1 N2 C3 -97(100) 3_656 . . . ?
O2 Cd1 N2 C2 -12.4(4) 4_566 . . . ?
O2 Cd1 N2 C2 167.6(4) 2_645 . . . ?
O1 Cd1 N2 C2 -100.1(4) 4_666 . . . ?
O1 Cd1 N2 C2 79.9(4) 2_545 . . . ?
N2 Cd1 N2 C2 93(100) 3_656 . . . ?
C7 C8 N3 N5 0.7(4) . . . . ?
C7 C8 N3 C6 179.2(3) . . . . ?
C5 C6 N3 C8 -76.3(5) . . . . ?
C5 C6 N3 N5 102.1(4) . . . . ?
C8 C7 N4 N5 0.8(5) . . . . ?
C4 C7 N4 N5 -177.0(4) . . . . ?
C8 N3 N5 N4 -0.2(5) . . . . ?
C6 N3 N5 N4 -178.8(3) . . . . ?
C7 N4 N5 N3 -0.4(5) . . . . ?
O2 C5 O1 Cd1 -122.8(4) . . . 2 ?
C6 C5 O1 Cd1 58.3(4) . . . 2 ?
O1 C5 O2 Cd1 25.8(6) . . . 2_655 ?
C6 C5 O2 Cd1 -155.3(3) . . . 2_655 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.065
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a
_database_code_depnum_ccdc_archive 'CCDC 1437789'
_audit_update_record             
;
2016-01-15 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H16 N10 O4 Pb'
_chemical_formula_weight         619.59

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pccn

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

_cell_length_a                   10.487(2)
_cell_length_b                   23.350(5)
_cell_length_c                   8.3772(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2051.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3777
_cell_measurement_theta_min      1.7442
_cell_measurement_theta_max      27.8804

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    8.272
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2885
_exptl_absorpt_correction_T_max  0.2885
_exptl_absorpt_process_details   ?

_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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7875
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         27.88
_reflns_number_total             2427
_reflns_number_gt                1648
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0198P)²+3.4289P] 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         2427
_refine_ls_number_parameters     141
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0687
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_restrained_S_all      1.168
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5876(10) 1.2070(4) 0.6554(12) 0.073(3) Uani 1 1 d . . .
H1A H 0.6083 1.2345 0.5793 0.087 Uiso 1 1 calc R . .
C2 C 0.4853(8) 1.1595(3) 0.8283(9) 0.0471(19) Uani 1 1 d . . .
H2A H 0.4215 1.1468 0.8968 0.057 Uiso 1 1 calc R . .
C3 C 0.6649(9) 1.1653(4) 0.7050(12) 0.068(3) Uani 1 1 d . . .
H3A H 0.7477 1.1586 0.6699 0.081 Uiso 1 1 calc R . .
C4 C 0.6364(8) 1.0808(3) 0.8936(9) 0.053(2) Uani 1 1 d . . .
H4A H 0.5972 1.0789 0.9984 0.063 Uiso 1 1 calc R . .
H4B H 0.7282 1.0799 0.9079 0.063 Uiso 1 1 calc R . .
C5 C 0.5959(7) 1.0299(3) 0.7972(9) 0.0395(18) Uani 1 1 d . . .
C6 C 0.6661(7) 0.9908(3) 0.7146(9) 0.0429(18) Uani 1 1 d . . .
H6A H 0.7543 0.9894 0.7036 0.052 Uiso 1 1 calc R . .
C9 C 0.6037(7) 0.9019(3) 0.5673(8) 0.0429(19) Uani 1 1 d . . .
H9A H 0.6709 0.9080 0.4897 0.051 Uiso 1 1 calc R . .
H9B H 0.5272 0.8908 0.5099 0.051 Uiso 1 1 calc R . .
C10 C 0.6423(7) 0.8536(3) 0.6798(8) 0.0394(18) Uani 1 1 d . . .
N1 N 0.4728(7) 1.2032(3) 0.7336(8) 0.0552(18) Uani 1 1 d . . .
N2 N 0.6002(6) 1.1346(2) 0.8164(7) 0.0444(16) Uani 1 1 d . . .
N3 N 0.5800(6) 0.9548(2) 0.6526(7) 0.0370(14) Uani 1 1 d . . .
N4 N 0.4611(6) 0.9695(2) 0.6914(8) 0.0448(16) Uani 1 1 d . . .
N5 N 0.4719(6) 1.0161(3) 0.7803(8) 0.0482(16) Uani 1 1 d . . .
O1 O 0.6881(5) 0.8098(2) 0.6160(5) 0.0476(14) Uani 1 1 d . . .
O2 O 0.6263(7) 0.8590(2) 0.8241(6) 0.084(2) Uani 1 1 d . . .
Pb1 Pb 0.7500 0.7500 0.84219(4) 0.03866(13) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.333(12) . ?
C1 N1 1.374(11) . ?
C1 H1A 0.9300 . ?
C2 N1 1.300(9) . ?
C2 N2 1.341(9) . ?
C2 H2A 0.9300 . ?
C3 N2 1.358(10) . ?
C3 H3A 0.9300 . ?
C4 N2 1.464(9) . ?
C4 C5 1.499(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N5 1.347(8) . ?
C5 C6 1.362(9) . ?
C6 N3 1.338(8) . ?
C6 H6A 0.9300 . ?
C9 N3 1.450(8) . ?
C9 C10 1.523(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 O2 1.227(8) . ?
C10 O1 1.251(8) . ?
N1 Pb1 2.656(7) 3_476 ?
N3 N4 1.333(8) . ?
N4 N5 1.324(8) . ?
O1 Pb1 2.441(5) . ?
O1 Pb1 2.762(5) 7_755 ?
O2 Pb1 2.861(5) . ?
Pb1 O1 2.441(5) 2_665 ?
Pb1 N1 2.656(7) 4_646 ?
Pb1 N1 2.656(7) 3_576 ?
Pb1 O1 2.762(5) 7_756 ?
Pb1 O1 2.762(5) 8_576 ?
Pb1 O2 2.861(5) 2_665 ?
Pb1 C10 2.997(7) 2_665 ?
Pb1 Pb1 4.1886(8) 7_756 ?
Pb1 Pb1 4.1886(8) 7_755 ?

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
C3 C1 N1 109.7(8) . . ?
C3 C1 H1A 125.1 . . ?
N1 C1 H1A 125.1 . . ?
N1 C2 N2 112.6(7) . . ?
N1 C2 H2A 123.7 . . ?
N2 C2 H2A 123.7 . . ?
C1 C3 N2 107.2(8) . . ?
C1 C3 H3A 126.4 . . ?
N2 C3 H3A 126.4 . . ?
N2 C4 C5 111.7(6) . . ?
N2 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
N2 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
N5 C5 C6 108.0(6) . . ?
N5 C5 C4 121.3(7) . . ?
C6 C5 C4 130.7(7) . . ?
N3 C6 C5 104.6(6) . . ?
N3 C6 H6A 127.7 . . ?
C5 C6 H6A 127.7 . . ?
N3 C9 C10 111.8(6) . . ?
N3 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N3 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
O2 C10 O1 123.9(7) . . ?
O2 C10 C9 119.8(6) . . ?
O1 C10 C9 116.3(6) . . ?
C2 N1 C1 104.7(7) . . ?
C2 N1 Pb1 123.9(6) . 3_476 ?
C1 N1 Pb1 129.1(6) . 3_476 ?
C2 N2 C3 105.8(7) . . ?
C2 N2 C4 124.9(7) . . ?
C3 N2 C4 128.8(7) . . ?
N4 N3 C6 112.1(6) . . ?
N4 N3 C9 119.9(6) . . ?
C6 N3 C9 127.6(6) . . ?
N5 N4 N3 105.5(6) . . ?
N4 N5 C5 109.7(6) . . ?
C10 O1 Pb1 103.8(4) . . ?
C10 O1 Pb1 149.1(4) . 7_755 ?
Pb1 O1 Pb1 107.06(16) . 7_755 ?
C10 O2 Pb1 84.2(4) . . ?
O1 Pb1 O1 78.2(2) 2_665 . ?
O1 Pb1 N1 79.2(2) 2_665 4_646 ?
O1 Pb1 N1 79.37(19) . 4_646 ?
O1 Pb1 N1 79.37(19) 2_665 3_576 ?
O1 Pb1 N1 79.2(2) . 3_576 ?
N1 Pb1 N1 152.3(3) 4_646 3_576 ?
O1 Pb1 O1 150.6(2) 2_665 7_756 ?
O1 Pb1 O1 114.72(18) . 7_756 ?
N1 Pb1 O1 127.80(19) 4_646 7_756 ?
N1 Pb1 O1 77.54(18) 3_576 7_756 ?
O1 Pb1 O1 114.72(18) 2_665 8_576 ?
O1 Pb1 O1 150.6(2) . 8_576 ?
N1 Pb1 O1 77.54(18) 4_646 8_576 ?
N1 Pb1 O1 127.80(19) 3_576 8_576 ?
O1 Pb1 O1 67.72(19) 7_756 8_576 ?
O1 Pb1 O2 47.91(15) 2_665 2_665 ?
O1 Pb1 O2 126.02(15) . 2_665 ?
N1 Pb1 O2 91.2(2) 4_646 2_665 ?
N1 Pb1 O2 87.4(2) 3_576 2_665 ?
O1 Pb1 O2 112.77(16) 7_756 2_665 ?
O1 Pb1 O2 72.60(16) 8_576 2_665 ?
O1 Pb1 O2 126.02(15) 2_665 . ?
O1 Pb1 O2 47.91(15) . . ?
N1 Pb1 O2 87.4(2) 4_646 . ?
N1 Pb1 O2 91.2(2) 3_576 . ?
O1 Pb1 O2 72.60(16) 7_756 . ?
O1 Pb1 O2 112.77(16) 8_576 . ?
O2 Pb1 O2 173.9(2) 2_665 . ?
O1 Pb1 C10 23.91(16) 2_665 2_665 ?
O1 Pb1 C10 102.08(18) . 2_665 ?
N1 Pb1 C10 83.7(2) 4_646 2_665 ?
N1 Pb1 C10 83.8(2) 3_576 2_665 ?
O1 Pb1 C10 134.14(18) 7_756 2_665 ?
O1 Pb1 C10 93.31(17) 8_576 2_665 ?
O2 Pb1 C10 24.04(15) 2_665 2_665 ?
O2 Pb1 C10 149.89(19) . 2_665 ?
O1 Pb1 Pb1 140.92(11) 2_665 7_756 ?
O1 Pb1 Pb1 140.92(11) . 7_756 ?
N1 Pb1 Pb1 103.84(15) 4_646 7_756 ?
N1 Pb1 Pb1 103.84(15) 3_576 7_756 ?
O1 Pb1 Pb1 33.86(10) 7_756 7_756 ?
O1 Pb1 Pb1 33.86(10) 8_576 7_756 ?
O2 Pb1 Pb1 93.04(10) 2_665 7_756 ?
O2 Pb1 Pb1 93.04(10) . 7_756 ?
C10 Pb1 Pb1 117.01(13) 2_665 7_756 ?
O1 Pb1 Pb1 39.08(11) 2_665 7_755 ?
O1 Pb1 Pb1 39.08(11) . 7_755 ?
N1 Pb1 Pb1 76.16(15) 4_646 7_755 ?
N1 Pb1 Pb1 76.16(15) 3_576 7_755 ?
O1 Pb1 Pb1 146.14(10) 7_756 7_755 ?
O1 Pb1 Pb1 146.14(10) 8_576 7_755 ?
O2 Pb1 Pb1 86.96(10) 2_665 7_755 ?
O2 Pb1 Pb1 86.96(10) . 7_755 ?
C10 Pb1 Pb1 62.99(13) 2_665 7_755 ?
Pb1 Pb1 Pb1 180 7_756 7_755 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C3 N2 -0.3(11) . . . . ?
N2 C4 C5 N5 -69.0(10) . . . . ?
N2 C4 C5 C6 110.8(9) . . . . ?
N5 C5 C6 N3 -0.6(8) . . . . ?
C4 C5 C6 N3 179.6(7) . . . . ?
N3 C9 C10 O2 14.1(11) . . . . ?
N3 C9 C10 O1 -166.7(6) . . . . ?
N2 C2 N1 C1 -0.1(9) . . . . ?
N2 C2 N1 Pb1 163.8(4) . . . 3_476 ?
C3 C1 N1 C2 0.3(10) . . . . ?
C3 C1 N1 Pb1 -162.5(6) . . . 3_476 ?
N1 C2 N2 C3 -0.1(9) . . . . ?
N1 C2 N2 C4 -172.4(6) . . . . ?
C1 C3 N2 C2 0.2(10) . . . . ?
C1 C3 N2 C4 172.1(7) . . . . ?
C5 C4 N2 C2 83.8(9) . . . . ?
C5 C4 N2 C3 -86.7(10) . . . . ?
C5 C6 N3 N4 0.2(8) . . . . ?
C5 C6 N3 C9 -173.1(6) . . . . ?
C10 C9 N3 N4 -97.3(8) . . . . ?
C10 C9 N3 C6 75.6(9) . . . . ?
C6 N3 N4 N5 0.2(8) . . . . ?
C9 N3 N4 N5 174.1(6) . . . . ?
N3 N4 N5 C5 -0.5(8) . . . . ?
C6 C5 N5 N4 0.7(9) . . . . ?
C4 C5 N5 N4 -179.5(6) . . . . ?
O2 C10 O1 Pb1 -5.4(10) . . . . ?
C9 C10 O1 Pb1 175.5(5) . . . . ?
O2 C10 O1 Pb1 174.2(7) . . . 7_755 ?
C9 C10 O1 Pb1 -4.9(14) . . . 7_755 ?
O1 C10 O2 Pb1 4.5(8) . . . . ?
C9 C10 O2 Pb1 -176.4(7) . . . . ?
C10 O1 Pb1 O1 179.8(6) . . . 2_665 ?
Pb1 O1 Pb1 O1 0.0 7_755 . . 2_665 ?
C10 O1 Pb1 N1 98.7(5) . . . 4_646 ?
Pb1 O1 Pb1 N1 -81.1(2) 7_755 . . 4_646 ?
C10 O1 Pb1 N1 -98.9(5) . . . 3_576 ?
Pb1 O1 Pb1 N1 81.3(2) 7_755 . . 3_576 ?
C10 O1 Pb1 O1 -28.1(4) . . . 7_756 ?
Pb1 O1 Pb1 O1 152.0(2) 7_755 . . 7_756 ?
C10 O1 Pb1 O1 59.9(6) . . . 8_576 ?
Pb1 O1 Pb1 O1 -119.9(2) 7_755 . . 8_576 ?
C10 O1 Pb1 O2 -177.6(5) . . . 2_665 ?
Pb1 O1 Pb1 O2 2.6(3) 7_755 . . 2_665 ?
C10 O1 Pb1 O2 2.6(5) . . . . ?
Pb1 O1 Pb1 O2 -177.2(4) 7_755 . . . ?
C10 O1 Pb1 C10 179.9(3) . . . 2_665 ?
Pb1 O1 Pb1 C10 0.1(2) 7_755 . . 2_665 ?
C10 O1 Pb1 Pb1 -0.2(6) . . . 7_756 ?
Pb1 O1 Pb1 Pb1 180 7_755 . . 7_756 ?
C10 O1 Pb1 Pb1 179.8(6) . . . 7_755 ?
C10 O2 Pb1 O1 -6.0(7) . . . 2_665 ?
C10 O2 Pb1 O1 -2.6(5) . . . . ?
C10 O2 Pb1 N1 -80.6(6) . . . 4_646 ?
C10 O2 Pb1 N1 71.7(6) . . . 3_576 ?
C10 O2 Pb1 O1 148.3(6) . . . 7_756 ?
C10 O2 Pb1 O1 -155.9(5) . . . 8_576 ?
C10 O2 Pb1 O2 -4.3(5) . . . 2_665 ?
C10 O2 Pb1 C10 -7.9(10) . . . 2_665 ?
C10 O2 Pb1 Pb1 175.7(5) . . . 7_756 ?
C10 O2 Pb1 Pb1 -4.3(5) . . . 7_755 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.88
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.483
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.134
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1437790'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Co N10 O10'
_chemical_formula_weight         579.41

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.7702(16)
_cell_length_b                   9.0412(18)
_cell_length_c                   9.2461(18)
_cell_angle_alpha                94.47(3)
_cell_angle_beta                 107.46(3)
_cell_angle_gamma                95.08(3)
_cell_volume                     613.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2263
_cell_measurement_theta_min      2.2752
_cell_measurement_theta_max      31.0825

_exptl_crystal_description       Prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             301
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8610
_exptl_absorpt_correction_T_max  0.8610
_exptl_absorpt_process_details   ?

_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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5983
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2153
_reflns_number_gt                1958
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0345P)²+0.3676P] 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         2153
_refine_ls_number_parameters     201
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0820
_refine_ls_wR_factor_gt          0.0791
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2554(4) -0.0716(3) 0.6547(3) 0.0440(7) Uani 1 1 d . . .
H1 H 0.1992 -0.1596 0.6743 0.062(9) Uiso 1 1 d R . .
C2 C 0.2238(4) -0.0205(3) 0.5157(3) 0.0482(7) Uani 1 1 d . . .
H2 H 0.1427 -0.0659 0.4240 0.076(11) Uiso 1 1 d R . .
C3 C 0.4272(4) 0.1339(3) 0.6865(3) 0.0366(6) Uani 1 1 d . . .
H3A H 0.5122 0.2163 0.7311 0.037(7) Uiso 1 1 d R . .
C4 C 0.3539(4) 0.2051(3) 0.4195(3) 0.0419(7) Uani 1 1 d . . .
H4A H 0.3203 0.1433 0.3226 0.052(9) Uiso 1 1 d R . .
H4B H 0.4805 0.2448 0.4435 0.054(9) Uiso 1 1 d R . .
C5 C 0.2427(3) 0.3329(3) 0.4028(3) 0.0332(6) Uani 1 1 d . . .
C6 C 0.1079(3) 0.3649(3) 0.2796(3) 0.0343(6) Uani 1 1 d . . .
H6 H 0.0589 0.2942 0.1921 0.067(10) Uiso 1 1 d R . .
C7 C -0.0353(3) 0.6037(3) 0.2267(3) 0.0377(6) Uani 1 1 d . . .
H7A H -0.0732 0.6741 0.2920 0.043(8) Uiso 1 1 d R . .
H7B H -0.1432 0.5481 0.1550 0.052(9) Uiso 1 1 d R . .
C8 C 0.0732(3) 0.6907(3) 0.1403(3) 0.0310(6) Uani 1 1 d . . .
Co1 Co 0.5000 0.0000 1.0000 0.02615(15) Uani 1 2 d S . .
H3W H 0.539(4) 0.314(3) 1.095(3) 0.050(8) Uiso 1 1 d . . .
H4W H 0.185(5) -0.037(4) 1.054(4) 0.070(12) Uiso 1 1 d . . .
H9W H 0.386(6) 0.494(5) 0.158(5) 0.099(15) Uiso 1 1 d . . .
H3WA H 0.656(4) 0.265(4) 0.999(4) 0.061(11) Uiso 1 1 d . . .
H4WA H 0.188(5) 0.093(4) 0.995(4) 0.077(12) Uiso 1 1 d . . .
H9WA H 0.567(7) 0.489(5) 0.296(6) 0.134(18) Uiso 1 1 d . . .
N1 N 0.3346(3) 0.1101(2) 0.5376(2) 0.0332(5) Uani 1 1 d . . .
N2 N 0.3828(3) 0.0266(2) 0.7630(2) 0.0308(5) Uani 1 1 d . . .
N3 N 0.0733(3) 0.5022(2) 0.3200(2) 0.0322(5) Uani 1 1 d . . .
N4 N 0.1803(3) 0.5559(2) 0.4608(3) 0.0408(5) Uani 1 1 d . . .
N5 N 0.2835(3) 0.4517(3) 0.5115(2) 0.0390(5) Uani 1 1 d . . .
O1 O 0.0240(3) 0.8144(2) 0.1055(3) 0.0538(6) Uani 1 1 d . . .
O2 O 0.1993(2) 0.6335(2) 0.1103(2) 0.0409(5) Uani 1 1 d . . .
O3 O 0.5959(3) 0.2283(2) 1.0464(2) 0.0399(5) Uani 1 1 d . . .
O4 O 0.2536(3) 0.0352(2) 1.0442(2) 0.0386(5) Uani 1 1 d . . .
O9 O 0.4904(4) 0.4543(3) 0.1858(3) 0.0593(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.360(4) . ?
C1 N2 1.371(3) . ?
C1 H1 0.9300 . ?
C2 N1 1.362(3) . ?
C2 H2 0.9293 . ?
C3 N2 1.325(3) . ?
C3 N1 1.338(3) . ?
C3 H3A 0.9295 . ?
C4 N1 1.475(3) . ?
C4 C5 1.493(4) . ?
C4 H4A 0.9686 . ?
C4 H4B 0.9696 . ?
C5 N5 1.358(3) . ?
C5 C6 1.367(3) . ?
C6 N3 1.341(3) . ?
C6 H6 0.9487 . ?
C7 N3 1.457(3) . ?
C7 C8 1.534(3) . ?
C7 H7A 0.9674 . ?
C7 H7B 0.9670 . ?
C8 O2 1.240(3) . ?
C8 O1 1.249(3) . ?
Co1 O3 2.0973(19) . ?
Co1 O3 2.0973(19) 2_657 ?
Co1 O4 2.1195(19) 2_657 ?
Co1 O4 2.1195(19) . ?
Co1 N2 2.148(2) 2_657 ?
Co1 N2 2.148(2) . ?
N3 N4 1.343(3) . ?
N4 N5 1.315(3) . ?
O3 H3W 1.07(3) . ?
O3 H3WA 0.79(3) . ?
O4 H4W 0.84(4) . ?
O4 H4WA 0.82(4) . ?
O9 H9W 0.89(4) . ?
O9 H9WA 1.02(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 109.8(2) . . ?
C2 C1 H1 125.5 . . ?
N2 C1 H1 124.7 . . ?
C1 C2 N1 106.4(2) . . ?
C1 C2 H2 126.7 . . ?
N1 C2 H2 126.9 . . ?
N2 C3 N1 112.1(2) . . ?
N2 C3 H3A 123.9 . . ?
N1 C3 H3A 124.0 . . ?
N1 C4 C5 114.5(2) . . ?
N1 C4 H4A 108.5 . . ?
C5 C4 H4A 108.9 . . ?
N1 C4 H4B 108.8 . . ?
C5 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
N5 C5 C6 108.1(2) . . ?
N5 C5 C4 121.5(2) . . ?
C6 C5 C4 129.8(2) . . ?
N3 C6 C5 104.7(2) . . ?
N3 C6 H6 134.5 . . ?
C5 C6 H6 120.8 . . ?
N3 C7 C8 111.4(2) . . ?
N3 C7 H7A 109.0 . . ?
C8 C7 H7A 108.8 . . ?
N3 C7 H7B 109.8 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.0 . . ?
O2 C8 O1 125.8(2) . . ?
O2 C8 C7 118.4(2) . . ?
O1 C8 C7 115.9(2) . . ?
O3 Co1 O3 180 . 2_657 ?
O3 Co1 O4 87.59(9) . 2_657 ?
O3 Co1 O4 92.41(9) 2_657 2_657 ?
O3 Co1 O4 92.41(9) . . ?
O3 Co1 O4 87.59(9) 2_657 . ?
O4 Co1 O4 180 2_657 . ?
O3 Co1 N2 89.73(8) . 2_657 ?
O3 Co1 N2 90.27(8) 2_657 2_657 ?
O4 Co1 N2 91.39(8) 2_657 2_657 ?
O4 Co1 N2 88.61(8) . 2_657 ?
O3 Co1 N2 90.27(8) . . ?
O3 Co1 N2 89.73(8) 2_657 . ?
O4 Co1 N2 88.61(8) 2_657 . ?
O4 Co1 N2 91.39(8) . . ?
N2 Co1 N2 180 2_657 . ?
C3 N1 C2 106.9(2) . . ?
C3 N1 C4 126.3(2) . . ?
C2 N1 C4 126.8(2) . . ?
C3 N2 C1 104.7(2) . . ?
C3 N2 Co1 128.02(17) . . ?
C1 N2 Co1 127.05(16) . . ?
C6 N3 N4 111.4(2) . . ?
C6 N3 C7 129.4(2) . . ?
N4 N3 C7 118.2(2) . . ?
N5 N4 N3 106.5(2) . . ?
N4 N5 C5 109.3(2) . . ?
Co1 O3 H3W 127.3(15) . . ?
Co1 O3 H3WA 120(2) . . ?
H3W O3 H3WA 109(3) . . ?
Co1 O4 H4W 120(2) . . ?
Co1 O4 H4WA 119(3) . . ?
H4W O4 H4WA 107(3) . . ?
H9W O9 H9WA 113(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N1 0.7(3) . . . . ?
N1 C4 C5 N5 70.6(3) . . . . ?
N1 C4 C5 C6 -119.1(3) . . . . ?
N5 C5 C6 N3 -0.1(3) . . . . ?
C4 C5 C6 N3 -171.4(3) . . . . ?
N3 C7 C8 O2 26.4(3) . . . . ?
N3 C7 C8 O1 -154.0(2) . . . . ?
N2 C3 N1 C2 -0.1(3) . . . . ?
N2 C3 N1 C4 -178.4(2) . . . . ?
C1 C2 N1 C3 -0.4(3) . . . . ?
C1 C2 N1 C4 177.9(2) . . . . ?
C5 C4 N1 C3 -85.4(3) . . . . ?
C5 C4 N1 C2 96.7(3) . . . . ?
N1 C3 N2 C1 0.6(3) . . . . ?
N1 C3 N2 Co1 175.61(16) . . . . ?
C2 C1 N2 C3 -0.8(3) . . . . ?
C2 C1 N2 Co1 -175.91(19) . . . . ?
O3 Co1 N2 C3 21.8(2) . . . . ?
O3 Co1 N2 C3 -158.2(2) 2_657 . . . ?
O4 Co1 N2 C3 -65.8(2) 2_657 . . . ?
O4 Co1 N2 C3 114.2(2) . . . . ?
N2 Co1 N2 C3 -93(100) 2_657 . . . ?
O3 Co1 N2 C1 -164.2(2) . . . . ?
O3 Co1 N2 C1 15.8(2) 2_657 . . . ?
O4 Co1 N2 C1 108.2(2) 2_657 . . . ?
O4 Co1 N2 C1 -71.8(2) . . . . ?
N2 Co1 N2 C1 81(100) 2_657 . . . ?
C5 C6 N3 N4 0.3(3) . . . . ?
C5 C6 N3 C7 168.8(2) . . . . ?
C8 C7 N3 C6 -82.1(3) . . . . ?
C8 C7 N3 N4 85.8(3) . . . . ?
C6 N3 N4 N5 -0.4(3) . . . . ?
C7 N3 N4 N5 -170.4(2) . . . . ?
N3 N4 N5 C5 0.3(3) . . . . ?
C6 C5 N5 N4 -0.2(3) . . . . ?
C4 C5 N5 N4 172.0(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
O9 H9W O2 0.89(4) 1.98(4) 2.847(3) 164(4) .
O9 H9WA N4 1.02(5) 2.59(5) 3.507(4) 149(4) 2_666
O9 H9WA N5 1.02(5) 1.82(5) 2.838(3) 176(4) 2_666
O4 H4WA O1 0.82(4) 1.93(4) 2.728(3) 162(4) 2_566
O4 H4W O1 0.84(4) 1.94(4) 2.764(3) 171(3) 1_546
O3 H3WA O2 0.79(3) 1.95(3) 2.740(3) 176(3) 2_666
O3 H3W O9 1.07(3) 1.60(3) 2.651(3) 169(2) 1_556

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.048
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1437791'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Mn N10 O10'
_chemical_formula_weight         575.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.8231(16)
_cell_length_b                   9.0961(18)
_cell_length_c                   9.2962(19)
_cell_angle_alpha                94.66(3)
_cell_angle_beta                 107.53(3)
_cell_angle_gamma                95.54(3)
_cell_volume                     623.6(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2143
_cell_measurement_theta_min      2.2648
_cell_measurement_theta_max      30.9030

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             299
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8894
_exptl_absorpt_correction_T_max  0.8894
_exptl_absorpt_process_details   ?

_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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5509
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2190
_reflns_number_gt                1952
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0409P)²+0.3034P] 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         2190
_refine_ls_number_parameters     193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0927
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5779(4) 0.3651(3) -0.1780(3) 0.0395(6) Uani 1 1 d . . .
H1 H 0.4937 0.2824 -0.2239 0.047 Uiso 1 1 calc R . .
C2 C 0.7466(4) 0.5716(3) -0.1430(3) 0.0462(7) Uani 1 1 d . . .
H2 H 0.8027 0.6603 -0.1603 0.055 Uiso 1 1 calc R . .
C3 C 0.7762(4) 0.5202(3) -0.0058(3) 0.0489(7) Uani 1 1 d . . .
H3 H 0.8548 0.5663 0.0866 0.059 Uiso 1 1 calc R . .
C4 C 0.6483(4) 0.2924(3) 0.0858(3) 0.0426(7) Uani 1 1 d . . .
H4A H 0.5219 0.2527 0.0608 0.051 Uiso 1 1 calc R . .
H4B H 0.6823 0.3528 0.1834 0.051 Uiso 1 1 calc R . .
C5 C 0.7584(3) 0.1659(3) 0.1002(3) 0.0332(6) Uani 1 1 d . . .
C6 C 0.8928(3) 0.1342(3) 0.2220(3) 0.0338(6) Uani 1 1 d . . .
H6 H 0.9486 0.1939 0.3135 0.041 Uiso 1 1 calc R . .
C7 C 1.0341(3) -0.1032(3) 0.2719(3) 0.0352(6) Uani 1 1 d . . .
H7A H 1.1424 -0.0471 0.3432 0.042 Uiso 1 1 calc R . .
H7B H 1.0709 -0.1734 0.2063 0.042 Uiso 1 1 calc R . .
C8 C 0.9276(3) -0.1883(3) 0.3593(3) 0.0299(5) Uani 1 1 d . . .
H5W H 0.822(5) 0.414(4) -0.495(4) 0.067(11) Uiso 1 1 d . . .
H7W H 0.335(4) 0.222(4) -0.494(4) 0.066(10) Uiso 1 1 d . . .
H9W H 0.452(5) 0.019(4) 0.222(5) 0.082(13) Uiso 1 1 d . . .
H5WA H 0.813(4) 0.538(4) -0.556(4) 0.057(11) Uiso 1 1 d . . .
H7WA H 0.442(4) 0.201(3) -0.581(3) 0.048(9) Uiso 1 1 d . . .
H9WA H 0.608(6) 0.006(4) 0.335(5) 0.090(14) Uiso 1 1 d . . .
Mn1 Mn 0.5000 0.5000 -0.5000 0.02658(17) Uani 1 2 d S . .
N1 N 0.6213(3) 0.4730(2) -0.2521(2) 0.0340(5) Uani 1 1 d . . .
N2 N 0.6687(3) 0.3881(2) -0.0296(2) 0.0341(5) Uani 1 1 d . . .
N3 N 0.9267(3) -0.0020(2) 0.1804(2) 0.0312(5) Uani 1 1 d . . .
N4 N 0.8195(3) -0.0548(2) 0.0397(2) 0.0389(5) Uani 1 1 d . . .
N5 N 0.7169(3) 0.0486(2) -0.0092(2) 0.0390(5) Uani 1 1 d . . .
O1 O 0.9782(2) -0.3087(2) 0.3981(2) 0.0510(5) Uani 1 1 d . . .
O2 O 0.8011(2) -0.13214(19) 0.3873(2) 0.0402(4) Uani 1 1 d . . .
O5 O 0.7553(3) 0.4668(2) -0.5428(2) 0.0402(5) Uani 1 1 d . . .
O7 O 0.3985(3) 0.2650(2) -0.5487(2) 0.0412(5) Uani 1 1 d . . .
O9 O 0.5075(3) 0.0416(2) 0.3128(3) 0.0536(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.319(3) . ?
C1 N2 1.337(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.356(4) . ?
C2 N1 1.370(3) . ?
C2 H2 0.9300 . ?
C3 N2 1.360(3) . ?
C3 H3 0.9300 . ?
C4 N2 1.470(3) . ?
C4 C5 1.494(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N5 1.355(3) . ?
C5 C6 1.365(3) . ?
C6 N3 1.343(3) . ?
C6 H6 0.9300 . ?
C7 N3 1.457(3) . ?
C7 C8 1.530(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O2 1.241(3) . ?
C8 O1 1.244(3) . ?
Mn1 O7 2.1686(19) . ?
Mn1 O7 2.1686(19) 2_664 ?
Mn1 O5 2.1939(19) . ?
Mn1 O5 2.1939(19) 2_664 ?
Mn1 N1 2.256(2) 2_664 ?
Mn1 N1 2.256(2) . ?
N3 N4 1.343(3) . ?
N4 N5 1.316(3) . ?
O5 H5W 0.81(4) . ?
O5 H5WA 0.79(3) . ?
O7 H7W 0.89(4) . ?
O7 H7WA 0.79(3) . ?
O9 H9W 0.82(4) . ?
O9 H9WA 0.85(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 112.3(2) . . ?
N1 C1 H1 123.8 . . ?
N2 C1 H1 123.8 . . ?
C3 C2 N1 109.6(2) . . ?
C3 C2 H2 125.2 . . ?
N1 C2 H2 125.2 . . ?
C2 C3 N2 106.6(2) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
N2 C4 C5 114.2(2) . . ?
N2 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
N2 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
N5 C5 C6 108.2(2) . . ?
N5 C5 C4 121.5(2) . . ?
C6 C5 C4 129.7(2) . . ?
N3 C6 C5 104.8(2) . . ?
N3 C6 H6 127.6 . . ?
C5 C6 H6 127.6 . . ?
N3 C7 C8 111.43(19) . . ?
N3 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N3 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
O2 C8 O1 125.6(2) . . ?
O2 C8 C7 118.3(2) . . ?
O1 C8 C7 116.2(2) . . ?
O7 Mn1 O7 180 . 2_664 ?
O7 Mn1 O5 93.30(9) . . ?
O7 Mn1 O5 86.70(9) 2_664 . ?
O7 Mn1 O5 86.70(9) . 2_664 ?
O7 Mn1 O5 93.30(9) 2_664 2_664 ?
O5 Mn1 O5 180 . 2_664 ?
O7 Mn1 N1 89.74(8) . 2_664 ?
O7 Mn1 N1 90.26(8) 2_664 2_664 ?
O5 Mn1 N1 88.88(8) . 2_664 ?
O5 Mn1 N1 91.12(8) 2_664 2_664 ?
O7 Mn1 N1 90.26(8) . . ?
O7 Mn1 N1 89.74(8) 2_664 . ?
O5 Mn1 N1 91.12(8) . . ?
O5 Mn1 N1 88.88(8) 2_664 . ?
N1 Mn1 N1 180 2_664 . ?
C1 N1 C2 104.8(2) . . ?
C1 N1 Mn1 127.80(17) . . ?
C2 N1 Mn1 127.24(17) . . ?
C1 N2 C3 106.6(2) . . ?
C1 N2 C4 126.3(2) . . ?
C3 N2 C4 127.0(2) . . ?
N4 N3 C6 111.1(2) . . ?
N4 N3 C7 118.3(2) . . ?
C6 N3 C7 129.5(2) . . ?
N5 N4 N3 106.63(19) . . ?
N4 N5 C5 109.2(2) . . ?
Mn1 O5 H5W 121(3) . . ?
Mn1 O5 H5WA 117(2) . . ?
H5W O5 H5WA 109(3) . . ?
Mn1 O7 H7W 121(2) . . ?
Mn1 O7 H7WA 128(2) . . ?
H7W O7 H7WA 106(3) . . ?
H9W O9 H9WA 110(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.1(3) . . . . ?
N2 C4 C5 N5 -71.0(3) . . . . ?
N2 C4 C5 C6 118.6(3) . . . . ?
N5 C5 C6 N3 -0.1(3) . . . . ?
C4 C5 C6 N3 171.3(2) . . . . ?
N3 C7 C8 O2 -24.3(3) . . . . ?
N3 C7 C8 O1 156.6(2) . . . . ?
N2 C1 N1 C2 -0.7(3) . . . . ?
N2 C1 N1 Mn1 -176.00(16) . . . . ?
C3 C2 N1 C1 0.3(3) . . . . ?
C3 C2 N1 Mn1 175.70(19) . . . . ?
O7 Mn1 N1 C1 -20.2(2) . . . . ?
O7 Mn1 N1 C1 159.8(2) 2_664 . . . ?
O5 Mn1 N1 C1 -113.5(2) . . . . ?
O5 Mn1 N1 C1 66.5(2) 2_664 . . . ?
N1 Mn1 N1 C1 78(100) 2_664 . . . ?
O7 Mn1 N1 C2 165.4(2) . . . . ?
O7 Mn1 N1 C2 -14.6(2) 2_664 . . . ?
O5 Mn1 N1 C2 72.1(2) . . . . ?
O5 Mn1 N1 C2 -107.9(2) 2_664 . . . ?
N1 Mn1 N1 C2 -97(100) 2_664 . . . ?
N1 C1 N2 C3 0.7(3) . . . . ?
N1 C1 N2 C4 177.9(2) . . . . ?
C2 C3 N2 C1 -0.5(3) . . . . ?
C2 C3 N2 C4 -177.6(2) . . . . ?
C5 C4 N2 C1 85.0(3) . . . . ?
C5 C4 N2 C3 -98.4(3) . . . . ?
C5 C6 N3 N4 -0.1(3) . . . . ?
C5 C6 N3 C7 -168.5(2) . . . . ?
C8 C7 N3 N4 -87.0(3) . . . . ?
C8 C7 N3 C6 80.7(3) . . . . ?
C6 N3 N4 N5 0.2(3) . . . . ?
C7 N3 N4 N5 170.1(2) . . . . ?
N3 N4 N5 C5 -0.3(3) . . . . ?
C6 C5 N5 N4 0.2(3) . . . . ?
C4 C5 N5 N4 -172.0(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
O9 H9WA O2 0.85(4) 2.03(4) 2.859(3) 164(4) .
O9 H9W N5 0.82(4) 2.03(4) 2.843(3) 172(4) 2_655
O7 H7WA O9 0.79(3) 1.88(3) 2.662(3) 170(3) 1_554
O5 H5WA O1 0.79(3) 1.97(4) 2.754(3) 171(3) 1_564
O7 H7W O2 0.89(4) 1.84(4) 2.737(3) 178(3) 2_655
O5 H5W O1 0.81(4) 1.93(4) 2.725(3) 167(3) 2_755

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.067
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1437792'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 N10 Ni O10'
_chemical_formula_weight         579.17

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.7318(15)
_cell_length_b                   8.9961(18)
_cell_length_c                   9.1815(18)
_cell_angle_alpha                94.40(3)
_cell_angle_beta                 107.22(3)
_cell_angle_gamma                95.01(3)
_cell_volume                     604.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1841
_cell_measurement_theta_min      2.2858
_cell_measurement_theta_max      27.8644

_exptl_crystal_description       Prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             302
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8443
_exptl_absorpt_correction_T_max  0.8443
_exptl_absorpt_process_details   ?

_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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6203
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         27.87
_reflns_number_total             2849
_reflns_number_gt                2397
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0481P)²+0.2410P] 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         2849
_refine_ls_number_parameters     192
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1105
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.227
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0721(5) 0.3653(4) 0.8085(3) 0.0373(7) Uani 1 1 d . . .
H1A H -0.0135 0.2827 0.7637 0.053(11) Uiso 1 1 d R . .
C2 C 0.2757(5) 0.5205(4) 0.9797(4) 0.0479(9) Uani 1 1 d . . .
H2A H 0.3575 0.5670 1.0710 0.063(12) Uiso 1 1 d R . .
C3 C 0.2440(5) 0.5708(4) 0.8395(4) 0.0448(9) Uani 1 1 d . . .
H3A H 0.2990 0.6596 0.8194 0.068(13) Uiso 1 1 d R . .
C4 C 0.1446(5) 0.2948(4) 1.0773(4) 0.0438(8) Uani 1 1 d . . .
H4A H 0.1780 0.3569 1.1747 0.050(10) Uiso 1 1 d R . .
H4B H 0.0172 0.2556 1.0529 0.063(13) Uiso 1 1 d R . .
C5 C 0.2552(4) 0.1667(3) 1.0950(3) 0.0336(7) Uani 1 1 d . . .
C6 C 0.3909(4) 0.1339(4) 1.2186(3) 0.0356(7) Uani 1 1 d . . .
H6A H 0.4470 0.1948 1.3099 0.046(10) Uiso 1 1 d R . .
C7 C 0.5356(4) -0.1052(4) 1.2732(4) 0.0374(7) Uani 1 1 d . . .
H7A H 0.5822 -0.1735 1.2035 0.040(9) Uiso 1 1 d R . .
H7B H 0.6476 -0.0475 1.3428 0.051(11) Uiso 1 1 d R . .
C8 C 0.4272(4) -0.1931(3) 1.3594(3) 0.0315(7) Uani 1 1 d . . .
H3 H -0.05(2) 0.023(12) 0.221(5) 0.46(10) Uiso 1 1 d D . .
H2W H -0.035(4) 0.221(2) 0.409(3) 0.072(15) Uiso 1 1 d D . .
H3W H 0.116(7) 0.015(13) 0.337(17) 0.57(13) Uiso 1 1 d D . .
N1 N 0.1649(4) 0.3891(3) 0.9586(3) 0.0345(6) Uani 1 1 d . . .
N2 N 0.1170(3) 0.4726(3) 0.7317(3) 0.0307(6) Uani 1 1 d . . .
N3 N 0.4261(4) -0.0034(3) 1.1800(3) 0.0345(6) Uani 1 1 d . . .
N4 N 0.3194(4) -0.0570(3) 1.0385(3) 0.0420(7) Uani 1 1 d . . .
N5 N 0.2160(4) 0.0474(3) 0.9868(3) 0.0408(7) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.5000 0.5000 0.02631(17) Uani 1 2 d SD . .
O1 O 0.2420(3) 0.4623(2) 0.4534(2) 0.0359(5) Uani 1 1 d D . .
H1 H 0.3048 0.4204 0.5207 0.066(14) Uiso 1 1 d RD . .
H1W H 0.3334 0.5475 0.4345 0.081(14) Uiso 1 1 d RD . .
O2 O -0.0976(3) 0.2743(2) 0.4519(3) 0.0380(5) Uani 1 1 d D . .
H2 H -0.1011 0.2390 0.5282 0.12(2) Uiso 1 1 d RD . .
O3 O 0.0120(5) 0.0465(3) 0.3159(3) 0.0635(8) Uani 1 1 d D . .
O5 O 0.3009(3) -0.1350(3) 1.3912(3) 0.0410(6) Uani 1 1 d . . .
O6 O 0.4743(3) -0.3170(3) 1.3934(3) 0.0556(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.319(4) . ?
C1 N1 1.343(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.358(5) . ?
C2 N1 1.363(4) . ?
C2 H2A 0.9290 . ?
C3 N2 1.365(4) . ?
C3 H3A 0.9292 . ?
C4 N1 1.467(4) . ?
C4 C5 1.485(5) . ?
C4 H4A 0.9698 . ?
C4 H4B 0.9699 . ?
C5 N5 1.353(4) . ?
C5 C6 1.369(4) . ?
C6 N3 1.332(4) . ?
C6 H6A 0.9295 . ?
C7 N3 1.455(4) . ?
C7 C8 1.526(4) . ?
C7 H7A 1.0153 . ?
C7 H7B 0.9848 . ?
C8 O6 1.237(4) . ?
C8 O5 1.243(4) . ?
N2 Ni1 2.094(2) . ?
N3 N4 1.341(4) . ?
N4 N5 1.313(4) . ?
Ni1 O2 2.070(2) 2_566 ?
Ni1 O2 2.070(2) . ?
Ni1 O1 2.088(2) 2_566 ?
Ni1 O1 2.088(2) . ?
Ni1 N2 2.094(2) 2_566 ?
O1 H1 0.8060 . ?
O1 H1W 1.0562 . ?
O2 H2W 0.861(11) . ?
O2 H2 0.7970 . ?
O3 H3 0.850(12) . ?
O3 H3W 0.850(12) . ?

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
N2 C1 N1 112.0(3) . . ?
N2 C1 H1A 123.9 . . ?
N1 C1 H1A 124.1 . . ?
C3 C2 N1 106.2(3) . . ?
C3 C2 H2A 126.3 . . ?
N1 C2 H2A 127.5 . . ?
C2 C3 N2 110.1(3) . . ?
C2 C3 H3A 125.3 . . ?
N2 C3 H3A 124.7 . . ?
N1 C4 C5 114.6(3) . . ?
N1 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
N1 C4 H4B 108.6 . . ?
C5 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
N5 C5 C6 107.5(3) . . ?
N5 C5 C4 121.7(3) . . ?
C6 C5 C4 130.3(3) . . ?
N3 C6 C5 105.5(3) . . ?
N3 C6 H6A 127.3 . . ?
C5 C6 H6A 127.3 . . ?
N3 C7 C8 111.2(3) . . ?
N3 C7 H7A 108.1 . . ?
C8 C7 H7A 112.3 . . ?
N3 C7 H7B 109.0 . . ?
C8 C7 H7B 112.3 . . ?
H7A C7 H7B 103.6 . . ?
O6 C8 O5 125.3(3) . . ?
O6 C8 C7 116.6(3) . . ?
O5 C8 C7 118.1(3) . . ?
C1 N1 C2 106.7(3) . . ?
C1 N1 C4 126.3(3) . . ?
C2 N1 C4 126.9(3) . . ?
C1 N2 C3 105.0(3) . . ?
C1 N2 Ni1 127.8(2) . . ?
C3 N2 Ni1 127.0(2) . . ?
C6 N3 N4 110.9(3) . . ?
C6 N3 C7 130.1(3) . . ?
N4 N3 C7 118.2(3) . . ?
N5 N4 N3 106.8(3) . . ?
N4 N5 C5 109.3(3) . . ?
O2 Ni1 O2 180 2_566 . ?
O2 Ni1 O1 92.04(9) 2_566 2_566 ?
O2 Ni1 O1 87.96(9) . 2_566 ?
O2 Ni1 O1 87.96(9) 2_566 . ?
O2 Ni1 O1 92.04(9) . . ?
O1 Ni1 O1 180 2_566 . ?
O2 Ni1 N2 89.19(10) 2_566 . ?
O2 Ni1 N2 90.81(10) . . ?
O1 Ni1 N2 88.91(9) 2_566 . ?
O1 Ni1 N2 91.09(9) . . ?
O2 Ni1 N2 90.81(10) 2_566 2_566 ?
O2 Ni1 N2 89.19(10) . 2_566 ?
O1 Ni1 N2 91.09(9) 2_566 2_566 ?
O1 Ni1 N2 88.91(9) . 2_566 ?
N2 Ni1 N2 180 . 2_566 ?
Ni1 O1 H1 109.9 . . ?
Ni1 O1 H1W 124.2 . . ?
H1 O1 H1W 104.1 . . ?
Ni1 O2 H2W 114.4(17) . . ?
Ni1 O2 H2 110.6 . . ?
H2W O2 H2 107.9 . . ?
H3 O3 H3W 110(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
N1 C2 C3 N2 -0.5(4) . . . . ?
N1 C4 C5 N5 -70.2(4) . . . . ?
N1 C4 C5 C6 118.6(4) . . . . ?
N5 C5 C6 N3 -0.5(4) . . . . ?
C4 C5 C6 N3 171.7(3) . . . . ?
N3 C7 C8 O6 153.5(3) . . . . ?
N3 C7 C8 O5 -27.2(4) . . . . ?
N2 C1 N1 C2 0.3(4) . . . . ?
N2 C1 N1 C4 178.0(3) . . . . ?
C3 C2 N1 C1 0.1(4) . . . . ?
C3 C2 N1 C4 -177.6(3) . . . . ?
C5 C4 N1 C1 85.7(4) . . . . ?
C5 C4 N1 C2 -97.1(4) . . . . ?
N1 C1 N2 C3 -0.6(4) . . . . ?
N1 C1 N2 Ni1 -174.6(2) . . . . ?
C2 C3 N2 C1 0.7(4) . . . . ?
C2 C3 N2 Ni1 174.8(2) . . . . ?
C5 C6 N3 N4 0.2(4) . . . . ?
C5 C6 N3 C7 -169.2(3) . . . . ?
C8 C7 N3 C6 83.0(4) . . . . ?
C8 C7 N3 N4 -85.7(4) . . . . ?
C6 N3 N4 N5 0.2(4) . . . . ?
C7 N3 N4 N5 171.0(3) . . . . ?
N3 N4 N5 C5 -0.5(4) . . . . ?
C6 C5 N5 N4 0.7(4) . . . . ?
C4 C5 N5 N4 -172.3(3) . . . . ?
C1 N2 Ni1 O2 157.9(3) . . . 2_566 ?
C3 N2 Ni1 O2 -14.9(3) . . . 2_566 ?
C1 N2 Ni1 O2 -22.1(3) . . . . ?
C3 N2 Ni1 O2 165.1(3) . . . . ?
C1 N2 Ni1 O1 65.8(3) . . . 2_566 ?
C3 N2 Ni1 O1 -106.9(3) . . . 2_566 ?
C1 N2 Ni1 O1 -114.2(3) . . . . ?
C3 N2 Ni1 O1 73.1(3) . . . . ?
C1 N2 Ni1 N2 -66(100) . . . 2_566 ?
C3 N2 Ni1 N2 121(100) . . . 2_566 ?

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
O2 H2W O3 0.861(11) 1.845(14) 2.649(4) 154(3) .
O3 H3W O5 0.850(12) 2.03(6) 2.834(4) 157(15) 1_554
O3 H3 N5 0.850(12) 1.99(3) 2.832(4) 170(18) 2_556
O2 H2 O5 0.80 2.08 2.718(3) 136.6 2_557
O1 H1W O6 1.06 1.70 2.758(3) 176.8 1_564
O1 H1 O6 0.81 2.00 2.730(3) 150.7 2_657

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.87
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.067
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9
_database_code_depnum_ccdc_archive 'CCDC 1437793'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 N10 O10 Zn'
_chemical_formula_weight         585.87

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

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

_cell_length_a                   7.7881(16)
_cell_length_b                   9.0380(18)
_cell_length_c                   9.1899(18)
_cell_angle_alpha                94.47(3)
_cell_angle_beta                 107.49(3)
_cell_angle_gamma                95.27(3)
_cell_volume                     610.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1977
_cell_measurement_theta_min      2.2770
_cell_measurement_theta_max      27.8565

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             304
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8133
_exptl_absorpt_correction_T_max  0.8133
_exptl_absorpt_process_details   ?

_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  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6755
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         27.86
_reflns_number_total             2874
_reflns_number_gt                2520
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0278P)²+0.3757P] 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         2874
_refine_ls_number_parameters     193
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0803
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4272(3) 0.1345(3) 0.6891(3) 0.0373(6) Uani 1 1 d . . .
H1A H 0.5128 0.2168 0.7345 0.045 Uiso 1 1 calc R . .
C2 C 0.2555(4) -0.0707(3) 0.6554(3) 0.0446(6) Uani 1 1 d . . .
H2A H 0.1986 -0.1590 0.6740 0.054 Uiso 1 1 calc R . .
C3 C 0.2250(4) -0.0198(3) 0.5162(3) 0.0478(7) Uani 1 1 d . . .
H3A H 0.1447 -0.0655 0.4235 0.057 Uiso 1 1 calc R . .
C4 C 0.3552(4) 0.2061(3) 0.4212(3) 0.0416(6) Uani 1 1 d . . .
H4A H 0.3219 0.1447 0.3233 0.050 Uiso 1 1 calc R . .
H4B H 0.4820 0.2455 0.4465 0.050 Uiso 1 1 calc R . .
C5 C 0.2449(3) 0.3335(3) 0.4039(3) 0.0331(5) Uani 1 1 d . . .
C6 C 0.1094(3) 0.3648(3) 0.2808(3) 0.0342(5) Uani 1 1 d . . .
H6A H 0.0536 0.3042 0.1890 0.041 Uiso 1 1 calc R . .
C7 C -0.0348(3) 0.6029(3) 0.2275(3) 0.0365(5) Uani 1 1 d . . .
H7A H -0.0748 0.6723 0.2929 0.044 Uiso 1 1 calc R . .
H7B H -0.1416 0.5459 0.1544 0.044 Uiso 1 1 calc R . .
C8 C 0.0729(3) 0.6905(3) 0.1411(3) 0.0315(5) Uani 1 1 d . . .
H3W H 0.809(5) 0.040(4) 0.936(4) 0.075(12) Uiso 1 1 d . . .
H4W H 0.546(4) 0.299(2) 1.082(3) 0.072(11) Uiso 1 1 d D . .
H5W H 0.372(6) 0.497(5) 1.160(5) 0.123(16) Uiso 1 1 d . . .
H3WA H 0.812(4) -0.085(4) 1.009(4) 0.064(11) Uiso 1 1 d . . .
H4WA H 0.662(3) 0.269(3) 0.998(3) 0.051(8) Uiso 1 1 d D . .
H5WA H 0.567(9) 0.489(7) 1.301(8) 0.21(3) Uiso 1 1 d . . .
N1 N 0.3825(3) 0.0272(2) 0.7647(2) 0.0319(4) Uani 1 1 d . . .
N2 N 0.3345(3) 0.1110(2) 0.5387(2) 0.0343(4) Uani 1 1 d . . .
N5 N 0.0741(3) 0.5019(2) 0.3209(2) 0.0327(4) Uani 1 1 d . . .
N6 N 0.1817(3) 0.5558(2) 0.4621(2) 0.0397(5) Uani 1 1 d . . .
N7 N 0.2848(3) 0.4521(2) 0.5129(2) 0.0394(5) Uani 1 1 d . . .
O1 O 0.0238(3) 0.8138(2) 0.1064(3) 0.0542(5) Uani 1 1 d . . .
O2 O 0.1987(2) 0.63385(19) 0.1103(2) 0.0408(4) Uani 1 1 d . . .
O3 O 0.7475(2) -0.0365(2) 0.9536(2) 0.0380(4) Uani 1 1 d . . .
O4 O 0.5992(3) 0.22907(18) 1.0487(2) 0.0394(4) Uani 1 1 d D . .
O5 O 0.4889(3) 0.4551(2) 1.1841(3) 0.0593(6) Uani 1 1 d . . .
Zn1 Zn 0.5000 0.0000 1.0000 0.02855(12) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.316(3) . ?
C1 N2 1.343(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.354(4) . ?
C2 N1 1.369(3) . ?
C2 H2A 0.9300 . ?
C3 N2 1.356(3) . ?
C3 H3A 0.9300 . ?
C4 N2 1.468(3) . ?
C4 C5 1.489(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N7 1.354(3) . ?
C5 C6 1.364(3) . ?
C6 N5 1.341(3) . ?
C6 H6A 0.9300 . ?
C7 N5 1.455(3) . ?
C7 C8 1.529(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O2 1.240(3) . ?
C8 O1 1.246(3) . ?
N1 Zn1 2.123(2) . ?
N5 N6 1.340(3) . ?
N6 N7 1.312(3) . ?
O3 Zn1 2.1433(18) . ?
O3 H3W 0.86(4) . ?
O3 H3WA 0.79(3) . ?
O4 Zn1 2.1065(17) . ?
O4 H4W 0.870(10) . ?
O4 H4WA 0.848(10) . ?
O5 H5W 0.99(5) . ?
O5 H5WA 1.07(7) . ?
Zn1 O4 2.1065(18) 2_657 ?
Zn1 N1 2.123(2) 2_657 ?
Zn1 O3 2.1433(18) 2_657 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 111.9(2) . . ?
N1 C1 H1A 124.0 . . ?
N2 C1 H1A 124.0 . . ?
C3 C2 N1 109.9(2) . . ?
C3 C2 H2A 125.0 . . ?
N1 C2 H2A 125.0 . . ?
C2 C3 N2 106.4(2) . . ?
C2 C3 H3A 126.8 . . ?
N2 C3 H3A 126.8 . . ?
N2 C4 C5 114.6(2) . . ?
N2 C4 H4A 108.6 . . ?
C5 C4 H4A 108.6 . . ?
N2 C4 H4B 108.6 . . ?
C5 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
N7 C5 C6 107.8(2) . . ?
N7 C5 C4 121.6(2) . . ?
C6 C5 C4 130.1(2) . . ?
N5 C6 C5 105.1(2) . . ?
N5 C6 H6A 127.5 . . ?
C5 C6 H6A 127.5 . . ?
N5 C7 C8 111.29(19) . . ?
N5 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N5 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O2 C8 O1 125.6(2) . . ?
O2 C8 C7 118.4(2) . . ?
O1 C8 C7 116.0(2) . . ?
C1 N1 C2 104.9(2) . . ?
C1 N1 Zn1 127.66(16) . . ?
C2 N1 Zn1 127.22(17) . . ?
C1 N2 C3 106.9(2) . . ?
C1 N2 C4 126.1(2) . . ?
C3 N2 C4 127.0(2) . . ?
N6 N5 C6 111.0(2) . . ?
N6 N5 C7 118.3(2) . . ?
C6 N5 C7 129.8(2) . . ?
N7 N6 N5 106.67(19) . . ?
N6 N7 C5 109.4(2) . . ?
Zn1 O3 H3W 117(2) . . ?
Zn1 O3 H3WA 117(2) . . ?
H3W O3 H3WA 110(3) . . ?
Zn1 O4 H4W 126(2) . . ?
Zn1 O4 H4WA 120.1(18) . . ?
H4W O4 H4WA 108(2) . . ?
H5W O5 H5WA 110(4) . . ?
O4 Zn1 O4 180 2_657 . ?
O4 Zn1 N1 90.54(8) 2_657 2_657 ?
O4 Zn1 N1 89.46(8) . 2_657 ?
O4 Zn1 N1 89.46(8) 2_657 . ?
O4 Zn1 N1 90.54(8) . . ?
N1 Zn1 N1 180 2_657 . ?
O4 Zn1 O3 92.44(8) 2_657 . ?
O4 Zn1 O3 87.56(8) . . ?
N1 Zn1 O3 91.17(8) 2_657 . ?
N1 Zn1 O3 88.83(8) . . ?
O4 Zn1 O3 87.56(8) 2_657 2_657 ?
O4 Zn1 O3 92.44(8) . 2_657 ?
N1 Zn1 O3 88.83(8) 2_657 2_657 ?
N1 Zn1 O3 91.17(8) . 2_657 ?
O3 Zn1 O3 180 . 2_657 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.2(3) . . . . ?
N2 C4 C5 N7 70.7(3) . . . . ?
N2 C4 C5 C6 -117.8(3) . . . . ?
N7 C5 C6 N5 0.3(3) . . . . ?
C4 C5 C6 N5 -172.2(2) . . . . ?
N5 C7 C8 O2 26.6(3) . . . . ?
N5 C7 C8 O1 -154.0(2) . . . . ?
N2 C1 N1 C2 0.7(3) . . . . ?
N2 C1 N1 Zn1 175.09(15) . . . . ?
C3 C2 N1 C1 -0.5(3) . . . . ?
C3 C2 N1 Zn1 -174.98(18) . . . . ?
N1 C1 N2 C3 -0.6(3) . . . . ?
N1 C1 N2 C4 -178.0(2) . . . . ?
C2 C3 N2 C1 0.2(3) . . . . ?
C2 C3 N2 C4 177.6(2) . . . . ?
C5 C4 N2 C1 -85.9(3) . . . . ?
C5 C4 N2 C3 97.2(3) . . . . ?
C5 C6 N5 N6 0.2(3) . . . . ?
C5 C6 N5 C7 168.5(2) . . . . ?
C8 C7 N5 N6 85.4(3) . . . . ?
C8 C7 N5 C6 -82.2(3) . . . . ?
C6 N5 N6 N7 -0.6(3) . . . . ?
C7 N5 N6 N7 -170.42(19) . . . . ?
N5 N6 N7 C5 0.8(3) . . . . ?
C6 C5 N7 N6 -0.7(3) . . . . ?
C4 C5 N7 N6 172.5(2) . . . . ?
C1 N1 Zn1 O4 -158.3(2) . . . 2_657 ?
C2 N1 Zn1 O4 14.9(2) . . . 2_657 ?
C1 N1 Zn1 O4 21.7(2) . . . . ?
C2 N1 Zn1 O4 -165.1(2) . . . . ?
C1 N1 Zn1 N1 103(100) . . . 2_657 ?
C2 N1 Zn1 N1 -84(100) . . . 2_657 ?
C1 N1 Zn1 O3 -65.9(2) . . . . ?
C2 N1 Zn1 O3 107.3(2) . . . . ?
C1 N1 Zn1 O3 114.1(2) . . . 2_657 ?
C2 N1 Zn1 O3 -72.7(2) . . . 2_657 ?

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
O4 H4W O5 0.870(10) 1.797(13) 2.651(3) 167(3) .
O3 H3WA O1 0.79(3) 1.96(3) 2.729(3) 161(3) 1_646
O4 H4WA O2 0.848(10) 1.884(10) 2.730(2) 177(3) 2_666
O3 H3W O1 0.86(4) 1.91(4) 2.763(3) 170(3) 2_666
O5 H5WA N6 1.07(7) 2.54(7) 3.499(3) 149(5) 2_667
O5 H5WA N7 1.07(7) 1.76(7) 2.824(3) 174(5) 2_667
O5 H5W O2 0.99(5) 1.89(5) 2.846(3) 161(4) 1_556

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.86
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.062

#===END




