# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1478775'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_audit_creation_date             2016-07-06
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H48 Co7 N10 O35, 2(H2 O), 2(H2 O)'
_chemical_formula_sum            'C68 H56 Co7 N10 O39'
_chemical_formula_weight         2049.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 O1 Co1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.5995(2)
_cell_length_b                   12.1967(3)
_cell_length_c                   16.3411(4)
_cell_angle_alpha                98.732(2)
_cell_angle_beta                 107.645(2)
_cell_angle_gamma                109.102(2)
_cell_volume                     1826.91(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    13841
_cell_measurement_temperature    288.53(10)
_cell_measurement_theta_max      71.4310
_cell_measurement_theta_min      4.5380
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1031
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34095
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.648
_diffrn_reflns_theta_min         4.563
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      288.53(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   57.00  107.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  178.0000  -30.0000 50

#__ type_ start__ end____ width___ exp.time_
  2 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega    1.00   74.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000 -150.0000 73

#__ type_ start__ end____ width___ exp.time_
  4 omega  -32.00   62.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -77.0000  -30.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega  -32.00   62.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -77.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega  -34.00   54.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -38.0000   60.0000 88

#__ type_ start__ end____ width___ exp.time_
  7 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
  8 omega   16.00  104.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   38.0000  -60.0000 88

#__ type_ start__ end____ width___ exp.time_
  9 omega    1.00   74.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000  -30.0000 73

#__ type_ start__ end____ width___ exp.time_
 10 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
 11 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 12 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000 -150.0000 84

#__ type_ start__ end____ width___ exp.time_
 13 omega  -32.00   52.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -57.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 14 omega   87.00  178.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
 15 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

#__ type_ start__ end____ width___ exp.time_
 16 omega   87.00  178.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -150.0000 91

#__ type_ start__ end____ width___ exp.time_
 17 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
 18 omega   39.00  110.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -90.0000 71

#__ type_ start__ end____ width___ exp.time_
 19 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
 20 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

#__ type_ start__ end____ width___ exp.time_
 21 omega   91.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85

#__ type_ start__ end____ width___ exp.time_
 22 omega   40.00  135.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 23 omega   38.00  116.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000   60.0000 78

#__ type_ start__ end____ width___ exp.time_
 24 omega   39.00  110.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -60.0000 71

#__ type_ start__ end____ width___ exp.time_
 25 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

#__ type_ start__ end____ width___ exp.time_
 26 omega   39.00  110.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   90.0000 71

#__ type_ start__ end____ width___ exp.time_
 27 omega   40.00   98.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 58

#__ type_ start__ end____ width___ exp.time_
 28 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
 29 omega   40.00   98.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

#__ type_ start__ end____ width___ exp.time_
 30 omega   39.00  110.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 71

#__ type_ start__ end____ width___ exp.time_
 31 omega   40.00  135.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -30.0000 95

#__ type_ start__ end____ width___ exp.time_
 32 omega   57.00  107.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  178.0000  120.0000 50

#__ type_ start__ end____ width___ exp.time_
 33 omega  -36.00   65.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -19.0000  150.0000 101

#__ type_ start__ end____ width___ exp.time_
 34 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
 35 omega   16.00  104.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   38.0000 -150.0000 88

#__ type_ start__ end____ width___ exp.time_
 36 omega  -32.00   52.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -57.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 37 omega    1.00   74.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000  150.0000 73

#__ type_ start__ end____ width___ exp.time_
 38 omega    0.00   27.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   93.0000  162.2068 27

#__ type_ start__ end____ width___ exp.time_
 39 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 40 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
 41 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 42 omega    1.00   74.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000   60.0000 73

#__ type_ start__ end____ width___ exp.time_
 43 omega    6.00  107.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   19.0000 -180.0000 101

#__ type_ start__ end____ width___ exp.time_
 44 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000  -30.0000 95

#__ type_ start__ end____ width___ exp.time_
 45 omega   87.00  178.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -90.0000 91

#__ type_ start__ end____ width___ exp.time_
 46 omega   70.00  178.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000    0.0000 108

#__ type_ start__ end____ width___ exp.time_
 47 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 48 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 49 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95

#__ type_ start__ end____ width___ exp.time_
 50 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
 51 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
 52 omega   91.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 85

#__ type_ start__ end____ width___ exp.time_
 53 omega   87.00  166.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  120.0000 79

#__ type_ start__ end____ width___ exp.time_
 54 omega   91.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1258670000
_diffrn_orient_matrix_UB_12      -0.0945098000
_diffrn_orient_matrix_UB_13      0.0122188000
_diffrn_orient_matrix_UB_21      -0.0951822000
_diffrn_orient_matrix_UB_22      -0.0252777000
_diffrn_orient_matrix_UB_23      -0.0987034000
_diffrn_orient_matrix_UB_31      0.0519017000
_diffrn_orient_matrix_UB_32      -0.0990048000
_diffrn_orient_matrix_UB_33      -0.0268333000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5876
_reflns_number_total             7067
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7067
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0349
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0397P)²+1.7212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0854
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Others
 Sof(O9)=1-FVAR(1)
 Sof(O10)=FVAR(1)
 Sof(O5W)=1-FVAR(2)
 Sof(O5WA)=FVAR(2)
 Fixed Sof: O15(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O16(H16), O4W(H4WA,H4WB)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C8(H8), C10(H10), C12(H12), C19(H19), C21(H21),
 C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
  C34(H34)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.49555(4) 0.49448(4) 1.23610(3) 0.01583(10) Uani 1 1 d . . . . .
Co2 Co 0.34910(4) 0.46606(4) 0.50826(3) 0.01643(10) Uani 1 1 d . . . . .
Co3 Co 0.35040(4) 0.29058(4) 0.32560(3) 0.01747(10) Uani 1 1 d . . . . .
Co4 Co 0.0000 0.0000 0.5000 0.03545(19) Uani 1 2 d S T P . .
O1W O 0.61496(19) 0.60633(17) 1.37486(11) 0.0186(4) Uani 1 1 d . . . . .
H1WA H 0.5754 0.6548 1.3715 0.028 Uiso 1 1 d R . . . .
H1WB H 0.6971 0.6265 1.3732 0.028 Uiso 1 1 d R . . . .
O1 O 0.4414(2) 0.62825(17) 1.19668(13) 0.0240(4) Uani 1 1 d . . . . .
O2W O 0.0726(3) -0.1431(2) 0.49187(16) 0.0484(7) Uani 1 1 d . . . . .
H2WA H 0.1628 -0.1364 0.5229 0.073 Uiso 1 1 d R . . . .
H2WB H 0.0081 -0.2053 0.4492 0.073 Uiso 1 1 d R . . . .
O2 O 0.4762(3) 0.7436(2) 1.32752(14) 0.0387(6) Uani 1 1 d . . . . .
O3 O 0.3966(3) 1.12779(19) 1.33613(14) 0.0321(5) Uani 1 1 d . . . . .
O3W O -0.1966(3) -0.1254(2) 0.48482(15) 0.0481(7) Uani 1 1 d . . . . .
H3WA H -0.1857 -0.1729 0.5190 0.072 Uiso 1 1 d R . . . .
H3WB H -0.2493 -0.0898 0.4992 0.072 Uiso 1 1 d R . . . .
O4 O 0.2792(2) 1.15229(19) 1.20960(14) 0.0297(5) Uani 1 1 d . . . . .
O5W O 0.3292(15) -0.155(5) 0.537(3) 0.23(2) Uani 0.39(3) 1 d . . . A 2
O5WA O 0.3133(15) -0.2140(10) 0.4688(16) 0.155(7) Uani 0.61(3) 1 d . . . A 1
O5 O -0.1504(2) 0.77957(19) 0.67117(15) 0.0313(5) Uani 1 1 d . . . . .
O6 O -0.1458(2) 0.6791(2) 0.54724(13) 0.0282(5) Uani 1 1 d . . . . .
O7 O 0.2802(2) 0.57851(19) 0.57288(12) 0.0252(4) Uani 1 1 d . . . . .
O8 O 0.4615(2) 0.63896(17) 0.70584(12) 0.0200(4) Uani 1 1 d . . . . .
O9 O 0.0961(9) 0.8414(9) 0.9379(5) 0.087(3) Uani 0.445(7) 1 d . U . . .
O10 O 0.4306(6) 0.8459(7) 0.9661(3) 0.080(2) Uani 0.555(7) 1 d . U . . .
O11 O -0.3124(2) 0.54743(19) 0.21593(13) 0.0257(4) Uani 1 1 d . . . . .
O12 O -0.1406(2) 0.6529(2) 0.35014(13) 0.0306(5) Uani 1 1 d . . . . .
O13 O 0.2798(2) 0.5249(2) 0.39532(12) 0.0266(5) Uani 1 1 d . . . . .
O14 O 0.3058(2) 0.43211(17) 0.27612(12) 0.0208(4) Uani 1 1 d . . . . .
O15 O -0.1609(7) 0.5244(8) -0.0202(4) 0.079(2) Uani 0.5 1 d . . . . .
O16 O 0.45447(19) 0.38206(16) 0.45508(11) 0.0174(4) Uani 1 1 d . . . . .
H16 H 0.4687 0.3271 0.4792 0.026 Uiso 1 1 d R . . . .
N1 N 0.2083(3) 0.8138(3) 0.96449(17) 0.0371(7) Uani 1 1 d . . . . .
N2 N 0.2863(3) 0.8005(3) 0.92541(18) 0.0462(8) Uani 1 1 d . . . . .
N3 N -0.0409(3) 0.5124(3) 0.01699(16) 0.0297(6) Uani 1 1 d . . . . .
N4 N 0.3813(3) 0.3706(2) 1.10390(14) 0.0213(5) Uani 1 1 d . . . . .
N5 N 0.0699(3) 0.0416(2) 0.64649(17) 0.0359(7) Uani 1 1 d . . . . .
C1 C 0.3227(3) 0.7664(3) 1.1032(2) 0.0280(7) Uani 1 1 d . . . . .
H1 H 0.3210 0.6966 1.0699 0.034 Uiso 1 1 calc R . . . .
C2 C 0.3765(3) 0.7961(3) 1.19599(19) 0.0223(6) Uani 1 1 d . . . . .
C3 C 0.3800(3) 0.9013(3) 1.24515(18) 0.0241(6) Uani 1 1 d . . . . .
H3 H 0.4169 0.9217 1.3073 0.029 Uiso 1 1 calc R . . . .
C4 C 0.3284(3) 0.9757(3) 1.20162(19) 0.0251(6) Uani 1 1 d . . . . .
C5 C 0.2728(4) 0.9458(3) 1.1089(2) 0.0293(7) Uani 1 1 d . . . . .
H5 H 0.2371 0.9954 1.0797 0.035 Uiso 1 1 calc R . . . .
C6 C 0.2712(4) 0.8424(3) 1.06066(19) 0.0296(7) Uani 1 1 d . . . . .
C7 C 0.2303(4) 0.7704(3) 0.82831(19) 0.0321(7) Uani 1 1 d . . . . .
C8 C 0.1021(3) 0.7756(3) 0.77660(19) 0.0279(7) Uani 1 1 d . . . . .
H8 H 0.0504 0.8060 0.8037 0.033 Uiso 1 1 calc R . . . .
C9 C 0.0528(3) 0.7349(3) 0.68437(18) 0.0205(6) Uani 1 1 d . . . . .
C10 C 0.1284(3) 0.6872(3) 0.64388(17) 0.0194(5) Uani 1 1 d . . . . .
H10 H 0.0924 0.6563 0.5821 0.023 Uiso 1 1 calc R . . . .
C11 C 0.2589(3) 0.6859(3) 0.69652(18) 0.0200(6) Uani 1 1 d . . . . .
C12 C 0.3096(3) 0.7289(3) 0.78849(19) 0.0306(7) Uani 1 1 d . . . . .
H12 H 0.3976 0.7299 0.8236 0.037 Uiso 1 1 calc R . . . .
C13 C 0.4360(3) 0.7169(3) 1.24450(19) 0.0233(6) Uani 1 1 d . . . . .
C14 C 0.3349(3) 1.0917(3) 1.25245(19) 0.0250(6) Uani 1 1 d . . . . .
C15 C -0.0919(3) 0.7313(3) 0.62990(18) 0.0211(6) Uani 1 1 d . . . . .
C16 C 0.3376(3) 0.6301(2) 0.65465(17) 0.0188(5) Uani 1 1 d . . . . .
C17 C -0.1826(3) 0.5946(3) 0.27073(18) 0.0208(6) Uani 1 1 d . . . . .
C18 C -0.0753(3) 0.5719(3) 0.23538(18) 0.0199(6) Uani 1 1 d . . . . .
C19 C -0.1003(3) 0.5538(3) 0.14459(18) 0.0239(6) Uani 1 1 d . . . . .
H19 H -0.1803 0.5614 0.1065 0.029 Uiso 1 1 calc R . . . .
C20 C -0.0071(3) 0.5246(3) 0.11097(18) 0.0226(6) Uani 1 1 d . . . . .
C21 C 0.1081(3) 0.5049(3) 0.16528(17) 0.0212(6) Uani 1 1 d . . . . .
H21 H 0.1673 0.4810 0.1415 0.025 Uiso 1 1 calc R . . . .
C22 C 0.1328(3) 0.5216(2) 0.25523(17) 0.0180(5) Uani 1 1 d . . . . .
C23 C 0.0444(3) 0.5585(2) 0.29078(17) 0.0186(5) Uani 1 1 d . . . . .
H23 H 0.0655 0.5743 0.3520 0.022 Uiso 1 1 calc R . . . .
C24 C 0.2500(3) 0.4930(2) 0.31387(17) 0.0186(5) Uani 1 1 d . . . . .
C25 C 0.2460(3) 0.2866(3) 1.07198(19) 0.0269(6) Uani 1 1 d . . . . .
H25 H 0.1958 0.2782 1.1100 0.032 Uiso 1 1 calc R . . . .
C26 C 0.1772(3) 0.2116(3) 0.98508(19) 0.0317(7) Uani 1 1 d . . . . .
H26 H 0.0833 0.1547 0.9662 0.038 Uiso 1 1 calc R . . . .
C27 C 0.2486(3) 0.2215(3) 0.92670(18) 0.0270(6) Uani 1 1 d . . . . .
C28 C 0.3887(3) 0.3090(3) 0.95937(19) 0.0303(7) Uani 1 1 d . . . . .
H28 H 0.4407 0.3200 0.9224 0.036 Uiso 1 1 calc R . . . .
C29 C 0.4496(3) 0.3790(3) 1.04642(19) 0.0284(7) Uani 1 1 d . . . . .
H29 H 0.5440 0.4358 1.0669 0.034 Uiso 1 1 calc R . . . .
C30 C -0.0107(4) 0.0702(3) 0.6877(2) 0.0411(9) Uani 1 1 d . . . . .
H30 H -0.1062 0.0530 0.6533 0.049 Uiso 1 1 calc R . . . .
C31 C 0.0395(4) 0.1238(3) 0.7785(2) 0.0357(8) Uani 1 1 d . . . . .
H31 H -0.0209 0.1424 0.8041 0.043 Uiso 1 1 calc R . . . .
C32 C 0.1813(3) 0.1493(3) 0.83090(19) 0.0299(7) Uani 1 1 d . . . . .
C33 C 0.2624(4) 0.1127(3) 0.7894(2) 0.0386(8) Uani 1 1 d . . . . .
H33 H 0.3561 0.1234 0.8227 0.046 Uiso 1 1 calc R . . . .
C34 C 0.2035(4) 0.0602(3) 0.6981(2) 0.0386(8) Uani 1 1 d . . . . .
H34 H 0.2599 0.0365 0.6713 0.046 Uiso 1 1 calc R . . . .
O4W O -0.3916(7) -0.0574(7) 0.5137(4) 0.178(3) Uani 1 1 d . . . . .
H4WA H -0.4426 -0.1096 0.5323 0.267 Uiso 1 1 d R . . . .
H4WB H -0.4450 -0.0520 0.4651 0.267 Uiso 1 1 d R . . . .


_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
Co1 O1W 2.1898(18) . ?
Co1 O1 2.0284(19) . ?
Co1 O8 2.1091(19) 2_667 ?
Co1 O11 2.069(2) 1_656 ?
Co1 O14 2.2360(19) 1_556 ?
Co1 N4 2.155(2) . ?
Co2 O1W 2.2055(17) 2_667 ?
Co2 O6 2.106(2) 2_566 ?
Co2 O7 2.052(2) . ?
Co2 O13 2.0943(18) . ?
Co2 O16 2.0296(19) . ?
Co2 O16 2.1231(19) 2_666 ?
Co3 O3 2.214(2) 1_544 ?
Co3 O4 2.082(2) 1_544 ?
Co3 O5 2.031(2) 2_566 ?
Co3 O8 2.1470(19) 2_666 ?
Co3 O14 2.1409(19) . ?
Co3 O16 2.0002(18) . ?
Co3 C14 2.465(3) 1_544 ?
Co4 O2W 2.128(3) . ?
Co4 O2W 2.128(3) 2_556 ?
Co4 O3W 2.056(2) 2_556 ?
Co4 O3W 2.056(2) . ?
Co4 N5 2.202(2) 2_556 ?
Co4 N5 2.201(2) . ?
O1W Co2 2.2055(17) 2_667 ?
O1 C13 1.262(4) . ?
O2 C13 1.246(4) . ?
O3 Co3 2.214(2) 1_566 ?
O3 C14 1.256(4) . ?
O4 Co3 2.082(2) 1_566 ?
O4 C14 1.256(3) . ?
O5 Co3 2.031(2) 2_566 ?
O5 C15 1.248(4) . ?
O6 Co2 2.106(2) 2_566 ?
O6 C15 1.261(3) . ?
O7 C16 1.246(3) . ?
O8 Co1 2.1090(19) 2_667 ?
O8 Co3 2.1470(19) 2_666 ?
O8 C16 1.285(3) . ?
O9 N1 1.307(7) . ?
O10 N2 1.344(6) . ?
O11 Co1 2.069(2) 1_454 ?
O11 C17 1.267(3) . ?
O12 C17 1.245(3) . ?
O13 C24 1.237(3) . ?
O14 Co1 2.2360(19) 1_554 ?
O14 C24 1.285(3) . ?
O15 N3 1.300(6) . ?
O16 Co2 2.1231(18) 2_666 ?
N1 N2 1.222(4) . ?
N1 C6 1.443(4) . ?
N2 C7 1.454(4) . ?
N3 N3 1.250(5) 2_565 ?
N3 C20 1.439(3) . ?
N4 C25 1.342(4) . ?
N4 C29 1.346(4) . ?
N5 C30 1.333(5) . ?
N5 C34 1.332(5) . ?
C1 C2 1.389(4) . ?
C1 C6 1.392(4) . ?
C2 C3 1.390(4) . ?
C2 C13 1.512(4) . ?
C3 C4 1.383(4) . ?
C4 C5 1.388(4) . ?
C4 C14 1.498(4) . ?
C5 C6 1.373(4) . ?
C7 C8 1.393(4) . ?
C7 C12 1.377(4) . ?
C8 C9 1.384(4) . ?
C9 C10 1.389(4) . ?
C9 C15 1.505(4) . ?
C10 C11 1.397(4) . ?
C11 C12 1.382(4) . ?
C11 C16 1.484(4) . ?
C14 Co3 2.465(3) 1_566 ?
C17 C18 1.503(4) . ?
C18 C19 1.394(4) . ?
C18 C23 1.393(4) . ?
C19 C20 1.380(4) . ?
C20 C21 1.391(4) . ?
C21 C22 1.382(4) . ?
C22 C23 1.395(4) . ?
C22 C24 1.498(4) . ?
C25 C26 1.388(4) . ?
C26 C27 1.382(4) . ?
C27 C28 1.392(4) . ?
C27 C32 1.493(4) . ?
C28 C29 1.372(4) . ?
C30 C31 1.384(4) . ?
C31 C32 1.385(4) . ?
C32 C33 1.383(5) . ?
C33 C34 1.382(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
O1W Co1 O14 85.66(7) . 1_556 ?
O1 Co1 O1W 92.16(8) . . ?
O1 Co1 O8 170.29(8) . 2_667 ?
O1 Co1 O11 95.25(8) . 1_656 ?
O1 Co1 O14 91.16(8) . 1_556 ?
O1 Co1 N4 93.17(8) . . ?
O8 Co1 O1W 81.72(7) 2_667 . ?
O8 Co1 O14 80.91(7) 2_667 1_556 ?
O8 Co1 N4 92.91(8) 2_667 . ?
O11 Co1 O1W 88.64(8) 1_656 . ?
O11 Co1 O8 92.15(8) 1_656 2_667 ?
O11 Co1 O14 171.59(7) 1_656 1_556 ?
O11 Co1 N4 91.52(9) 1_656 . ?
N4 Co1 O1W 174.63(8) . . ?
N4 Co1 O14 93.57(8) . 1_556 ?
O6 Co2 O1W 85.64(7) 2_566 2_667 ?
O6 Co2 O16 171.24(7) 2_566 2_666 ?
O7 Co2 O1W 87.59(7) . 2_667 ?
O7 Co2 O6 94.06(9) . 2_566 ?
O7 Co2 O13 87.75(8) . . ?
O7 Co2 O16 87.30(8) . 2_666 ?
O13 Co2 O1W 170.65(8) . 2_667 ?
O13 Co2 O6 86.61(8) . 2_566 ?
O13 Co2 O16 84.80(8) . 2_666 ?
O16 Co2 O1W 103.07(7) 2_666 2_667 ?
O16 Co2 O1W 93.14(7) . 2_667 ?
O16 Co2 O6 96.93(8) . 2_566 ?
O16 Co2 O7 169.00(8) . . ?
O16 Co2 O13 92.98(8) . . ?
O16 Co2 O16 81.85(8) . 2_666 ?
O3 Co3 C14 30.54(8) 1_544 1_544 ?
O4 Co3 O3 61.12(8) 1_544 1_544 ?
O4 Co3 O8 83.89(8) 1_544 2_666 ?
O4 Co3 O14 103.27(8) 1_544 . ?
O4 Co3 C14 30.60(9) 1_544 1_544 ?
O5 Co3 O3 95.48(9) 2_566 1_544 ?
O5 Co3 O4 88.33(9) 2_566 1_544 ?
O5 Co3 O8 168.32(8) 2_566 2_666 ?
O5 Co3 O14 91.09(8) 2_566 . ?
O5 Co3 C14 93.08(9) 2_566 1_544 ?
O8 Co3 O3 88.39(8) 2_666 1_544 ?
O8 Co3 C14 84.65(9) 2_666 1_544 ?
O14 Co3 O3 162.75(8) . 1_544 ?
O14 Co3 O8 82.28(7) . 2_666 ?
O14 Co3 C14 133.32(9) . 1_544 ?
O16 Co3 O3 96.96(8) . 1_544 ?
O16 Co3 O4 157.92(8) . 1_544 ?
O16 Co3 O5 96.94(8) . 2_566 ?
O16 Co3 O8 93.51(7) . 2_666 ?
O16 Co3 O14 98.07(7) . . ?
O16 Co3 C14 127.39(9) . 1_544 ?
O2W Co4 O2W 180.00(5) . 2_556 ?
O2W Co4 N5 87.28(10) 2_556 . ?
O2W Co4 N5 87.28(10) . 2_556 ?
O2W Co4 N5 92.72(10) . . ?
O2W Co4 N5 92.72(10) 2_556 2_556 ?
O3W Co4 O2W 92.25(11) 2_556 . ?
O3W Co4 O2W 87.75(11) 2_556 2_556 ?
O3W Co4 O2W 87.75(11) . . ?
O3W Co4 O2W 92.25(11) . 2_556 ?
O3W Co4 O3W 180.00(11) 2_556 . ?
O3W Co4 N5 89.30(10) 2_556 . ?
O3W Co4 N5 90.70(10) 2_556 2_556 ?
O3W Co4 N5 89.30(10) . 2_556 ?
O3W Co4 N5 90.70(10) . . ?
N5 Co4 N5 180.0 . 2_556 ?
Co1 O1W Co2 124.24(9) . 2_667 ?
C13 O1 Co1 127.64(18) . . ?
C14 O3 Co3 85.89(17) . 1_566 ?
C14 O4 Co3 91.81(18) . 1_566 ?
C15 O5 Co3 129.34(19) . 2_566 ?
C15 O6 Co2 119.62(18) . 2_566 ?
C16 O7 Co2 123.96(18) . . ?
Co1 O8 Co3 100.16(8) 2_667 2_666 ?
C16 O8 Co1 126.10(17) . 2_667 ?
C16 O8 Co3 121.49(16) . 2_666 ?
C17 O11 Co1 131.28(18) . 1_454 ?
C24 O13 Co2 138.9(2) . . ?
Co3 O14 Co1 96.43(7) . 1_554 ?
C24 O14 Co1 130.35(17) . 1_554 ?
C24 O14 Co3 120.23(16) . . ?
Co2 O16 Co2 98.15(8) . 2_666 ?
Co3 O16 Co2 117.64(8) . 2_666 ?
Co3 O16 Co2 115.34(9) . . ?
O9 N1 C6 111.7(4) . . ?
N2 N1 O9 129.4(4) . . ?
N2 N1 C6 115.5(3) . . ?
O10 N2 C7 115.7(3) . . ?
N1 N2 O10 122.5(4) . . ?
N1 N2 C7 118.9(3) . . ?
O15 N3 C20 111.5(3) . . ?
N3 N3 O15 130.1(4) 2_565 . ?
N3 N3 C20 118.4(3) 2_565 . ?
C25 N4 Co1 126.27(19) . . ?
C25 N4 C29 116.1(2) . . ?
C29 N4 Co1 117.6(2) . . ?
C30 N5 Co4 120.8(2) . . ?
C34 N5 Co4 121.4(2) . . ?
C34 N5 C30 116.8(3) . . ?
C2 C1 C6 119.2(3) . . ?
C1 C2 C3 120.0(3) . . ?
C1 C2 C13 120.6(3) . . ?
C3 C2 C13 119.4(2) . . ?
C4 C3 C2 120.0(3) . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 C14 121.4(3) . . ?
C5 C4 C14 118.2(3) . . ?
C6 C5 C4 119.4(3) . . ?
C1 C6 N1 121.7(3) . . ?
C5 C6 N1 117.1(3) . . ?
C5 C6 C1 121.1(3) . . ?
C8 C7 N2 124.1(3) . . ?
C12 C7 N2 115.2(3) . . ?
C12 C7 C8 120.7(3) . . ?
C9 C8 C7 119.1(3) . . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 C15 118.4(3) . . ?
C10 C9 C15 120.8(2) . . ?
C9 C10 C11 119.6(2) . . ?
C10 C11 C16 120.3(2) . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 C16 119.8(3) . . ?
C7 C12 C11 120.2(3) . . ?
O1 C13 C2 116.5(2) . . ?
O2 C13 O1 125.1(3) . . ?
O2 C13 C2 118.3(3) . . ?
O3 C14 Co3 63.57(16) . 1_566 ?
O3 C14 C4 120.3(3) . . ?
O4 C14 Co3 57.59(15) . 1_566 ?
O4 C14 O3 121.1(3) . . ?
O4 C14 C4 118.6(3) . . ?
C4 C14 Co3 174.9(2) . 1_566 ?
O5 C15 O6 125.0(3) . . ?
O5 C15 C9 116.6(3) . . ?
O6 C15 C9 118.3(3) . . ?
O7 C16 O8 124.4(3) . . ?
O7 C16 C11 118.4(2) . . ?
O8 C16 C11 117.2(2) . . ?
O11 C17 C18 115.5(2) . . ?
O12 C17 O11 125.1(3) . . ?
O12 C17 C18 119.4(2) . . ?
C19 C18 C17 120.3(2) . . ?
C23 C18 C17 120.9(2) . . ?
C23 C18 C19 118.6(3) . . ?
C20 C19 C18 120.4(3) . . ?
C19 C20 N3 115.5(2) . . ?
C19 C20 C21 121.0(2) . . ?
C21 C20 N3 123.5(3) . . ?
C22 C21 C20 118.8(3) . . ?
C21 C22 C23 120.4(2) . . ?
C21 C22 C24 119.8(2) . . ?
C23 C22 C24 119.7(2) . . ?
C18 C23 C22 120.5(2) . . ?
O13 C24 O14 125.1(2) . . ?
O13 C24 C22 116.7(2) . . ?
O14 C24 C22 118.1(2) . . ?
N4 C25 C26 123.3(3) . . ?
C27 C26 C25 119.9(3) . . ?
C26 C27 C28 116.9(3) . . ?
C26 C27 C32 123.8(3) . . ?
C28 C27 C32 119.2(3) . . ?
C29 C28 C27 119.6(3) . . ?
N4 C29 C28 124.0(3) . . ?
N5 C30 C31 123.8(3) . . ?
C30 C31 C32 119.0(3) . . ?
C31 C32 C27 121.9(3) . . ?
C33 C32 C27 120.5(3) . . ?
C33 C32 C31 117.4(3) . . ?
C34 C33 C32 119.6(3) . . ?
N5 C34 C33 123.3(3) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form

_vrf_PLAT420_1                   
;
PROBLEM: D-H Without Acceptor       O16    --  H16    ...     Please Check   
RESPONSE: H16 is the brige atom in the cluster, which doesn't have an accepor.
;
####################################################################### 
# 
# 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 1478776'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_audit_creation_date             2016-08-18
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.13(C416 H336 N64 Ni40 O208), 4(H2 O)'
_chemical_formula_sum            'C52 H50 N8 Ni5 O30'
_chemical_formula_weight         1560.55
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_H-M_alt        'C c c e'
_space_group_name_Hall           '-C 2b 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y+1/2, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z'
'x+1/2, -y+1, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y-1/2, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z'
'-x+1/2, y, z-1/2'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   11.84540(14)
_cell_length_b                   28.3935(3)
_cell_length_c                   34.5364(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11615.7(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    24770
_cell_measurement_temperature    291.57(10)
_cell_measurement_theta_max      71.3890
_cell_measurement_theta_min      5.5680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6384
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            51611
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.570
_diffrn_reflns_theta_min         4.242
_diffrn_ambient_temperature      291.57(10)
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   57.00  109.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  178.0000 -150.0000 52

#__ type_ start__ end____ width___ exp.time_
  2 omega  -32.00   56.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -38.0000   30.0000 88

#__ type_ start__ end____ width___ exp.time_
  3 omega   20.00  104.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000 -150.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega   57.00  109.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  178.0000  -30.0000 52

#__ type_ start__ end____ width___ exp.time_
  5 omega  -31.00   64.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
  6 omega   39.00  110.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  150.0000 71

#__ type_ start__ end____ width___ exp.time_
  7 omega   41.00  126.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -150.0000 85

#__ type_ start__ end____ width___ exp.time_
  8 omega   40.00   98.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 58

#__ type_ start__ end____ width___ exp.time_
  9 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

#__ type_ start__ end____ width___ exp.time_
 10 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
 11 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -28.0000 -134.0000 53

#__ type_ start__ end____ width___ exp.time_
 12 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
 13 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

#__ type_ start__ end____ width___ exp.time_
 14 omega   40.00   98.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

#__ type_ start__ end____ width___ exp.time_
 15 omega   41.00  126.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -30.0000 85

#__ type_ start__ end____ width___ exp.time_
 16 omega   20.00  104.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
 17 omega   10.00  105.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   77.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
 18 omega   20.00  104.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000   90.0000 84

#__ type_ start__ end____ width___ exp.time_
 19 omega   18.00  106.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   38.0000    0.0000 88

#__ type_ start__ end____ width___ exp.time_
 20 omega   70.00  178.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   60.0000 108

#__ type_ start__ end____ width___ exp.time_
 21 omega   87.00  178.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
 22 omega   70.00  178.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108

#__ type_ start__ end____ width___ exp.time_
 23 omega   38.00  116.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000    0.0000 78

#__ type_ start__ end____ width___ exp.time_
 24 omega   90.00  175.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
 25 omega   91.00  148.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   90.0000 57

#__ type_ start__ end____ width___ exp.time_
 26 omega   87.00  178.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5357
_reflns_number_total             5660
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.872
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         5660
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0622P)²+52.4618P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1355
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H13 of C13, H26 of C26, H25 of C25, H18 of C18, H21 of
  C21, H23 of C23, H17 of C17, H15 of C15, H24 of C24, H20 of C20, H3A of C3A,
  H3B of C3B, H5A of C5A, H5B of C5B, H11 of C11
 At 1.5 times of:
  All O(H) groups, H6 of C26, All O(H,H) groups
2. Restrained distances
 C7-C2B \\sim C7-C2A \\sim C3A-C2A \\sim C3B-C2B
 with sigma of 0.02
 N0-C4A \\sim N0A-C4B
 with sigma of 0.02
3. Rigid bond restraints
 O5, N0, C4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O5 \\sim N0 \\sim C4A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C6A) \\sim Ueq, Uanis(C6B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C2B) \\sim Ueq, Uanis(C2A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O5WA) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 O5, N0, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N0A, C2B, C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
6. Others
 Fixed Sof: O5(0.5) O11(0.5) N0(0.5) N0A(0.5) C2A(0.5) C2B(0.5) C3A(0.5)
 H3A(0.5) C3B(0.5) H3B(0.5) C4A(0.5) C4B(0.5) C5A(0.5) H5A(0.5) C5B(0.5)
 H5B(0.5) C6A(0.5) C6B(0.5) H7B(0.5) H7A(0.5) O5WA(0.2) H5WA(0.2) H5WB(0.2)
 O5WB(0.8) H5WC(0.8) H5WD(0.8) O6W(0.8) H6WA(0.8) H6WB(0.8) O7W(0.2) H7WA(0.2)
 H7WB(0.2)
7.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2W), O3W(H3WA,H3WB), O4W(H4W), O5WA(H5WA,H5WB),
 O5WB(H5WC,H5WD), O6W(H6WA,H6WB), O7W(H7WA,H7WB)
7.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C5A(H5A), C5B(H5B), C7(H7B), C7(H7A), C11(H11), C13(H13),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.7500 0.5000 0.07962(2) 0.02050(17) Uani 1 2 d S T P . .
Ni2 Ni 0.7500 0.5000 0.16855(2) 0.0275(2) Uani 1 2 d S T P . .
Ni3 Ni 0.78365(5) 0.39007(2) 0.12687(2) 0.02189(15) Uani 1 1 d . . . . .
Ni4 Ni 0.7500 0.0000 0.08514(2) 0.02411(18) Uani 1 2 d S T P . .
O1 O 0.3842(2) 0.60552(8) -0.10962(7) 0.0343(5) Uani 1 1 d . . . . .
O1W O 0.9150(2) 0.53034(9) 0.16921(8) 0.0429(6) Uani 1 1 d . . . . .
H1WA H 0.9215 0.5586 0.1594 0.064 Uiso 1 1 d R . . . .
H1WB H 0.9606 0.5058 0.1634 0.064 Uiso 1 1 d R . . . .
O2 O 0.39430(18) 0.54147(7) -0.07205(7) 0.0280(5) Uani 1 1 d . . . . .
O2W O 0.7500 0.0000 0.02539(9) 0.0396(8) Uani 1 2 d S T P . .
H2W H 0.7163 0.0200 0.0114 0.059 Uiso 1 1 d R . . . .
O3 O 0.66929(19) 0.54648(7) 0.03824(6) 0.0266(5) Uani 1 1 d . . . . .
O3W O 0.9195(2) 0.01478(9) 0.08515(8) 0.0385(6) Uani 1 1 d . . . . .
H3WA H 0.9779 0.0005 0.0803 0.058 Uiso 1 1 d R . . . .
H3WB H 0.9512 0.0387 0.1008 0.058 Uiso 1 1 d R . . . .
O4 O 0.6713(2) 0.61545(7) 0.07015(7) 0.0355(6) Uani 1 1 d . . . . .
O4W O 0.7500 0.0000 0.14633(11) 0.0516(10) Uani 1 2 d S T P . .
H4W H 0.7977 0.0142 0.1584 0.077 Uiso 1 1 d R . . . .
O5 O 0.4689(6) 0.7460(3) 0.02849(16) 0.0605(13) Uani 0.5 1 d . U . A -2
O6 O 0.80776(19) 0.45964(7) 0.12429(6) 0.0227(4) Uani 1 1 d . . . . .
O7 O 0.8024(3) 0.45656(8) 0.21139(7) 0.0419(6) Uani 1 1 d . . . . .
O8 O 0.7272(2) 0.39224(8) 0.18425(6) 0.0337(5) Uani 1 1 d . . . . .
O9 O 1.0531(2) 0.37679(9) 0.35425(8) 0.0435(6) Uani 1 1 d . . . . .
O10 O 0.9544(2) 0.44304(9) 0.34686(8) 0.0441(6) Uani 1 1 d . . . . .
O11 O 0.8724(7) 0.23774(18) 0.30055(16) 0.062(2) Uani 0.5 1 d . . . . .
N0 N 0.5038(8) 0.73830(17) -0.00766(19) 0.0496(11) Uani 0.5 1 d D U . B -2
N0A N 0.5323(5) 0.73651(17) -0.03229(15) 0.0291(10) Uani 0.5 1 d D U . C -1
N1 N 0.7671(2) 0.31697(9) 0.12621(7) 0.0257(5) Uani 1 1 d . . . . .
N2 N 0.7282(2) 0.07276(9) 0.08854(8) 0.0286(6) Uani 1 1 d . . . . .
N3 N 0.8639(3) 0.25854(9) 0.26716(8) 0.0328(6) Uani 1 1 d . . . . .
C1 C 0.4105(2) 0.58458(11) -0.07893(9) 0.0247(6) Uani 1 1 d . . . . .
C2A C 0.4649(9) 0.6142(3) -0.0453(2) 0.0242(11) Uani 0.5 1 d D U . B -2
C2B C 0.4754(8) 0.6108(3) -0.0506(2) 0.0195(10) Uani 0.5 1 d D U . C -1
C3A C 0.4614(11) 0.6636(3) -0.0441(2) 0.0331(17) Uani 0.5 1 d D U . B -2
H3A H 0.4244 0.6805 -0.0633 0.040 Uiso 0.5 1 calc R . . B -2
C3B C 0.4754(10) 0.6595(2) -0.0535(2) 0.0284(15) Uani 0.5 1 d D U . C -1
H3B H 0.4405 0.6742 -0.0744 0.034 Uiso 0.5 1 calc R . . C -1
C4A C 0.5145(11) 0.6869(3) -0.0133(2) 0.0472(12) Uani 0.5 1 d D U . B -2
C4B C 0.5278(7) 0.6861(2) -0.02512(19) 0.0282(10) Uani 0.5 1 d D U . C -1
C5A C 0.5738(13) 0.6625(3) 0.0140(3) 0.039(2) Uani 0.5 1 d . U . B -2
H5A H 0.6117 0.6785 0.0336 0.046 Uiso 0.5 1 calc R . . B -2
C5B C 0.5855(11) 0.6640(3) 0.0056(2) 0.0265(14) Uani 0.5 1 d . U . C -1
H5B H 0.6211 0.6822 0.0244 0.032 Uiso 0.5 1 calc R . . C -1
C6A C 0.5770(9) 0.6134(4) 0.0121(3) 0.0239(11) Uani 0.5 1 d . U . B -2
C6B C 0.5892(9) 0.6152(4) 0.0078(3) 0.0196(10) Uani 0.5 1 d . U . C -1
C7 C 0.5268(3) 0.58917(10) -0.01841(8) 0.0240(6) Uani 1 1 d D . . . .
H7B H 0.5187 0.5569 -0.0148 0.029 Uiso 0.5 1 calc R . . B -1
H7A H 0.5348 0.5567 -0.0206 0.029 Uiso 0.5 1 calc R . . B -2
C8 C 0.6465(3) 0.58954(10) 0.04234(8) 0.0238(6) Uani 1 1 d . . . . .
C9 C 0.7788(3) 0.41346(11) 0.21097(9) 0.0295(7) Uani 1 1 d . . . . .
C10 C 0.8181(3) 0.38504(10) 0.24470(9) 0.0267(6) Uani 1 1 d . . . . .
C11 C 0.8671(3) 0.40578(10) 0.27700(9) 0.0264(6) Uani 1 1 d . . . . .
H11 H 0.8676 0.4384 0.2794 0.032 Uiso 1 1 calc R . . . .
C12 C 0.9153(3) 0.37804(11) 0.30564(8) 0.0251(6) Uani 1 1 d . . . . .
C13 C 0.9130(3) 0.32919(11) 0.30208(9) 0.0286(6) Uani 1 1 d . . . . .
H13 H 0.9451 0.3103 0.3211 0.034 Uiso 1 1 calc R . . . .
C14 C 0.8625(3) 0.30894(10) 0.26985(9) 0.0280(6) Uani 1 1 d . . . . .
C15 C 0.8146(3) 0.33649(11) 0.24116(8) 0.0292(7) Uani 1 1 d . . . . .
H15 H 0.7806 0.3226 0.2198 0.035 Uiso 1 1 calc R . . . .
C16 C 0.9784(3) 0.40102(11) 0.33833(9) 0.0300(7) Uani 1 1 d . . . . .
C17 C 0.8501(3) 0.29259(11) 0.10960(11) 0.0332(7) Uani 1 1 d . . . . .
H17 H 0.9158 0.3085 0.1028 0.040 Uiso 1 1 calc R . . . .
C18 C 0.8434(3) 0.24496(11) 0.10194(11) 0.0354(7) Uani 1 1 d . . . . .
H18 H 0.9031 0.2296 0.0899 0.043 Uiso 1 1 calc R . . . .
C19 C 0.7475(3) 0.22025(11) 0.11228(10) 0.0298(7) Uani 1 1 d . . . . .
C20 C 0.6629(3) 0.24516(12) 0.13099(12) 0.0398(8) Uani 1 1 d . . . . .
H20 H 0.5980 0.2298 0.1394 0.048 Uiso 1 1 calc R . . . .
C21 C 0.6757(3) 0.29295(11) 0.13711(11) 0.0346(7) Uani 1 1 d . . . . .
H21 H 0.6177 0.3092 0.1494 0.042 Uiso 1 1 calc R . . . .
C22 C 0.7375(3) 0.16923(11) 0.10361(10) 0.0297(7) Uani 1 1 d . . . . .
C23 C 0.6743(3) 0.13952(12) 0.12653(10) 0.0345(7) Uani 1 1 d . . . . .
H23 H 0.6340 0.1513 0.1475 0.041 Uiso 1 1 calc R . . . .
C24 C 0.6713(3) 0.09197(12) 0.11805(11) 0.0335(7) Uani 1 1 d . . . . .
H24 H 0.6277 0.0724 0.1336 0.040 Uiso 1 1 calc R . . . .
C25 C 0.7872(3) 0.10154(11) 0.06575(10) 0.0334(7) Uani 1 1 d . . . . .
H25 H 0.8257 0.0889 0.0447 0.040 Uiso 1 1 calc R . . . .
C26 C 0.7933(3) 0.14940(12) 0.07216(11) 0.0366(8) Uani 1 1 d . . . . .
H26 H 0.8348 0.1684 0.0555 0.044 Uiso 1 1 calc R . . . .
H6 H 0.876(4) 0.4606(17) 0.1272(14) 0.055 Uiso 1 1 d R . . . .
O5WA O 0.460(4) 0.4815(16) 0.2409(11) 0.15(2) Uani 0.2 1 d . U . D -2
H5WA H 0.4581 0.4576 0.2261 0.232 Uiso 0.2 1 d R . . D -2
H5WB H 0.5271 0.4857 0.2489 0.232 Uiso 0.2 1 d R . . D -2
O5WB O 0.3851(9) 0.4690(3) 0.2227(3) 0.143(4) Uani 0.8 1 d . . . E -1
H5WC H 0.3888 0.4395 0.2187 0.214 Uiso 0.8 1 d R . . E -1
H5WD H 0.3350 0.4747 0.2397 0.214 Uiso 0.8 1 d R . . E -1
O6W O 0.5002(5) 0.3644(3) 0.20806(18) 0.145(3) Uani 0.8 1 d . . . F 1
H6WA H 0.5234 0.3800 0.2275 0.218 Uiso 0.8 1 d R . . F 1
H6WB H 0.5396 0.3611 0.1982 0.218 Uiso 0.8 1 d R . . F 1
O7W O 0.445(2) 0.2637(14) 0.2149(7) 0.142(14) Uani 0.2 1 d . . . G -1
H7WA H 0.4570 0.2923 0.2212 0.212 Uiso 0.2 1 d R . . G -1
H7WB H 0.5024 0.2472 0.2213 0.212 Uiso 0.2 1 d R . . G -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.092(2) 9_665 ?
Ni1 O2 2.092(2) 14 ?
Ni1 O3 2.167(2) . ?
Ni1 O3 2.167(2) 6_655 ?
Ni1 O6 2.040(2) . ?
Ni1 O6 2.040(2) 6_655 ?
Ni2 O1W 2.136(3) . ?
Ni2 O1W 2.136(3) 6_655 ?
Ni2 O6 2.029(2) . ?
Ni2 O6 2.029(2) 6_655 ?
Ni2 O7 2.024(2) 6_655 ?
Ni2 O7 2.024(2) . ?
Ni3 O1 2.079(2) 9_665 ?
Ni3 O4 2.036(2) 6_655 ?
Ni3 O6 1.998(2) . ?
Ni3 O8 2.093(2) . ?
Ni3 O9 2.075(2) 4_755 ?
Ni3 N1 2.085(3) . ?
Ni4 O2W 2.064(3) . ?
Ni4 O3W 2.051(2) 6_645 ?
Ni4 O3W 2.051(2) . ?
Ni4 O4W 2.113(4) . ?
Ni4 N2 2.085(3) . ?
Ni4 N2 2.085(3) 6_645 ?
O1 Ni3 2.079(2) 9_665 ?
O1 C1 1.254(4) . ?
O1W H1WA 0.8729 . ?
O1W H1WB 0.9039 . ?
O2 Ni1 2.092(2) 9_665 ?
O2 C1 1.262(4) . ?
O2W H2W 0.8457 . ?
O3 C8 1.260(4) . ?
O3W H3WA 0.8190 . ?
O3W H3WB 0.9457 . ?
O4 Ni3 2.036(2) 6_655 ?
O4 C8 1.245(4) . ?
O4W H4W 0.8102 . ?
O5 N0 1.365(8) 2_665 ?
O6 H6 0.81(5) . ?
O7 C9 1.256(4) . ?
O8 C9 1.260(4) . ?
O9 Ni3 2.075(2) 4_755 ?
O9 C16 1.249(4) . ?
O10 C16 1.261(4) . ?
O11 N3 1.300(6) . ?
N0 C4A 1.479(8) . ?
N0A N0 1.191(7) 2_665 ?
N0A C4B 1.452(7) . ?
N1 C17 1.332(4) . ?
N1 C21 1.334(4) . ?
N2 C24 1.338(4) . ?
N2 C25 1.333(4) . ?
N3 N3 1.281(5) 3 ?
N3 C14 1.434(4) . ?
C1 C2A 1.571(9) . ?
C1 C2B 1.450(9) . ?
C2A C3A 1.403(9) . ?
C2A C7 1.381(8) . ?
C2B C3B 1.386(8) . ?
C2B C7 1.408(8) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.400(11) . ?
C3B H3B 0.9300 . ?
C3B C4B 1.387(10) . ?
C4A C5A 1.365(12) . ?
C4B C5B 1.408(10) . ?
C5A H5A 0.9300 . ?
C5A C6A 1.398(15) . ?
C5B H5B 0.9300 . ?
C5B C6B 1.389(13) . ?
C6A C7 1.393(12) . ?
C6A C8 1.491(12) . ?
C6B C7 1.384(12) . ?
C6B C8 1.553(11) . ?
C7 H7B 0.9300 . ?
C7 H7A 0.9300 . ?
C9 C10 1.492(4) . ?
C10 C11 1.389(4) . ?
C10 C15 1.384(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.387(4) . ?
C12 C13 1.393(4) . ?
C12 C16 1.503(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.388(4) . ?
C14 C15 1.384(4) . ?
C15 H15 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.380(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.381(5) . ?
C19 C20 1.386(5) . ?
C19 C22 1.484(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.381(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.378(5) . ?
C22 C26 1.391(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.382(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.379(5) . ?
C26 H26 0.9300 . ?
O5WA H5WA 0.8493 . ?
O5WA H5WB 0.8504 . ?
O5WB H5WC 0.8499 . ?
O5WB H5WD 0.8507 . ?
O6W H6WA 0.8487 . ?
O6W H6WB 0.5848 . ?
O7W H7WA 0.8500 . ?
O7W H7WB 0.8502 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O2 165.65(13) 9_665 14 ?
O2 Ni1 O3 86.29(9) 9_665 6_655 ?
O2 Ni1 O3 84.26(8) 14 6_655 ?
O2 Ni1 O3 84.26(8) 9_665 . ?
O2 Ni1 O3 86.29(9) 14 . ?
O3 Ni1 O3 97.50(11) . 6_655 ?
O6 Ni1 O2 97.85(9) 6_655 9_665 ?
O6 Ni1 O2 97.85(9) . 14 ?
O6 Ni1 O2 93.00(9) 6_655 14 ?
O6 Ni1 O2 93.00(9) . 9_665 ?
O6 Ni1 O3 90.50(8) 6_655 . ?
O6 Ni1 O3 171.34(9) . . ?
O6 Ni1 O3 90.50(8) . 6_655 ?
O6 Ni1 O3 171.35(9) 6_655 6_655 ?
O6 Ni1 O6 81.73(12) . 6_655 ?
O1W Ni2 O1W 178.77(15) . 6_655 ?
O6 Ni2 O1W 95.09(10) . 6_655 ?
O6 Ni2 O1W 95.09(10) 6_655 . ?
O6 Ni2 O1W 85.84(10) 6_655 6_655 ?
O6 Ni2 O1W 85.83(10) . . ?
O6 Ni2 O6 82.25(12) 6_655 . ?
O7 Ni2 O1W 91.55(11) 6_655 . ?
O7 Ni2 O1W 91.55(11) . 6_655 ?
O7 Ni2 O1W 87.55(11) . . ?
O7 Ni2 O1W 87.55(11) 6_655 6_655 ?
O7 Ni2 O6 176.65(9) . 6_655 ?
O7 Ni2 O6 176.65(9) 6_655 . ?
O7 Ni2 O6 95.92(9) 6_655 6_655 ?
O7 Ni2 O6 95.92(9) . . ?
O7 Ni2 O7 86.05(15) . 6_655 ?
O1 Ni3 O8 87.93(10) 9_665 . ?
O1 Ni3 N1 88.10(10) 9_665 . ?
O4 Ni3 O1 88.84(11) 6_655 9_665 ?
O4 Ni3 O8 175.63(10) 6_655 . ?
O4 Ni3 O9 92.53(12) 6_655 4_755 ?
O4 Ni3 N1 86.41(9) 6_655 . ?
O6 Ni3 O1 93.69(9) . 9_665 ?
O6 Ni3 O4 89.76(9) . 6_655 ?
O6 Ni3 O8 93.38(9) . . ?
O6 Ni3 O9 93.48(10) . 4_755 ?
O6 Ni3 N1 175.74(10) . . ?
O9 Ni3 O1 172.71(10) 4_755 9_665 ?
O9 Ni3 O8 90.32(11) 4_755 . ?
O9 Ni3 N1 84.84(10) 4_755 . ?
N1 Ni3 O8 90.54(9) . . ?
O2W Ni4 O4W 180.0 . . ?
O2W Ni4 N2 93.23(8) . 6_645 ?
O2W Ni4 N2 93.23(8) . . ?
O3W Ni4 O2W 90.01(8) . . ?
O3W Ni4 O2W 90.01(8) 6_645 . ?
O3W Ni4 O3W 179.97(16) . 6_645 ?
O3W Ni4 O4W 89.99(8) 6_645 . ?
O3W Ni4 O4W 89.99(8) . . ?
O3W Ni4 N2 94.68(10) . 6_645 ?
O3W Ni4 N2 94.68(10) 6_645 . ?
O3W Ni4 N2 85.32(10) 6_645 6_645 ?
O3W Ni4 N2 85.32(10) . . ?
N2 Ni4 O4W 86.77(8) . . ?
N2 Ni4 O4W 86.77(8) 6_645 . ?
N2 Ni4 N2 173.55(16) . 6_645 ?
C1 O1 Ni3 120.5(2) . 9_665 ?
Ni2 O1W H1WA 116.6 . . ?
Ni2 O1W H1WB 103.6 . . ?
H1WA O1W H1WB 124.6 . . ?
C1 O2 Ni1 130.33(19) . 9_665 ?
Ni4 O2W H2W 124.8 . . ?
C8 O3 Ni1 127.67(19) . . ?
Ni4 O3W H3WA 136.5 . . ?
Ni4 O3W H3WB 122.4 . . ?
H3WA O3W H3WB 97.9 . . ?
C8 O4 Ni3 139.3(2) . 6_655 ?
Ni4 O4W H4W 121.0 . . ?
Ni1 O6 H6 114(3) . . ?
Ni2 O6 Ni1 98.01(9) . . ?
Ni2 O6 H6 103(3) . . ?
Ni3 O6 Ni1 122.76(10) . . ?
Ni3 O6 Ni2 118.46(10) . . ?
Ni3 O6 H6 100(4) . . ?
C9 O7 Ni2 121.1(2) . . ?
C9 O8 Ni3 123.5(2) . . ?
C16 O9 Ni3 134.3(2) . 4_755 ?
C17 N1 Ni3 116.9(2) . . ?
C17 N1 C21 117.0(3) . . ?
C21 N1 Ni3 125.6(2) . . ?
C24 N2 Ni4 120.6(2) . . ?
C25 N2 Ni4 120.6(2) . . ?
C25 N2 C24 117.6(3) . . ?
O11 N3 C14 113.4(3) . . ?
N3 N3 O11 130.5(4) 3 . ?
N3 N3 C14 116.0(3) 3 . ?
O1 C1 O2 125.5(3) . . ?
O1 C1 C2A 118.2(4) . . ?
O1 C1 C2B 117.3(4) . . ?
O2 C1 C2A 116.3(4) . . ?
O2 C1 C2B 116.9(4) . . ?
C3A C2A C1 123.1(6) . . ?
C7 C2A C1 116.1(6) . . ?
C7 C2A C3A 120.6(7) . . ?
C3B C2B C1 117.5(6) . . ?
C3B C2B C7 119.6(7) . . ?
C7 C2B C1 122.5(6) . . ?
C2A C3A H3A 120.6 . . ?
C4A C3A C2A 118.9(7) . . ?
C4A C3A H3A 120.6 . . ?
C2B C3B H3B 120.3 . . ?
C2B C3B C4B 119.5(7) . . ?
C4B C3B H3B 120.3 . . ?
C3A C4A N0 121.9(7) . . ?
C5A C4A N0 116.9(7) . . ?
C5A C4A C3A 121.1(7) . . ?
C3B C4B N0A 115.6(6) . . ?
C3B C4B C5B 120.5(6) . . ?
C5B C4B N0A 123.3(7) . . ?
C4A C5A H5A 120.4 . . ?
C4A C5A C6A 119.2(9) . . ?
C6A C5A H5A 120.4 . . ?
C4B C5B H5B 119.9 . . ?
C6B C5B C4B 120.2(8) . . ?
C6B C5B H5B 119.9 . . ?
C5A C6A C8 115.8(9) . . ?
C7 C6A C5A 121.1(9) . . ?
C7 C6A C8 122.8(8) . . ?
C5B C6B C8 121.7(8) . . ?
C7 C6B C5B 118.6(8) . . ?
C7 C6B C8 119.0(7) . . ?
C2A C7 C6A 118.9(6) . . ?
C2A C7 H7A 120.6 . . ?
C2B C7 H7B 119.5 . . ?
C6A C7 H7A 120.6 . . ?
C6B C7 C2B 121.0(6) . . ?
C6B C7 H7B 119.5 . . ?
O3 C8 C6A 118.7(5) . . ?
O3 C8 C6B 117.6(5) . . ?
O4 C8 O3 127.6(3) . . ?
O4 C8 C6A 113.7(5) . . ?
O4 C8 C6B 114.7(5) . . ?
O7 C9 O8 125.6(3) . . ?
O7 C9 C10 116.7(3) . . ?
O8 C9 C10 117.7(3) . . ?
C11 C10 C9 121.9(3) . . ?
C15 C10 C9 117.4(3) . . ?
C15 C10 C11 120.4(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 C16 119.6(3) . . ?
C13 C12 C16 120.5(3) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.4(3) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 N3 117.4(3) . . ?
C15 C14 N3 121.5(3) . . ?
C15 C14 C13 121.1(3) . . ?
C10 C15 H15 120.4 . . ?
C14 C15 C10 119.2(3) . . ?
C14 C15 H15 120.4 . . ?
O9 C16 O10 125.3(3) . . ?
O9 C16 C12 116.4(3) . . ?
O10 C16 C12 118.3(3) . . ?
N1 C17 H17 118.3 . . ?
N1 C17 C18 123.3(3) . . ?
C18 C17 H17 118.3 . . ?
C17 C18 H18 120.2 . . ?
C17 C18 C19 119.7(3) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C20 117.1(3) . . ?
C18 C19 C22 120.6(3) . . ?
C20 C19 C22 122.3(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H20 120.2 . . ?
N1 C21 C20 123.2(3) . . ?
N1 C21 H21 118.4 . . ?
C20 C21 H21 118.4 . . ?
C23 C22 C19 121.7(3) . . ?
C23 C22 C26 117.3(3) . . ?
C26 C22 C19 121.0(3) . . ?
C22 C23 H23 120.3 . . ?
C22 C23 C24 119.3(3) . . ?
C24 C23 H23 120.3 . . ?
N2 C24 C23 123.2(3) . . ?
N2 C24 H24 118.4 . . ?
C23 C24 H24 118.4 . . ?
N2 C25 H25 118.8 . . ?
N2 C25 C26 122.5(3) . . ?
C26 C25 H25 118.8 . . ?
C22 C26 H26 120.0 . . ?
C25 C26 C22 120.0(3) . . ?
C25 C26 H26 120.0 . . ?
H5WA O5WA H5WB 109.5 . . ?
H5WC O5WB H5WD 109.5 . . ?
H6WA O6W H6WB 106.6 . . ?
H7WA O7W H7WB 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
Ni1 O2 C1 O1 -47.7(5) 9_665 . . . ?
Ni1 O2 C1 C2A 130.3(4) 9_665 . . . ?
Ni1 O2 C1 C2B 139.0(4) 9_665 . . . ?
Ni1 O3 C8 O4 4.5(5) . . . . ?
Ni1 O3 C8 C6A -172.0(5) . . . . ?
Ni1 O3 C8 C6B 179.3(4) . . . . ?
Ni2 O7 C9 O8 3.8(5) . . . . ?
Ni2 O7 C9 C10 -177.8(2) . . . . ?
Ni3 O1 C1 O2 62.0(4) 9_665 . . . ?
Ni3 O1 C1 C2A -115.9(5) 9_665 . . . ?
Ni3 O1 C1 C2B -124.7(4) 9_665 . . . ?
Ni3 O4 C8 O3 -20.1(6) 6_655 . . . ?
Ni3 O4 C8 C6A 156.6(5) 6_655 . . . ?
Ni3 O4 C8 C6B 165.0(4) 6_655 . . . ?
Ni3 O8 C9 O7 58.5(5) . . . . ?
Ni3 O8 C9 C10 -119.8(3) . . . . ?
Ni3 O9 C16 O10 -41.2(6) 4_755 . . . ?
Ni3 O9 C16 C12 136.9(3) 4_755 . . . ?
Ni3 N1 C17 C18 -170.2(3) . . . . ?
Ni3 N1 C21 C20 170.4(3) . . . . ?
Ni4 N2 C24 C23 165.7(3) . . . . ?
Ni4 N2 C25 C26 -166.3(3) . . . . ?
O1 C1 C2A C3A 15.5(11) . . . . ?
O1 C1 C2A C7 -158.6(5) . . . . ?
O1 C1 C2B C3B 18.6(9) . . . . ?
O1 C1 C2B C7 -168.5(5) . . . . ?
O2 C1 C2A C3A -162.6(8) . . . . ?
O2 C1 C2A C7 23.3(9) . . . . ?
O2 C1 C2B C3B -167.6(7) . . . . ?
O2 C1 C2B C7 5.3(9) . . . . ?
O7 C9 C10 C11 7.0(5) . . . . ?
O7 C9 C10 C15 -166.5(3) . . . . ?
O8 C9 C10 C11 -174.4(3) . . . . ?
O8 C9 C10 C15 12.0(5) . . . . ?
O11 N3 C14 C13 24.9(6) . . . . ?
O11 N3 C14 C15 -156.3(5) . . . . ?
N0 C4A C5A C6A 173.6(12) . . . . ?
N0A C4B C5B C6B -171.8(9) . . . . ?
N1 C17 C18 C19 -1.1(6) . . . . ?
N2 C25 C26 C22 0.6(6) . . . . ?
N3 N3 C14 C13 -150.9(2) 3 . . . ?
N3 N3 C14 C15 27.9(4) 3 . . . ?
N3 C14 C15 C10 -178.3(3) . . . . ?
C1 C2A C3A C4A -178.6(9) . . . . ?
C1 C2A C7 C6A -179.9(6) . . . . ?
C1 C2B C3B C4B 174.3(8) . . . . ?
C1 C2B C7 C6B 179.2(6) . . . . ?
C2A C3A C4A N0 -173.1(11) . . . . ?
C2A C3A C4A C5A 3.3(18) . . . . ?
C2B C3B C4B N0A 174.8(8) . . . . ?
C2B C3B C4B C5B 3.1(14) . . . . ?
C3A C2A C7 C6A 5.9(12) . . . . ?
C3A C4A C5A C6A -3.0(19) . . . . ?
C3B C2B C7 C6B -8.0(12) . . . . ?
C3B C4B C5B C6B -0.7(15) . . . . ?
C4A C5A C6A C7 4.1(18) . . . . ?
C4A C5A C6A C8 178.2(10) . . . . ?
C4B C5B C6B C7 -5.9(15) . . . . ?
C4B C5B C6B C8 -176.8(8) . . . . ?
C5A C6A C7 C2A -5.6(14) . . . . ?
C5A C6A C8 O3 -167.4(8) . . . . ?
C5A C6A C8 O4 15.5(11) . . . . ?
C5B C6B C7 C2B 10.2(12) . . . . ?
C5B C6B C8 O3 -164.2(8) . . . . ?
C5B C6B C8 O4 11.3(11) . . . . ?
C7 C2A C3A C4A -4.8(16) . . . . ?
C7 C2B C3B C4B 1.2(14) . . . . ?
C7 C6A C8 O3 6.5(10) . . . . ?
C7 C6A C8 O4 -170.5(6) . . . . ?
C7 C6B C8 O3 25.0(9) . . . . ?
C7 C6B C8 O4 -159.6(6) . . . . ?
C8 C6A C7 C2A -179.2(7) . . . . ?
C8 C6B C7 C2B -178.6(6) . . . . ?
C9 C10 C11 C12 -172.0(3) . . . . ?
C9 C10 C15 C14 172.5(3) . . . . ?
C10 C11 C12 C13 -0.8(5) . . . . ?
C10 C11 C12 C16 173.7(3) . . . . ?
C11 C10 C15 C14 -1.2(5) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C11 C12 C16 O9 -153.8(3) . . . . ?
C11 C12 C16 O10 24.4(5) . . . . ?
C12 C13 C14 N3 179.0(3) . . . . ?
C12 C13 C14 C15 0.2(5) . . . . ?
C13 C12 C16 O9 20.7(5) . . . . ?
C13 C12 C16 O10 -161.1(3) . . . . ?
C13 C14 C15 C10 0.4(5) . . . . ?
C15 C10 C11 C12 1.4(5) . . . . ?
C16 C12 C13 C14 -174.4(3) . . . . ?
C17 N1 C21 C20 -1.8(5) . . . . ?
C17 C18 C19 C20 -1.5(5) . . . . ?
C17 C18 C19 C22 178.7(3) . . . . ?
C18 C19 C20 C21 2.4(6) . . . . ?
C18 C19 C22 C23 150.6(4) . . . . ?
C18 C19 C22 C26 -28.4(5) . . . . ?
C19 C20 C21 N1 -0.7(6) . . . . ?
C19 C22 C23 C24 -177.5(3) . . . . ?
C19 C22 C26 C25 176.9(3) . . . . ?
C20 C19 C22 C23 -29.1(5) . . . . ?
C20 C19 C22 C26 151.9(4) . . . . ?
C21 N1 C17 C18 2.8(5) . . . . ?
C22 C19 C20 C21 -177.9(3) . . . . ?
C22 C23 C24 N2 0.7(6) . . . . ?
C23 C22 C26 C25 -2.2(5) . . . . ?
C24 N2 C25 C26 1.6(5) . . . . ?
C25 N2 C24 C23 -2.2(5) . . . . ?
C26 C22 C23 C24 1.6(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1478777'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_audit_creation_date             2016-07-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H12 N4 O18 Zn3, C10 H10 N2, H2 O'
_chemical_formula_sum            'C42 H24 N6 O19 Zn3'
_chemical_formula_weight         1112.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 O1 Zn1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0180 0.0090 '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 0.0310 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0490 0.0320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5490 0.6780 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.6379(4)
_cell_length_b                   10.2081(3)
_cell_length_c                   12.1115(5)
_cell_angle_alpha                112.980(3)
_cell_angle_beta                 99.703(3)
_cell_angle_gamma                95.828(3)
_cell_volume                     1062.78(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    12953
_cell_measurement_temperature    290.88(19)
_cell_measurement_theta_max      71.3620
_cell_measurement_theta_min      4.7800
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19866
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.550
_diffrn_reflns_theta_min         4.736
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.88(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -120.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega  -35.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -19.0000   90.0000 101

#__ type_ start__ end____ width___ exp.time_
  6 omega    1.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000   60.0000 75

#__ type_ start__ end____ width___ exp.time_
  7 omega   21.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203 -122.0000    9.0000 67

#__ type_ start__ end____ width___ exp.time_
  8 omega   57.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000   60.0000 52

#__ type_ start__ end____ width___ exp.time_
  9 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
 10 omega   38.00   91.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

#__ type_ start__ end____ width___ exp.time_
 11 omega   39.00  110.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   90.0000 71

#__ type_ start__ end____ width___ exp.time_
 12 omega   39.00  110.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   30.0000 71

#__ type_ start__ end____ width___ exp.time_
 13 omega   38.00   91.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
 14 omega   40.00   98.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
 15 omega   39.00  110.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -60.0000 71

#__ type_ start__ end____ width___ exp.time_
 16 omega   37.00  146.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000  120.0000 109

#__ type_ start__ end____ width___ exp.time_
 17 omega   38.00   91.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
 18 omega   40.00   98.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
 19 omega   38.00  116.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000 -120.0000 78

#__ type_ start__ end____ width___ exp.time_
 20 omega   38.00   91.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

#__ type_ start__ end____ width___ exp.time_
 21 omega   37.00  146.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -150.0000 109

#__ type_ start__ end____ width___ exp.time_
 22 omega   40.00   98.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

#__ type_ start__ end____ width___ exp.time_
 23 omega   40.00  135.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 24 omega   38.00   91.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
 25 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
 26 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  -30.0000 94

#__ type_ start__ end____ width___ exp.time_
 27 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
 28 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
 29 omega   55.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203 -178.0000  -90.0000 54

#__ type_ start__ end____ width___ exp.time_
 30 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000 -150.0000 84

#__ type_ start__ end____ width___ exp.time_
 31 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000 -150.0000 84

#__ type_ start__ end____ width___ exp.time_
 32 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
 33 omega   91.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 85

#__ type_ start__ end____ width___ exp.time_
 34 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
 35 omega   70.00  178.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   90.0000 108

#__ type_ start__ end____ width___ exp.time_
 36 omega   70.00  178.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -180.0000 108

#__ type_ start__ end____ width___ exp.time_
 37 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
 38 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 39 omega   70.00  178.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000    0.0000 108

#__ type_ start__ end____ width___ exp.time_
 40 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
 41 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 95

#__ type_ start__ end____ width___ exp.time_
 42 omega   70.00  178.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108

#__ type_ start__ end____ width___ exp.time_
 43 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 44 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
 45 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 46 omega   81.00  123.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 42

#__ type_ start__ end____ width___ exp.time_
 47 omega   81.00  176.00   1.0000    1.4900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0235893000
_diffrn_orient_matrix_UB_12      -0.0654746000
_diffrn_orient_matrix_UB_13      0.0919216000
_diffrn_orient_matrix_UB_21      0.0523575000
_diffrn_orient_matrix_UB_22      0.1507786000
_diffrn_orient_matrix_UB_23      0.1073954000
_diffrn_orient_matrix_UB_31      -0.1546772000
_diffrn_orient_matrix_UB_32      0.0282162000
_diffrn_orient_matrix_UB_33      -0.0120650000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3883
_reflns_number_total             4106
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.667
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4106
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0856P)²+2.0570P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1445
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 C23, C22, C26, C25, N4, C24, N3, C17, C18, C19, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(O9)=1-FVAR(1)
 Sof(O10)=FVAR(1)
 Fixed Sof: C23(0.5) H23(0.5) C22(0.5) C26(0.5) H26(0.5) C25(0.5) H25(0.5)
 N4(0.5) H4(0.5) C24(0.5) H24(0.5) N3(0.5) H3a(0.5) C17(0.5) H17(0.5) C18(0.5)
 H18(0.5) C19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) O1W(0.5) H1Wa(0.5)
 H1Wb(0.5)
4.a Riding coordinates:
 O1W(H1Wa,H1Wb)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14), C23(H23), C26(H26),
 C25(H25), N4(H4), C24(H24), N3(H3a), C17(H17), C18(H18), C20(H20), C21(H21)
4.c Fitted hexagon refined as free rotating group:
 C23(C22,C26,C25,N4,C24), N3(C17,C18,C19,C20,C21)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7704(3) 0.6809(3) 1.0790(3) 0.0221(6) Uani 1 1 d . . . . .
C2 C 0.6132(3) 0.6718(3) 1.0321(3) 0.0210(6) Uani 1 1 d . . . . .
C3 C 0.5588(3) 0.6064(4) 0.9055(3) 0.0233(6) Uani 1 1 d . . . . .
H3 H 0.6190 0.5707 0.8527 0.028 Uiso 1 1 calc R . . . .
C4 C 0.4158(3) 0.5947(3) 0.8586(3) 0.0223(6) Uani 1 1 d . . . . .
C5 C 0.3219(3) 0.6443(3) 0.9356(3) 0.0203(6) Uani 1 1 d . . . . .
H5 H 0.2254 0.6366 0.9029 0.024 Uiso 1 1 calc R . . . .
C6 C 0.3763(3) 0.7054(3) 1.0621(3) 0.0201(6) Uani 1 1 d . . . . .
C7 C 0.5216(3) 0.7198(3) 1.1101(3) 0.0217(6) Uani 1 1 d . . . . .
H7 H 0.5573 0.7619 1.1949 0.026 Uiso 1 1 calc R . . . .
C8 C 0.2785(3) 0.7551(3) 1.1485(3) 0.0244(7) Uani 1 1 d . . . . .
C9 C 0.2018(4) 0.4697(4) 0.5488(3) 0.0245(7) Uani 1 1 d . . . . .
C10 C 0.1649(4) 0.5467(3) 0.4798(3) 0.0245(7) Uani 1 1 d . . . . .
H10 H 0.1799 0.6473 0.5171 0.029 Uiso 1 1 calc R . . . .
C11 C 0.1052(3) 0.4729(3) 0.3543(3) 0.0219(6) Uani 1 1 d . . . . .
C12 C 0.0813(4) 0.3220(3) 0.2990(3) 0.0252(7) Uani 1 1 d . . . . .
H12 H 0.0437 0.2724 0.2147 0.030 Uiso 1 1 calc R . . . .
C13 C 0.1139(4) 0.2457(3) 0.3705(3) 0.0255(7) Uani 1 1 d . . . . .
C14 C 0.1745(4) 0.3192(4) 0.4964(3) 0.0267(7) Uani 1 1 d . . . . .
H14 H 0.1963 0.2685 0.5443 0.032 Uiso 1 1 calc R . . . .
C15 C 0.0624(3) 0.5569(3) 0.2793(3) 0.0214(6) Uani 1 1 d . . . . .
C16 C 0.0837(4) 0.0827(4) 0.3116(3) 0.0305(7) Uani 1 1 d . . . . .
N1 N 0.2576(3) 0.5523(3) 0.6788(3) 0.0314(7) Uani 1 1 d . . . . .
N2 N 0.3631(3) 0.5163(3) 0.7266(3) 0.0303(6) Uani 1 1 d . . . . .
O1 O 0.8279(3) 0.7672(3) 1.1890(2) 0.0325(6) Uani 1 1 d . . . . .
O2 O 0.8323(2) 0.6024(3) 1.0041(2) 0.0286(5) Uani 1 1 d . . . . .
O3 O 0.3300(3) 0.8347(4) 1.2578(3) 0.0479(8) Uani 1 1 d . . . . .
O4 O 0.1425(2) 0.7150(2) 1.1037(2) 0.0228(5) Uani 1 1 d . . . . .
O5 O 0.0846(3) 0.6926(3) 0.3360(2) 0.0296(5) Uani 1 1 d . . . . .
O6 O 0.0063(3) 0.4860(2) 0.1675(2) 0.0251(5) Uani 1 1 d . . . . .
O7 O 0.0469(4) 0.0176(3) 0.1976(3) 0.0528(9) Uani 1 1 d . . . . .
O8 O 0.0943(3) 0.0145(3) 0.3783(2) 0.0364(6) Uani 1 1 d . . . . .
O9 O 0.2364(9) 0.6840(8) 0.7245(6) 0.036(2) Uani 0.353(9) 1 d . . . . .
O10 O 0.4425(6) 0.4391(8) 0.6671(5) 0.081(3) Uani 0.647(9) 1 d . . . . .
Zn1 Zn 1.04224(4) 0.81060(4) 1.24116(4) 0.02078(16) Uani 1 1 d . . . . .
Zn2 Zn 1.0000 0.5000 1.0000 0.01850(17) Uani 1 2 d S T P . .
C23 C 0.4569(9) 0.0218(11) 0.0502(8) 0.086(3) Uani 0.5 1 d . U . A -1
H23 H 0.3783 0.0390 0.0854 0.103 Uiso 0.5 1 calc R . . A -1
C22 C 0.5925(10) 0.0484(9) 0.1245(5) 0.071(3) Uani 0.5 1 d G U . A -1
C26 C 0.7100(8) 0.0227(8) 0.0718(8) 0.071(3) Uani 0.5 1 d G U . A -1
H26 H 0.8007 0.0405 0.1215 0.086 Uiso 0.5 1 calc R . . A -1
C25 C 0.6919(11) -0.0296(8) -0.0552(8) 0.094(4) Uani 0.5 1 d G U . A -1
H25 H 0.7705 -0.0468 -0.0905 0.112 Uiso 0.5 1 calc R . . A -1
N4 N 0.5563(13) -0.0563(7) -0.1296(5) 0.096(3) Uani 0.5 1 d G U . A -1
H4 H 0.5451 -0.0887 -0.2082 0.115 Uiso 0.5 1 calc R . . A -1
C24 C 0.4388(9) -0.0306(10) -0.0769(7) 0.092(4) Uani 0.5 1 d G U . A -1
H24 H 0.3481 -0.0484 -0.1266 0.110 Uiso 0.5 1 calc R . . A -1
N3 N 0.6200(7) 0.1408(7) 0.5033(4) 0.064(2) Uani 0.5 1 d . U . A -1
H3A H 0.6307 0.1561 0.5796 0.077 Uiso 0.5 1 calc R . . A -1
C17 C 0.5136(7) 0.1936(7) 0.4493(6) 0.069(3) Uani 0.5 1 d G U . A -1
H17 H 0.4539 0.2455 0.4956 0.083 Uiso 0.5 1 calc R . . A -1
C18 C 0.4964(7) 0.1688(7) 0.3261(6) 0.067(3) Uani 0.5 1 d G U . A -1
H18 H 0.4251 0.2042 0.2900 0.080 Uiso 0.5 1 calc R . . A -1
C19 C 0.5856(8) 0.0913(6) 0.2569(4) 0.055(2) Uani 0.5 1 d G U . A -1
C20 C 0.6921(7) 0.0385(6) 0.3109(5) 0.052(2) Uani 0.5 1 d G U . A -1
H20 H 0.7518 -0.0133 0.2646 0.062 Uiso 0.5 1 calc R . . A -1
C21 C 0.7093(6) 0.0633(7) 0.4341(5) 0.058(2) Uani 0.5 1 d G U . A -1
H21 H 0.7805 0.0280 0.4703 0.069 Uiso 0.5 1 calc R . . A -1
O1W O 0.8408(15) -0.039(3) -0.0097(14) 0.182(9) Uani 0.5 1 d . . . A 1
H1WA H 0.8854 -0.0229 0.0550 0.272 Uiso 0.5 1 d R . . A 1
H1WB H 0.8686 -0.0450 -0.0675 0.272 Uiso 0.5 1 d R . . A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.506(4) . ?
C1 O1 1.262(4) . ?
C1 O2 1.238(4) . ?
C2 C3 1.389(4) . ?
C2 C7 1.386(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.373(5) . ?
C4 C5 1.397(4) . ?
C4 N2 1.449(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(4) . ?
C6 C7 1.392(4) . ?
C6 C8 1.502(4) . ?
C7 H7 0.9300 . ?
C8 O3 1.231(4) . ?
C8 O4 1.288(4) . ?
C9 C10 1.383(5) . ?
C9 C14 1.390(5) . ?
C9 N1 1.437(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.389(4) . ?
C11 C12 1.395(4) . ?
C11 C15 1.512(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.393(5) . ?
C13 C14 1.395(5) . ?
C13 C16 1.505(4) . ?
C14 H14 0.9300 . ?
C15 O5 1.258(4) . ?
C15 O6 1.248(4) . ?
C16 O7 1.243(5) . ?
C16 O8 1.255(5) . ?
C16 Zn1 2.532(3) 1_444 ?
N1 N2 1.244(4) . ?
N1 O9 1.292(8) . ?
N2 O10 1.261(6) . ?
O1 Zn1 2.005(2) . ?
O2 Zn2 2.010(2) . ?
O4 Zn1 2.030(2) 1_455 ?
O4 Zn2 2.222(2) 1_455 ?
O5 Zn1 1.990(2) 1_454 ?
O6 Zn2 2.079(2) 1_454 ?
O7 Zn1 2.367(3) 1_444 ?
O8 Zn1 2.037(3) 1_444 ?
Zn1 C16 2.532(3) 1_666 ?
Zn1 O4 2.030(2) 1_655 ?
Zn1 O5 1.990(2) 1_656 ?
Zn1 O7 2.367(3) 1_666 ?
Zn1 O8 2.037(3) 1_666 ?
Zn1 Zn2 3.2948(4) . ?
Zn2 O2 2.010(2) 2_767 ?
Zn2 O4 2.222(2) 1_655 ?
Zn2 O4 2.222(2) 2_667 ?
Zn2 O6 2.079(2) 2_666 ?
Zn2 O6 2.079(2) 1_656 ?
Zn2 Zn1 3.2948(4) 2_767 ?
C23 H23 0.9300 . ?
C23 C22 1.3900 . ?
C23 C24 1.3900 . ?
C22 C26 1.3900 . ?
C22 C19 1.504(7) . ?
C26 H26 0.9300 . ?
C26 C25 1.3900 . ?
C26 O1W 1.748(18) . ?
C25 H25 0.9300 . ?
C25 N4 1.3900 . ?
C25 O1W 1.475(16) . ?
N4 H4 0.8600 . ?
N4 C24 1.3900 . ?
C24 H24 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C17 1.3900 . ?
N3 C21 1.3900 . ?
C17 H17 0.9300 . ?
C17 C18 1.3900 . ?
C18 H18 0.9300 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C20 H20 0.9300 . ?
C20 C21 1.3900 . ?
C21 H21 0.9300 . ?
O1W H1WA 0.7730 . ?
O1W H1WB 0.7729 . ?

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 C2 118.3(3) . . ?
O2 C1 C2 116.0(3) . . ?
O2 C1 O1 125.7(3) . . ?
C3 C2 C1 117.8(3) . . ?
C7 C2 C1 122.5(3) . . ?
C7 C2 C3 119.6(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.8(3) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 121.5(3) . . ?
C3 C4 N2 117.3(3) . . ?
C5 C4 N2 120.9(3) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.3(3) . . ?
C6 C5 H5 120.8 . . ?
C5 C6 C7 120.4(3) . . ?
C5 C6 C8 120.2(3) . . ?
C7 C6 C8 119.3(3) . . ?
C2 C7 C6 120.3(3) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
O3 C8 C6 119.5(3) . . ?
O3 C8 O4 122.4(3) . . ?
O4 C8 C6 118.0(3) . . ?
C10 C9 C14 121.4(3) . . ?
C10 C9 N1 116.8(3) . . ?
C14 C9 N1 121.7(3) . . ?
C9 C10 H10 120.2 . . ?
C9 C10 C11 119.6(3) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C12 120.0(3) . . ?
C10 C11 C15 119.6(3) . . ?
C12 C11 C15 120.4(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 120.5(3) . . ?
C12 C13 C16 119.8(3) . . ?
C14 C13 C16 119.7(3) . . ?
C9 C14 C13 118.7(3) . . ?
C9 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
O5 C15 C11 116.7(3) . . ?
O6 C15 C11 117.4(3) . . ?
O6 C15 O5 125.8(3) . . ?
C13 C16 Zn1 172.4(3) . 1_444 ?
O7 C16 C13 119.5(3) . . ?
O7 C16 O8 120.9(3) . . ?
O7 C16 Zn1 68.0(2) . 1_444 ?
O8 C16 C13 119.6(3) . . ?
O8 C16 Zn1 52.87(17) . 1_444 ?
N2 N1 C9 116.4(3) . . ?
N2 N1 O9 120.9(4) . . ?
O9 N1 C9 116.8(4) . . ?
N1 N2 C4 116.7(3) . . ?
N1 N2 O10 124.3(4) . . ?
O10 N2 C4 117.4(3) . . ?
C1 O1 Zn1 118.2(2) . . ?
C1 O2 Zn2 140.1(2) . . ?
C8 O4 Zn1 107.96(19) . 1_455 ?
C8 O4 Zn2 133.3(2) . 1_455 ?
Zn1 O4 Zn2 101.51(9) 1_455 1_455 ?
C15 O5 Zn1 118.9(2) . 1_454 ?
C15 O6 Zn2 139.8(2) . 1_454 ?
C16 O7 Zn1 82.8(2) . 1_444 ?
C16 O8 Zn1 97.7(2) . 1_444 ?
C16 Zn1 Zn2 143.89(9) 1_666 . ?
O1 Zn1 C16 99.32(11) . 1_666 ?
O1 Zn1 O4 114.34(10) . 1_655 ?
O1 Zn1 O7 90.01(13) . 1_666 ?
O1 Zn1 O8 105.87(11) . 1_666 ?
O1 Zn1 Zn2 80.76(7) . . ?
O4 Zn1 C16 111.38(11) 1_655 1_666 ?
O4 Zn1 O7 90.84(10) 1_655 1_666 ?
O4 Zn1 O8 129.14(10) 1_655 1_666 ?
O4 Zn1 Zn2 41.35(6) 1_655 . ?
O5 Zn1 C16 130.15(11) 1_656 1_666 ?
O5 Zn1 O1 103.39(11) 1_656 . ?
O5 Zn1 O4 98.58(10) 1_656 1_655 ?
O5 Zn1 O7 158.51(11) 1_656 1_666 ?
O5 Zn1 O8 101.12(10) 1_656 1_666 ?
O5 Zn1 Zn2 83.80(7) 1_656 . ?
O7 Zn1 C16 29.15(11) 1_666 1_666 ?
O7 Zn1 Zn2 115.29(7) 1_666 . ?
O8 Zn1 C16 29.41(11) 1_666 1_666 ?
O8 Zn1 O7 58.55(10) 1_666 1_666 ?
O8 Zn1 Zn2 170.35(8) 1_666 . ?
O2 Zn2 O2 180.0 . 2_767 ?
O2 Zn2 O4 91.65(9) . 2_667 ?
O2 Zn2 O4 91.65(9) 2_767 1_655 ?
O2 Zn2 O4 88.35(9) 2_767 2_667 ?
O2 Zn2 O4 88.35(9) . 1_655 ?
O2 Zn2 O6 96.17(10) 2_767 2_666 ?
O2 Zn2 O6 83.83(10) 2_767 1_656 ?
O2 Zn2 O6 83.83(10) . 2_666 ?
O2 Zn2 O6 96.17(10) . 1_656 ?
O2 Zn2 Zn1 64.80(7) 2_767 2_767 ?
O2 Zn2 Zn1 64.80(7) . . ?
O2 Zn2 Zn1 115.20(7) 2_767 . ?
O2 Zn2 Zn1 115.20(7) . 2_767 ?
O4 Zn2 O4 180.0 1_655 2_667 ?
O4 Zn2 Zn1 37.14(6) 2_667 2_767 ?
O4 Zn2 Zn1 142.86(6) 1_655 2_767 ?
O4 Zn2 Zn1 142.86(6) 2_667 . ?
O4 Zn2 Zn1 37.14(6) 1_655 . ?
O6 Zn2 O4 92.16(9) 1_656 2_667 ?
O6 Zn2 O4 87.84(9) 1_656 1_655 ?
O6 Zn2 O4 87.84(9) 2_666 2_667 ?
O6 Zn2 O4 92.16(9) 2_666 1_655 ?
O6 Zn2 O6 180.0 2_666 1_656 ?
O6 Zn2 Zn1 115.65(6) 1_656 2_767 ?
O6 Zn2 Zn1 115.65(6) 2_666 . ?
O6 Zn2 Zn1 64.35(6) 2_666 2_767 ?
O6 Zn2 Zn1 64.35(6) 1_656 . ?
Zn1 Zn2 Zn1 179.999(13) 2_767 . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C22 C19 111.1(6) . . ?
C26 C22 C23 120.0 . . ?
C26 C22 C19 128.7(6) . . ?
C22 C26 H26 120.0 . . ?
C22 C26 C25 120.0 . . ?
C22 C26 O1W 170.3(8) . . ?
C25 C26 H26 120.0 . . ?
C25 C26 O1W 54.6(6) . . ?
O1W C26 H26 66.0 . . ?
C26 C25 H25 120.0 . . ?
C26 C25 N4 120.0 . . ?
C26 C25 O1W 75.2(8) . . ?
N4 C25 H25 120.0 . . ?
N4 C25 O1W 162.5(10) . . ?
O1W C25 H25 45.8 . . ?
C25 N4 H4 120.0 . . ?
C24 N4 C25 120.0 . . ?
C24 N4 H4 120.0 . . ?
C23 C24 H24 120.0 . . ?
N4 C24 C23 120.0 . . ?
N4 C24 H24 120.0 . . ?
C17 N3 H3A 120.0 . . ?
C17 N3 C21 120.0 . . ?
C21 N3 H3A 120.0 . . ?
N3 C17 H17 120.0 . . ?
N3 C17 C18 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C22 131.8(5) . . ?
C18 C19 C20 120.0 . . ?
C20 C19 C22 108.2(5) . . ?
C19 C20 H20 120.0 . . ?
C19 C20 C21 120.0 . . ?
C21 C20 H20 120.0 . . ?
N3 C21 H21 120.0 . . ?
C20 C21 N3 120.0 . . ?
C20 C21 H21 120.0 . . ?
C26 O1W H1WA 82.9 . . ?
C26 O1W H1WB 143.8 . . ?
C25 O1W C26 50.2(5) . . ?
C25 O1W H1WA 133.0 . . ?
C25 O1W H1WB 97.5 . . ?
H1WA O1W H1WB 127.8 . . ?

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
C1 C2 C3 C4 179.5(3) . . . . ?
C1 C2 C7 C6 -178.3(3) . . . . ?
C2 C1 O1 Zn1 -167.4(2) . . . . ?
C2 C1 O2 Zn2 -152.2(3) . . . . ?
C2 C3 C4 C5 -1.4(5) . . . . ?
C2 C3 C4 N2 -175.7(3) . . . . ?
C3 C2 C7 C6 -1.3(5) . . . . ?
C3 C4 C5 C6 -0.6(5) . . . . ?
C3 C4 N2 N1 -151.8(3) . . . . ?
C3 C4 N2 O10 14.6(6) . . . . ?
C4 C5 C6 C7 1.6(5) . . . . ?
C4 C5 C6 C8 -177.6(3) . . . . ?
C5 C4 N2 N1 33.9(5) . . . . ?
C5 C4 N2 O10 -159.7(5) . . . . ?
C5 C6 C7 C2 -0.7(5) . . . . ?
C5 C6 C8 O3 -165.3(3) . . . . ?
C5 C6 C8 O4 12.9(4) . . . . ?
C6 C8 O4 Zn1 -176.3(2) . . . 1_455 ?
C6 C8 O4 Zn2 57.3(4) . . . 1_455 ?
C7 C2 C3 C4 2.3(5) . . . . ?
C7 C6 C8 O3 15.4(5) . . . . ?
C7 C6 C8 O4 -166.4(3) . . . . ?
C8 C6 C7 C2 178.6(3) . . . . ?
C9 C10 C11 C12 0.8(5) . . . . ?
C9 C10 C11 C15 178.9(3) . . . . ?
C9 N1 N2 C4 -177.2(3) . . . . ?
C9 N1 N2 O10 17.4(7) . . . . ?
C10 C9 C14 C13 2.6(5) . . . . ?
C10 C9 N1 N2 -136.8(4) . . . . ?
C10 C9 N1 O9 16.4(6) . . . . ?
C10 C11 C12 C13 1.7(5) . . . . ?
C10 C11 C15 O5 0.5(5) . . . . ?
C10 C11 C15 O6 -178.5(3) . . . . ?
C11 C12 C13 C14 -2.0(5) . . . . ?
C11 C12 C13 C16 178.0(3) . . . . ?
C11 C15 O5 Zn1 176.2(2) . . . 1_454 ?
C11 C15 O6 Zn2 -145.0(3) . . . 1_454 ?
C12 C11 C15 O5 178.6(3) . . . . ?
C12 C11 C15 O6 -0.4(5) . . . . ?
C12 C13 C14 C9 -0.1(5) . . . . ?
C12 C13 C16 O7 9.0(6) . . . . ?
C12 C13 C16 O8 -170.1(3) . . . . ?
C13 C16 O7 Zn1 179.7(3) . . . 1_444 ?
C13 C16 O8 Zn1 -179.5(3) . . . 1_444 ?
C14 C9 C10 C11 -2.9(5) . . . . ?
C14 C9 N1 N2 48.5(5) . . . . ?
C14 C9 N1 O9 -158.2(5) . . . . ?
C14 C13 C16 O7 -170.9(4) . . . . ?
C14 C13 C16 O8 9.9(5) . . . . ?
C15 C11 C12 C13 -176.4(3) . . . . ?
C16 C13 C14 C9 179.9(3) . . . . ?
N1 C9 C10 C11 -177.6(3) . . . . ?
N1 C9 C14 C13 177.0(3) . . . . ?
N2 C4 C5 C6 173.5(3) . . . . ?
O1 C1 C2 C3 164.1(3) . . . . ?
O1 C1 C2 C7 -18.9(5) . . . . ?
O1 C1 O2 Zn2 28.6(6) . . . . ?
O2 C1 C2 C3 -15.2(4) . . . . ?
O2 C1 C2 C7 161.8(3) . . . . ?
O2 C1 O1 Zn1 11.8(5) . . . . ?
O3 C8 O4 Zn1 1.8(4) . . . 1_455 ?
O3 C8 O4 Zn2 -124.6(3) . . . 1_455 ?
O5 C15 O6 Zn2 36.2(5) . . . 1_454 ?
O6 C15 O5 Zn1 -5.0(4) . . . 1_454 ?
O7 C16 O8 Zn1 1.3(4) . . . 1_444 ?
O8 C16 O7 Zn1 -1.2(4) . . . 1_444 ?
O9 N1 N2 C4 30.7(6) . . . . ?
O9 N1 N2 O10 -134.7(7) . . . . ?
C23 C22 C26 C25 0.0 . . . . ?
C23 C22 C19 C18 -33.4(7) . . . . ?
C23 C22 C19 C20 146.6(4) . . . . ?
C22 C23 C24 N4 0.0 . . . . ?
C22 C26 C25 N4 0.0 . . . . ?
C22 C26 C25 O1W -170.4(10) . . . . ?
C22 C19 C20 C21 180.0(6) . . . . ?
C26 C22 C19 C18 152.3(5) . . . . ?
C26 C22 C19 C20 -27.7(8) . . . . ?
C26 C25 N4 C24 0.0 . . . . ?
C25 N4 C24 C23 0.0 . . . . ?
N4 C25 O1W C26 -151(2) . . . . ?
C24 C23 C22 C26 0.0 . . . . ?
C24 C23 C22 C19 -174.8(6) . . . . ?
N3 C17 C18 C19 0.0 . . . . ?
C17 N3 C21 C20 0.0 . . . . ?
C17 C18 C19 C22 -180.0(7) . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C22 C26 C25 173.8(7) . . . . ?
C19 C20 C21 N3 0.0 . . . . ?
C21 N3 C17 C18 0.0 . . . . ?
O1W C26 C25 N4 170.4(10) . . . . ?
O1W C25 N4 C24 148(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1478778'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_audit_creation_date             2016-08-10
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2016.05.11 svn.r3296 for OlexSys, GUI svn.r3563)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H12 N4 O18 Zn3, C13 H16 N2, H2 O'
_chemical_formula_sum            'C45 H30 N6 O19 Zn3'
_chemical_formula_weight         1154.86
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.67809(16)
_cell_length_b                   10.27573(15)
_cell_length_c                   11.9152(2)
_cell_angle_alpha                112.1787(15)
_cell_angle_beta                 101.8630(14)
_cell_angle_gamma                93.0017(13)
_cell_volume                     1062.75(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    12393
_cell_measurement_temperature    288.53(10)
_cell_measurement_theta_max      71.3360
_cell_measurement_theta_min      5.4530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.529
_diffrn_reflns_theta_min         4.696
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -32.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -77.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega    1.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000  -30.0000 73

#__ type_ start__ end____ width___ exp.time_
  3 omega   57.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  178.0000  -30.0000 50

#__ type_ start__ end____ width___ exp.time_
  4 omega  -32.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -77.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000  150.0000 73

#__ type_ start__ end____ width___ exp.time_
  6 omega   16.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   38.0000 -180.0000 88

#__ type_ start__ end____ width___ exp.time_
  7 omega  -34.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203    0.0000  150.0000 139

#__ type_ start__ end____ width___ exp.time_
  8 omega   18.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000  -60.0000 84

#__ type_ start__ end____ width___ exp.time_
  9 omega   55.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203 -178.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -120.0000 71

#__ type_ start__ end____ width___ exp.time_
 11 omega   40.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 58

#__ type_ start__ end____ width___ exp.time_
 12 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
 13 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95

#__ type_ start__ end____ width___ exp.time_
 14 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   90.0000 71

#__ type_ start__ end____ width___ exp.time_
 15 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000    0.0000 71

#__ type_ start__ end____ width___ exp.time_
 16 omega   70.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  150.0000 108

#__ type_ start__ end____ width___ exp.time_
 17 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -60.0000 71

#__ type_ start__ end____ width___ exp.time_
 18 omega   40.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

#__ type_ start__ end____ width___ exp.time_
 19 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
 20 omega   91.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 85

#__ type_ start__ end____ width___ exp.time_
 21 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

#__ type_ start__ end____ width___ exp.time_
 22 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

#__ type_ start__ end____ width___ exp.time_
 23 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
 24 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

#__ type_ start__ end____ width___ exp.time_
 25 omega   40.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 58

#__ type_ start__ end____ width___ exp.time_
 26 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 71

#__ type_ start__ end____ width___ exp.time_
 27 omega   38.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000 -150.0000 78

#__ type_ start__ end____ width___ exp.time_
 28 omega    8.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
 29 omega  -34.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -38.0000   90.0000 88

#__ type_ start__ end____ width___ exp.time_
 30 omega   18.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 31 omega    8.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000 -120.0000 95

#__ type_ start__ end____ width___ exp.time_
 32 omega   16.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   38.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
 33 omega    8.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
 34 omega   18.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
 35 omega    8.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 36 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
 37 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 91

#__ type_ start__ end____ width___ exp.time_
 38 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
 39 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 91

#__ type_ start__ end____ width___ exp.time_
 40 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 41 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
 42 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 91

#__ type_ start__ end____ width___ exp.time_
 43 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 95

#__ type_ start__ end____ width___ exp.time_
 44 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -150.0000 91

#__ type_ start__ end____ width___ exp.time_
 45 omega   70.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 108

#__ type_ start__ end____ width___ exp.time_
 46 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -60.0000 91

#__ type_ start__ end____ width___ exp.time_
 47 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 48 omega   81.00  161.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 80

#__ type_ start__ end____ width___ exp.time_
 49 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4059
_reflns_number_total             4100
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         4100
_refine_ls_number_restraints     258
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0349P)²+1.2862P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0798
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C6B-C5A \\sim C6A-C5B \\sim C7-C6B \\sim C7-C6A
 with sigma of 0.02
 C3A-C2A \\sim C3B-C2B \\sim C7-C2A \\sim C7-C2B
 with sigma of 0.02
 C13B-C12 \\sim C14B-C13A \\sim C14A-C13B \\sim C13A-C12
 with sigma of 0.02
 C12-C11B \\sim C12-C11A \\sim C11B-C10B \\sim C11A-C10A
 with sigma of 0.02
3. Restrained planarity
 C7, C2A, C3A, C4A, C5A, C6B
 with sigma of 0.1
 C14A, C9A, C10A, C11A, C12, C13B
 with sigma of 0.1
4. Rigid bond restraints
 N2, N1A, O0AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
N2 \\sim N1A \\sim O0AA: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N1A \\sim O0AA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C3A \\sim C2A \\sim C7: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
C12 \\sim C13B \\sim C14A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
6. Rigid body (RIGU) restrains
 C29, C18, C19, C17, C20, C22, N3, C21, C23, C24, C25, C26, C28, C27, N4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6B, H7B, H12A, C13B, N1A, N2, O0AA, C5A, H5A, C4A, C3A, H3A, C2A, C9A, C14A,
 H14A, C10A, H10A, C11A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Fixed Sof: C2B(0.65) C3B(0.65) H3B(0.65) C4B(0.65) C5B(0.65) H5B(0.65)
 C6B(0.35) H7A(0.65) H7B(0.35) C9B(0.65) C10B(0.65) H10B(0.65) C11B(0.65)
 H12(0.65) H12A(0.35) C13B(0.35) C14B(0.65) H14B(0.65) N1(0.65) N1A(0.35)
 N2(0.35) N2A(0.65) O9(0.65) C18(0.5) H18(0.5) C19(0.5) C20(0.5) H20(0.5)
 C21(0.5) H21(0.5) N3(0.5) H3(0.5) C17(0.5) H17(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C24(0.5) H24A(0.5) H24B(0.5) C25(0.5)
 C29(0.5) H29(0.5) C28(0.5) H28(0.5) N4(0.5) H4(0.5) C27(0.5) H27(0.5) C26(0.5)
 H26(0.5) O0AA(0.35) C5A(0.35) H5A(0.35) C4A(0.35) C3A(0.35) H3A(0.35)
 C6A(0.65) C2A(0.35) C9A(0.35) C14A(0.35) H14A(0.35) C10A(0.35) H10A(0.35)
 C11A(0.35) C13A(0.65) O1AA(0.5) H1AA(0.5) H1AB(0.5)
8.a Riding coordinates:
 O1AA(H1AA,H1AB)
8.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C22(H22A,H22B), C24(H24A,H24B)
8.c Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C5B(H5B), C7(H7A), C7(H7B), C10B(H10B), C12(H12), C12(H12A),
 C14B(H14B), C18(H18), C20(H20), C21(H21), N3(H3), C17(H17), C29(H29), C28(H28),
  N4(H4), C27(H27), C26(H26), C5A(H5A), C3A(H3A), C14A(H14A), C10A(H10A)
8.d Fitted hexagon refined as free rotating group:
 C18(C19,C20,C21,N3,C17), C25(C29,C28,N4,C27,C26)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0618(2) 0.0355(2) -0.2224(2) 0.0222(4) Uani 1 1 d . . . . .
C2B C 0.0958(8) -0.0532(8) -0.1489(8) 0.0216(11) Uani 0.65 1 d D . . A 1
C3B C 0.1529(4) 0.0173(5) -0.0203(4) 0.0234(9) Uani 0.65 1 d D . . A 1
H3B H 0.1688 0.1160 0.0165 0.028 Uiso 0.65 1 calc R . . A 1
C4B C 0.1858(4) -0.0601(4) 0.0517(3) 0.0223(8) Uani 0.65 1 d . . . A 1
C5B C 0.1587(7) -0.2071(6) 0.0000(5) 0.0241(12) Uani 0.65 1 d D . . A 1
H5B H 0.1809 -0.2585 0.0494 0.029 Uiso 0.65 1 calc R . . A 1
C6B C 0.114(3) -0.2905(18) -0.1440(13) 0.020(4) Uani 0.35 1 d D U . A 2
C7 C 0.0706(2) -0.2004(2) -0.2037(2) 0.0243(4) Uani 1 1 d D U . . .
H7A H 0.0364 -0.2482 -0.2897 0.029 Uiso 0.65 1 calc R . . A 1
H7B H 0.0119 -0.2399 -0.2841 0.029 Uiso 0.35 1 calc R U . A 2
C8 C 0.0695(3) -0.4399(2) -0.1926(2) 0.0304(5) Uani 1 1 d . . . . .
C9B C 0.4121(6) 0.0907(8) 0.3633(5) 0.0211(11) Uani 0.65 1 d . . . A 1
C10B C 0.3161(10) 0.1363(10) 0.4383(6) 0.0207(14) Uani 0.65 1 d D . . A 1
H10B H 0.2188 0.1261 0.4038 0.025 Uiso 0.65 1 calc R . . A 1
C11B C 0.3725(7) 0.1976(17) 0.5669(7) 0.0173(18) Uani 0.65 1 d D . . A 1
C12 C 0.5181(2) 0.2169(2) 0.61914(19) 0.0210(4) Uani 1 1 d D U . . .
H12 H 0.5530 0.2598 0.7054 0.025 Uiso 0.65 1 calc R . . A 1
H12A H 0.5624 0.2495 0.7038 0.025 Uiso 0.35 1 calc R U . A 2
C13B C 0.599(2) 0.167(4) 0.5298(15) 0.0208(8) Uani 0.35 1 d D U . A 2
C14B C 0.5582(6) 0.1051(7) 0.4137(6) 0.0216(12) Uani 0.65 1 d D . . A 1
H14B H 0.6193 0.0703 0.3620 0.026 Uiso 0.65 1 calc R . . A 1
C15 C 0.7648(2) 0.1775(2) 0.5858(2) 0.0236(4) Uani 1 1 d . . . . .
C16 C 0.2763(2) 0.2467(2) 0.6599(2) 0.0242(4) Uani 1 1 d . . . . .
N1 N 0.2345(3) 0.0183(4) 0.1839(3) 0.0295(7) Uani 0.65 1 d . . . A 1
N1A N 0.3398(6) -0.0274(6) 0.1563(6) 0.0255(9) Uani 0.35 1 d . U . A 2
N2 N 0.3083(8) 0.0767(7) 0.2390(6) 0.0252(10) Uani 0.35 1 d . U . A 2
N2A N 0.3598(3) 0.0141(4) 0.2293(3) 0.0280(7) Uani 0.65 1 d . . . A 1
O1 O 0.08292(19) 0.16853(17) -0.16182(15) 0.0297(4) Uani 1 1 d . . . . .
O2 O 0.01053(17) -0.02852(17) -0.33709(14) 0.0263(3) Uani 1 1 d . . . . .
O3 O 0.0252(3) -0.5013(2) -0.30684(19) 0.0531(6) Uani 1 1 d . . . . .
O4 O 0.0885(2) -0.50791(18) -0.12238(17) 0.0356(4) Uani 1 1 d . . . . .
O5 O 0.82919(17) 0.10504(19) 0.50861(16) 0.0333(4) Uani 1 1 d . . . . .
O6 O 0.82134(17) 0.25591(18) 0.69867(16) 0.0327(4) Uani 1 1 d . . . . .
O7 O 0.32795(19) 0.3170(2) 0.77213(16) 0.0423(5) Uani 1 1 d . . . . .
O8 O 0.14046(15) 0.20851(16) 0.61247(14) 0.0241(3) Uani 1 1 d . . . . .
O9 O 0.4425(5) -0.0857(5) 0.1688(5) 0.0539(13) Uani 0.65 1 d . . . A 1
Zn1 Zn 0.03398(3) 0.29255(3) -0.25444(3) 0.02174(9) Uani 1 1 d . . . . .
Zn2 Zn 0.0000 0.0000 -0.5000 0.02051(11) Uani 1 2 d S T P . .
C18 C 0.5460(4) 0.3447(6) 0.1565(4) 0.0562(19) Uani 0.5 1 d . U . B -1
H18 H 0.6343 0.3133 0.1663 0.067 Uiso 0.5 1 calc R . . B -1
C19 C 0.4914(4) 0.4100(5) 0.2600(3) 0.0331(10) Uani 0.5 1 d G U . B -1
C20 C 0.3594(5) 0.4570(5) 0.2453(3) 0.0377(13) Uani 0.5 1 d G U . B -1
H20 H 0.3228 0.5007 0.3146 0.045 Uiso 0.5 1 calc R . . B -1
C21 C 0.2821(4) 0.4387(5) 0.1271(4) 0.0356(12) Uani 0.5 1 d G U . B -1
H21 H 0.1938 0.4701 0.1172 0.043 Uiso 0.5 1 calc R . . B -1
N3 N 0.3367(5) 0.3734(7) 0.0235(3) 0.0441(14) Uani 0.5 1 d G U . B -1
H3 H 0.2889 0.3621 -0.0496 0.053 Uiso 0.5 1 calc R . . B -1
C17 C 0.4687(5) 0.3264(7) 0.0383(3) 0.068(3) Uani 0.5 1 d G U . B -1
H17 H 0.5053 0.2828 -0.0310 0.082 Uiso 0.5 1 calc R . . B -1
C23 C 0.5370(5) 0.5037(6) 0.5008(5) 0.0330(11) Uani 0.5 1 d . U . B -1
H23A H 0.4646 0.4342 0.5000 0.040 Uiso 0.5 1 calc R . . B -1
H23B H 0.4941 0.5878 0.5036 0.040 Uiso 0.5 1 calc R . . B -1
C22 C 0.5921(6) 0.4431(6) 0.3828(5) 0.0364(10) Uani 0.5 1 d . U . B -1
H22A H 0.6719 0.5102 0.3911 0.044 Uiso 0.5 1 calc R . . B -1
H22B H 0.6294 0.3566 0.3804 0.044 Uiso 0.5 1 calc R . . B -1
C24 C 0.6606(6) 0.5419(6) 0.6161(5) 0.0366(10) Uani 0.5 1 d . U . B -1
H24A H 0.7103 0.4601 0.6054 0.044 Uiso 0.5 1 calc R . . B -1
H24B H 0.7270 0.6180 0.6193 0.044 Uiso 0.5 1 calc R . . B -1
C25 C 0.6220(5) 0.5870(5) 0.7389(3) 0.0326(11) Uani 0.5 1 d . U . B -1
C29 C 0.5124(5) 0.6657(6) 0.7681(3) 0.0512(16) Uani 0.5 1 d G U . B -1
H29 H 0.4542 0.6886 0.7077 0.061 Uiso 0.5 1 calc R . . B -1
C28 C 0.4897(5) 0.7104(5) 0.8876(4) 0.0544(17) Uani 0.5 1 d G U . B -1
H28 H 0.4163 0.7631 0.9072 0.065 Uiso 0.5 1 calc R . . B -1
N4 N 0.5767(6) 0.6762(5) 0.9779(3) 0.0423(12) Uani 0.5 1 d G U . B -1
H4 H 0.5626 0.7039 1.0518 0.051 Uiso 0.5 1 calc R . . B -1
C27 C 0.6863(5) 0.5975(6) 0.9487(4) 0.0344(12) Uani 0.5 1 d G U . B -1
H27 H 0.7445 0.5747 1.0091 0.041 Uiso 0.5 1 calc R . . B -1
C26 C 0.7090(5) 0.5528(5) 0.8292(5) 0.0394(13) Uani 0.5 1 d G U . B -1
H26 H 0.7824 0.5001 0.8096 0.047 Uiso 0.5 1 calc R . . B -1
O0AA O 0.4493(9) -0.0249(11) 0.1683(9) 0.061(3) Uani 0.35 1 d . U . A 2
C5A C 0.1919(13) -0.2267(12) -0.0209(10) 0.023(2) Uani 0.35 1 d D U . A 2
H5A H 0.2130 -0.2815 0.0255 0.028 Uiso 0.35 1 calc R U . A 2
C4A C 0.2383(9) -0.0828(8) 0.0336(7) 0.0217(12) Uani 0.35 1 d . U . A 2
C3A C 0.1982(9) 0.0049(11) -0.0259(9) 0.0235(9) Uani 0.35 1 d D U . A 2
H3A H 0.2280 0.1023 0.0141 0.028 Uiso 0.35 1 calc R U . A 2
C6A C 0.0977(16) -0.2757(8) -0.1271(7) 0.0194(17) Uani 0.65 1 d D . . A 1
C2A C 0.1119(17) -0.0536(15) -0.1474(15) 0.0236(8) Uani 0.35 1 d D U . A 2
C9A C 0.3924(15) 0.1259(12) 0.3683(12) 0.021(2) Uani 0.35 1 d . U . A 2
C14A C 0.5351(16) 0.1212(16) 0.4029(14) 0.0208(10) Uani 0.35 1 d D U . A 2
H14A H 0.5879 0.0882 0.3433 0.025 Uiso 0.35 1 calc R U . A 2
C10A C 0.3158(19) 0.1740(15) 0.4532(14) 0.018(3) Uani 0.35 1 d D U . A 2
H10A H 0.2200 0.1787 0.4248 0.021 Uiso 0.35 1 calc R U . A 2
C11A C 0.3702(16) 0.218(3) 0.5815(17) 0.020(3) Uani 0.35 1 d D U . A 2
C13A C 0.6112(10) 0.172(2) 0.5426(7) 0.0195(12) Uani 0.65 1 d D . . A 1
O1AA O 0.8060(7) 0.4614(10) 0.4777(7) 0.120(3) Uani 0.5 1 d . . . C -2
H1AA H 0.8439 0.4710 0.4224 0.179 Uiso 0.5 1 d R . . C -2
H1AB H 0.8710 0.4725 0.5419 0.179 Uiso 0.5 1 d R . . C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2B 1.491(10) . ?
C1 O1 1.264(3) . ?
C1 O2 1.247(3) . ?
C1 C2A 1.54(2) . ?
C2B C3B 1.396(7) . ?
C2B C7 1.388(8) . ?
C3B H3B 0.9300 . ?
C3B C4B 1.379(6) . ?
C4B C5B 1.385(6) . ?
C4B N1 1.431(4) . ?
C5B H5B 0.9300 . ?
C5B C6A 1.387(6) . ?
C6B C7 1.398(13) . ?
C6B C8 1.426(19) . ?
C6B C5A 1.385(13) . ?
C7 H7A 0.9300 . ?
C7 H7B 0.9300 . ?
C7 C6A 1.397(7) . ?
C7 C2A 1.396(13) . ?
C8 O3 1.232(3) . ?
C8 O4 1.270(3) . ?
C8 Zn1 2.547(2) 1_545 ?
C8 C6A 1.550(8) . ?
C9B C10B 1.397(8) . ?
C9B C14B 1.394(7) . ?
C9B N2A 1.450(6) . ?
C10B H10B 0.9300 . ?
C10B C11B 1.391(6) . ?
C11B C12 1.389(7) . ?
C11B C16 1.550(8) . ?
C12 H12 0.9300 . ?
C12 H12A 0.9300 . ?
C12 C13B 1.411(13) . ?
C12 C11A 1.410(13) . ?
C12 C13A 1.386(8) . ?
C13B C15 1.58(2) . ?
C13B C14A 1.393(14) . ?
C14B H14B 0.9300 . ?
C14B C13A 1.391(7) . ?
C15 O5 1.248(3) . ?
C15 O6 1.261(3) . ?
C15 C13A 1.460(10) . ?
C16 O7 1.231(3) . ?
C16 O8 1.295(3) . ?
C16 C11A 1.40(2) . ?
N1 N2A 1.232(5) . ?
N1A N2 1.253(9) . ?
N1A O0AA 1.038(10) . ?
N1A C4A 1.466(10) . ?
N2 C9A 1.464(14) . ?
N2A O9 1.406(6) . ?
O1 Zn1 1.9942(16) . ?
O2 Zn2 2.0532(15) . ?
O3 Zn1 2.425(2) 1_545 ?
O4 Zn1 2.0170(17) 1_545 ?
O5 Zn2 2.0202(16) 1_656 ?
O6 Zn1 1.9941(16) 1_656 ?
O8 Zn1 2.0133(15) 1_556 ?
O8 Zn2 2.2389(15) 1_556 ?
Zn1 C8 2.547(2) 1_565 ?
Zn1 O3 2.425(2) 1_565 ?
Zn1 O4 2.0169(17) 1_565 ?
Zn1 O6 1.9941(16) 1_454 ?
Zn1 O8 2.0133(15) 1_554 ?
Zn2 O2 2.0532(15) 2_554 ?
Zn2 O5 2.0202(16) 1_454 ?
Zn2 O5 2.0202(16) 2_655 ?
Zn2 O8 2.2390(15) 2 ?
Zn2 O8 2.2390(15) 1_554 ?
C18 H18 0.9300 . ?
C18 C19 1.3900 . ?
C18 C17 1.3900 . ?
C19 C20 1.3900 . ?
C19 C22 1.486(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.3900 . ?
C21 H21 0.9300 . ?
C21 N3 1.3900 . ?
N3 H3 0.8600 . ?
N3 C17 1.3900 . ?
C17 H17 0.9300 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C22 1.528(7) . ?
C23 C24 1.530(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.492(6) . ?
C25 C29 1.3900 . ?
C25 C26 1.3900 . ?
C29 H29 0.9300 . ?
C29 C28 1.3900 . ?
C28 H28 0.9300 . ?
C28 N4 1.3900 . ?
N4 H4 0.8600 . ?
N4 C27 1.3900 . ?
C27 H27 0.9300 . ?
C27 C26 1.3900 . ?
C26 H26 0.9300 . ?
C5A H5A 0.9300 . ?
C5A C4A 1.377(13) . ?
C4A C3A 1.368(13) . ?
C3A H3A 0.9300 . ?
C3A C2A 1.396(14) . ?
C9A C14A 1.367(18) . ?
C9A C10A 1.336(19) . ?
C14A H14A 0.9300 . ?
C10A H10A 0.9300 . ?
C10A C11A 1.394(13) . ?
O1AA H1AA 0.8505 . ?
O1AA H1AB 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 C2B 116.8(3) . . ?
O1 C1 C2A 116.1(5) . . ?
O2 C1 C2B 117.0(3) . . ?
O2 C1 O1 126.2(2) . . ?
O2 C1 C2A 117.7(5) . . ?
C3B C2B C1 117.5(5) . . ?
C7 C2B C1 122.3(6) . . ?
C7 C2B C3B 120.2(7) . . ?
C2B C3B H3B 120.2 . . ?
C4B C3B C2B 119.7(5) . . ?
C4B C3B H3B 120.2 . . ?
C3B C4B C5B 121.4(4) . . ?
C3B C4B N1 116.9(4) . . ?
C5B C4B N1 121.4(4) . . ?
C4B C5B H5B 120.8 . . ?
C4B C5B C6A 118.3(5) . . ?
C6A C5B H5B 120.8 . . ?
C7 C6B C8 125.7(12) . . ?
C5A C6B C7 116.8(13) . . ?
C5A C6B C8 116.9(10) . . ?
C2B C7 H7A 120.6 . . ?
C2B C7 C6A 118.8(5) . . ?
C6B C7 H7B 118.7 . . ?
C6A C7 H7A 120.6 . . ?
C2A C7 C6B 122.7(11) . . ?
C2A C7 H7B 118.7 . . ?
C6B C8 Zn1 169.5(8) . 1_545 ?
O3 C8 C6B 116.9(6) . . ?
O3 C8 O4 121.7(2) . . ?
O3 C8 Zn1 70.22(14) . 1_545 ?
O3 C8 C6A 121.5(3) . . ?
O4 C8 C6B 121.1(5) . . ?
O4 C8 Zn1 51.46(11) . 1_545 ?
O4 C8 C6A 116.8(3) . . ?
C6A C8 Zn1 168.2(3) . 1_545 ?
C10B C9B N2A 120.1(5) . . ?
C14B C9B C10B 122.1(5) . . ?
C14B C9B N2A 117.6(5) . . ?
C9B C10B H10B 121.5 . . ?
C11B C10B C9B 117.0(7) . . ?
C11B C10B H10B 121.5 . . ?
C10B C11B C16 121.9(6) . . ?
C12 C11B C10B 121.9(7) . . ?
C12 C11B C16 116.3(5) . . ?
C11B C12 H12 120.0 . . ?
C13B C12 H12A 119.7 . . ?
C11A C12 H12A 119.7 . . ?
C11A C12 C13B 120.7(12) . . ?
C13A C12 C11B 119.9(5) . . ?
C13A C12 H12 120.0 . . ?
C12 C13B C15 115.1(12) . . ?
C14A C13B C12 120.3(17) . . ?
C14A C13B C15 124.6(11) . . ?
C9B C14B H14B 120.4 . . ?
C13A C14B C9B 119.1(7) . . ?
C13A C14B H14B 120.4 . . ?
O5 C15 C13B 114.0(7) . . ?
O5 C15 O6 125.4(2) . . ?
O5 C15 C13A 117.7(4) . . ?
O6 C15 C13B 120.5(7) . . ?
O6 C15 C13A 116.9(4) . . ?
O7 C16 C11B 121.2(3) . . ?
O7 C16 O8 122.8(2) . . ?
O7 C16 C11A 117.2(7) . . ?
O8 C16 C11B 116.0(3) . . ?
O8 C16 C11A 119.8(6) . . ?
N2A N1 C4B 115.4(3) . . ?
N2 N1A C4A 115.6(6) . . ?
O0AA N1A N2 112.0(9) . . ?
O0AA N1A C4A 123.5(9) . . ?
N1A N2 C9A 119.1(7) . . ?
N1 N2A C9B 116.8(4) . . ?
N1 N2A O9 124.5(4) . . ?
O9 N2A C9B 116.6(4) . . ?
C1 O1 Zn1 118.63(14) . . ?
C1 O2 Zn2 139.84(14) . . ?
C8 O3 Zn1 81.22(15) . 1_545 ?
C8 O4 Zn1 99.04(15) . 1_545 ?
C15 O5 Zn2 140.70(16) . 1_656 ?
C15 O6 Zn1 115.71(14) . 1_656 ?
C16 O8 Zn1 109.86(13) . 1_556 ?
C16 O8 Zn2 134.60(14) . 1_556 ?
Zn1 O8 Zn2 99.58(6) 1_556 1_556 ?
O1 Zn1 C8 133.77(8) . 1_565 ?
O1 Zn1 O3 161.66(7) . 1_565 ?
O1 Zn1 O4 104.58(7) . 1_565 ?
O1 Zn1 O6 102.05(7) . 1_454 ?
O1 Zn1 O8 97.93(7) . 1_554 ?
O3 Zn1 C8 28.57(7) 1_565 1_565 ?
O4 Zn1 C8 29.51(8) 1_565 1_565 ?
O4 Zn1 O3 58.07(7) 1_565 1_565 ?
O6 Zn1 C8 99.24(8) 1_454 1_565 ?
O6 Zn1 O3 89.56(8) 1_454 1_565 ?
O6 Zn1 O4 106.21(7) 1_454 1_565 ?
O6 Zn1 O8 118.94(7) 1_454 1_554 ?
O8 Zn1 C8 106.77(7) 1_554 1_565 ?
O8 Zn1 O3 88.55(7) 1_554 1_565 ?
O8 Zn1 O4 123.31(7) 1_554 1_565 ?
O2 Zn2 O2 180.0 . 2_554 ?
O2 Zn2 O8 91.61(6) 2_554 1_554 ?
O2 Zn2 O8 91.61(6) . 2 ?
O2 Zn2 O8 88.39(6) 2_554 2 ?
O2 Zn2 O8 88.39(6) . 1_554 ?
O5 Zn2 O2 96.08(7) 1_454 . ?
O5 Zn2 O2 83.92(7) 2_655 . ?
O5 Zn2 O2 96.08(7) 2_655 2_554 ?
O5 Zn2 O2 83.92(7) 1_454 2_554 ?
O5 Zn2 O5 180.0 2_655 1_454 ?
O5 Zn2 O8 91.38(6) 2_655 1_554 ?
O5 Zn2 O8 88.62(6) 2_655 2 ?
O5 Zn2 O8 88.62(6) 1_454 1_554 ?
O5 Zn2 O8 91.38(6) 1_454 2 ?
O8 Zn2 O8 180.00(6) 2 1_554 ?
C19 C18 H18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 C22 115.1(4) . . ?
C20 C19 C22 124.3(4) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 120.0 . . ?
C20 C21 N3 120.0 . . ?
N3 C21 H21 120.0 . . ?
C21 N3 H3 120.0 . . ?
C17 N3 C21 120.0 . . ?
C17 N3 H3 120.0 . . ?
C18 C17 H17 120.0 . . ?
N3 C17 C18 120.0 . . ?
N3 C17 H17 120.0 . . ?
H23A C23 H23B 108.2 . . ?
C22 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C22 C23 C24 109.6(4) . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
C19 C22 C23 118.4(5) . . ?
C19 C22 H22A 107.7 . . ?
C19 C22 H22B 107.7 . . ?
C23 C22 H22A 107.7 . . ?
C23 C22 H22B 107.7 . . ?
H22A C22 H22B 107.1 . . ?
C23 C24 H24A 108.2 . . ?
C23 C24 H24B 108.2 . . ?
H24A C24 H24B 107.4 . . ?
C25 C24 C23 116.3(5) . . ?
C25 C24 H24A 108.2 . . ?
C25 C24 H24B 108.2 . . ?
C29 C25 C24 124.0(4) . . ?
C29 C25 C26 120.0 . . ?
C26 C25 C24 115.9(4) . . ?
C25 C29 H29 120.0 . . ?
C25 C29 C28 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C28 H28 120.0 . . ?
C29 C28 N4 120.0 . . ?
N4 C28 H28 120.0 . . ?
C28 N4 H4 120.0 . . ?
C28 N4 C27 120.0 . . ?
C27 N4 H4 120.0 . . ?
N4 C27 H27 120.0 . . ?
C26 C27 N4 120.0 . . ?
C26 C27 H27 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C6B C5A H5A 119.7 . . ?
C4A C5A C6B 120.6(12) . . ?
C4A C5A H5A 119.7 . . ?
C5A C4A N1A 117.2(7) . . ?
C3A C4A N1A 120.7(7) . . ?
C3A C4A C5A 122.0(8) . . ?
C4A C3A H3A 120.4 . . ?
C4A C3A C2A 119.2(11) . . ?
C2A C3A H3A 120.4 . . ?
C5B C6A C7 121.5(6) . . ?
C5B C6A C8 121.3(5) . . ?
C7 C6A C8 116.9(5) . . ?
C7 C2A C1 118.6(11) . . ?
C3A C2A C1 123.2(10) . . ?
C3A C2A C7 118.2(15) . . ?
C14A C9A N2 124.8(12) . . ?
C10A C9A N2 113.8(11) . . ?
C10A C9A C14A 121.4(13) . . ?
C13B C14A H14A 120.9 . . ?
C9A C14A C13B 118.2(15) . . ?
C9A C14A H14A 120.9 . . ?
C9A C10A H10A 117.9 . . ?
C9A C10A C11A 124.3(15) . . ?
C11A C10A H10A 117.9 . . ?
C16 C11A C12 125.5(13) . . ?
C10A C11A C12 115.1(15) . . ?
C10A C11A C16 119.2(12) . . ?
C12 C13A C14B 119.8(7) . . ?
C12 C13A C15 125.3(6) . . ?
C14B C13A C15 114.6(6) . . ?
H1AA O1AA H1AB 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
C1 C2B C3B C4B 179.8(4) . . . . ?
C1 C2B C7 C6A -176.3(9) . . . . ?
C2B C1 O1 Zn1 -178.2(3) . . . . ?
C2B C1 O2 Zn2 -152.8(3) . . . . ?
C2B C3B C4B C5B -2.3(7) . . . . ?
C2B C3B C4B N1 -175.7(5) . . . . ?
C2B C7 C6A C5B -4.9(15) . . . . ?
C2B C7 C6A C8 -179.4(8) . . . . ?
C3B C2B C7 C6A 2.8(10) . . . . ?
C3B C4B C5B C6A 0.2(10) . . . . ?
C3B C4B N1 N2A -112.9(4) . . . . ?
C4B C5B C6A C7 3.4(15) . . . . ?
C4B C5B C6A C8 177.6(8) . . . . ?
C4B N1 N2A C9B -179.1(5) . . . . ?
C4B N1 N2A O9 -16.1(6) . . . . ?
C5B C4B N1 N2A 73.6(6) . . . . ?
C6B C7 C2A C1 178.3(16) . . . . ?
C6B C7 C2A C3A -1.1(17) . . . . ?
C6B C8 O3 Zn1 171.5(12) . . . 1_545 ?
C6B C8 O4 Zn1 -170.9(13) . . . 1_545 ?
C6B C5A C4A N1A -169.9(14) . . . . ?
C6B C5A C4A C3A 6.8(18) . . . . ?
C7 C2B C3B C4B 0.7(8) . . . . ?
C7 C6B C8 O3 23(3) . . . . ?
C7 C6B C8 O4 -164.3(15) . . . . ?
C7 C6B C8 Zn1 153(3) . . . 1_545 ?
C7 C6B C5A C4A -8(3) . . . . ?
C8 C6B C7 C2A 176.1(17) . . . . ?
C8 C6B C5A C4A -179.6(14) . . . . ?
C9B C10B C11B C12 1.9(18) . . . . ?
C9B C10B C11B C16 -177.5(11) . . . . ?
C9B C14B C13A C12 3(2) . . . . ?
C9B C14B C13A C15 178.1(10) . . . . ?
C10B C9B C14B C13A -2.7(13) . . . . ?
C10B C9B N2A N1 14.9(9) . . . . ?
C10B C9B N2A O9 -149.4(7) . . . . ?
C10B C11B C12 C13A -1(2) . . . . ?
C10B C11B C16 O7 -170.6(9) . . . . ?
C10B C11B C16 O8 9.9(16) . . . . ?
C11B C12 C13A C14B -2(2) . . . . ?
C11B C12 C13A C15 -175.6(14) . . . . ?
C11B C16 O8 Zn1 -176.5(7) . . . 1_556 ?
C11B C16 O8 Zn2 56.3(8) . . . 1_556 ?
C12 C11B C16 O7 10.0(15) . . . . ?
C12 C11B C16 O8 -169.5(8) . . . . ?
C12 C13B C15 O5 164(2) . . . . ?
C12 C13B C15 O6 -17(4) . . . . ?
C12 C13B C14A C9A 0(4) . . . . ?
C13B C12 C11A C16 171(3) . . . . ?
C13B C12 C11A C10A -3(4) . . . . ?
C13B C15 O5 Zn2 -151.0(17) . . . 1_656 ?
C13B C15 O6 Zn1 -166.6(18) . . . 1_656 ?
C14B C9B C10B C11B 0.1(12) . . . . ?
C14B C9B N2A N1 -170.6(5) . . . . ?
C14B C9B N2A O9 25.1(8) . . . . ?
C15 C13B C14A C9A -176(2) . . . . ?
C16 C11B C12 C13A 178.2(12) . . . . ?
N1 C4B C5B C6A 173.4(8) . . . . ?
N1A N2 C9A C14A 33.5(15) . . . . ?
N1A N2 C9A C10A -144.8(9) . . . . ?
N1A C4A C3A C2A 174.0(9) . . . . ?
N2 N1A C4A C5A -129.5(8) . . . . ?
N2 N1A C4A C3A 53.8(10) . . . . ?
N2 C9A C14A C13B -178(2) . . . . ?
N2 C9A C10A C11A 176(2) . . . . ?
N2A C9B C10B C11B 174.3(10) . . . . ?
N2A C9B C14B C13A -177.1(11) . . . . ?
O1 C1 C2B C3B -2.3(7) . . . . ?
O1 C1 C2B C7 176.7(4) . . . . ?
O1 C1 O2 Zn2 30.0(4) . . . . ?
O1 C1 C2A C7 169.4(8) . . . . ?
O1 C1 C2A C3A -11.2(14) . . . . ?
O2 C1 C2B C3B -179.8(4) . . . . ?
O2 C1 C2B C7 -0.8(7) . . . . ?
O2 C1 O1 Zn1 -1.0(3) . . . . ?
O2 C1 C2A C7 -13.7(14) . . . . ?
O2 C1 C2A C3A 165.7(8) . . . . ?
O3 C8 O4 Zn1 1.9(3) . . . 1_545 ?
O3 C8 C6A C5B -174.6(8) . . . . ?
O3 C8 C6A C7 -0.1(14) . . . . ?
O4 C8 O3 Zn1 -1.6(2) . . . 1_545 ?
O4 C8 C6A C5B 8.4(14) . . . . ?
O4 C8 C6A C7 -177.2(7) . . . . ?
O5 C15 O6 Zn1 12.0(3) . . . 1_656 ?
O5 C15 C13A C12 163.8(12) . . . . ?
O5 C15 C13A C14B -10.5(17) . . . . ?
O6 C15 O5 Zn2 30.3(4) . . . 1_656 ?
O6 C15 C13A C12 -16(2) . . . . ?
O6 C15 C13A C14B 169.2(9) . . . . ?
O7 C16 O8 Zn1 4.1(3) . . . 1_556 ?
O7 C16 O8 Zn2 -123.1(2) . . . 1_556 ?
O7 C16 C11A C12 23(3) . . . . ?
O7 C16 C11A C10A -162.6(17) . . . . ?
O8 C16 C11A C12 -161.6(19) . . . . ?
O8 C16 C11A C10A 13(3) . . . . ?
Zn1 C8 C6A C5B 12(4) 1_545 . . . ?
Zn1 C8 C6A C7 -173.2(18) 1_545 . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C18 C19 C22 C23 -175.0(4) . . . . ?
C19 C18 C17 N3 0.0 . . . . ?
C19 C20 C21 N3 0.0 . . . . ?
C20 C19 C22 C23 14.2(7) . . . . ?
C20 C21 N3 C17 0.0 . . . . ?
C21 N3 C17 C18 0.0 . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C22 -171.2(4) . . . . ?
C23 C24 C25 C29 -35.4(6) . . . . ?
C23 C24 C25 C26 148.4(4) . . . . ?
C22 C19 C20 C21 170.3(5) . . . . ?
C22 C23 C24 C25 -173.2(4) . . . . ?
C24 C23 C22 C19 -175.0(4) . . . . ?
C24 C25 C29 C28 -176.1(5) . . . . ?
C24 C25 C26 C27 176.4(4) . . . . ?
C25 C29 C28 N4 0.0 . . . . ?
C29 C25 C26 C27 0.0 . . . . ?
C29 C28 N4 C27 0.0 . . . . ?
C28 N4 C27 C26 0.0 . . . . ?
N4 C27 C26 C25 0.0 . . . . ?
C26 C25 C29 C28 0.0 . . . . ?
O0AA N1A N2 C9A -40.0(13) . . . . ?
O0AA N1A C4A C5A 85.9(12) . . . . ?
O0AA N1A C4A C3A -90.9(12) . . . . ?
C5A C6B C7 C2A 5(3) . . . . ?
C5A C6B C8 O3 -166.3(13) . . . . ?
C5A C6B C8 O4 7(2) . . . . ?
C5A C6B C8 Zn1 -36(7) . . . 1_545 ?
C5A C4A C3A C2A -2.5(13) . . . . ?
C4A N1A N2 C9A 171.3(9) . . . . ?
C4A C3A C2A C1 -179.7(11) . . . . ?
C4A C3A C2A C7 -0.3(14) . . . . ?
C6A C8 O3 Zn1 -178.5(7) . . . 1_545 ?
C6A C8 O4 Zn1 179.0(7) . . . 1_545 ?
C2A C1 O1 Zn1 175.6(7) . . . . ?
C2A C1 O2 Zn2 -146.6(7) . . . . ?
C9A C10A C11A C12 4(3) . . . . ?
C9A C10A C11A C16 -170.9(19) . . . . ?
C14A C13B C15 O5 -19(4) . . . . ?
C14A C13B C15 O6 160(2) . . . . ?
C14A C9A C10A C11A -3(2) . . . . ?
C10A C9A C14A C13B 0(2) . . . . ?
C11A C12 C13B C15 178(2) . . . . ?
C11A C12 C13B C14A 1(5) . . . . ?
C11A C16 O8 Zn1 -171.0(16) . . . 1_556 ?
C11A C16 O8 Zn2 61.8(16) . . . 1_556 ?
C13A C15 O5 Zn2 -149.9(9) . . . 1_656 ?
C13A C15 O6 Zn1 -167.8(9) . . . 1_656 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1478779'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_audit_creation_date             2016-07-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H12 Cd3 N4 O18, 2(C2 H8 N), 3(H2 O)'
_chemical_formula_sum            'C36 H34 Cd3 N6 O21'
_chemical_formula_weight         1223.89
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cd1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.8669(2)
_cell_length_b                   10.4250(2)
_cell_length_c                   12.4397(3)
_cell_angle_alpha                111.3156(19)
_cell_angle_beta                 102.5684(18)
_cell_angle_gamma                93.8625(17)
_cell_volume                     1148.29(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    13779
_cell_measurement_temperature    290.56(17)
_cell_measurement_theta_max      71.4660
_cell_measurement_theta_min      4.6150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.772
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            "'clear light yellow'"
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21241
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.546
_diffrn_reflns_theta_min         4.613
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.56(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    7.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   19.0000  -30.0000 101

#__ type_ start__ end____ width___ exp.time_
  2 omega    1.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000   90.0000 75

#__ type_ start__ end____ width___ exp.time_
  3 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  150.0000 84

#__ type_ start__ end____ width___ exp.time_
  5 omega    2.00   29.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   91.0000  -75.3243 27

#__ type_ start__ end____ width___ exp.time_
  6 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  7 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  8 omega   13.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203 -113.0000  -13.0000 70

#__ type_ start__ end____ width___ exp.time_
  9 omega   40.00   98.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
 10 omega   38.00   91.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
 11 omega   39.00  110.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   60.0000 71

#__ type_ start__ end____ width___ exp.time_
 12 omega   38.00   91.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
 13 omega   38.00  116.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000  -30.0000 78

#__ type_ start__ end____ width___ exp.time_
 14 omega   91.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85

#__ type_ start__ end____ width___ exp.time_
 15 omega   57.00  150.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 93

#__ type_ start__ end____ width___ exp.time_
 16 omega   37.00  146.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000  120.0000 109

#__ type_ start__ end____ width___ exp.time_
 17 omega   39.00  110.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  150.0000 71

#__ type_ start__ end____ width___ exp.time_
 18 omega   90.00  175.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -30.0000 85

#__ type_ start__ end____ width___ exp.time_
 19 omega   39.00  110.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000    0.0000 71

#__ type_ start__ end____ width___ exp.time_
 20 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 21 omega   41.00  126.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  120.0000 85

#__ type_ start__ end____ width___ exp.time_
 22 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
 23 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   90.0000 84

#__ type_ start__ end____ width___ exp.time_
 24 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 25 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -150.0000 94

#__ type_ start__ end____ width___ exp.time_
 26 omega   57.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000 -150.0000 52

#__ type_ start__ end____ width___ exp.time_
 27 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 28 omega   70.00  178.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108

#__ type_ start__ end____ width___ exp.time_
 29 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 95

#__ type_ start__ end____ width___ exp.time_
 30 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 95

#__ type_ start__ end____ width___ exp.time_
 31 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
 32 omega   91.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
 33 omega   70.00  178.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   60.0000 108

#__ type_ start__ end____ width___ exp.time_
 34 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 35 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
 36 omega   90.00  175.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -90.0000 85

#__ type_ start__ end____ width___ exp.time_
 37 omega   90.00  175.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  120.0000 85

#__ type_ start__ end____ width___ exp.time_
 38 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
 39 omega   91.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 85

#__ type_ start__ end____ width___ exp.time_
 40 omega    7.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   19.0000  150.0000 101

#__ type_ start__ end____ width___ exp.time_
 41 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -60.0000 84

#__ type_ start__ end____ width___ exp.time_
 42 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
 43 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
 44 omega   18.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   38.0000  -60.0000 88

#__ type_ start__ end____ width___ exp.time_
 45 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
 46 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
 47 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0376607000
_diffrn_orient_matrix_UB_12      0.0316538000
_diffrn_orient_matrix_UB_13      -0.1136650000
_diffrn_orient_matrix_UB_21      -0.0711363000
_diffrn_orient_matrix_UB_22      -0.1526990000
_diffrn_orient_matrix_UB_23      -0.0731865000
_diffrn_orient_matrix_UB_31      -0.1406856000
_diffrn_orient_matrix_UB_32      0.0389102000
_diffrn_orient_matrix_UB_33      0.0261166000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4250
_reflns_number_total             4417
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0628P)²+2.5296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1106
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N3-C17 = N3-C18
 1.4 with sigma of 0.01
 C18-C17
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C17, C18, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O10)=1-FVAR(1)
 Sof(O9)=FVAR(1)
 Fixed Sof: O2W(0.5) H2Wa(0.5) H2Wb(0.5)
6.a Riding coordinates:
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), O1W(H1Wa,H1Wb), O2W(H2Wa,H2Wb)
6.b Secondary CH2 refined with riding coordinates:
 N3(H3a,H3b)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.2614(4) 0.3028(5) 0.4080(4) 0.0314(9) Uani 1 1 d . . . . .
C2 C -0.1054(4) 0.3224(4) 0.4619(4) 0.0262(8) Uani 1 1 d . . . . .
C3 C -0.0524(4) 0.3960(4) 0.5844(4) 0.0285(8) Uani 1 1 d . . . . .
H3 H -0.1122 0.4338 0.6319 0.034 Uiso 1 1 calc R . . . .
C4 C 0.0893(4) 0.4121(4) 0.6344(4) 0.0268(8) Uani 1 1 d . . . . .
C5 C 0.1819(4) 0.3600(4) 0.5659(4) 0.0254(8) Uani 1 1 d . . . . .
H5 H 0.2776 0.3721 0.6013 0.031 Uiso 1 1 calc R . . . .
C6 C 0.1285(4) 0.2893(4) 0.4432(4) 0.0239(8) Uani 1 1 d . . . . .
C7 C -0.0154(4) 0.2695(4) 0.3914(4) 0.0258(8) Uani 1 1 d . . . . .
H7 H -0.0510 0.2208 0.3094 0.031 Uiso 1 1 calc R . . . .
C8 C 0.2262(4) 0.2364(4) 0.3668(4) 0.0259(8) Uani 1 1 d . . . . .
C9 C 0.2985(5) 0.5299(4) 0.9409(4) 0.0302(9) Uani 1 1 d . . . . .
C10 C 0.3266(5) 0.6752(5) 0.9896(4) 0.0316(9) Uani 1 1 d . . . . .
H10 H 0.3056 0.7251 0.9411 0.038 Uiso 1 1 calc R . . . .
C11 C 0.3863(5) 0.7443(4) 1.1113(4) 0.0303(9) Uani 1 1 d . . . . .
C12 C 0.4168(5) 0.6685(4) 1.1829(4) 0.0303(9) Uani 1 1 d . . . . .
H12 H 0.4562 0.7151 1.2647 0.036 Uiso 1 1 calc R . . . .
C13 C 0.3888(4) 0.5237(4) 1.1333(4) 0.0270(8) Uani 1 1 d . . . . .
C14 C 0.3318(5) 0.4543(4) 1.0109(4) 0.0290(9) Uani 1 1 d . . . . .
H14 H 0.3163 0.3573 0.9765 0.035 Uiso 1 1 calc R . . . .
C15 C 0.4228(5) 0.4414(5) 1.2105(4) 0.0296(9) Uani 1 1 d . . . . .
C16 C 0.4144(5) 0.9010(5) 1.1655(4) 0.0340(10) Uani 1 1 d . . . . .
Cd1 Cd -0.54670(3) 0.17885(3) 0.25827(2) 0.02397(11) Uani 1 1 d . . . . .
Cd2 Cd -0.5000 0.5000 0.5000 0.02238(12) Uani 1 2 d S T P . .
N1 N 0.1416(4) 0.4905(4) 0.7622(3) 0.0335(8) Uani 1 1 d . . . . .
N2 N 0.2431(5) 0.4517(4) 0.8146(3) 0.0380(9) Uani 1 1 d . . . . .
O1 O -0.3105(3) 0.2246(4) 0.3003(3) 0.0485(9) Uani 1 1 d . . . . .
O2 O -0.3339(4) 0.3634(5) 0.4758(4) 0.0505(9) Uani 1 1 d . . . . .
O3 O 0.1814(4) 0.1457(4) 0.2647(3) 0.0450(9) Uani 1 1 d . . . . .
O4 O 0.3576(3) 0.2862(3) 0.4111(3) 0.0305(6) Uani 1 1 d . . . . .
O5 O 0.3947(4) 0.3106(3) 1.1583(3) 0.0436(8) Uani 1 1 d . . . . .
O6 O 0.4766(4) 0.5070(4) 1.3190(3) 0.0424(8) Uani 1 1 d . . . . .
O7 O 0.3892(5) 0.9661(3) 1.0990(3) 0.0502(10) Uani 1 1 d . . . . .
O8 O 0.4610(5) 0.9618(3) 1.2762(3) 0.0513(10) Uani 1 1 d . . . . .
O9 O 0.0653(7) 0.5740(8) 0.8131(5) 0.075(3) Uani 0.703(12) 1 d . . . . .
O10 O 0.2503(19) 0.3172(13) 0.7779(11) 0.063(5) Uani 0.297(12) 1 d . . . . .
C17 C -0.028(2) -0.174(3) -0.001(2) 0.261(10) Uani 1 1 d D U . . .
H17A H 0.0498 -0.2254 -0.0078 0.391 Uiso 1 1 d R . . . .
H17B H -0.0206 -0.1072 -0.0367 0.391 Uiso 1 1 d R . . . .
H17C H -0.1145 -0.2380 -0.0421 0.391 Uiso 1 1 d R . . . .
C18 C 0.015(2) -0.137(2) 0.2186(19) 0.269(10) Uani 1 1 d D U . . .
H18A H -0.0636 -0.1555 0.2471 0.404 Uiso 1 1 d R . . . .
H18B H 0.0830 -0.0624 0.2816 0.404 Uiso 1 1 d R . . . .
H18C H 0.0580 -0.2192 0.1936 0.404 Uiso 1 1 d R . . . .
N3 N -0.019(3) -0.100(2) 0.120(2) 0.334(12) Uani 1 1 d D U . . .
H3A H 0.0406 -0.0221 0.1404 0.401 Uiso 1 1 calc R . . . .
H3B H -0.1031 -0.0741 0.1204 0.401 Uiso 1 1 calc R . . . .
O1W O -0.2527(10) -0.0156(13) 0.1152(7) 0.176(5) Uani 1 1 d . . . . .
H1WA H -0.2870 -0.0044 0.0472 0.264 Uiso 1 1 d R . . . .
H1WB H -0.2683 0.0607 0.1633 0.264 Uiso 1 1 d R . . . .
O2W O 0.684(2) 1.023(2) 1.5205(17) 0.163(7) Uani 0.5 1 d . U . . .
H2WA H 0.6242 1.0064 1.4545 0.244 Uiso 0.5 1 d R . . . .
H2WB H 0.6404 1.0262 1.5734 0.244 Uiso 0.5 1 d R . . . .


_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 1.506(6) . ?
C1 O1 1.251(6) . ?
C1 O2 1.248(6) . ?
C2 C3 1.391(6) . ?
C2 C7 1.384(6) . ?
C3 C4 1.373(6) . ?
C4 C5 1.387(6) . ?
C4 N1 1.451(5) . ?
C5 C6 1.389(6) . ?
C6 C7 1.393(6) . ?
C6 C8 1.492(6) . ?
C8 O3 1.236(5) . ?
C8 O4 1.282(5) . ?
C9 C10 1.394(6) . ?
C9 C14 1.377(6) . ?
C9 N2 1.438(5) . ?
C10 C11 1.386(6) . ?
C11 C12 1.391(6) . ?
C11 C16 1.503(6) . ?
C12 C13 1.388(6) . ?
C13 C14 1.389(6) . ?
C13 C15 1.506(6) . ?
C15 O5 1.259(5) . ?
C15 O6 1.241(5) . ?
C16 Cd1 2.664(4) 1_666 ?
C16 O7 1.245(6) . ?
C16 O8 1.249(6) . ?
Cd1 C16 2.664(4) 1_444 ?
Cd1 O1 2.252(3) . ?
Cd1 O4 2.267(3) 1_455 ?
Cd1 O5 2.192(3) 1_454 ?
Cd1 O7 2.305(3) 1_444 ?
Cd1 O8 2.357(3) 1_444 ?
Cd2 O2 2.241(4) 2_466 ?
Cd2 O2 2.241(4) . ?
Cd2 O4 2.297(3) 2_566 ?
Cd2 O4 2.297(3) 1_455 ?
Cd2 O6 2.242(3) 2_567 ?
Cd2 O6 2.242(3) 1_454 ?
N1 N2 1.247(5) . ?
N1 O9 1.272(7) . ?
N2 O10 1.320(13) . ?
O4 Cd1 2.267(3) 1_655 ?
O4 Cd2 2.297(3) 1_655 ?
O5 Cd1 2.192(3) 1_656 ?
O6 Cd2 2.242(3) 1_656 ?
O7 Cd1 2.305(3) 1_666 ?
O8 Cd1 2.357(3) 1_666 ?
C17 N3 1.405(10) . ?
C18 N3 1.394(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 118.6(4) . . ?
O2 C1 C2 117.1(4) . . ?
O2 C1 O1 124.3(4) . . ?
C3 C2 C1 118.8(4) . . ?
C7 C2 C1 121.0(4) . . ?
C7 C2 C3 120.1(4) . . ?
C4 C3 C2 119.1(4) . . ?
C3 C4 C5 121.9(4) . . ?
C3 C4 N1 117.8(4) . . ?
C5 C4 N1 120.2(4) . . ?
C4 C5 C6 118.6(4) . . ?
C5 C6 C7 120.2(4) . . ?
C5 C6 C8 119.7(4) . . ?
C7 C6 C8 120.1(4) . . ?
C2 C7 C6 120.0(4) . . ?
O3 C8 C6 120.7(4) . . ?
O3 C8 O4 121.4(4) . . ?
O4 C8 C6 117.9(3) . . ?
C10 C9 N2 121.7(4) . . ?
C14 C9 C10 121.3(4) . . ?
C14 C9 N2 116.8(4) . . ?
C11 C10 C9 118.9(4) . . ?
C10 C11 C12 120.0(4) . . ?
C10 C11 C16 119.6(4) . . ?
C12 C11 C16 120.4(4) . . ?
C13 C12 C11 120.5(4) . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 C15 120.6(4) . . ?
C14 C13 C15 119.8(4) . . ?
C9 C14 C13 119.6(4) . . ?
O5 C15 C13 116.6(4) . . ?
O6 C15 C13 117.9(4) . . ?
O6 C15 O5 125.5(4) . . ?
C11 C16 Cd1 177.7(3) . 1_666 ?
O7 C16 C11 119.1(4) . . ?
O7 C16 Cd1 59.9(2) . 1_666 ?
O7 C16 O8 122.1(4) . . ?
O8 C16 C11 118.8(4) . . ?
O8 C16 Cd1 62.2(2) . 1_666 ?
O1 Cd1 C16 99.92(15) . 1_444 ?
O1 Cd1 O4 115.76(12) . 1_455 ?
O1 Cd1 O7 105.16(15) . 1_444 ?
O1 Cd1 O8 91.76(15) . 1_444 ?
O4 Cd1 C16 118.00(13) 1_455 1_444 ?
O4 Cd1 O7 132.82(13) 1_455 1_444 ?
O4 Cd1 O8 99.06(13) 1_455 1_444 ?
O5 Cd1 C16 125.38(14) 1_454 1_444 ?
O5 Cd1 O1 100.37(15) 1_454 . ?
O5 Cd1 O4 97.07(13) 1_454 1_455 ?
O5 Cd1 O7 97.69(12) 1_454 1_444 ?
O5 Cd1 O8 153.14(12) 1_454 1_444 ?
O7 Cd1 C16 27.84(14) 1_444 1_444 ?
O7 Cd1 O8 55.79(12) 1_444 1_444 ?
O8 Cd1 C16 27.95(14) 1_444 1_444 ?
O2 Cd2 O2 180.0 . 2_466 ?
O2 Cd2 O4 81.06(13) 2_466 2_566 ?
O2 Cd2 O4 98.94(13) 2_466 1_455 ?
O2 Cd2 O4 81.06(13) . 1_455 ?
O2 Cd2 O4 98.94(13) . 2_566 ?
O2 Cd2 O6 92.33(15) . 1_454 ?
O2 Cd2 O6 87.67(15) . 2_567 ?
O2 Cd2 O6 87.67(15) 2_466 1_454 ?
O2 Cd2 O6 92.33(15) 2_466 2_567 ?
O4 Cd2 O4 180.00(17) 1_455 2_566 ?
O6 Cd2 O4 89.06(12) 2_567 2_566 ?
O6 Cd2 O4 90.94(12) 2_567 1_455 ?
O6 Cd2 O4 90.94(12) 1_454 2_566 ?
O6 Cd2 O4 89.06(12) 1_454 1_455 ?
O6 Cd2 O6 180.0 2_567 1_454 ?
N2 N1 C4 116.3(4) . . ?
N2 N1 O9 125.3(4) . . ?
O9 N1 C4 117.1(4) . . ?
N1 N2 C9 117.2(4) . . ?
N1 N2 O10 118.8(7) . . ?
O10 N2 C9 115.2(6) . . ?
C1 O1 Cd1 109.8(3) . . ?
C1 O2 Cd2 145.6(3) . . ?
C8 O4 Cd1 103.2(2) . 1_655 ?
C8 O4 Cd2 138.6(3) . 1_655 ?
Cd1 O4 Cd2 100.62(11) 1_655 1_655 ?
C15 O5 Cd1 120.0(3) . 1_656 ?
C15 O6 Cd2 144.1(3) . 1_656 ?
C16 O7 Cd1 92.3(3) . 1_666 ?
C16 O8 Cd1 89.8(3) . 1_666 ?
C18 N3 C17 131.5(19) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1478781'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_audit_creation_date             2016-08-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H12 Co3 N4 O18, H2 O, C13 H16 N2'
_chemical_formula_sum            'C45 H30 Co3 N6 O19'
_chemical_formula_weight         1135.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 O1 Co1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.6701(2)
_cell_length_b                   10.2782(2)
_cell_length_c                   11.9406(3)
_cell_angle_alpha                112.322(2)
_cell_angle_beta                 101.936(2)
_cell_angle_gamma                92.9815(19)
_cell_volume                     1062.88(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7018
_cell_measurement_temperature    288.85(12)
_cell_measurement_theta_max      71.1530
_cell_measurement_theta_min      4.6890
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             575
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15802
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.504
_diffrn_reflns_theta_min         4.128
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      288.85(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -31.00   63.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega   20.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -90.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega  -35.00   66.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -19.0000 -180.0000 101

#__ type_ start__ end____ width___ exp.time_
  4 omega   57.00  109.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000   90.0000 52

#__ type_ start__ end____ width___ exp.time_
  5 omega  -35.00   66.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -19.0000  -90.0000 101

#__ type_ start__ end____ width___ exp.time_
  6 omega    1.00   76.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000 -150.0000 75

#__ type_ start__ end____ width___ exp.time_
  7 omega   20.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  8 omega    1.00   76.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000  -30.0000 75

#__ type_ start__ end____ width___ exp.time_
  9 omega   40.00   98.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  110.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -120.0000 71

#__ type_ start__ end____ width___ exp.time_
 11 omega   39.00  110.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  150.0000 71

#__ type_ start__ end____ width___ exp.time_
 12 omega   91.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 85

#__ type_ start__ end____ width___ exp.time_
 13 omega   39.00  110.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   60.0000 71

#__ type_ start__ end____ width___ exp.time_
 14 omega   41.00  126.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 85

#__ type_ start__ end____ width___ exp.time_
 15 omega   38.00  116.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000 -150.0000 78

#__ type_ start__ end____ width___ exp.time_
 16 omega   38.00   91.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

#__ type_ start__ end____ width___ exp.time_
 17 omega   39.00  110.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -30.0000 71

#__ type_ start__ end____ width___ exp.time_
 18 omega   38.00   91.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

#__ type_ start__ end____ width___ exp.time_
 19 omega   38.00   91.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

#__ type_ start__ end____ width___ exp.time_
 20 omega   38.00   91.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

#__ type_ start__ end____ width___ exp.time_
 21 omega   91.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
 22 omega   40.00   98.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
 23 omega   91.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 85

#__ type_ start__ end____ width___ exp.time_
 24 omega   70.00  178.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  120.0000 108

#__ type_ start__ end____ width___ exp.time_
 25 omega   10.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
 26 omega   20.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   90.0000 84

#__ type_ start__ end____ width___ exp.time_
 27 omega   20.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
 28 omega  -31.00   53.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
 29 omega   10.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
 30 omega   10.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  -60.0000 94

#__ type_ start__ end____ width___ exp.time_
 31 omega   10.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -150.0000 94

#__ type_ start__ end____ width___ exp.time_
 32 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 95

#__ type_ start__ end____ width___ exp.time_
 33 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
 34 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 35 omega   91.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 85

#__ type_ start__ end____ width___ exp.time_
 36 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
 37 omega   87.00  178.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
 38 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 39 omega   70.00  178.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1568920000
_diffrn_orient_matrix_UB_12      -0.0096806000
_diffrn_orient_matrix_UB_13      -0.0061544000
_diffrn_orient_matrix_UB_21      0.0028298000
_diffrn_orient_matrix_UB_22      0.1278828000
_diffrn_orient_matrix_UB_23      -0.0373239000
_diffrn_orient_matrix_UB_31      0.0495481000
_diffrn_orient_matrix_UB_32      0.1018002000
_diffrn_orient_matrix_UB_33      0.1388026000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3675
_reflns_number_total             4104
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         4104
_refine_ls_number_restraints     330
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0508P)²+1.1550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1004
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C5A, C6, C6A, C7, C7A, C8, C9, C10, C11, C12, C13, C14,
 C15, C16, C18, C19, C20, C21, C17, C22, C23, C24, C25, C29, C28, C27, C26, N1,
 N1A, N2, N2A, N4, N3, O5, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O5)=Sof(N1)=Sof(N2)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7)=1-FVAR(1)
 Sof(O5A)=Sof(N1A)=Sof(N2A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=FVAR(1)
 Fixed Sof: O1W(0.5) H1Wa(0.5) H1Wb(0.5) C18(0.5) H18(0.5) C19(0.5) C20(0.5)
 H20(0.5) C21(0.5) H21(0.5) N4(0.5) H4(0.5) C17(0.5) H17(0.5) C22(0.5)
 H22a(0.5) H22b(0.5) C23(0.5) H23a(0.5) H23b(0.5) C24(0.5) H24a(0.5) H24b(0.5)
 C25(0.5) C29(0.5) H29(0.5) C28(0.5) H28(0.5) N3(0.5) H3a(0.5) C27(0.5)
 H27(0.5) C26(0.5) H26(0.5)
5.a Riding coordinates:
 O1W(H1Wa,H1Wb)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C5A(H5A), C7(H7), C7A(H7A), C10(H10), C12(H12), C14(H14),
 C18(H18), C20(H20), C21(H21), N4(H4), C17(H17), C29(H29), C28(H28), N3(H3a),
 C27(H27), C26(H26)
5.d Fitted hexagon refined as free rotating group:
 C18(C19,C20,C21,N4,C17), C25(C29,C28,N3,C27,C26)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co -0.53791(4) 0.20498(4) -0.74889(4) 0.01951(12) Uani 1 1 d . . . . .
Co2 Co -0.5000 0.5000 -0.5000 0.01583(14) Uani 1 2 d S T P . .
O1 O 0.4841(2) 0.5330(2) 0.33837(18) 0.0254(4) Uani 1 1 d . . . . .
O2 O 0.4173(2) 0.3342(2) 0.16345(19) 0.0286(4) Uani 1 1 d . . . . .
O3 O 0.4740(3) 1.0056(2) 0.3011(2) 0.0407(6) Uani 1 1 d . . . . .
O4 O 0.4078(2) 1.0055(2) 0.1147(2) 0.0313(5) Uani 1 1 d . . . . .
O5 O 0.0507(16) 0.5134(19) -0.1675(14) 0.062(4) Uani 0.289(9) 1 d . U . A 1
O5A O 0.0542(6) 0.5768(6) -0.1719(5) 0.0519(14) Uani 0.711(9) 1 d . U . A 2
O6 O -0.3271(2) 0.3980(2) -0.5144(2) 0.0322(5) Uani 1 1 d . . . . .
O7 O -0.3224(2) 0.2384(2) -0.7020(2) 0.0324(5) Uani 1 1 d . . . . .
O8 O 0.36366(19) 0.2922(2) -0.60821(18) 0.0225(4) Uani 1 1 d . . . . .
O9 O 0.1802(2) 0.1833(3) -0.7704(2) 0.0387(5) Uani 1 1 d . . . . .
N1 N 0.1583(9) 0.5259(10) -0.1575(10) 0.021(2) Uani 0.289(9) 1 d . U . A 1
N1A N 0.2647(5) 0.4789(4) -0.1851(4) 0.0286(11) Uani 0.711(9) 1 d . U . A 2
N2 N 0.1913(12) 0.4232(12) -0.2409(10) 0.025(2) Uani 0.289(9) 1 d . U . A 1
N2A N 0.1402(4) 0.4848(5) -0.2310(4) 0.0273(10) Uani 0.711(9) 1 d . U . A 2
C1 C 0.4362(3) 0.4677(3) 0.2235(3) 0.0210(5) Uani 1 1 d . U . . .
C2 C 0.3977(3) 0.5548(3) 0.1482(3) 0.0230(6) Uani 1 1 d . U . . .
C3 C 0.4282(3) 0.7024(3) 0.2022(3) 0.0230(5) Uani 1 1 d . U . . .
H3 H 0.4711 0.7500 0.2890 0.028 Uiso 1 1 calc R . . . .
C4 C 0.3963(3) 0.7807(3) 0.1296(3) 0.0237(6) Uani 1 1 d . U . . .
C5 C 0.307(2) 0.726(2) 0.0195(17) 0.024(4) Uani 0.289(9) 1 d . U . A 1
H5 H 0.2772 0.7845 -0.0232 0.029 Uiso 0.289(9) 1 calc R . . A 1
C5A C 0.3399(9) 0.7063(8) -0.0024(6) 0.0242(16) Uani 0.711(9) 1 d . U . A 2
H5A H 0.3214 0.7572 -0.0545 0.029 Uiso 0.711(9) 1 calc R . . A 2
C6 C 0.2572(14) 0.5822(12) -0.0347(10) 0.019(2) Uani 0.289(9) 1 d . U . A 1
C6A C 0.3129(6) 0.5598(5) -0.0529(4) 0.0220(10) Uani 0.711(9) 1 d . U . A 2
C7 C 0.2997(18) 0.496(2) 0.0265(17) 0.024(4) Uani 0.289(9) 1 d . U . A 1
H7 H 0.2644 0.3969 -0.0117 0.028 Uiso 0.289(9) 1 calc R . . A 1
C7A C 0.3456(8) 0.4827(8) 0.0200(7) 0.0250(15) Uani 0.711(9) 1 d . U . A 2
H7A H 0.3325 0.3818 -0.0173 0.030 Uiso 0.711(9) 1 calc R . . A 2
C8 C 0.4290(3) 0.9398(3) 0.1871(3) 0.0249(6) Uani 1 1 d . U . . .
C9 C 0.0932(3) 0.3991(4) -0.3663(3) 0.0319(7) Uani 1 1 d . U . . .
C10 C 0.1848(3) 0.3515(3) -0.4434(3) 0.0275(6) Uani 1 1 d . U . . .
H10 H 0.2838 0.3574 -0.4089 0.033 Uiso 1 1 calc R . . . .
C11 C 0.1302(3) 0.2949(3) -0.5719(2) 0.0196(5) Uani 1 1 d . U . . .
C12 C -0.0164(3) 0.2811(3) -0.6211(2) 0.0191(5) Uani 1 1 d . U . . .
H12 H -0.0544 0.2399 -0.7090 0.023 Uiso 1 1 calc R . . . .
C13 C -0.1072(3) 0.3273(3) -0.5419(3) 0.0208(5) Uani 1 1 d . U . . .
C14 C -0.0516(3) 0.3888(3) -0.4140(3) 0.0273(6) Uani 1 1 d . U . . .
H14 H -0.1125 0.4235 -0.3595 0.033 Uiso 1 1 calc R . . . .
C15 C -0.2643(3) 0.3208(3) -0.5904(3) 0.0219(6) Uani 1 1 d . U . . .
C16 C 0.2284(3) 0.2540(3) -0.6576(3) 0.0221(5) Uani 1 1 d . U . . .
O1W O 1.3125(8) 0.9678(12) 0.4804(8) 0.114(4) Uani 0.5 1 d . . . B -1
H1WA H 1.3260 0.9283 0.4092 0.171 Uiso 0.5 1 d R . . B -1
H1WB H 1.3685 0.9786 0.5384 0.171 Uiso 0.5 1 d R . . B -1
C18 C 1.0485(6) 0.8434(8) 0.1570(6) 0.058(3) Uani 0.5 1 d . U . C -1
H18 H 1.1394 0.8124 0.1675 0.069 Uiso 0.5 1 calc R . . C -1
C19 C 0.9934(6) 0.9087(6) 0.2602(4) 0.0317(14) Uani 0.5 1 d G U . C -1
C20 C 0.8605(7) 0.9539(6) 0.2448(5) 0.037(2) Uani 0.5 1 d G U . C -1
H20 H 0.8228 0.9986 0.3153 0.044 Uiso 0.5 1 calc R . . C -1
C21 C 0.7827(6) 0.9339(8) 0.1263(6) 0.0331(18) Uani 0.5 1 d G U . C -1
H21 H 0.6918 0.9649 0.1158 0.040 Uiso 0.5 1 calc R . . C -1
N4 N 0.8378(8) 0.8686(10) 0.0232(4) 0.043(2) Uani 0.5 1 d G U . C -1
H4 H 0.7886 0.8559 -0.0518 0.052 Uiso 0.5 1 calc R . . C -1
C17 C 0.9708(8) 0.8233(10) 0.0386(5) 0.074(5) Uani 0.5 1 d G U . C -1
H17 H 1.0085 0.7787 -0.0319 0.089 Uiso 0.5 1 calc R . . C -1
C22 C 1.0940(8) 0.9415(7) 0.3835(6) 0.0376(14) Uani 0.5 1 d . U . C -1
H22A H 1.1764 1.0093 0.3925 0.045 Uiso 0.5 1 calc R . . C -1
H22B H 1.1309 0.8527 0.3813 0.045 Uiso 0.5 1 calc R . . C -1
C23 C 1.0378(6) 1.0029(8) 0.4998(7) 0.0313(15) Uani 0.5 1 d . U . C -1
H23A H 0.9632 0.9322 0.4985 0.038 Uiso 0.5 1 calc R . . C -1
H23B H 0.9941 1.0885 0.5016 0.038 Uiso 0.5 1 calc R . . C -1
C24 C 1.1600(7) 1.0423(7) 0.6164(6) 0.0371(14) Uani 0.5 1 d . U . C -1
H24A H 1.2113 0.9593 0.6064 0.044 Uiso 0.5 1 calc R . . C -1
H24B H 1.2280 1.1203 0.6204 0.044 Uiso 0.5 1 calc R . . C -1
C25 C 1.1191(8) 1.0873(6) 0.7377(5) 0.0341(18) Uani 0.5 1 d . U . C -1
C29 C 1.0106(7) 1.1684(8) 0.7658(5) 0.054(2) Uani 0.5 1 d G U . C -1
H29 H 0.9524 1.1916 0.7036 0.065 Uiso 0.5 1 calc R . . C -1
C28 C 0.9875(7) 1.2156(7) 0.8851(6) 0.056(3) Uani 0.5 1 d G U . C -1
H28 H 0.9133 1.2710 0.9043 0.067 Uiso 0.5 1 calc R . . C -1
N3 N 1.0728(8) 1.1817(7) 0.9762(4) 0.0422(17) Uani 0.5 1 d G U . C -1
H3A H 1.0581 1.2116 1.0517 0.051 Uiso 0.5 1 calc R . . C -1
C27 C 1.1812(9) 1.1006(9) 0.9481(5) 0.034(2) Uani 0.5 1 d G U . C -1
H27 H 1.2395 1.0774 1.0103 0.041 Uiso 0.5 1 calc R . . C -1
C26 C 1.2044(8) 1.0534(8) 0.8288(7) 0.039(2) Uani 0.5 1 d G U . C -1
H26 H 1.2785 0.9980 0.8096 0.046 Uiso 0.5 1 calc R . . C -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 1.9941(19) 1_454 ?
Co1 O3 2.344(2) 1_444 ?
Co1 O4 2.033(2) 1_444 ?
Co1 O7 2.018(2) . ?
Co1 O8 2.0341(19) 1_455 ?
Co1 C8 2.518(3) 1_444 ?
Co2 O1 2.0601(18) 1_454 ?
Co2 O1 2.0601(18) 2_565 ?
Co2 O6 2.0218(19) 2_464 ?
Co2 O6 2.0218(19) . ?
Co2 O8 2.2083(19) 1_455 ?
Co2 O8 2.2083(18) 2_564 ?
O1 Co2 2.0601(18) 1_656 ?
O1 C1 1.245(3) . ?
O2 Co1 1.9941(19) 1_656 ?
O2 C1 1.266(3) . ?
O3 Co1 2.344(2) 1_666 ?
O3 C8 1.235(4) . ?
O4 Co1 2.033(2) 1_666 ?
O4 C8 1.277(3) . ?
O5 N1 1.018(16) . ?
O5A N2A 1.379(7) . ?
O6 C15 1.246(3) . ?
O7 C15 1.262(4) . ?
O8 Co1 2.0340(19) 1_655 ?
O8 Co2 2.2083(18) 1_655 ?
O8 C16 1.290(3) . ?
O9 C16 1.233(4) . ?
N1 N2 1.255(16) . ?
N1 C6 1.455(15) . ?
N1A N2A 1.230(7) . ?
N1A C6A 1.434(6) . ?
N2 C9 1.520(11) . ?
N2A C9 1.471(5) . ?
C1 C2 1.502(3) . ?
C2 C3 1.391(4) . ?
C2 C7 1.442(18) . ?
C2 C7A 1.388(8) . ?
C3 C4 1.393(4) . ?
C4 C5 1.31(2) . ?
C4 C5A 1.432(7) . ?
C4 C8 1.500(4) . ?
C5 C6 1.38(2) . ?
C5A C6A 1.380(8) . ?
C6 C7 1.38(2) . ?
C6A C7A 1.387(8) . ?
C8 Co1 2.518(3) 1_666 ?
C9 C10 1.383(4) . ?
C9 C14 1.380(4) . ?
C10 C11 1.388(4) . ?
C11 C12 1.395(4) . ?
C11 C16 1.498(4) . ?
C12 C13 1.391(4) . ?
C13 C14 1.383(4) . ?
C13 C15 1.498(4) . ?
C18 C19 1.3900 . ?
C18 C17 1.3900 . ?
C19 C20 1.3900 . ?
C19 C22 1.491(8) . ?
C20 C21 1.3900 . ?
C21 N4 1.3900 . ?
N4 C17 1.3900 . ?
C22 C23 1.519(10) . ?
C23 C24 1.530(9) . ?
C24 C25 1.488(8) . ?
C25 C29 1.3900 . ?
C25 C26 1.3900 . ?
C29 C28 1.3900 . ?
C28 N3 1.3900 . ?
N3 C27 1.3900 . ?
C27 C26 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O3 163.81(8) 1_454 1_444 ?
O2 Co1 O4 105.09(8) 1_454 1_444 ?
O2 Co1 O7 101.64(9) 1_454 . ?
O2 Co1 O8 98.75(8) 1_454 1_455 ?
O2 Co1 C8 135.11(9) 1_454 1_444 ?
O3 Co1 C8 29.15(9) 1_444 1_444 ?
O4 Co1 O3 59.39(8) 1_444 1_444 ?
O4 Co1 O8 125.94(8) 1_444 1_455 ?
O4 Co1 C8 30.25(9) 1_444 1_444 ?
O7 Co1 O3 87.86(9) . 1_444 ?
O7 Co1 O4 105.09(9) . 1_444 ?
O7 Co1 O8 116.62(8) . 1_455 ?
O7 Co1 C8 97.75(9) . 1_444 ?
O8 Co1 O3 88.40(8) 1_455 1_444 ?
O8 Co1 C8 107.98(9) 1_455 1_444 ?
O1 Co2 O1 180.0 1_454 2_565 ?
O1 Co2 O8 90.14(7) 1_454 2_564 ?
O1 Co2 O8 89.86(7) 2_565 2_564 ?
O1 Co2 O8 89.86(7) 1_454 1_455 ?
O1 Co2 O8 90.14(7) 2_565 1_455 ?
O6 Co2 O1 95.55(9) . 1_454 ?
O6 Co2 O1 84.45(9) 2_464 1_454 ?
O6 Co2 O1 84.45(9) . 2_565 ?
O6 Co2 O1 95.55(9) 2_464 2_565 ?
O6 Co2 O6 180.0 2_464 . ?
O6 Co2 O8 91.50(8) 2_464 1_455 ?
O6 Co2 O8 88.50(8) 2_464 2_564 ?
O6 Co2 O8 91.50(8) . 2_564 ?
O6 Co2 O8 88.50(8) . 1_455 ?
O8 Co2 O8 180.00(11) 2_564 1_455 ?
C1 O1 Co2 139.44(18) . 1_656 ?
C1 O2 Co1 120.95(18) . 1_656 ?
C8 O3 Co1 83.26(17) . 1_666 ?
C8 O4 Co1 96.41(18) . 1_666 ?
C15 O6 Co2 143.6(2) . . ?
C15 O7 Co1 115.92(18) . . ?
Co1 O8 Co2 101.14(7) 1_655 1_655 ?
C16 O8 Co1 106.21(17) . 1_655 ?
C16 O8 Co2 133.79(17) . 1_655 ?
O5 N1 N2 109.9(15) . . ?
O5 N1 C6 121.4(13) . . ?
N2 N1 C6 116.5(10) . . ?
N2A N1A C6A 114.9(4) . . ?
N1 N2 C9 108.7(9) . . ?
O5A N2A C9 119.7(4) . . ?
N1A N2A O5A 125.9(5) . . ?
N1A N2A C9 113.7(4) . . ?
O1 C1 O2 126.2(2) . . ?
O1 C1 C2 117.3(2) . . ?
O2 C1 C2 116.4(2) . . ?
C3 C2 C1 121.3(2) . . ?
C3 C2 C7 115.2(8) . . ?
C7 C2 C1 122.0(8) . . ?
C7A C2 C1 117.6(4) . . ?
C7A C2 C3 120.7(4) . . ?
C2 C3 C4 120.4(3) . . ?
C3 C4 C5A 118.8(4) . . ?
C3 C4 C8 120.6(3) . . ?
C5 C4 C3 121.7(10) . . ?
C5 C4 C8 115.6(10) . . ?
C5A C4 C8 120.4(4) . . ?
C4 C5 C6 120.0(17) . . ?
C6A C5A C4 119.1(6) . . ?
C5 C6 N1 118.0(12) . . ?
C5 C6 C7 120.6(14) . . ?
C7 C6 N1 121.4(11) . . ?
C5A C6A N1A 121.8(5) . . ?
C5A C6A C7A 121.6(5) . . ?
C7A C6A N1A 116.3(5) . . ?
C6 C7 C2 120.1(15) . . ?
C6A C7A C2 119.2(6) . . ?
O3 C8 Co1 67.59(15) . 1_666 ?
O3 C8 O4 120.9(3) . . ?
O3 C8 C4 121.1(3) . . ?
O4 C8 Co1 53.34(14) . 1_666 ?
O4 C8 C4 117.9(3) . . ?
C4 C8 Co1 171.0(2) . 1_666 ?
C10 C9 N2 100.3(5) . . ?
C10 C9 N2A 124.3(3) . . ?
C14 C9 N2 136.7(5) . . ?
C14 C9 N2A 113.4(3) . . ?
C14 C9 C10 121.6(3) . . ?
C9 C10 C11 119.2(3) . . ?
C10 C11 C12 119.7(2) . . ?
C10 C11 C16 120.3(2) . . ?
C12 C11 C16 120.0(2) . . ?
C13 C12 C11 120.3(2) . . ?
C12 C13 C15 122.2(2) . . ?
C14 C13 C12 119.8(2) . . ?
C14 C13 C15 117.9(2) . . ?
C9 C14 C13 119.4(3) . . ?
O6 C15 O7 125.4(3) . . ?
O6 C15 C13 115.9(3) . . ?
O7 C15 C13 118.7(2) . . ?
O8 C16 C11 117.4(2) . . ?
O9 C16 O8 122.2(3) . . ?
O9 C16 C11 120.4(2) . . ?
C19 C18 C17 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 C22 115.0(5) . . ?
C20 C19 C22 124.5(5) . . ?
C19 C20 C21 120.0 . . ?
N4 C21 C20 120.0 . . ?
C21 N4 C17 120.0 . . ?
N4 C17 C18 120.0 . . ?
C19 C22 C23 117.9(6) . . ?
C22 C23 C24 109.8(5) . . ?
C25 C24 C23 116.3(6) . . ?
C29 C25 C24 123.9(5) . . ?
C29 C25 C26 120.0 . . ?
C26 C25 C24 115.9(5) . . ?
C25 C29 C28 120.0 . . ?
N3 C28 C29 120.0 . . ?
C28 N3 C27 120.0 . . ?
N3 C27 C26 120.0 . . ?
C27 C26 C25 120.0 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1478782'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_audit_creation_date             2016-07-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H12 Mn3 N4 O18, C10 H10 N2, 2(H2 O)'
_chemical_formula_sum            'C42 H26 Mn3 N6 O20'
_chemical_formula_weight         1099.51
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 O1 N1 Mn1 Cl1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.7826(2)
_cell_length_b                   10.3101(2)
_cell_length_c                   12.1333(3)
_cell_angle_alpha                112.088(2)
_cell_angle_beta                 101.488(2)
_cell_angle_gamma                94.1132(18)
_cell_volume                     1096.64(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    11878
_cell_measurement_temperature    289.03(10)
_cell_measurement_theta_max      71.3850
_cell_measurement_theta_min      4.6550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             555
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20392
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.503
_diffrn_reflns_theta_min         4.055
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      289.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega    7.00  108.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   19.0000  150.0000 101

#__ type_ start__ end____ width___ exp.time_
  3 omega   20.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  150.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega    1.00   76.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000   60.0000 75

#__ type_ start__ end____ width___ exp.time_
  5 omega   55.00  109.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203 -178.0000   30.0000 54

#__ type_ start__ end____ width___ exp.time_
  6 omega  -31.00   53.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
  7 omega   20.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  8 omega  -31.00   63.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  9 omega  -32.00   56.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -38.0000 -120.0000 88

#__ type_ start__ end____ width___ exp.time_
 10 omega    1.00   76.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000 -180.0000 75

#__ type_ start__ end____ width___ exp.time_
 11 omega   38.00  116.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000    0.0000 78

#__ type_ start__ end____ width___ exp.time_
 12 omega   39.00  110.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 71

#__ type_ start__ end____ width___ exp.time_
 13 omega   39.00  110.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -150.0000 71

#__ type_ start__ end____ width___ exp.time_
 14 omega   87.00  178.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
 15 omega   38.00  116.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000  120.0000 78

#__ type_ start__ end____ width___ exp.time_
 16 omega  101.00  178.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  112.0000  -60.0000 77

#__ type_ start__ end____ width___ exp.time_
 17 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 85

#__ type_ start__ end____ width___ exp.time_
 18 omega   40.00  135.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 19 omega   38.00   91.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
 20 omega   38.00   91.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

#__ type_ start__ end____ width___ exp.time_
 21 omega   38.00   91.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
 22 omega   40.00   98.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 58

#__ type_ start__ end____ width___ exp.time_
 23 omega   37.00  146.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 109

#__ type_ start__ end____ width___ exp.time_
 24 omega   90.00  175.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -120.0000 85

#__ type_ start__ end____ width___ exp.time_
 25 omega   40.00  135.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
 26 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
 27 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
 28 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -120.0000 94

#__ type_ start__ end____ width___ exp.time_
 29 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
 30 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
 31 omega   57.00  109.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000  -30.0000 52

#__ type_ start__ end____ width___ exp.time_
 32 omega  -35.00   66.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -19.0000  -30.0000 101

#__ type_ start__ end____ width___ exp.time_
 33 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  150.0000 94

#__ type_ start__ end____ width___ exp.time_
 34 omega   57.00  109.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000   90.0000 52

#__ type_ start__ end____ width___ exp.time_
 35 omega   18.00  106.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   38.0000  -90.0000 88

#__ type_ start__ end____ width___ exp.time_
 36 omega   20.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 37 omega   20.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 38 omega   87.00  178.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 91

#__ type_ start__ end____ width___ exp.time_
 39 omega   70.00  178.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -180.0000 108

#__ type_ start__ end____ width___ exp.time_
 40 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 85

#__ type_ start__ end____ width___ exp.time_
 41 omega   90.00  145.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 55

#__ type_ start__ end____ width___ exp.time_
 42 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
 43 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
 44 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -90.0000 85

#__ type_ start__ end____ width___ exp.time_
 45 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 46 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 47 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
 48 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 85

#__ type_ start__ end____ width___ exp.time_
 49 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0319963000
_diffrn_orient_matrix_UB_12      0.0197501000
_diffrn_orient_matrix_UB_13      0.1354139000
_diffrn_orient_matrix_UB_21      0.1511231000
_diffrn_orient_matrix_UB_22      0.0735290000
_diffrn_orient_matrix_UB_23      0.0204740000
_diffrn_orient_matrix_UB_31      -0.0515114000
_diffrn_orient_matrix_UB_32      0.1445814000
_diffrn_orient_matrix_UB_33      0.0348693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4007
_reflns_number_total             4219
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0425
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0802P)²+0.8834P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1298
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C21-C20 = C20-C19 = C19-C18 = C18-C17
 1.38 with sigma of 0.01
 C22-C23 = C23-C24 = C22-C26 = C26-C25
 1.38 with sigma of 0.01
 C21-N3 = N3-C17 = C24-N4 = N4-C25
 1.34 with sigma of 0.01
3. Rigid bond restraints
 C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, N3, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O9(0.5) O10(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5) C19(0.5)
 C20(0.5) H20(0.5) C21(0.5) H21(0.5) C22(0.5) C23(0.5) H23(0.5) C24(0.5)
 H24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) N3(0.5) H3a(0.5) N4(0.5) H4(0.5)
 O2W(0.5) H2Wa(0.5) H2Wb(0.5) O1W(0.5) H1Wa(0.5) H1Wb(0.5)
6.a Riding coordinates:
 O2W(H2Wa,H2Wb), O1W(H1Wa,H1Wb)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), N3(H3a), N4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7670(3) 0.6969(3) 0.6007(3) 0.0306(6) Uani 1 1 d . . . . .
C2 C 0.6118(3) 0.6798(3) 0.5470(2) 0.0253(5) Uani 1 1 d . . . . .
C3 C 0.5606(3) 0.6131(3) 0.4204(2) 0.0289(5) Uani 1 1 d . . . . .
H3 H 0.6218 0.5794 0.3703 0.035 Uiso 1 1 calc R . . . .
C4 C 0.4177(3) 0.5977(3) 0.3702(2) 0.0278(5) Uani 1 1 d . . . . .
C5 C 0.3231(3) 0.6442(3) 0.4423(2) 0.0253(5) Uani 1 1 d . . . . .
H5 H 0.2273 0.6334 0.4068 0.030 Uiso 1 1 calc R . . . .
C6 C 0.3747(3) 0.7073(3) 0.5688(2) 0.0237(5) Uani 1 1 d . . . . .
C7 C 0.5192(3) 0.7262(3) 0.6211(2) 0.0256(5) Uani 1 1 d . . . . .
H7 H 0.5535 0.7701 0.7058 0.031 Uiso 1 1 calc R . . . .
C8 C 0.2741(3) 0.7529(3) 0.6490(2) 0.0282(5) Uani 1 1 d . . . . .
C9 C 0.2037(3) 0.4667(3) 0.0590(2) 0.0307(6) Uani 1 1 d . . . . .
C10 C 0.1776(3) 0.3194(3) 0.0111(3) 0.0319(6) Uani 1 1 d . . . . .
H10 H 0.1997 0.2710 0.0617 0.038 Uiso 1 1 calc R . . . .
C11 C 0.1178(3) 0.2456(3) -0.1138(3) 0.0297(6) Uani 1 1 d . . . . .
C12 C 0.0855(3) 0.3190(3) -0.1892(2) 0.0293(6) Uani 1 1 d . . . . .
H12 H 0.0478 0.2693 -0.2730 0.035 Uiso 1 1 calc R . . . .
C13 C 0.1098(3) 0.4667(3) -0.1388(2) 0.0271(5) Uani 1 1 d . . . . .
C14 C 0.1680(3) 0.5407(3) -0.0140(2) 0.0301(6) Uani 1 1 d . . . . .
H14 H 0.1828 0.6393 0.0203 0.036 Uiso 1 1 calc R . . . .
C15 C 0.0887(3) 0.0868(3) -0.1674(3) 0.0322(6) Uani 1 1 d . . . . .
C16 C 0.0699(3) 0.5470(3) -0.2180(2) 0.0280(5) Uani 1 1 d . . . . .
Mn1 Mn 1.04286(4) 0.81502(4) 0.74738(4) 0.02540(15) Uani 1 1 d . . . . .
Mn2 Mn 1.0000 0.5000 0.5000 0.02074(16) Uani 1 2 d S T P . .
N1 N 0.3676(3) 0.5197(3) 0.2384(2) 0.0374(6) Uani 1 1 d . . . . .
N2 N 0.2589(3) 0.5491(3) 0.1879(2) 0.0398(6) Uani 1 1 d . . . . .
O1 O 0.8178(2) 0.7803(3) 0.7100(2) 0.0473(6) Uani 1 1 d . . . . .
O2 O 0.8386(2) 0.6280(3) 0.5314(2) 0.0473(6) Uani 1 1 d . . . . .
O3 O 0.3187(2) 0.8336(3) 0.7587(2) 0.0498(6) Uani 1 1 d . . . . .
O4 O 0.14225(19) 0.7089(2) 0.60051(18) 0.0296(4) Uani 1 1 d . . . . .
O5 O 0.1039(3) 0.0222(2) -0.0975(2) 0.0444(5) Uani 1 1 d . . . . .
O6 O 0.0492(3) 0.0198(2) -0.2817(2) 0.0429(5) Uani 1 1 d . . . . .
O7 O 0.0217(2) 0.4773(2) -0.33006(18) 0.0386(5) Uani 1 1 d . . . . .
O8 O 0.0868(2) 0.6801(2) -0.16382(19) 0.0387(5) Uani 1 1 d . . . . .
O9 O 0.4506(5) 0.4504(6) 0.1813(4) 0.0569(15) Uani 0.5 1 d . . . . .
O10 O 0.2407(9) 0.6808(7) 0.2286(6) 0.084(2) Uani 0.5 1 d . . . . .
C17 C 0.3054(9) -0.0752(9) 0.0807(8) 0.065(2) Uani 0.5 1 d D U . A -1
H17 H 0.2250 -0.0425 0.0528 0.078 Uiso 0.5 1 calc R . . A -1
C18 C 0.3489(8) -0.0506(8) 0.2050(7) 0.0586(18) Uani 0.5 1 d D U . A -1
H18 H 0.2965 -0.0050 0.2601 0.070 Uiso 0.5 1 calc R . . A -1
C19 C 0.4712(9) -0.0959(8) 0.2432(7) 0.063(2) Uani 0.5 1 d D U . A -1
C20 C 0.5359(9) -0.1739(10) 0.1566(7) 0.071(2) Uani 0.5 1 d D U . A -1
H20 H 0.6168 -0.2089 0.1799 0.086 Uiso 0.5 1 calc R . . A -1
C21 C 0.4835(9) -0.2010(11) 0.0368(8) 0.089(3) Uani 0.5 1 d D U . A -1
H21 H 0.5239 -0.2612 -0.0220 0.107 Uiso 0.5 1 calc R . . A -1
C22 C 0.5506(8) -0.0535(7) 0.3772(6) 0.0488(16) Uani 0.5 1 d D U . A -1
C23 C 0.6923(8) -0.0392(9) 0.4224(8) 0.0634(19) Uani 0.5 1 d D U . A -1
H23 H 0.7515 -0.0610 0.3690 0.076 Uiso 0.5 1 calc R . . A -1
C24 C 0.7478(10) 0.0068(10) 0.5448(9) 0.085(3) Uani 0.5 1 d D U . A -1
H24 H 0.8450 0.0168 0.5743 0.102 Uiso 0.5 1 calc R . . A -1
C25 C 0.5288(14) 0.0280(18) 0.5850(9) 0.074(3) Uani 0.5 1 d D U . A -1
H25 H 0.4735 0.0546 0.6415 0.089 Uiso 0.5 1 calc R . . A -1
C26 C 0.4681(14) -0.0223(14) 0.4609(8) 0.068(3) Uani 0.5 1 d D U . A -1
H26 H 0.3703 -0.0353 0.4333 0.082 Uiso 0.5 1 calc R . . A -1
N3 N 0.3785(8) -0.1448(8) 0.0031(6) 0.0702(19) Uani 0.5 1 d D U . A -1
H3A H 0.3554 -0.1525 -0.0715 0.084 Uiso 0.5 1 calc R . . A -1
N4 N 0.6672(12) 0.0375(9) 0.6222(8) 0.096(3) Uani 0.5 1 d D U . A -1
H4 H 0.7051 0.0646 0.6992 0.115 Uiso 0.5 1 calc R . . A -1
O2W O 0.1600(11) 0.024(2) 0.5094(13) 0.191(8) Uani 0.5 1 d . . . B -1
H2WA H 0.1823 0.0605 0.5892 0.286 Uiso 0.5 1 d R . . B -1
H2WB H 0.0687 0.0116 0.4826 0.286 Uiso 0.5 1 d R . . B -1
O1W O 0.7568(12) 0.0712(10) 0.8632(9) 0.114(3) Uani 0.5 1 d . . . C -1
H1WA H 0.7606 -0.0157 0.8337 0.171 Uiso 0.5 1 d R . . C -1
H1WB H 0.7871 0.0890 0.9352 0.171 Uiso 0.5 1 d R . . C -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.497(3) . ?
C1 O1 1.251(4) . ?
C1 O2 1.249(4) . ?
C2 C3 1.390(4) . ?
C2 C7 1.386(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.381(4) . ?
C4 C5 1.388(4) . ?
C4 N1 1.451(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.388(3) . ?
C6 C7 1.396(4) . ?
C6 C8 1.497(4) . ?
C7 H7 0.9300 . ?
C8 O3 1.240(3) . ?
C8 O4 1.276(3) . ?
C9 C10 1.389(4) . ?
C9 C14 1.383(4) . ?
C9 N2 1.435(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.391(4) . ?
C11 C12 1.395(4) . ?
C11 C15 1.498(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.392(4) . ?
C13 C14 1.387(4) . ?
C13 C16 1.503(4) . ?
C14 H14 0.9300 . ?
C15 Mn1 2.565(3) 1_444 ?
C15 O5 1.255(4) . ?
C15 O6 1.255(4) . ?
C16 O7 1.245(3) . ?
C16 O8 1.260(3) . ?
Mn1 C15 2.564(3) 1_666 ?
Mn1 O1 2.132(2) . ?
Mn1 O4 2.1667(19) 1_655 ?
Mn1 O5 2.193(2) 1_666 ?
Mn1 O6 2.266(2) 1_666 ?
Mn1 O8 2.076(2) 1_656 ?
Mn2 O2 2.131(2) 2_766 ?
Mn2 O2 2.131(2) . ?
Mn2 O4 2.2319(18) 1_655 ?
Mn2 O4 2.2319(18) 2_666 ?
Mn2 O7 2.1323(19) 2_665 ?
Mn2 O7 2.1323(19) 1_656 ?
N1 N2 1.235(4) . ?
N1 O9 1.259(5) . ?
N2 O10 1.297(7) . ?
O4 Mn1 2.1667(19) 1_455 ?
O4 Mn2 2.2319(18) 1_455 ?
O5 Mn1 2.193(2) 1_444 ?
O6 Mn1 2.266(2) 1_444 ?
O7 Mn2 2.1323(19) 1_454 ?
O8 Mn1 2.076(2) 1_454 ?
C17 H17 0.9300 . ?
C17 C18 1.400(8) . ?
C17 N3 1.322(8) . ?
C18 H18 0.9300 . ?
C18 C19 1.373(8) . ?
C19 C20 1.362(8) . ?
C19 C22 1.533(10) . ?
C20 H20 0.9300 . ?
C20 C21 1.353(8) . ?
C21 H21 0.9300 . ?
C21 N3 1.286(8) . ?
C22 C23 1.361(8) . ?
C22 C26 1.380(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.356(8) . ?
C24 H24 0.9300 . ?
C24 N4 1.308(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.379(9) . ?
C25 N4 1.323(9) . ?
C26 H26 0.9300 . ?
N3 H3A 0.8600 . ?
N4 H4 0.8600 . ?
O2W H2WA 0.8699 . ?
O2W H2WB 0.8701 . ?
O1W H1WA 0.8373 . ?
O1W H1WB 0.8092 . ?

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 C2 119.0(3) . . ?
O2 C1 C2 117.1(3) . . ?
O2 C1 O1 123.9(3) . . ?
C3 C2 C1 118.7(2) . . ?
C7 C2 C1 121.2(2) . . ?
C7 C2 C3 120.0(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.1(2) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 122.0(2) . . ?
C3 C4 N1 117.3(2) . . ?
C5 C4 N1 120.6(2) . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.5(2) . . ?
C6 C5 H5 120.8 . . ?
C5 C6 C7 120.3(2) . . ?
C5 C6 C8 119.6(2) . . ?
C7 C6 C8 120.2(2) . . ?
C2 C7 C6 120.1(2) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
O3 C8 C6 120.4(2) . . ?
O3 C8 O4 121.5(3) . . ?
O4 C8 C6 118.1(2) . . ?
C10 C9 N2 121.5(2) . . ?
C14 C9 C10 121.5(2) . . ?
C14 C9 N2 116.8(2) . . ?
C9 C10 H10 120.6 . . ?
C9 C10 C11 118.8(2) . . ?
C11 C10 H10 120.6 . . ?
C10 C11 C12 120.3(2) . . ?
C10 C11 C15 119.7(2) . . ?
C12 C11 C15 120.1(2) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.0(2) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C16 120.5(2) . . ?
C14 C13 C12 120.0(2) . . ?
C14 C13 C16 119.5(2) . . ?
C9 C14 C13 119.5(2) . . ?
C9 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C11 C15 Mn1 178.2(2) . 1_444 ?
O5 C15 C11 119.5(3) . . ?
O5 C15 Mn1 58.72(15) . 1_444 ?
O5 C15 O6 120.8(3) . . ?
O6 C15 C11 119.7(3) . . ?
O6 C15 Mn1 62.04(15) . 1_444 ?
O7 C16 C13 117.8(2) . . ?
O7 C16 O8 125.8(2) . . ?
O8 C16 C13 116.4(2) . . ?
O1 Mn1 C15 99.41(9) . 1_666 ?
O1 Mn1 O4 118.56(9) . 1_655 ?
O1 Mn1 O5 103.39(10) . 1_666 ?
O1 Mn1 O6 92.76(10) . 1_666 ?
O4 Mn1 C15 115.24(8) 1_655 1_666 ?
O4 Mn1 O5 131.68(8) 1_655 1_666 ?
O4 Mn1 O6 94.72(8) 1_655 1_666 ?
O5 Mn1 C15 29.27(9) 1_666 1_666 ?
O5 Mn1 O6 58.57(8) 1_666 1_666 ?
O6 Mn1 C15 29.30(9) 1_666 1_666 ?
O8 Mn1 C15 129.86(9) 1_656 1_666 ?
O8 Mn1 O1 99.45(10) 1_656 . ?
O8 Mn1 O4 95.03(8) 1_656 1_655 ?
O8 Mn1 O5 100.93(8) 1_656 1_666 ?
O8 Mn1 O6 158.34(9) 1_656 1_666 ?
O2 Mn2 O2 180.0 2_766 . ?
O2 Mn2 O4 97.08(9) 2_766 1_655 ?
O2 Mn2 O4 82.92(9) 2_766 2_666 ?
O2 Mn2 O4 97.08(9) . 2_666 ?
O2 Mn2 O4 82.92(9) . 1_655 ?
O2 Mn2 O7 93.31(9) 2_766 2_665 ?
O2 Mn2 O7 93.31(9) . 1_656 ?
O2 Mn2 O7 86.69(9) 2_766 1_656 ?
O2 Mn2 O7 86.69(9) . 2_665 ?
O4 Mn2 O4 180.0 1_655 2_666 ?
O7 Mn2 O4 88.66(8) 2_665 2_666 ?
O7 Mn2 O4 91.34(8) 1_656 2_666 ?
O7 Mn2 O4 91.34(8) 2_665 1_655 ?
O7 Mn2 O4 88.66(8) 1_656 1_655 ?
O7 Mn2 O7 180.0 2_665 1_656 ?
N2 N1 C4 116.7(2) . . ?
N2 N1 O9 123.6(3) . . ?
O9 N1 C4 118.0(3) . . ?
N1 N2 C9 117.1(2) . . ?
N1 N2 O10 117.7(4) . . ?
O10 N2 C9 116.6(4) . . ?
C1 O1 Mn1 109.8(2) . . ?
C1 O2 Mn2 150.2(2) . . ?
C8 O4 Mn1 103.98(16) . 1_455 ?
C8 O4 Mn2 137.02(17) . 1_455 ?
Mn1 O4 Mn2 102.11(7) 1_455 1_455 ?
C15 O5 Mn1 92.01(17) . 1_444 ?
C15 O6 Mn1 88.66(17) . 1_444 ?
C16 O7 Mn2 140.40(18) . 1_454 ?
C16 O8 Mn1 123.91(18) . 1_454 ?
C18 C17 H17 120.0 . . ?
N3 C17 H17 120.0 . . ?
N3 C17 C18 120.0(7) . . ?
C17 C18 H18 121.0 . . ?
C19 C18 C17 118.0(7) . . ?
C19 C18 H18 121.0 . . ?
C18 C19 C22 125.3(7) . . ?
C20 C19 C18 118.2(7) . . ?
C20 C19 C22 116.2(7) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.6(8) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 119.6 . . ?
N3 C21 C20 120.9(8) . . ?
N3 C21 H21 119.6 . . ?
C23 C22 C19 127.4(7) . . ?
C23 C22 C26 117.0(8) . . ?
C26 C22 C19 115.5(7) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.5(8) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 119.4 . . ?
N4 C24 C23 121.2(9) . . ?
N4 C24 H24 119.4 . . ?
C26 C25 H25 120.6 . . ?
N4 C25 H25 120.6 . . ?
N4 C25 C26 118.7(10) . . ?
C22 C26 H26 119.6 . . ?
C25 C26 C22 120.8(10) . . ?
C25 C26 H26 119.6 . . ?
C17 N3 H3A 119.2 . . ?
C21 N3 C17 121.5(7) . . ?
C21 N3 H3A 119.2 . . ?
C24 N4 C25 121.7(9) . . ?
C24 N4 H4 119.2 . . ?
C25 N4 H4 119.2 . . ?
H2WA O2W H2WB 109.5 . . ?
H1WA O1W H1WB 99.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -179.6(2) . . . . ?
C1 C2 C7 C6 -179.1(2) . . . . ?
C2 C1 O1 Mn1 -167.86(19) . . . . ?
C2 C1 O2 Mn2 -137.3(4) . . . . ?
C2 C3 C4 C5 -1.3(4) . . . . ?
C2 C3 C4 N1 -176.2(2) . . . . ?
C3 C2 C7 C6 -0.6(4) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C3 C4 N1 N2 -153.5(3) . . . . ?
C3 C4 N1 O9 12.2(5) . . . . ?
C4 C5 C6 C7 1.6(4) . . . . ?
C4 C5 C6 C8 -177.5(2) . . . . ?
C4 N1 N2 C9 -176.3(3) . . . . ?
C4 N1 N2 O10 36.8(6) . . . . ?
C5 C4 N1 N2 31.4(4) . . . . ?
C5 C4 N1 O9 -162.9(4) . . . . ?
C5 C6 C7 C2 -1.2(4) . . . . ?
C5 C6 C8 O3 -165.5(3) . . . . ?
C5 C6 C8 O4 12.9(4) . . . . ?
C6 C8 O4 Mn1 -175.79(19) . . . 1_455 ?
C6 C8 O4 Mn2 58.4(4) . . . 1_455 ?
C7 C2 C3 C4 1.8(4) . . . . ?
C7 C6 C8 O3 15.4(4) . . . . ?
C7 C6 C8 O4 -166.2(2) . . . . ?
C8 C6 C7 C2 177.9(2) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C9 C10 C11 C15 180.0(3) . . . . ?
C10 C9 C14 C13 -2.5(4) . . . . ?
C10 C9 N2 N1 52.6(4) . . . . ?
C10 C9 N2 O10 -160.1(5) . . . . ?
C10 C11 C12 C13 -1.7(4) . . . . ?
C10 C11 C15 O5 7.9(4) . . . . ?
C10 C11 C15 O6 -172.3(3) . . . . ?
C11 C12 C13 C14 0.9(4) . . . . ?
C11 C12 C13 C16 -177.4(2) . . . . ?
C11 C15 O5 Mn1 -179.5(2) . . . 1_444 ?
C11 C15 O6 Mn1 179.5(2) . . . 1_444 ?
C12 C11 C15 O5 -172.5(3) . . . . ?
C12 C11 C15 O6 7.4(4) . . . . ?
C12 C13 C14 C9 1.2(4) . . . . ?
C12 C13 C16 O7 -3.7(4) . . . . ?
C12 C13 C16 O8 175.5(3) . . . . ?
C13 C16 O7 Mn2 -156.1(2) . . . 1_454 ?
C13 C16 O8 Mn1 178.92(17) . . . 1_454 ?
C14 C9 C10 C11 1.8(4) . . . . ?
C14 C9 N2 N1 -132.0(3) . . . . ?
C14 C9 N2 O10 15.3(6) . . . . ?
C14 C13 C16 O7 178.0(3) . . . . ?
C14 C13 C16 O8 -2.9(4) . . . . ?
C15 C11 C12 C13 178.7(3) . . . . ?
C16 C13 C14 C9 179.5(3) . . . . ?
N1 C4 C5 C6 174.4(2) . . . . ?
N2 C9 C10 C11 177.0(3) . . . . ?
N2 C9 C14 C13 -178.0(3) . . . . ?
O1 C1 C2 C3 165.8(3) . . . . ?
O1 C1 C2 C7 -15.6(4) . . . . ?
O1 C1 O2 Mn2 44.3(6) . . . . ?
O2 C1 C2 C3 -12.7(4) . . . . ?
O2 C1 C2 C7 165.9(3) . . . . ?
O2 C1 O1 Mn1 10.5(4) . . . . ?
O3 C8 O4 Mn1 2.6(3) . . . 1_455 ?
O3 C8 O4 Mn2 -123.1(3) . . . 1_455 ?
O5 C15 O6 Mn1 -0.6(3) . . . 1_444 ?
O6 C15 O5 Mn1 0.7(3) . . . 1_444 ?
O7 C16 O8 Mn1 -2.0(4) . . . 1_454 ?
O8 C16 O7 Mn2 24.8(5) . . . 1_454 ?
O9 N1 N2 C9 18.9(6) . . . . ?
O9 N1 N2 O10 -128.0(6) . . . . ?
C17 C18 C19 C20 -6.2(12) . . . . ?
C17 C18 C19 C22 167.2(7) . . . . ?
C18 C17 N3 C21 5.6(13) . . . . ?
C18 C19 C20 C21 2.5(14) . . . . ?
C18 C19 C22 C23 -148.5(8) . . . . ?
C18 C19 C22 C26 29.2(12) . . . . ?
C19 C20 C21 N3 5.5(15) . . . . ?
C19 C22 C23 C24 176.4(8) . . . . ?
C19 C22 C26 C25 -174.8(8) . . . . ?
C20 C19 C22 C23 25.0(11) . . . . ?
C20 C19 C22 C26 -157.3(9) . . . . ?
C20 C21 N3 C17 -9.7(15) . . . . ?
C22 C19 C20 C21 -171.5(8) . . . . ?
C22 C23 C24 N4 0.5(14) . . . . ?
C23 C22 C26 C25 3.2(12) . . . . ?
C23 C24 N4 C25 -1.4(17) . . . . ?
C26 C22 C23 C24 -1.4(12) . . . . ?
C26 C25 N4 C24 3.2(17) . . . . ?
N3 C17 C18 C19 2.5(12) . . . . ?
N4 C25 C26 C22 -4.1(14) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
