# 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_jv65
_database_code_depnum_ccdc_archive 'CCDC 1441122'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H50 Br N4 O18 S2'
_chemical_formula_sum            'C52 H50 Br N4 O18 S2'
_chemical_formula_weight         1162.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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

_cell_length_a                   12.4860(10)
_cell_length_b                   14.7786(10)
_cell_length_c                   13.7673(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.077(3)
_cell_angle_gamma                90
_cell_volume                     2464.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    38298
_cell_measurement_theta_min      1.976
_cell_measurement_theta_max      28.383

_exptl_crystal_description       plates
_exptl_crystal_colour            'clear white'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_F_000             1202
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.003
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38298
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.976
_diffrn_reflns_theta_max         28.383
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6127
_reflns_number_gt                4444
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014/6 (Sheldrick, 2014)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0483P)²+1.2838P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6127
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.1009
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Br1 Br 0.0000 0.0000 0.0000 0.03336(10) Uani 1 2 d S . P . .
S11 S 0.54144(4) 0.42269(3) -0.13112(4) 0.01829(12) Uani 1 1 d . . . . .
N1 N 0.75735(14) 0.20555(12) -0.24868(13) 0.0211(4) Uani 1 1 d . . . . .
N2 N 0.71040(14) 0.32181(12) -0.75278(12) 0.0203(4) Uani 1 1 d . . . . .
O1 O 0.32663(13) -0.02975(12) -0.11326(13) 0.0321(4) Uani 1 1 d . . . . .
H1 H 0.2775 -0.0683 -0.1120 0.048 Uiso 1 1 calc R U . . .
O2 O 0.42350(14) -0.15233(11) -0.13629(13) 0.0350(4) Uani 1 1 d . . . . .
O3 O 1.08900(13) 0.64429(11) -0.86444(12) 0.0329(4) Uani 1 1 d . . . . .
O4 O 1.17168(12) 0.51419(10) -0.88804(12) 0.0276(4) Uani 1 1 d . . . . .
H4 H 1.2223 0.5489 -0.8957 0.041 Uiso 1 1 calc R U . . .
O11 O 0.53748(14) 0.51232(10) -0.17423(12) 0.0310(4) Uani 1 1 d . . . . .
O12 O 0.65506(11) 0.39078(11) -0.09358(11) 0.0264(3) Uani 1 1 d . . . . .
O13 O 0.47917(12) 0.35606(10) -0.20148(11) 0.0280(3) Uani 1 1 d . . . . .
O14 O 0.48745(13) 0.42717(10) -0.04354(11) 0.0260(3) Uani 1 1 d . . . . .
H14 H 0.4964 0.3777 -0.0126 0.039 Uiso 1 1 calc R U . . .
C1 C 0.41660(18) -0.07131(16) -0.12484(15) 0.0251(5) Uani 1 1 d . . . . .
C2 C 0.50874(18) -0.00619(14) -0.12418(15) 0.0218(4) Uani 1 1 d . . . . .
C3 C 0.49517(18) 0.08613(15) -0.11233(16) 0.0248(5) Uani 1 1 d . . . . .
H3 H 0.4276 0.1082 -0.1014 0.030 Uiso 1 1 calc R U . . .
C4 C 0.57885(19) 0.14612(15) -0.11631(16) 0.0256(5) Uani 1 1 d . . . . .
H4A H 0.5687 0.2091 -0.1083 0.031 Uiso 1 1 calc R U . . .
C5 C 0.67781(17) 0.11425(14) -0.13206(14) 0.0214(4) Uani 1 1 d . . . . .
C6 C 0.69268(18) 0.02122(15) -0.14160(16) 0.0240(5) Uani 1 1 d . . . . .
H6 H 0.7610 -0.0011 -0.1506 0.029 Uiso 1 1 calc R U . . .
C7 C 0.60831(18) -0.03848(15) -0.13804(15) 0.0236(4) Uani 1 1 d . . . . .
H7 H 0.6186 -0.1016 -0.1451 0.028 Uiso 1 1 calc R U . . .
C8 C 0.76730(19) 0.18053(15) -0.14084(15) 0.0257(5) Uani 1 1 d . . . . .
H8A H 0.7612 0.2357 -0.1018 0.031 Uiso 1 1 calc R U . . .
H8B H 0.8406 0.1531 -0.1126 0.031 Uiso 1 1 calc R U . . .
C9 C 0.68705(18) 0.27092(15) -0.29171(16) 0.0252(5) Uani 1 1 d . . . . .
H9 H 0.6448 0.3019 -0.2533 0.030 Uiso 1 1 calc R U . . .
C10 C 0.67538(18) 0.29358(14) -0.39036(16) 0.0235(4) Uani 1 1 d . . . . .
H10 H 0.6247 0.3396 -0.4198 0.028 Uiso 1 1 calc R U . . .
C11 C 0.73759(17) 0.24940(14) -0.44790(15) 0.0202(4) Uani 1 1 d . . . . .
C12 C 0.8086(2) 0.18148(16) -0.40108(17) 0.0297(5) Uani 1 1 d . . . . .
H12 H 0.8518 0.1491 -0.4375 0.036 Uiso 1 1 calc R U . . .
C13 C 0.81673(19) 0.16097(16) -0.30203(17) 0.0290(5) Uani 1 1 d . . . . .
H13 H 0.8654 0.1143 -0.2710 0.035 Uiso 1 1 calc R U . . .
C14 C 0.72830(17) 0.27455(14) -0.55473(15) 0.0202(4) Uani 1 1 d . . . . .
C15 C 0.6540(2) 0.33968(18) -0.60292(19) 0.0411(7) Uani 1 1 d . . . . .
H15 H 0.6075 0.3689 -0.5674 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6465(2) 0.36260(18) -0.70096(18) 0.0359(6) Uani 1 1 d . . . . .
H16 H 0.5956 0.4078 -0.7322 0.043 Uiso 1 1 calc R U . . .
C17 C 0.78210(18) 0.25839(15) -0.70897(16) 0.0248(5) Uani 1 1 d . . . . .
H17 H 0.8264 0.2293 -0.7468 0.030 Uiso 1 1 calc R U . . .
C18 C 0.79366(17) 0.23396(15) -0.61072(15) 0.0230(4) Uani 1 1 d . . . . .
H18 H 0.8463 0.1894 -0.5811 0.028 Uiso 1 1 calc R U . . .
C19 C 0.70313(18) 0.34745(16) -0.86002(15) 0.0245(5) Uani 1 1 d . . . . .
H19A H 0.6349 0.3828 -0.8864 0.029 Uiso 1 1 calc R U . . .
H19B H 0.6994 0.2920 -0.9010 0.029 Uiso 1 1 calc R U . . .
C20 C 0.80242(17) 0.40297(14) -0.86789(14) 0.0205(4) Uani 1 1 d . . . . .
C21 C 0.80074(17) 0.49684(15) -0.85805(15) 0.0227(4) Uani 1 1 d . . . . .
H21 H 0.7362 0.5259 -0.8486 0.027 Uiso 1 1 calc R U . . .
C22 C 0.89276(17) 0.54801(15) -0.86200(15) 0.0231(4) Uani 1 1 d . . . . .
H22 H 0.8908 0.6120 -0.8558 0.028 Uiso 1 1 calc R U . . .
C23 C 0.98780(17) 0.50583(14) -0.87502(14) 0.0196(4) Uani 1 1 d . . . . .
C24 C 1.08709(18) 0.56277(15) -0.87537(15) 0.0235(4) Uani 1 1 d . . . . .
C25 C 0.98827(17) 0.41235(15) -0.88688(15) 0.0223(4) Uani 1 1 d . . . . .
H25 H 1.0524 0.3832 -0.8973 0.027 Uiso 1 1 calc R U . . .
C26 C 0.89595(18) 0.36144(15) -0.88361(15) 0.0235(4) Uani 1 1 d . . . . .
H26 H 0.8970 0.2977 -0.8922 0.028 Uiso 1 1 calc R U . . .
O1W O 0.14832(13) -0.12389(11) -0.11204(12) 0.0322(4) Uani 1 1 d . . . . .
H1WA H 0.1056 -0.1192 -0.1692 0.048 Uiso 1 1 d R U . . .
H1WB H 0.1169 -0.0901 -0.0785 0.048 Uiso 1 1 d R U . . .


_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
S11 O11 1.4475(15) . ?
S11 O12 1.4648(15) . ?
S11 O13 1.4649(15) . ?
S11 O14 1.5193(15) . ?
N1 C13 1.337(3) . ?
N1 C9 1.342(3) . ?
N1 C8 1.506(3) . ?
N2 C17 1.335(3) . ?
N2 C16 1.336(3) . ?
N2 C19 1.505(3) . ?
O1 C1 1.323(3) . ?
O2 C1 1.214(3) . ?
O3 C24 1.214(3) . ?
O4 C24 1.323(3) . ?
C1 C2 1.498(3) . ?
C2 C7 1.387(3) . ?
C2 C3 1.389(3) . ?
C3 C4 1.381(3) . ?
C4 C5 1.388(3) . ?
C5 C6 1.398(3) . ?
C5 C8 1.513(3) . ?
C6 C7 1.384(3) . ?
C9 C10 1.372(3) . ?
C10 C11 1.399(3) . ?
C11 C12 1.390(3) . ?
C11 C14 1.494(3) . ?
C12 C13 1.376(3) . ?
C14 C18 1.388(3) . ?
C14 C15 1.388(3) . ?
C15 C16 1.373(3) . ?
C17 C18 1.373(3) . ?
C19 C20 1.512(3) . ?
C20 C26 1.382(3) . ?
C20 C21 1.394(3) . ?
C21 C22 1.388(3) . ?
C22 C23 1.390(3) . ?
C23 C25 1.391(3) . ?
C23 C24 1.499(3) . ?
C25 C26 1.386(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 S11 O12 111.89(9) . . ?
O11 S11 O13 112.60(10) . . ?
O12 S11 O13 109.25(9) . . ?
O11 S11 O14 107.94(9) . . ?
O12 S11 O14 108.22(9) . . ?
O13 S11 O14 106.71(9) . . ?
C13 N1 C9 120.17(18) . . ?
C13 N1 C8 119.80(18) . . ?
C9 N1 C8 120.01(17) . . ?
C17 N2 C16 119.83(18) . . ?
C17 N2 C19 119.59(17) . . ?
C16 N2 C19 120.58(18) . . ?
O2 C1 O1 124.2(2) . . ?
O2 C1 C2 123.8(2) . . ?
O1 C1 C2 111.98(19) . . ?
C7 C2 C3 119.5(2) . . ?
C7 C2 C1 119.39(19) . . ?
C3 C2 C1 121.07(19) . . ?
C4 C3 C2 120.7(2) . . ?
C3 C4 C5 119.9(2) . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 C8 119.73(19) . . ?
C6 C5 C8 120.78(19) . . ?
C7 C6 C5 120.3(2) . . ?
C6 C7 C2 120.1(2) . . ?
N1 C8 C5 110.64(17) . . ?
N1 C9 C10 120.88(19) . . ?
C9 C10 C11 120.5(2) . . ?
C12 C11 C10 117.01(19) . . ?
C12 C11 C14 121.62(18) . . ?
C10 C11 C14 121.37(18) . . ?
C13 C12 C11 120.2(2) . . ?
N1 C13 C12 121.3(2) . . ?
C18 C14 C15 116.68(19) . . ?
C18 C14 C11 121.59(18) . . ?
C15 C14 C11 121.73(18) . . ?
C16 C15 C14 121.3(2) . . ?
N2 C16 C15 120.5(2) . . ?
N2 C17 C18 121.87(19) . . ?
C17 C18 C14 119.89(19) . . ?
N2 C19 C20 110.61(16) . . ?
C26 C20 C21 119.36(19) . . ?
C26 C20 C19 120.59(19) . . ?
C21 C20 C19 120.05(19) . . ?
C22 C21 C20 120.4(2) . . ?
C21 C22 C23 120.1(2) . . ?
C22 C23 C25 119.25(19) . . ?
C22 C23 C24 118.76(19) . . ?
C25 C23 C24 122.00(19) . . ?
O3 C24 O4 124.2(2) . . ?
O3 C24 C23 123.2(2) . . ?
O4 C24 C23 112.52(19) . . ?
C26 C25 C23 120.5(2) . . ?
C20 C26 C25 120.3(2) . . ?

_refine_diff_density_max         0.892
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.071

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_da349_sq
_database_code_depnum_ccdc_archive 'CCDC 1441123'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 Br Cu N2 O4'
_chemical_formula_sum            'C26 H20 Br Cu N2 O4'
_chemical_formula_weight         567.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'

_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.
;

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

_cell_length_a                   13.2570(5)
_cell_length_b                   13.2570(5)
_cell_length_c                   31.1199(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5469.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    26392
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      28.529

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_F_000             2288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.291
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26392
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.670
_diffrn_reflns_theta_max         28.529
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3472
_reflns_number_gt                2307
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014/6 (Sheldrick, 2014)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1265P)²+8.0880P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.87(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3472
_refine_ls_number_parameters     156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0652
_refine_ls_wR_factor_ref         0.2188
_refine_ls_wR_factor_gt          0.1920
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cu1 Cu -1.5000 -1.5000 -0.04584(4) 0.0500(4) Uani 1 2 d S T P . .
Br1 Br -1.5000 -1.5000 -0.12868(4) 0.0824(5) Uani 1 2 d S T P . .
N1 N -1.2815(6) -0.8622(6) 0.0244(3) 0.0626(19) Uani 1 1 d . . . . .
O1 O -1.4534(5) -1.3639(4) -0.04378(19) 0.0577(14) Uani 1 1 d . . . . .
O2 O -1.4484(4) -1.3604(4) 0.0288(2) 0.0565(14) Uani 1 1 d . . . . .
C1 C -1.4360(6) -1.3216(6) -0.0082(3) 0.0548(19) Uani 1 1 d . . . . .
C2 C -1.3967(6) -1.2171(6) -0.0098(3) 0.0504(18) Uani 1 1 d . . . . .
C3 C -1.3474(7) -1.1746(7) 0.0245(3) 0.061(2) Uani 1 1 d . . . . .
H3 H -1.3373 -1.2131 0.0498 0.073 Uiso 1 1 calc R U . . .
C4 C -1.3115(7) -1.0749(7) 0.0226(3) 0.064(2) Uani 1 1 d . . . . .
H4 H -1.2774 -1.0464 0.0466 0.076 Uiso 1 1 calc R U . . .
C5 C -1.3261(7) -1.0192(6) -0.0137(3) 0.0561(19) Uani 1 1 d . . . . .
C6 C -1.3816(7) -1.0573(6) -0.0487(3) 0.060(2) Uani 1 1 d . . . . .
H6 H -1.3953 -1.0166 -0.0732 0.072 Uiso 1 1 calc R U . . .
C7 C -1.4159(7) -1.1572(7) -0.0463(3) 0.0577(19) Uani 1 1 d . . . . .
H7 H -1.4526 -1.1849 -0.0697 0.069 Uiso 1 1 calc R U . . .
C8 C -1.2829(10) -0.9143(7) -0.0190(3) 0.074(3) Uani 1 1 d . . . . .
H8A H -1.3247 -0.8752 -0.0395 0.089 Uiso 1 1 calc R U . . .
H8B H -1.2135 -0.9185 -0.0307 0.089 Uiso 1 1 calc R U . . .
C9 C -1.1962(7) -0.8620(7) 0.0476(3) 0.064(2) Uani 1 1 d . . . . .
H9 H -1.1367 -0.8920 0.0364 0.077 Uiso 1 1 calc R U . . .
C10 C -1.1953(7) -0.8180(7) 0.0880(3) 0.063(2) Uani 1 1 d . . . . .
H10 H -1.1352 -0.8176 0.1046 0.076 Uiso 1 1 calc R U . . .
C11 C -1.2840(6) -0.7738(6) 0.1042(3) 0.0552(19) Uani 1 1 d . . . . .
C12 C -1.3725(7) -0.7762(7) 0.0792(3) 0.059(2) Uani 1 1 d . . . . .
H12 H -1.4336 -0.7476 0.0895 0.071 Uiso 1 1 calc R U . . .
C13 C -1.3677(9) -0.8221(8) 0.0387(4) 0.076(3) Uani 1 1 d . . . . .
H13 H -1.4264 -0.8247 0.0212 0.091 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.909(5) 2_225 ?
Cu1 O1 1.909(5) . ?
Cu1 O2 2.044(5) 3_525 ?
Cu1 O2 2.044(5) 4_255 ?
Cu1 Br1 2.5779(18) . ?
Cu1 Cu1 2.853(3) 3_525 ?
N1 C13 1.337(15) . ?
N1 C9 1.342(13) . ?
N1 C8 1.518(13) . ?
O1 C1 1.264(10) . ?
O2 C1 1.270(11) . ?
O2 Cu1 2.044(5) 3_525 ?
C1 C2 1.480(11) . ?
C2 C3 1.371(13) . ?
C2 C7 1.412(12) . ?
C3 C4 1.406(13) . ?
C4 C5 1.364(12) . ?
C5 C6 1.408(12) . ?
C5 C8 1.512(12) . ?
C6 C7 1.402(12) . ?
C9 C10 1.385(14) . ?
C10 C11 1.407(12) . ?
C11 C12 1.407(13) . ?
C11 C11 1.441(19) 14_434 ?
C12 C13 1.401(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 176.1(4) 2_225 . ?
O1 Cu1 O2 88.2(2) 2_225 3_525 ?
O1 Cu1 O2 90.8(2) . 3_525 ?
O1 Cu1 O2 90.8(2) 2_225 4_255 ?
O1 Cu1 O2 88.2(2) . 4_255 ?
O2 Cu1 O2 149.9(3) 3_525 4_255 ?
O1 Cu1 Br1 91.93(18) 2_225 . ?
O1 Cu1 Br1 91.93(18) . . ?
O2 Cu1 Br1 105.06(17) 3_525 . ?
O2 Cu1 Br1 105.06(17) 4_255 . ?
O1 Cu1 Cu1 88.07(18) 2_225 3_525 ?
O1 Cu1 Cu1 88.07(18) . 3_525 ?
O2 Cu1 Cu1 74.94(17) 3_525 3_525 ?
O2 Cu1 Cu1 74.94(17) 4_255 3_525 ?
Br1 Cu1 Cu1 180.0 . 3_525 ?
C13 N1 C9 122.7(9) . . ?
C13 N1 C8 117.9(9) . . ?
C9 N1 C8 119.4(9) . . ?
C1 O1 Cu1 120.6(5) . . ?
C1 O2 Cu1 130.2(5) . 3_525 ?
O1 C1 O2 126.2(7) . . ?
O1 C1 C2 116.7(8) . . ?
O2 C1 C2 117.1(7) . . ?
C3 C2 C7 118.7(8) . . ?
C3 C2 C1 121.8(8) . . ?
C7 C2 C1 119.4(8) . . ?
C2 C3 C4 121.1(9) . . ?
C5 C4 C3 119.7(9) . . ?
C4 C5 C6 121.4(7) . . ?
C4 C5 C8 122.3(8) . . ?
C6 C5 C8 116.3(7) . . ?
C7 C6 C5 117.9(8) . . ?
C6 C7 C2 121.0(8) . . ?
C5 C8 N1 109.0(8) . . ?
N1 C9 C10 119.8(9) . . ?
C9 C10 C11 119.5(9) . . ?
C10 C11 C12 119.3(9) . . ?
C10 C11 C11 120.3(6) . 14_434 ?
C12 C11 C11 120.4(6) . 14_434 ?
C13 C12 C11 118.0(9) . . ?
N1 C13 C12 120.7(10) . . ?

_refine_diff_density_max         1.247
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.109

_shelxl_version_number           2013-3



####################################################################### 
# 
# 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_da346
_database_code_depnum_ccdc_archive 'CCDC 1441124'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C180 H198 Br2 Mn4 N12 O81'
_chemical_formula_sum            'C180 H198 Br2 Mn4 N12 O81'
_chemical_formula_weight         4205.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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.
;

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

_cell_length_a                   34.9259(6)
_cell_length_b                   34.9259(6)
_cell_length_c                   27.7797(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     29346.3(12)
_cell_formula_units_Z            6
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    99516
_cell_measurement_theta_min      1.991
_cell_measurement_theta_max      28.893

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_F_000             13080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.759
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            99516
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.991
_diffrn_reflns_theta_max         28.293
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16211
_reflns_number_gt                10150
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0954P)²+62.8052P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16211
_refine_ls_number_parameters     864
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0615
_refine_ls_wR_factor_ref         0.1890
_refine_ls_wR_factor_gt          0.1627
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Mn1 Mn 0.15604(2) -0.18350(2) 1.02297(2) 0.02966(13) Uani 1 1 d . . . . .
Mn2 Mn 0.0000 0.0000 0.30651(3) 0.02732(18) Uani 1 3 d S T P . .
Br1 Br 0.05635(4) -0.05689(4) 0.16083(5) 0.0524(3) Uani 0.3333 1 d . . P A 1
Br2 Br 0.0865(3) -0.0847(2) 0.1441(3) 0.204(3) Uani 0.1667 1 d . . P B 2
Br3 Br 0.0407(3) -0.0406(3) 0.1679(2) 0.170(3) Uani 0.1667 1 d . . P C 3
O1 O 0.16828(7) -0.22675(8) 0.98265(8) 0.0397(5) Uani 1 1 d . . . . .
O2 O 0.11380(8) -0.29618(8) 0.99267(8) 0.0459(6) Uani 1 1 d . . . . .
O3 O 0.04099(8) -0.39978(7) 0.32655(8) 0.0395(5) Uani 1 1 d . . . . .
O4 O -0.00393(8) -0.46675(7) 0.35601(8) 0.0420(6) Uani 1 1 d . . . . .
N1 N 0.15842(8) -0.31441(8) 0.74589(9) 0.0302(5) Uani 1 1 d . . . . .
N2 N 0.00708(8) -0.34356(8) 0.56407(8) 0.0286(5) Uani 1 1 d . . . . .
C1 C 0.14469(10) -0.26636(11) 0.96949(11) 0.0322(7) Uani 1 1 d . . . . .
C2 C 0.15641(10) -0.27741(10) 0.92092(10) 0.0281(6) Uani 1 1 d . . . . .
C3 C 0.18223(10) -0.24397(10) 0.88818(10) 0.0290(6) Uani 1 1 d . . . . .
H3 H 0.1921 -0.2140 0.8962 0.035 Uiso 1 1 calc R U . . .
C4 C 0.19353(10) -0.25412(10) 0.84411(11) 0.0313(6) Uani 1 1 d . . . . .
H4 H 0.2112 -0.2312 0.8221 0.038 Uiso 1 1 calc R U . . .
C5 C 0.17903(10) -0.29780(10) 0.83229(11) 0.0323(7) Uani 1 1 d . . . . .
C6 C 0.15414(11) -0.33101(10) 0.86499(11) 0.0359(7) Uani 1 1 d . . . . .
H6 H 0.1451 -0.3608 0.8573 0.043 Uiso 1 1 calc R U . . .
C7 C 0.14228(11) -0.32100(10) 0.90884(11) 0.0346(7) Uani 1 1 d . . . . .
H7 H 0.1244 -0.3441 0.9307 0.042 Uiso 1 1 calc R U . . .
C8 C 0.19090(11) -0.30934(12) 0.78419(11) 0.0367(7) Uani 1 1 d . . . . .
H8A H 0.2208 -0.2858 0.7747 0.044 Uiso 1 1 calc R U . . .
H8B H 0.1915 -0.3373 0.7872 0.044 Uiso 1 1 calc R U . . .
C9 C 0.17162(11) -0.28589(11) 0.70854(11) 0.0361(7) Uani 1 1 d . . . . .
H9 H 0.2015 -0.2627 0.7067 0.043 Uiso 1 1 calc R U . . .
C10 C 0.14250(11) -0.29000(10) 0.67342(11) 0.0345(7) Uani 1 1 d . . . . .
H10 H 0.1524 -0.2696 0.6474 0.041 Uiso 1 1 calc R U . . .
C11 C 0.09865(10) -0.32351(9) 0.67519(10) 0.0268(6) Uani 1 1 d . . . . .
C12 C 0.08602(10) -0.35263(10) 0.71446(10) 0.0300(6) Uani 1 1 d . . . . .
H12 H 0.0563 -0.3760 0.7173 0.036 Uiso 1 1 calc R U . . .
C13 C 0.11663(11) -0.34724(10) 0.74873(11) 0.0321(7) Uani 1 1 d . . . . .
H13 H 0.1079 -0.3673 0.7750 0.039 Uiso 1 1 calc R U . . .
C14 C 0.06665(10) -0.32926(9) 0.63695(10) 0.0262(6) Uani 1 1 d . . . . .
C15 C 0.08070(11) -0.30698(10) 0.59292(10) 0.0320(7) Uani 1 1 d . . . . .
H15 H 0.1111 -0.2864 0.5877 0.025(8) Uiso 1 1 calc R . . . .
C16 C 0.05028(10) -0.31507(10) 0.55725(11) 0.0318(7) Uani 1 1 d . . . . .
H16 H 0.0600 -0.3002 0.5273 0.038 Uiso 1 1 calc R U . . .
C17 C -0.00742(10) -0.36434(10) 0.60631(11) 0.0316(7) Uani 1 1 d . . . . .
H17 H -0.0382 -0.3837 0.6111 0.038 Uiso 1 1 calc R U . . .
C18 C 0.02150(10) -0.35799(10) 0.64260(11) 0.0325(7) Uani 1 1 d . . . . .
H18 H 0.0107 -0.3734 0.6721 0.039 Uiso 1 1 calc R U . . .
C19 C -0.02526(11) -0.35157(11) 0.52448(11) 0.0337(7) Uani 1 1 d . . . . .
H19A H -0.0238 -0.3234 0.5158 0.040 Uiso 1 1 calc R U . . .
H19B H -0.0556 -0.3724 0.5358 0.040 Uiso 1 1 calc R U . . .
C20 C -0.01512(10) -0.37057(10) 0.48054(10) 0.0289(6) Uani 1 1 d . . . . .
C21 C 0.00879(11) -0.34370(10) 0.44242(11) 0.0323(7) Uani 1 1 d . . . . .
H21 H 0.0182 -0.3131 0.4433 0.039 Uiso 1 1 calc R U . . .
C22 C 0.01916(10) -0.36099(10) 0.40303(10) 0.0307(6) Uani 1 1 d . . . . .
H22 H 0.0362 -0.3421 0.3774 0.037 Uiso 1 1 calc R U . . .
C23 C 0.00457(9) -0.40602(10) 0.40096(10) 0.0257(6) Uani 1 1 d . . . . .
C24 C -0.01967(10) -0.43317(10) 0.43904(10) 0.0292(6) Uani 1 1 d . . . . .
H24 H -0.0296 -0.4639 0.4378 0.035 Uiso 1 1 calc R U . . .
C25 C -0.02943(10) -0.41565(10) 0.47870(10) 0.0295(6) Uani 1 1 d . . . . .
H25 H -0.0459 -0.4343 0.5047 0.035 Uiso 1 1 calc R U . . .
C26 C 0.01471(10) -0.42568(10) 0.35747(10) 0.0287(6) Uani 1 1 d . . . . .
O31 O 0.10461(7) -0.19153(7) 0.97205(7) 0.0354(5) Uani 1 1 d . . . . .
O32 O 0.09226(8) -0.13755(7) 0.99523(8) 0.0394(5) Uani 1 1 d . . . . .
O33 O 0.05563(7) 0.01549(7) 0.35219(8) 0.0340(5) Uani 1 1 d . . . . .
O34 O 0.07836(7) -0.03173(7) 0.33135(8) 0.0362(5) Uani 1 1 d . . . . .
N31 N 0.02730(8) -0.14671(8) 0.75000(8) 0.0283(5) Uani 1 1 d . . . . .
N32 N 0.15677(8) 0.00892(8) 0.57473(8) 0.0256(5) Uani 1 1 d . . . . .
C31 C 0.09014(10) -0.16580(10) 0.96554(11) 0.0315(7) Uani 1 1 d . . . . .
C32 C 0.06681(10) -0.16959(10) 0.91843(10) 0.0297(6) Uani 1 1 d . . . . .
C33 C 0.04010(11) -0.15094(11) 0.91401(11) 0.0364(7) Uani 1 1 d . . . . .
H33 H 0.0370 -0.1354 0.9404 0.044 Uiso 1 1 calc R U . . .
C34 C 0.01778(11) -0.15479(11) 0.87125(11) 0.0374(7) Uani 1 1 d . . . . .
H34 H -0.0007 -0.1422 0.8687 0.045 Uiso 1 1 calc R U . . .
C35 C 0.02241(10) -0.17686(10) 0.83242(10) 0.0292(6) Uani 1 1 d . . . . .
C36 C 0.04951(10) -0.19526(10) 0.83658(11) 0.0317(7) Uani 1 1 d . . . . .
H36 H 0.0531 -0.2103 0.8100 0.038 Uiso 1 1 calc R U . . .
C37 C 0.07133(10) -0.19174(10) 0.87946(11) 0.0315(7) Uani 1 1 d . . . . .
H37 H 0.0896 -0.2047 0.8821 0.038 Uiso 1 1 calc R U . . .
C38 C -0.00217(10) -0.18062(11) 0.78606(11) 0.0343(7) Uani 1 1 d . . . . .
H38A H -0.0136 -0.2105 0.7723 0.041 Uiso 1 1 calc R U . . .
H38B H -0.0277 -0.1766 0.7931 0.041 Uiso 1 1 calc R U . . .
C39 C 0.04065(11) -0.10393(11) 0.75723(11) 0.0332(7) Uani 1 1 d . . . . .
H39 H 0.0314 -0.0953 0.7853 0.040 Uiso 1 1 calc R U . . .
C40 C 0.06758(11) -0.07244(10) 0.72457(10) 0.0321(7) Uani 1 1 d . . . . .
H40 H 0.0768 -0.0422 0.7302 0.039 Uiso 1 1 calc R U . . .
C41 C 0.08147(9) -0.08456(9) 0.68333(9) 0.0240(6) Uani 1 1 d . . . . .
C42 C 0.06730(10) -0.12907(10) 0.67720(10) 0.0297(6) Uani 1 1 d . . . . .
H42 H 0.0764 -0.1386 0.6496 0.036 Uiso 1 1 calc R U . . .
C43 C 0.04022(10) -0.15954(10) 0.71061(10) 0.0318(7) Uani 1 1 d . . . . .
H43 H 0.0305 -0.1900 0.7058 0.038 Uiso 1 1 calc R U . . .
C44 C 0.10907(9) -0.05172(9) 0.64618(9) 0.0240(6) Uani 1 1 d . . . . .
C45 C 0.11986(10) -0.00750(10) 0.64956(10) 0.0301(6) Uani 1 1 d . . . . .
H45 H 0.1106 0.0022 0.6768 0.036 Uiso 1 1 calc R U . . .
C46 C 0.14356(10) 0.02188(10) 0.61395(11) 0.0300(6) Uani 1 1 d . . . . .
H46 H 0.1508 0.0519 0.6169 0.036 Uiso 1 1 calc R U . . .
C47 C 0.14760(10) -0.03346(10) 0.57053(10) 0.0288(6) Uani 1 1 d . . . . .
H47 H 0.1573 -0.0423 0.5429 0.035 Uiso 1 1 calc R U . . .
C48 C 0.12447(10) -0.06371(10) 0.60583(10) 0.0280(6) Uani 1 1 d . . . . .
H48 H 0.1189 -0.0932 0.6028 0.034 Uiso 1 1 calc R U . . .
C49 C 0.18074(10) 0.04084(10) 0.53485(10) 0.0307(6) Uani 1 1 d . . . . .
H49A H 0.2087 0.0411 0.5279 0.037 Uiso 1 1 calc R U . . .
H49B H 0.1883 0.0710 0.5451 0.037 Uiso 1 1 calc R U . . .
C50 C 0.15300(9) 0.02859(9) 0.48984(10) 0.0261(6) Uani 1 1 d . . . . .
C51 C 0.12033(10) 0.04019(10) 0.48456(11) 0.0290(6) Uani 1 1 d . . . . .
H51 H 0.1153 0.0557 0.5095 0.035 Uiso 1 1 calc R U . . .
C52 C 0.09516(10) 0.02896(9) 0.44257(11) 0.0286(6) Uani 1 1 d . . . . .
H52 H 0.0731 0.0370 0.4389 0.034 Uiso 1 1 calc R U . . .
C53 C 0.10221(9) 0.00600(9) 0.40586(10) 0.0264(6) Uani 1 1 d . . . . .
C54 C 0.13440(10) -0.00602(10) 0.41163(10) 0.0294(6) Uani 1 1 d . . . . .
H54 H 0.1390 -0.0223 0.3871 0.035 Uiso 1 1 calc R U . . .
C55 C 0.15987(10) 0.00575(10) 0.45323(11) 0.0307(6) Uani 1 1 d . . . . .
H55 H 0.1823 -0.0019 0.4566 0.037 Uiso 1 1 calc R U . . .
O71 O -0.14727(8) -0.37903(8) 0.74337(7) 0.0437(6) Uani 1 1 d . . . . .
O72 O -0.21866(8) -0.42565(8) 0.72795(8) 0.0410(6) Uani 1 1 d . . . . .
O73 O -0.11148(9) -0.34566(10) 0.49479(8) 0.0532(7) Uani 1 1 d . . . . .
O74 O -0.17621(9) -0.40699(8) 0.48192(8) 0.0450(6) Uani 1 1 d . . . . .
C71 C -0.17912(11) -0.40063(11) 0.71498(11) 0.0345(7) Uani 1 1 d . . . . .
C72 C -0.16945(11) -0.39622(11) 0.66165(10) 0.0331(7) Uani 1 1 d . . . . .
C73 C -0.13091(12) -0.36065(12) 0.64379(11) 0.0415(8) Uani 1 1 d . . . . .
H73 H -0.1096 -0.3398 0.6654 0.050 Uiso 1 1 calc R U . . .
C74 C -0.12333(12) -0.35531(12) 0.59447(11) 0.0396(8) Uani 1 1 d . . . . .
H74 H -0.0968 -0.3309 0.5826 0.047 Uiso 1 1 calc R U . . .
C75 C -0.15402(10) -0.38521(11) 0.56266(10) 0.0317(7) Uani 1 1 d . . . . .
C76 C -0.19193(11) -0.42160(11) 0.58041(11) 0.0338(7) Uani 1 1 d . . . . .
H76 H -0.2127 -0.4428 0.5587 0.041 Uiso 1 1 calc R U . . .
C77 C -0.19971(11) -0.42728(11) 0.62955(11) 0.0347(7) Uani 1 1 d . . . . .
H77 H -0.2257 -0.4523 0.6413 0.042 Uiso 1 1 calc R U . . .
C78 C -0.14634(11) -0.37856(12) 0.50880(11) 0.0352(7) Uani 1 1 d . . . . .
C79 C 0.07620(9) -0.00488(10) 0.35948(10) 0.0282(6) Uani 1 1 d . . . . .
O1W O 0.21348(7) -0.17071(7) 1.06924(7) 0.0322(5) Uani 1 1 d . . . . .
H1WA H 0.2354 -0.1482 1.0577 0.048 Uiso 1 1 d R U . . .
H1WB H 0.2174 -0.1593 1.0967 0.048 Uiso 1 1 d R U . . .
O2W O 0.14421(7) -0.13699(7) 1.06437(7) 0.0353(5) Uani 1 1 d . . . . .
H2WA H 0.1299 -0.1459 1.0902 0.053 Uiso 1 1 d R U . . .
H2WB H 0.1255 -0.1348 1.0474 0.053 Uiso 1 1 d R U . . .
O3W O 0.10777(7) -0.23733(7) 1.06971(7) 0.0345(5) Uani 1 1 d . . . . .
H3WA H 0.1031 -0.2624 1.0611 0.052 Uiso 1 1 d R U . . .
H3WB H 0.1039 -0.2338 1.0988 0.052 Uiso 1 1 d R U . . .
O4W O 0.02047(8) -0.04078(8) 0.26463(8) 0.0400(5) Uani 1 1 d . . . . .
H4WA H 0.0416 -0.0418 0.2778 0.060 Uiso 1 1 d R U . . .
H4WB H 0.0287 -0.0305 0.2368 0.060 Uiso 1 1 d R U . . .
O5W O 0.2752(3) -0.2985(3) 0.6893(3) 0.199(3) Uiso 1 1 d . . . . .
O6W O 0.2935(2) -0.2885(2) 0.7929(2) 0.172(2) Uiso 1 1 d . . . . .
O7W O 0.1735(5) -0.4141(6) 0.7212(6) 0.153(6) Uiso 0.4 1 d . . P D 1
O7W' O 0.1812(3) -0.3880(3) 0.7106(3) 0.118(3) Uiso 0.6 1 d . . P E 2
O8W O -0.0149(3) -0.2541(3) 0.5037(3) 0.0309(19) Uani 0.25 1 d . . P F 1
O8W' O 0.01933(16) -0.24523(13) 0.50915(14) 0.0664(11) Uani 0.75 1 d . . P G 2
O9W O 0.14234(9) -0.25373(8) 0.50307(8) 0.0467(6) Uani 1 1 d G . . H 2
H9WA H 0.1699 -0.2371 0.5042 0.070 Uiso 1 1 d R U . H 2
H9WB H 0.1338 -0.2572 0.4743 0.070 Uiso 1 1 d R U . H 2
O10W O 0.16510(11) -0.08650(10) 0.48595(9) 0.0665(9) Uani 1 1 d . . . I 2
H10A H 0.1536 -0.0958 0.4588 0.100 Uiso 1 1 d R U . I 2
H10B H 0.1908 -0.0828 0.4861 0.100 Uiso 1 1 d R U . I 2
O11W O -0.00727(9) -0.27126(9) 0.60363(9) 0.0520(7) Uani 1 1 d . . . J 2
H11A H 0.0170 -0.2604 0.6183 0.078 Uiso 1 1 d R U . J 2
H11B H -0.0027 -0.2629 0.5748 0.078 Uiso 1 1 d R U . J 2
O12W O -0.04909(8) -0.24143(8) 0.66302(9) 0.0463(6) Uani 1 1 d . . . K 2
H12A H -0.0358 -0.2485 0.6428 0.069 Uiso 1 1 d R U . K 2
H12B H -0.0690 -0.2402 0.6473 0.069 Uiso 1 1 d R U . K 2
O13W O -0.07183(8) -0.29160(8) 0.74519(8) 0.0462(6) Uani 1 1 d . . . L 2
H13A H -0.0681 -0.2760 0.7207 0.069 Uiso 1 1 d R U . L 2
H13B H -0.0938 -0.3163 0.7384 0.069 Uiso 1 1 d R U . L 2
O14W O 0.08054(10) -0.34295(9) 1.07551(9) 0.0591(7) Uani 1 1 d . . . M 2
H14A H 0.0651 -0.3694 1.0668 0.089 Uiso 1 1 d R U . M 2
H14B H 0.0895 -0.3288 1.0496 0.089 Uiso 1 1 d R U . M 2
O15W O 0.22314(10) -0.13789(9) 1.15973(8) 0.0583(8) Uani 1 1 d G . . N 2
H15A H 0.2089 -0.1244 1.1600 0.087 Uiso 1 1 d R U . N 2
H15B H 0.2286 -0.1418 1.1882 0.087 Uiso 1 1 d R U . N 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
Mn1 O1 2.089(2) . ?
Mn1 O4 2.150(2) 14_556 ?
Mn1 O2W 2.192(2) . ?
Mn1 O31 2.191(2) . ?
Mn1 O3W 2.212(2) . ?
Mn1 O1W 2.231(2) . ?
Mn2 O33 2.151(2) 2 ?
Mn2 O33 2.151(2) 3 ?
Mn2 O33 2.151(2) . ?
Mn2 O4W 2.216(2) 3 ?
Mn2 O4W 2.216(2) 2 ?
Mn2 O4W 2.216(2) . ?
O1 C1 1.260(4) . ?
O2 C1 1.241(4) . ?
O3 C26 1.252(4) . ?
O4 C26 1.244(4) . ?
O4 Mn1 2.150(2) 15_446 ?
N1 C13 1.333(4) . ?
N1 C9 1.350(4) . ?
N1 C8 1.500(4) . ?
N2 C17 1.339(4) . ?
N2 C16 1.342(4) . ?
N2 C19 1.499(4) . ?
C1 C2 1.515(4) . ?
C2 C7 1.387(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.385(4) . ?
C5 C6 1.385(4) . ?
C5 C8 1.512(4) . ?
C6 C7 1.386(4) . ?
C9 C10 1.364(5) . ?
C10 C11 1.388(4) . ?
C11 C12 1.404(4) . ?
C11 C14 1.481(4) . ?
C12 C13 1.372(4) . ?
C14 C18 1.391(4) . ?
C14 C15 1.400(4) . ?
C15 C16 1.375(4) . ?
C17 C18 1.364(4) . ?
C19 C20 1.513(4) . ?
C20 C21 1.384(4) . ?
C20 C25 1.395(4) . ?
C21 C22 1.383(4) . ?
C22 C23 1.391(4) . ?
C23 C24 1.390(4) . ?
C23 C26 1.517(4) . ?
C24 C25 1.383(4) . ?
O31 C31 1.245(4) . ?
O32 C31 1.259(4) . ?
O33 C79 1.254(4) . ?
O34 C79 1.252(4) . ?
N31 C39 1.339(4) . ?
N31 C43 1.343(4) . ?
N31 C38 1.499(4) . ?
N32 C46 1.347(4) . ?
N32 C47 1.354(4) . ?
N32 C49 1.496(4) . ?
C31 C32 1.512(4) . ?
C32 C37 1.385(4) . ?
C32 C33 1.385(4) . ?
C33 C34 1.390(4) . ?
C34 C35 1.381(4) . ?
C35 C36 1.390(4) . ?
C35 C38 1.516(4) . ?
C36 C37 1.386(4) . ?
C39 C40 1.372(4) . ?
C40 C41 1.390(4) . ?
C41 C42 1.386(4) . ?
C41 C44 1.485(4) . ?
C42 C43 1.372(4) . ?
C44 C48 1.395(4) . ?
C44 C45 1.398(4) . ?
C45 C46 1.366(4) . ?
C47 C48 1.370(4) . ?
C49 C50 1.507(4) . ?
C50 C55 1.385(4) . ?
C50 C51 1.396(4) . ?
C51 C52 1.394(4) . ?
C52 C53 1.393(4) . ?
C53 C54 1.392(4) . ?
C53 C79 1.511(4) . ?
C54 C55 1.389(4) . ?
O71 C71 1.261(4) . ?
O72 C71 1.262(4) . ?
O73 C78 1.247(4) . ?
O74 C78 1.263(4) . ?
C71 C72 1.510(4) . ?
C72 C73 1.389(5) . ?
C72 C77 1.394(4) . ?
C73 C74 1.390(4) . ?
C74 C75 1.379(5) . ?
C75 C76 1.389(5) . ?
C75 C78 1.517(4) . ?
C76 C77 1.387(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
O1 Mn1 O4 90.26(10) . 14_556 ?
O1 Mn1 O2W 178.82(10) . . ?
O4 Mn1 O2W 88.56(9) 14_556 . ?
O1 Mn1 O31 90.71(9) . . ?
O4 Mn1 O31 84.88(8) 14_556 . ?
O2W Mn1 O31 89.28(8) . . ?
O1 Mn1 O3W 92.56(9) . . ?
O4 Mn1 O3W 176.13(9) 14_556 . ?
O2W Mn1 O3W 88.62(8) . . ?
O31 Mn1 O3W 92.43(8) . . ?
O1 Mn1 O1W 87.99(8) . . ?
O4 Mn1 O1W 89.37(8) 14_556 . ?
O2W Mn1 O1W 91.90(8) . . ?
O31 Mn1 O1W 174.10(8) . . ?
O3W Mn1 O1W 93.37(8) . . ?
O33 Mn2 O33 88.74(9) 2 3 ?
O33 Mn2 O33 88.74(9) 2 . ?
O33 Mn2 O33 88.74(9) 3 . ?
O33 Mn2 O4W 90.19(8) 2 3 ?
O33 Mn2 O4W 86.00(8) 3 3 ?
O33 Mn2 O4W 174.65(9) . 3 ?
O33 Mn2 O4W 86.00(8) 2 2 ?
O33 Mn2 O4W 174.65(9) 3 2 ?
O33 Mn2 O4W 90.19(8) . 2 ?
O4W Mn2 O4W 94.97(8) 3 2 ?
O33 Mn2 O4W 174.65(9) 2 . ?
O33 Mn2 O4W 90.19(8) 3 . ?
O33 Mn2 O4W 86.00(8) . . ?
O4W Mn2 O4W 94.97(8) 3 . ?
O4W Mn2 O4W 94.97(8) 2 . ?
C1 O1 Mn1 133.8(2) . . ?
C26 O4 Mn1 131.5(2) . 15_446 ?
C13 N1 C9 120.2(3) . . ?
C13 N1 C8 119.8(3) . . ?
C9 N1 C8 119.9(3) . . ?
C17 N2 C16 120.4(3) . . ?
C17 N2 C19 119.8(3) . . ?
C16 N2 C19 119.8(2) . . ?
O2 C1 O1 126.0(3) . . ?
O2 C1 C2 118.7(3) . . ?
O1 C1 C2 115.3(3) . . ?
C7 C2 C3 119.1(3) . . ?
C7 C2 C1 120.1(3) . . ?
C3 C2 C1 120.7(3) . . ?
C4 C3 C2 120.6(3) . . ?
C5 C4 C3 119.8(3) . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 C8 120.3(3) . . ?
C6 C5 C8 119.8(3) . . ?
C5 C6 C7 120.4(3) . . ?
C6 C7 C2 120.2(3) . . ?
N1 C8 C5 111.5(3) . . ?
N1 C9 C10 120.7(3) . . ?
C9 C10 C11 120.9(3) . . ?
C10 C11 C12 116.9(3) . . ?
C10 C11 C14 121.9(3) . . ?
C12 C11 C14 121.1(3) . . ?
C13 C12 C11 119.9(3) . . ?
N1 C13 C12 121.3(3) . . ?
C18 C14 C15 117.1(3) . . ?
C18 C14 C11 121.5(3) . . ?
C15 C14 C11 121.3(3) . . ?
C16 C15 C14 119.7(3) . . ?
N2 C16 C15 121.2(3) . . ?
N2 C17 C18 120.7(3) . . ?
C17 C18 C14 120.9(3) . . ?
N2 C19 C20 110.7(2) . . ?
C21 C20 C25 119.4(3) . . ?
C21 C20 C19 120.9(3) . . ?
C25 C20 C19 119.6(3) . . ?
C22 C21 C20 120.7(3) . . ?
C21 C22 C23 119.9(3) . . ?
C24 C23 C22 119.6(3) . . ?
C24 C23 C26 119.9(3) . . ?
C22 C23 C26 120.6(3) . . ?
C25 C24 C23 120.3(3) . . ?
C24 C25 C20 120.0(3) . . ?
O4 C26 O3 125.6(3) . . ?
O4 C26 C23 116.2(3) . . ?
O3 C26 C23 118.2(3) . . ?
C31 O31 Mn1 127.2(2) . . ?
C79 O33 Mn2 130.8(2) . . ?
C39 N31 C43 120.4(3) . . ?
C39 N31 C38 120.0(3) . . ?
C43 N31 C38 119.6(3) . . ?
C46 N32 C47 120.2(2) . . ?
C46 N32 C49 120.5(2) . . ?
C47 N32 C49 119.3(2) . . ?
O31 C31 O32 125.8(3) . . ?
O31 C31 C32 117.3(3) . . ?
O32 C31 C32 117.0(3) . . ?
C37 C32 C33 119.0(3) . . ?
C37 C32 C31 121.3(3) . . ?
C33 C32 C31 119.7(3) . . ?
C32 C33 C34 120.5(3) . . ?
C35 C34 C33 120.3(3) . . ?
C34 C35 C36 119.3(3) . . ?
C34 C35 C38 119.5(3) . . ?
C36 C35 C38 121.2(3) . . ?
C37 C36 C35 120.1(3) . . ?
C32 C37 C36 120.7(3) . . ?
N31 C38 C35 111.3(2) . . ?
N31 C39 C40 120.8(3) . . ?
C39 C40 C41 120.3(3) . . ?
C42 C41 C40 117.4(3) . . ?
C42 C41 C44 120.7(3) . . ?
C40 C41 C44 121.9(3) . . ?
C43 C42 C41 120.5(3) . . ?
N31 C43 C42 120.6(3) . . ?
C48 C44 C45 117.0(3) . . ?
C48 C44 C41 121.7(3) . . ?
C45 C44 C41 121.3(3) . . ?
C46 C45 C44 120.5(3) . . ?
N32 C46 C45 120.9(3) . . ?
N32 C47 C48 120.5(3) . . ?
C47 C48 C44 120.7(3) . . ?
N32 C49 C50 111.2(2) . . ?
C55 C50 C51 119.5(3) . . ?
C55 C50 C49 120.1(3) . . ?
C51 C50 C49 120.5(3) . . ?
C52 C51 C50 119.9(3) . . ?
C53 C52 C51 120.4(3) . . ?
C54 C53 C52 119.4(3) . . ?
C54 C53 C79 119.8(3) . . ?
C52 C53 C79 120.8(3) . . ?
C55 C54 C53 120.0(3) . . ?
C50 C55 C54 120.8(3) . . ?
O71 C71 O72 124.6(3) . . ?
O71 C71 C72 117.8(3) . . ?
O72 C71 C72 117.5(3) . . ?
C73 C72 C77 119.1(3) . . ?
C73 C72 C71 120.6(3) . . ?
C77 C72 C71 120.3(3) . . ?
C72 C73 C74 120.4(3) . . ?
C75 C74 C73 120.4(3) . . ?
C74 C75 C76 119.3(3) . . ?
C74 C75 C78 120.3(3) . . ?
C76 C75 C78 120.3(3) . . ?
C77 C76 C75 120.6(3) . . ?
C76 C77 C72 120.0(3) . . ?
O73 C78 O74 125.6(3) . . ?
O73 C78 C75 117.7(3) . . ?
O74 C78 C75 116.7(3) . . ?
O34 C79 O33 126.2(3) . . ?
O34 C79 C53 117.8(3) . . ?
O33 C79 C53 116.0(3) . . ?

_refine_diff_density_max         1.130
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.078

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_da351
_database_code_depnum_ccdc_archive 'CCDC 1441125'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C180 H204 Br2 Co4 N12 O81'
_chemical_formula_sum            'C180 H204 Br2 Co4 N12 O81'
_chemical_formula_weight         4227.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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.
;

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

_cell_length_a                   35.0155(8)
_cell_length_b                   35.0155(8)
_cell_length_c                   27.5842(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     29289.5(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    89750
_cell_measurement_theta_min      1.996
_cell_measurement_theta_max      28.308

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_F_000             13164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.829
_shelx_estimated_absorpt_T_min   0.900
_shelx_estimated_absorpt_T_max   0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            89750
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.996
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16166
_reflns_number_gt                11507
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014/6 (Sheldrick, 2014)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0683P)²+74.4202P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16166
_refine_ls_number_parameters     875
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1436
_refine_ls_wR_factor_gt          0.1281
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.51022(2) 0.99531(2) 0.31057(2) 0.02159(8) Uani 1 1 d . . . . .
Co2 Co 0.6667 1.3333 1.02579(2) 0.02604(13) Uani 1 3 d S T P . .
Br1 Br 0.60997(3) 1.39071(3) 1.17109(3) 0.0459(2) Uani 0.3333 1 d . . P A 1
Br2 Br 0.6312(3) 1.3737(2) 1.16627(19) 0.189(3) Uani 0.1667 1 d . . P B 2
Br3 Br 0.5841(2) 1.4203(2) 1.1823(3) 0.191(2) Uiso 0.1667 1 d . . P C 3
O1 O 0.56000(5) 1.03632(6) 0.36029(6) 0.0273(4) Uani 1 1 d . . . . .
O2 O 0.57201(6) 1.10272(6) 0.33752(6) 0.0323(4) Uani 1 1 d . . . . .
O3 O 0.61320(6) 1.29633(6) 0.98065(6) 0.0308(4) Uani 1 1 d . . . . .
O4 O 0.59130(6) 1.22659(6) 1.00202(6) 0.0342(4) Uani 1 1 d . . . . .
N1 N 0.63856(6) 1.15800(7) 0.58346(7) 0.0262(4) Uani 1 1 d . . . . .
N2 N 0.50962(6) 1.18585(6) 0.75886(7) 0.0241(4) Uani 1 1 d . . . . .
C1 C 0.57476(8) 1.07662(8) 0.36705(8) 0.0252(5) Uani 1 1 d . . . . .
C2 C 0.59842(8) 1.09602(8) 0.41428(8) 0.0247(5) Uani 1 1 d . . . . .
C3 C 0.62538(9) 1.14127(9) 0.41862(9) 0.0311(5) Uani 1 1 d . . . . .
H3 H 0.6285 1.1599 0.3920 0.047 Uiso 1 1 calc R U . . .
C4 C 0.64783(9) 1.15960(9) 0.46148(9) 0.0325(6) Uani 1 1 d . . . . .
H4 H 0.6664 1.1906 0.4640 0.049 Uiso 1 1 calc R U . . .
C5 C 0.64321(8) 1.13273(8) 0.50072(8) 0.0267(5) Uani 1 1 d . . . . .
C6 C 0.61592(8) 1.08732(8) 0.49641(8) 0.0276(5) Uani 1 1 d . . . . .
H6 H 0.6124 1.0687 0.5231 0.041 Uiso 1 1 calc R U . . .
C7 C 0.59378(8) 1.06896(8) 0.45330(8) 0.0267(5) Uani 1 1 d . . . . .
H7 H 0.5755 1.0379 0.4505 0.040 Uiso 1 1 calc R U . . .
C8 C 0.66774(8) 1.15318(9) 0.54730(9) 0.0306(5) Uani 1 1 d . . . . .
H8A H 0.6788 1.1344 0.5612 0.046 Uiso 1 1 calc R U . . .
H8B H 0.6935 1.1825 0.5403 0.046 Uiso 1 1 calc R U . . .
C9 C 0.62642(9) 1.18854(8) 0.57656(9) 0.0319(6) Uani 1 1 d . . . . .
H9 H 0.6365 1.2069 0.5487 0.048 Uiso 1 1 calc R U . . .
C10 C 0.59976(9) 1.19352(8) 0.60923(9) 0.0305(5) Uani 1 1 d . . . . .
H10 H 0.5915 1.2153 0.6039 0.046 Uiso 1 1 calc R U . . .
C11 C 0.58465(7) 1.16682(7) 0.65029(8) 0.0225(5) Uani 1 1 d . . . . .
C12 C 0.59750(8) 1.13537(8) 0.65604(9) 0.0276(5) Uani 1 1 d . . . . .
H12 H 0.5875 1.1163 0.6834 0.041 Uiso 1 1 calc R U . . .
C13 C 0.62447(8) 1.13171(8) 0.62248(9) 0.0288(5) Uani 1 1 d . . . . .
H13 H 0.6332 1.1103 0.6270 0.043 Uiso 1 1 calc R U . . .
C14 C 0.55702(8) 1.17228(7) 0.68738(8) 0.0225(5) Uani 1 1 d . . . . .
C15 C 0.54682(8) 1.20602(8) 0.68385(9) 0.0288(5) Uani 1 1 d . . . . .
H15 H 0.5563 1.2249 0.6564 0.043 Uiso 1 1 calc R U . . .
C16 C 0.52324(8) 1.21210(8) 0.71972(9) 0.0285(5) Uani 1 1 d . . . . .
H16 H 0.5165 1.2351 0.7168 0.043 Uiso 1 1 calc R U . . .
C17 C 0.51797(8) 1.15241(8) 0.76324(8) 0.0267(5) Uani 1 1 d . . . . .
H17 H 0.5078 1.1339 0.7910 0.040 Uiso 1 1 calc R U . . .
C18 C 0.54106(8) 1.14491(8) 0.72805(8) 0.0263(5) Uani 1 1 d . . . . .
H18 H 0.5463 1.1209 0.7313 0.039 Uiso 1 1 calc R U . . .
C19 C 0.48586(8) 1.19434(9) 0.79886(8) 0.0285(5) Uani 1 1 d . . . . .
H19A H 0.4581 1.1668 0.8063 0.043 Uiso 1 1 calc R U . . .
H19B H 0.4783 1.2167 0.7882 0.043 Uiso 1 1 calc R U . . .
C20 C 0.51404(8) 1.21046(8) 0.84403(8) 0.0246(5) Uani 1 1 d . . . . .
C21 C 0.54667(8) 1.25466(8) 0.84867(9) 0.0268(5) Uani 1 1 d . . . . .
H21 H 0.5514 1.2748 0.8232 0.040 Uiso 1 1 calc R U . . .
C22 C 0.57219(8) 1.26918(8) 0.89033(9) 0.0266(5) Uani 1 1 d . . . . .
H22 H 0.5941 1.2994 0.8935 0.040 Uiso 1 1 calc R U . . .
C23 C 0.56572(8) 1.23953(8) 0.92768(8) 0.0245(5) Uani 1 1 d . . . . .
C24 C 0.53357(8) 1.19552(8) 0.92258(9) 0.0283(5) Uani 1 1 d . . . . .
H24 H 0.5293 1.1752 0.9477 0.042 Uiso 1 1 calc R U . . .
C25 C 0.50767(8) 1.18103(8) 0.88123(9) 0.0286(5) Uani 1 1 d . . . . .
H25 H 0.4855 1.1509 0.8783 0.043 Uiso 1 1 calc R U . . .
C26 C 0.59234(8) 1.25528(8) 0.97379(9) 0.0269(5) Uani 1 1 d . . . . .
N31 N 0.50897(7) 0.86011(7) 0.58620(7) 0.0245(4) Uani 1 1 d . . . . .
N32 N 0.65969(7) 0.98260(6) 0.76954(7) 0.0238(4) Uani 1 1 d . . . . .
O31 O 0.49828(6) 0.94263(6) 0.35233(6) 0.0293(4) Uani 1 1 d . . . . .
O32 O 0.55115(6) 0.92615(6) 0.33720(6) 0.0309(4) Uani 1 1 d . . . . .
O33 O 0.62652(6) 0.89120(6) 1.00762(6) 0.0337(4) Uani 1 1 d . . . . .
O34 O 0.67231(6) 0.87023(6) 0.97757(6) 0.0292(4) Uani 1 1 d . . . . .
C31 C 0.52129(7) 0.92538(7) 0.36271(8) 0.0229(5) Uani 1 1 d . . . . .
C32 C 0.51035(7) 0.90151(7) 0.41093(8) 0.0218(4) Uani 1 1 d . . . . .
C33 C 0.48443(8) 0.90821(8) 0.44438(8) 0.0245(5) Uani 1 1 d . . . . .
H33 H 0.4741 0.9280 0.4369 0.037 Uiso 1 1 calc R U . . .
C34 C 0.47366(8) 0.88624(8) 0.48843(8) 0.0252(5) Uani 1 1 d . . . . .
H34 H 0.4561 0.8911 0.5112 0.038 Uiso 1 1 calc R U . . .
C35 C 0.48855(8) 0.85712(8) 0.49934(8) 0.0255(5) Uani 1 1 d . . . . .
C36 C 0.51409(9) 0.85024(8) 0.46580(9) 0.0295(5) Uani 1 1 d . . . . .
H36 H 0.5240 0.8301 0.4730 0.044 Uiso 1 1 calc R U . . .
C37 C 0.52519(8) 0.87248(8) 0.42184(8) 0.0275(5) Uani 1 1 d . . . . .
H37 H 0.5429 0.8678 0.3992 0.041 Uiso 1 1 calc R U . . .
C38 C 0.47704(8) 0.83299(8) 0.54727(8) 0.0283(5) Uani 1 1 d . . . . .
H38A H 0.4469 0.8258 0.5569 0.043 Uiso 1 1 calc R U . . .
H38B H 0.4772 0.8050 0.5435 0.043 Uiso 1 1 calc R U . . .
C39 C 0.55088(8) 0.86871(8) 0.58376(8) 0.0266(5) Uani 1 1 d . . . . .
H39 H 0.5597 0.8573 0.5576 0.040 Uiso 1 1 calc R U . . .
C40 C 0.58107(8) 0.89379(8) 0.61868(8) 0.0258(5) Uani 1 1 d . . . . .
H40 H 0.6107 0.8999 0.6163 0.039 Uiso 1 1 calc R U . . .
C41 C 0.56839(8) 0.91036(8) 0.65767(8) 0.0233(5) Uani 1 1 d . . . . .
C42 C 0.52463(8) 0.90058(8) 0.65923(9) 0.0278(5) Uani 1 1 d . . . . .
H42 H 0.5148 0.9112 0.6853 0.042 Uiso 1 1 calc R U . . .
C43 C 0.49575(8) 0.87566(9) 0.62333(9) 0.0293(5) Uani 1 1 d . . . . .
H43 H 0.4660 0.8693 0.6247 0.044 Uiso 1 1 calc R U . . .
C44 C 0.60020(8) 0.93675(8) 0.69640(8) 0.0229(5) Uani 1 1 d . . . . .
C45 C 0.64525(8) 0.95280(8) 0.69048(8) 0.0276(5) Uani 1 1 d . . . . .
H45 H 0.6559 0.9477 0.6609 0.041 Uiso 1 1 calc R U . . .
C46 C 0.67430(8) 0.97593(8) 0.72723(8) 0.0269(5) Uani 1 1 d . . . . .
H46 H 0.7050 0.9873 0.7226 0.040 Uiso 1 1 calc R U . . .
C47 C 0.61652(8) 0.96796(8) 0.77613(8) 0.0275(5) Uani 1 1 d . . . . .
H47 H 0.6068 0.9734 0.8061 0.033 Uiso 1 1 calc R U . . .
C48 C 0.58623(8) 0.94532(8) 0.74037(8) 0.0270(5) Uani 1 1 d . . . . .
H48 H 0.5559 0.9355 0.7455 0.041 Uiso 1 1 calc R U . . .
C49 C 0.69189(8) 1.00728(8) 0.80947(8) 0.0269(5) Uani 1 1 d . . . . .
H49A H 0.6898 1.0336 0.8184 0.040 Uiso 1 1 calc R U . . .
H49B H 0.7223 1.0174 0.7980 0.040 Uiso 1 1 calc R U . . .
C50 C 0.68225(8) 0.97802(7) 0.85334(8) 0.0234(5) Uani 1 1 d . . . . .
C51 C 0.65828(8) 0.98059(8) 0.89196(8) 0.0277(5) Uani 1 1 d . . . . .
H51 H 0.6486 1.0016 0.8914 0.042 Uiso 1 1 calc R U . . .
C52 C 0.64836(8) 0.95256(8) 0.93145(8) 0.0266(5) Uani 1 1 d . . . . .
H52 H 0.6314 0.9541 0.9575 0.040 Uiso 1 1 calc R U . . .
C53 C 0.66298(7) 0.92225(7) 0.93321(8) 0.0218(4) Uani 1 1 d . . . . .
C54 C 0.68728(8) 0.91985(8) 0.89442(8) 0.0236(5) Uani 1 1 d . . . . .
H54 H 0.6974 0.8993 0.8952 0.035 Uiso 1 1 calc R U . . .
C55 C 0.69669(8) 0.94745(8) 0.85464(8) 0.0242(5) Uani 1 1 d . . . . .
H55 H 0.7130 0.9455 0.8282 0.036 Uiso 1 1 calc R U . . .
C56 C 0.65306(8) 0.89220(7) 0.97641(8) 0.0230(5) Uani 1 1 d . . . . .
O71 O 0.54046(6) 1.09203(6) -0.05997(6) 0.0350(4) Uani 1 1 d . . . . .
O72 O 0.56263(6) 1.04353(6) -0.07691(6) 0.0353(4) Uani 1 1 d . . . . .
O73 O 0.56408(6) 1.06990(6) 0.18668(6) 0.0376(4) Uani 1 1 d . . . . .
O74 O 0.56467(7) 1.00729(7) 0.17325(6) 0.0408(5) Uani 1 1 d . . . . .
C71 C 0.55361(8) 1.06585(8) -0.04774(8) 0.0291(5) Uani 1 1 d . . . . .
C72 C 0.55923(8) 1.06071(9) 0.00585(8) 0.0279(5) Uani 1 1 d . . . . .
C73 C 0.56049(8) 1.09167(9) 0.03876(9) 0.0292(5) Uani 1 1 d . . . . .
H H 0.5598 1.1169 0.0274 0.044 Uiso 1 1 calc R U . . .
C74 C 0.56278(8) 1.08536(9) 0.08806(8) 0.0284(5) Uani 1 1 d . . . . .
HA H 0.5637 1.1065 0.1104 0.043 Uiso 1 1 calc R U . . .
C75 C 0.56378(8) 1.04867(9) 0.10523(8) 0.0281(5) Uani 1 1 d . . . . .
C76 C 0.56399(9) 1.01876(9) 0.07255(9) 0.0347(6) Uani 1 1 d . . . . .
HB H 0.5656 0.9940 0.0840 0.052 Uiso 1 1 calc R U . . .
C77 C 0.56192(10) 1.02488(9) 0.02306(9) 0.0354(6) Uani 1 1 d . . . . .
HC H 0.5623 1.0044 0.0008 0.053 Uiso 1 1 calc R U . . .
C78 C 0.56426(8) 1.04113(9) 0.15922(8) 0.0296(5) Uani 1 1 d . . . . .
O4W O 0.62622(6) 1.35068(6) 1.06723(6) 0.0352(4) Uani 1 1 d . . . . .
H4WA H 0.6244 1.3713 1.0539 0.053 Uiso 1 1 d R U . . .
H4WB H 0.6287 1.3574 1.0967 0.053 Uiso 1 1 d R U . . .
O2W O 0.52014(6) 1.04979(6) 0.26979(6) 0.0273(4) Uani 1 1 d . . . . .
H2WA H 0.5328 1.0513 0.2434 0.041 Uiso 1 1 d R U . . .
H2WB H 0.5359 1.0733 0.2850 0.041 Uiso 1 1 d R U . . .
O3W O 0.55745(5) 0.98917(5) 0.26814(6) 0.0255(3) Uani 1 1 d . . . . .
H3WA H 0.5526 0.9901 0.2385 0.031 Uiso 1 1 d R U . . .
H3WB H 0.5563 0.9651 0.2740 0.031 Uiso 1 1 d R U . . .
O1W O 0.45663(5) 0.95117(5) 0.26542(6) 0.0260(3) Uani 1 1 d . . . . .
H1WA H 0.4597 0.9610 0.2371 0.031 Uiso 1 1 d R U . . .
H1WB H 0.4325 0.9473 0.2760 0.031 Uiso 1 1 d R U . . .
O5W' O 0.40208(15) 0.76302(11) 0.64333(13) 0.0713(11) Uani 0.75 1 d . . P D 1
O5W O 0.3715(3) 0.7509(3) 0.6527(4) 0.065(3) Uani 0.25 1 d . . P E 2
O6W O 0.3734(2) 0.7514(2) 0.5567(3) 0.0847(18) Uiso 0.5 1 d . . P F 1
O6W' O 0.3752(2) 0.7527(2) 0.5265(3) 0.0881(19) Uiso 0.5 1 d . . P G 2
O7W O 0.3272(6) 0.9107(5) 0.1710(5) 0.072(5) Uani 0.2 1 d . . P H 1
O7W' O 0.35519(10) 0.93253(10) 0.17675(10) 0.0429(7) Uani 0.8 1 d . . P I 2
O8W O 0.60096(19) 1.17661(14) 0.28172(16) 0.168(2) Uani 1 1 d . . . . .
HD H 0.6054 1.2003 0.2944 0.202 Uiso 1 1 d R U . . .
HE H 0.5898 1.1563 0.3024 0.202 Uiso 1 1 d R U . . .
O9W O 0.50100(9) 1.08374(7) -0.15189(8) 0.0578(6) Uani 1 1 d . . . . .
HF H 0.5125 1.0855 -0.1247 0.069 Uiso 1 1 d R U . . .
HG H 0.4795 1.0582 -0.1558 0.069 Uiso 1 1 d R U . . .
O10W O 0.55267(7) 0.95704(7) -0.07930(7) 0.0403(5) Uani 1 1 d . . . . .
HH H 0.5527 0.9809 -0.0756 0.048 Uiso 1 1 d R U . . .
HI H 0.5423 0.9414 -0.0544 0.081(14) Uiso 1 1 d R . . . .
O11W O 0.47561(6) 1.09405(7) -0.00273(7) 0.0394(4) Uani 1 1 d . . . . .
HJ H 0.4543 1.0852 -0.0220 0.047 Uiso 1 1 d R U . . .
HK H 0.4973 1.0954 -0.0173 0.047 Uiso 1 1 d R U . . .
O12W O 0.47677(8) 1.06420(7) 0.17064(7) 0.0411(5) Uani 1 1 d . . . . .
HL H 0.5045 1.0779 0.1710 0.16(3) Uiso 1 1 d R . . . .
H12B H 0.4711 1.0607 0.1409 0.245 Uiso 1 1 d R U . . .
O13W O 0.44559(7) 0.97406(7) 0.17466(6) 0.0419(5) Uani 1 1 d . . . . .
HN H 0.4565 1.0015 0.1732 0.050 Uiso 1 1 d R U . . .
HO H 0.4465 0.9667 0.1459 0.063 Uiso 1 1 d R U . . .
O14W O 0.59674(6) 0.93671(7) 1.06194(7) 0.0407(5) Uani 1 1 d . . . . .
HP H 0.6158 0.9600 1.0755 0.049 Uiso 1 1 d R U . . .
HQ H 0.6092 0.9239 1.0493 0.049 Uiso 1 1 d R U . . .
O15W O 0.58771(8) 0.90856(7) 0.25709(7) 0.0500(6) Uani 1 1 d . . . . .
HR H 0.6019 0.8954 0.2618 0.060 Uiso 1 1 d R U . . .
HS H 0.5782 0.9110 0.2842 0.060 Uiso 1 1 d R U . . .


_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 O31 2.0328(17) . ?
Co1 O34 2.0786(16) 15_556 ?
Co1 O2W 2.0890(16) . ?
Co1 O1 2.1163(16) . ?
Co1 O3W 2.1230(16) . ?
Co1 O1W 2.1356(16) . ?
Co2 O3 2.0757(17) 2_775 ?
Co2 O3 2.0757(17) . ?
Co2 O3 2.0757(17) 3_575 ?
Co2 O4W 2.1310(18) 2_775 ?
Co2 O4W 2.1310(18) 3_575 ?
Co2 O4W 2.1311(18) . ?
O1 C1 1.251(3) . ?
O2 C1 1.263(3) . ?
O3 C26 1.259(3) . ?
O4 C26 1.257(3) . ?
N1 C13 1.340(3) . ?
N1 C9 1.347(3) . ?
N1 C8 1.496(3) . ?
N2 C16 1.341(3) . ?
N2 C17 1.347(3) . ?
N2 C19 1.498(3) . ?
C1 C2 1.511(3) . ?
C2 C3 1.386(4) . ?
C2 C7 1.389(3) . ?
C3 C4 1.387(3) . ?
C4 C5 1.389(4) . ?
C5 C6 1.391(4) . ?
C5 C8 1.512(3) . ?
C6 C7 1.389(3) . ?
C9 C10 1.370(4) . ?
C10 C11 1.393(3) . ?
C11 C12 1.392(3) . ?
C11 C14 1.485(3) . ?
C12 C13 1.373(3) . ?
C14 C18 1.398(3) . ?
C14 C15 1.398(3) . ?
C15 C16 1.372(3) . ?
C17 C18 1.370(3) . ?
C19 C20 1.513(3) . ?
C20 C25 1.391(3) . ?
C20 C21 1.396(3) . ?
C21 C22 1.387(3) . ?
C22 C23 1.398(3) . ?
C23 C24 1.388(3) . ?
C23 C26 1.509(3) . ?
C24 C25 1.386(3) . ?
N31 C39 1.344(3) . ?
N31 C43 1.346(3) . ?
N31 C38 1.498(3) . ?
N32 C46 1.341(3) . ?
N32 C47 1.344(3) . ?
N32 C49 1.502(3) . ?
O31 C31 1.258(3) . ?
O32 C31 1.249(3) . ?
O33 C56 1.254(3) . ?
O34 C56 1.251(3) . ?
O34 Co1 2.0785(16) 14_456 ?
C31 C32 1.515(3) . ?
C32 C37 1.386(3) . ?
C32 C33 1.394(3) . ?
C33 C34 1.386(3) . ?
C34 C35 1.390(3) . ?
C35 C36 1.389(3) . ?
C35 C38 1.511(3) . ?
C36 C37 1.387(3) . ?
C39 C40 1.374(3) . ?
C40 C41 1.396(3) . ?
C41 C42 1.394(3) . ?
C41 C44 1.485(3) . ?
C42 C43 1.372(4) . ?
C44 C45 1.394(3) . ?
C44 C48 1.395(3) . ?
C45 C46 1.377(3) . ?
C47 C48 1.373(3) . ?
C49 C50 1.511(3) . ?
C50 C51 1.387(3) . ?
C50 C55 1.394(3) . ?
C51 C52 1.389(3) . ?
C52 C53 1.391(3) . ?
C53 C54 1.395(3) . ?
C53 C56 1.511(3) . ?
C54 C55 1.389(3) . ?
O71 C71 1.260(3) . ?
O72 C71 1.267(3) . ?
O73 C78 1.263(3) . ?
O74 C78 1.253(3) . ?
C71 C72 1.514(3) . ?
C72 C77 1.388(4) . ?
C72 C73 1.398(3) . ?
C73 C74 1.387(3) . ?
C74 C75 1.386(4) . ?
C75 C76 1.385(4) . ?
C75 C78 1.514(3) . ?
C76 C77 1.389(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O31 Co1 O34 88.49(7) . 15_556 ?
O31 Co1 O2W 177.07(7) . . ?
O34 Co1 O2W 88.59(7) 15_556 . ?
O31 Co1 O1 88.53(7) . . ?
O34 Co1 O1 84.45(6) 15_556 . ?
O2W Co1 O1 91.43(7) . . ?
O31 Co1 O3W 92.17(7) . . ?
O34 Co1 O3W 174.79(7) 15_556 . ?
O2W Co1 O3W 90.76(6) . . ?
O1 Co1 O3W 90.40(6) . . ?
O31 Co1 O1W 88.07(7) . . ?
O34 Co1 O1W 92.19(7) 15_556 . ?
O2W Co1 O1W 91.80(6) . . ?
O1 Co1 O1W 175.28(7) . . ?
O3W Co1 O1W 93.00(6) . . ?
O3 Co2 O3 87.72(7) 2_775 . ?
O3 Co2 O3 87.73(7) 2_775 3_575 ?
O3 Co2 O3 87.73(7) . 3_575 ?
O3 Co2 O4W 88.80(7) 2_775 2_775 ?
O3 Co2 O4W 89.38(7) . 2_775 ?
O3 Co2 O4W 175.56(7) 3_575 2_775 ?
O3 Co2 O4W 89.38(7) 2_775 3_575 ?
O3 Co2 O4W 175.56(8) . 3_575 ?
O3 Co2 O4W 88.80(7) 3_575 3_575 ?
O4W Co2 O4W 93.92(7) 2_775 3_575 ?
O3 Co2 O4W 175.56(8) 2_775 . ?
O3 Co2 O4W 88.80(7) . . ?
O3 Co2 O4W 89.37(7) 3_575 . ?
O4W Co2 O4W 93.93(7) 2_775 . ?
O4W Co2 O4W 93.92(7) 3_575 . ?
C1 O1 Co1 126.70(15) . . ?
C26 O3 Co2 129.06(16) . . ?
C13 N1 C9 120.3(2) . . ?
C13 N1 C8 119.7(2) . . ?
C9 N1 C8 120.0(2) . . ?
C16 N2 C17 120.7(2) . . ?
C16 N2 C19 119.9(2) . . ?
C17 N2 C19 119.3(2) . . ?
O1 C1 O2 125.6(2) . . ?
O1 C1 C2 117.4(2) . . ?
O2 C1 C2 117.0(2) . . ?
C3 C2 C7 119.6(2) . . ?
C3 C2 C1 119.7(2) . . ?
C7 C2 C1 120.7(2) . . ?
C2 C3 C4 120.5(2) . . ?
C3 C4 C5 120.2(2) . . ?
C4 C5 C6 119.2(2) . . ?
C4 C5 C8 119.7(2) . . ?
C6 C5 C8 121.1(2) . . ?
C7 C6 C5 120.5(2) . . ?
C2 C7 C6 120.0(2) . . ?
N1 C8 C5 111.19(19) . . ?
N1 C9 C10 120.9(2) . . ?
C9 C10 C11 120.2(2) . . ?
C12 C11 C10 117.3(2) . . ?
C12 C11 C14 120.8(2) . . ?
C10 C11 C14 121.8(2) . . ?
C13 C12 C11 120.4(2) . . ?
N1 C13 C12 120.8(2) . . ?
C18 C14 C15 116.9(2) . . ?
C18 C14 C11 121.9(2) . . ?
C15 C14 C11 121.3(2) . . ?
C16 C15 C14 120.6(2) . . ?
N2 C16 C15 120.6(2) . . ?
N2 C17 C18 120.6(2) . . ?
C17 C18 C14 120.6(2) . . ?
N2 C19 C20 110.93(19) . . ?
C25 C20 C21 119.5(2) . . ?
C25 C20 C19 119.9(2) . . ?
C21 C20 C19 120.6(2) . . ?
C22 C21 C20 120.2(2) . . ?
C21 C22 C23 120.2(2) . . ?
C24 C23 C22 119.4(2) . . ?
C24 C23 C26 120.1(2) . . ?
C22 C23 C26 120.6(2) . . ?
C25 C24 C23 120.6(2) . . ?
C24 C25 C20 120.2(2) . . ?
O4 C26 O3 126.0(2) . . ?
O4 C26 C23 117.7(2) . . ?
O3 C26 C23 116.3(2) . . ?
C39 N31 C43 120.3(2) . . ?
C39 N31 C38 119.43(19) . . ?
C43 N31 C38 120.2(2) . . ?
C46 N32 C47 120.4(2) . . ?
C46 N32 C49 119.8(2) . . ?
C47 N32 C49 119.85(19) . . ?
C31 O31 Co1 132.38(16) . . ?
C56 O34 Co1 129.76(15) . 14_456 ?
O32 C31 O31 126.3(2) . . ?
O32 C31 C32 119.0(2) . . ?
O31 C31 C32 114.8(2) . . ?
C37 C32 C33 119.6(2) . . ?
C37 C32 C31 120.7(2) . . ?
C33 C32 C31 119.6(2) . . ?
C34 C33 C32 120.4(2) . . ?
C33 C34 C35 119.9(2) . . ?
C36 C35 C34 119.5(2) . . ?
C36 C35 C38 120.0(2) . . ?
C34 C35 C38 120.4(2) . . ?
C37 C36 C35 120.6(2) . . ?
C32 C37 C36 119.9(2) . . ?
N31 C38 C35 111.5(2) . . ?
N31 C39 C40 120.9(2) . . ?
C39 C40 C41 120.2(2) . . ?
C42 C41 C40 117.4(2) . . ?
C42 C41 C44 121.4(2) . . ?
C40 C41 C44 121.2(2) . . ?
C43 C42 C41 120.3(2) . . ?
N31 C43 C42 120.9(2) . . ?
C45 C44 C48 117.6(2) . . ?
C45 C44 C41 120.8(2) . . ?
C48 C44 C41 121.6(2) . . ?
C46 C45 C44 120.3(2) . . ?
N32 C46 C45 120.6(2) . . ?
N32 C47 C48 121.3(2) . . ?
C47 C48 C44 119.7(2) . . ?
N32 C49 C50 110.37(19) . . ?
C51 C50 C55 119.6(2) . . ?
C51 C50 C49 120.6(2) . . ?
C55 C50 C49 119.8(2) . . ?
C50 C51 C52 120.1(2) . . ?
C51 C52 C53 120.6(2) . . ?
C52 C53 C54 119.2(2) . . ?
C52 C53 C56 121.0(2) . . ?
C54 C53 C56 119.8(2) . . ?
C55 C54 C53 120.2(2) . . ?
C54 C55 C50 120.3(2) . . ?
O34 C56 O33 125.8(2) . . ?
O34 C56 C53 116.2(2) . . ?
O33 C56 C53 118.0(2) . . ?
O71 C71 O72 125.0(2) . . ?
O71 C71 C72 117.7(2) . . ?
O72 C71 C72 117.4(2) . . ?
C77 C72 C73 119.3(2) . . ?
C77 C72 C71 120.9(2) . . ?
C73 C72 C71 119.8(2) . . ?
C74 C73 C72 119.7(2) . . ?
C75 C74 C73 120.9(2) . . ?
C76 C75 C74 119.4(2) . . ?
C76 C75 C78 120.2(2) . . ?
C74 C75 C78 120.4(2) . . ?
C75 C76 C77 120.2(3) . . ?
C72 C77 C76 120.5(2) . . ?
O74 C78 O73 125.2(2) . . ?
O74 C78 C75 118.4(2) . . ?
O73 C78 C75 116.5(2) . . ?

_refine_diff_density_max         0.926
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.070

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_an115
_database_code_depnum_ccdc_archive 'CCDC 1441126'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C180 H204 Br2 N12 Ni4 O81'
_chemical_formula_sum            'C180 H204 Br2 N12 Ni4 O81'
_chemical_formula_weight         4226.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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.
;

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

_cell_length_a                   35.0383(17)
_cell_length_b                   35.0383(17)
_cell_length_c                   27.5617(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     29304(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    81866
_cell_measurement_theta_min      1.923
_cell_measurement_theta_max      28.286

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             13188
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.887
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            81866
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.923
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16175
_reflns_number_gt                11058
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0983P)²+117.1401P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16175
_refine_ls_number_parameters     853
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.1942
_refine_ls_wR_factor_gt          0.1729
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.32901(2) 0.17687(2) 0.85614(2) 0.01931(11) Uani 1 1 d . . . . .
Ni2 Ni 0.6667 0.3333 0.14187(3) 0.02916(18) Uani 1 3 d S T P . .
Br1 Br 0.72474(6) 0.27706(6) -0.00204(6) 0.0801(6) Uani 0.3333 1 d . . P A 1
Br2 Br 0.7553(3) 0.2502(3) -0.0175(3) 0.168(3) Uiso 0.1667 1 d . . P B 2
Br3 Br 0.7060(3) 0.3020(3) 0.0023(3) 0.182(3) Uiso 0.1667 1 d . . P C 3
N1 N 0.49061(9) 0.30451(9) 0.58334(9) 0.0262(6) Uani 1 1 d . . . . .
N2 N 0.51930(9) 0.17605(9) 0.40764(9) 0.0242(6) Uani 1 1 d . . . . .
O1 O 0.36889(8) 0.22585(7) 0.80693(8) 0.0253(5) Uani 1 1 d . . . . .
O2 O 0.43515(8) 0.23727(8) 0.82950(8) 0.0312(5) Uani 1 1 d . . . . .
O3 O 0.63107(8) 0.28072(8) 0.18698(9) 0.0329(5) Uani 1 1 d . . . . .
O4 O 0.56147(9) 0.25917(9) 0.16532(9) 0.0369(6) Uani 1 1 d . . . . .
C1 C 0.40901(11) 0.24052(10) 0.80008(11) 0.0240(6) Uani 1 1 d . . . . .
C2 C 0.42845(11) 0.26410(10) 0.75272(11) 0.0233(6) Uani 1 1 d . . . . .
C3 C 0.47372(11) 0.29089(11) 0.74833(12) 0.0291(7) Uani 1 1 d . . . . .
H3 H 0.4923 0.2939 0.7749 0.035 Uiso 1 1 calc R U . . .
C4 C 0.49213(12) 0.31335(12) 0.70545(12) 0.0316(7) Uani 1 1 d . . . . .
H4 H 0.5232 0.3318 0.7029 0.038 Uiso 1 1 calc R U . . .
C5 C 0.46514(11) 0.30884(11) 0.66614(11) 0.0261(7) Uani 1 1 d . . . . .
C6 C 0.41978(11) 0.28173(11) 0.67035(11) 0.0271(7) Uani 1 1 d . . . . .
H6 H 0.4012 0.2783 0.6436 0.033 Uiso 1 1 calc R U . . .
C7 C 0.40145(11) 0.25957(11) 0.71357(11) 0.0253(7) Uani 1 1 d . . . . .
H7 H 0.3704 0.2413 0.7164 0.030 Uiso 1 1 calc R U . . .
C8 C 0.48550(12) 0.33330(11) 0.61936(11) 0.0293(7) Uani 1 1 d . . . . .
H8A H 0.4666 0.3441 0.6054 0.035 Uiso 1 1 calc R U . . .
H8B H 0.5147 0.3592 0.6264 0.035 Uiso 1 1 calc R U . . .
C9 C 0.52105(12) 0.29238(12) 0.59006(12) 0.0320(8) Uani 1 1 d . . . . .
H9 H 0.5392 0.3022 0.6182 0.038 Uiso 1 1 calc R U . . .
C10 C 0.52655(11) 0.26613(12) 0.55735(12) 0.0302(7) Uani 1 1 d . . . . .
H10 H 0.5485 0.2582 0.5626 0.036 Uiso 1 1 calc R U . . .
C11 C 0.49979(10) 0.25098(10) 0.51617(11) 0.0228(6) Uani 1 1 d . . . . .
C12 C 0.46814(11) 0.26332(11) 0.51039(12) 0.0268(7) Uani 1 1 d . . . . .
H12 H 0.4490 0.2532 0.4831 0.032 Uiso 1 1 calc R U . . .
C13 C 0.46434(12) 0.29023(12) 0.54406(11) 0.0291(7) Uani 1 1 d . . . . .
H13 H 0.4428 0.2989 0.5395 0.035 Uiso 1 1 calc R U . . .
C14 C 0.50541(10) 0.22332(10) 0.47912(11) 0.0218(6) Uani 1 1 d . . . . .
C15 C 0.53948(11) 0.21358(12) 0.48275(12) 0.0294(7) Uani 1 1 d . . . . .
H15 H 0.5586 0.2235 0.5101 0.035 Uiso 1 1 calc R U . . .
C16 C 0.54539(11) 0.18980(12) 0.44710(12) 0.0305(7) Uani 1 1 d . . . . .
H16 H 0.5683 0.1829 0.4503 0.037 Uiso 1 1 calc R U . . .
C17 C 0.48579(11) 0.18424(11) 0.40314(12) 0.0272(7) Uani 1 1 d . . . . .
H17 H 0.4673 0.1740 0.3753 0.033 Uiso 1 1 calc R U . . .
C18 C 0.47804(11) 0.20726(11) 0.43846(11) 0.0258(7) Uani 1 1 d . . . . .
H18 H 0.4539 0.2123 0.4352 0.031 Uiso 1 1 calc R U . . .
C19 C 0.52800(12) 0.15244(11) 0.36784(12) 0.0292(7) Uani 1 1 d . . . . .
H19A H 0.5005 0.1247 0.3602 0.035 Uiso 1 1 calc R U . . .
H19B H 0.5503 0.1448 0.3787 0.035 Uiso 1 1 calc R U . . .
C20 C 0.54440(11) 0.18071(10) 0.32283(11) 0.0245(6) Uani 1 1 d . . . . .
C21 C 0.58853(11) 0.21331(11) 0.31839(12) 0.0280(7) Uani 1 1 d . . . . .
H21 H 0.6086 0.2179 0.3440 0.034 Uiso 1 1 calc R U . . .
C22 C 0.60334(11) 0.23907(11) 0.27688(12) 0.0274(7) Uani 1 1 d . . . . .
H22 H 0.6335 0.2611 0.2740 0.033 Uiso 1 1 calc R U . . .
C23 C 0.57410(11) 0.23277(11) 0.23943(11) 0.0263(7) Uani 1 1 d . . . . .
C24 C 0.59018(12) 0.25994(11) 0.19344(12) 0.0283(7) Uani 1 1 d . . . . .
C25 C 0.52998(12) 0.20070(12) 0.24386(12) 0.0296(7) Uani 1 1 d . . . . .
H25 H 0.5099 0.1967 0.2186 0.036 Uiso 1 1 calc R U . . .
C26 C 0.51515(11) 0.17439(12) 0.28518(12) 0.0298(7) Uani 1 1 d . . . . .
H26 H 0.4851 0.1521 0.2878 0.036 Uiso 1 1 calc R U . . .
N31 N 0.19338(9) 0.17605(9) 0.58067(9) 0.0243(6) Uani 1 1 d . . . . .
N32 N 0.31571(8) 0.32622(9) 0.39675(9) 0.0234(5) Uani 1 1 d . . . . .
O31 O 0.27739(8) 0.16463(7) 0.81342(8) 0.0268(5) Uani 1 1 d . . . . .
O32 O 0.26066(8) 0.21710(8) 0.82994(8) 0.0297(5) Uani 1 1 d . . . . .
O33 O 0.22365(8) 0.29322(8) 0.15857(8) 0.0323(5) Uani 1 1 d . . . . .
O34 O 0.20329(7) 0.33961(8) 0.18840(8) 0.0266(5) Uani 1 1 d . . . . .
C31 C 0.25986(10) 0.18741(10) 0.80387(11) 0.0219(6) Uani 1 1 d . . . . .
C32 C 0.23564(10) 0.17685(10) 0.75585(10) 0.0209(6) Uani 1 1 d . . . . .
C33 C 0.24183(10) 0.15088(10) 0.72180(11) 0.0225(6) Uani 1 1 d . . . . .
H33 H 0.2615 0.1403 0.7288 0.027 Uiso 1 1 calc R U . . .
C34 C 0.21959(11) 0.14038(10) 0.67794(11) 0.0245(6) Uani 1 1 d . . . . .
H34 H 0.2242 0.1229 0.6550 0.029 Uiso 1 1 calc R U . . .
C35 C 0.19042(11) 0.15544(11) 0.66746(11) 0.0246(6) Uani 1 1 d . . . . .
C36 C 0.18406(11) 0.18085(12) 0.70159(12) 0.0288(7) Uani 1 1 d . . . . .
H36 H 0.1639 0.1909 0.6949 0.035 Uiso 1 1 calc R U . . .
C37 C 0.20672(11) 0.19184(11) 0.74532(11) 0.0261(7) Uani 1 1 d . . . . .
H37 H 0.2024 0.2097 0.7681 0.031 Uiso 1 1 calc R U . . .
C38 C 0.16608(11) 0.14407(11) 0.61967(11) 0.0282(7) Uani 1 1 d . . . . .
H38A H 0.1586 0.1139 0.6099 0.034 Uiso 1 1 calc R U . . .
H38B H 0.1382 0.1445 0.6236 0.034 Uiso 1 1 calc R U . . .
C39 C 0.20869(12) 0.16276(11) 0.54351(12) 0.0289(7) Uani 1 1 d . . . . .
H39 H 0.2021 0.1330 0.5421 0.035 Uiso 1 1 calc R U . . .
C40 C 0.23365(11) 0.19146(11) 0.50753(11) 0.0269(7) Uani 1 1 d . . . . .
H40 H 0.2442 0.1814 0.4816 0.032 Uiso 1 1 calc R U . . .
C41 C 0.24360(10) 0.23531(11) 0.50885(11) 0.0229(6) Uani 1 1 d . . . . .
C42 C 0.22704(11) 0.24799(11) 0.54802(11) 0.0266(7) Uani 1 1 d . . . . .
H42 H 0.2331 0.2776 0.5505 0.032 Uiso 1 1 calc R U . . .
C43 C 0.20189(11) 0.21764(11) 0.58307(11) 0.0265(7) Uani 1 1 d . . . . .
H43 H 0.1905 0.2265 0.6093 0.032 Uiso 1 1 calc R U . . .
C44 C 0.26988(10) 0.26698(11) 0.47025(11) 0.0223(6) Uani 1 1 d . . . . .
C45 C 0.27848(11) 0.25280(11) 0.42646(11) 0.0267(7) Uani 1 1 d . . . . .
H45 H 0.2687 0.2225 0.4215 0.032 Uiso 1 1 calc R U . . .
C46 C 0.30134(11) 0.28321(11) 0.39019(12) 0.0277(7) Uani 1 1 d . . . . .
H46 H 0.3069 0.2734 0.3603 0.033 Uiso 1 1 calc R U . . .
C47 C 0.30887(11) 0.34088(11) 0.43911(11) 0.0272(7) Uani 1 1 d . . . . .
H47 H 0.3201 0.3715 0.4437 0.033 Uiso 1 1 calc R U . . .
C48 C 0.28591(11) 0.31198(11) 0.47586(11) 0.0275(7) Uani 1 1 d . . . . .
H48 H 0.2809 0.3228 0.5054 0.033 Uiso 1 1 calc R U . . .
C49 C 0.34017(11) 0.35811(11) 0.35673(11) 0.0265(7) Uani 1 1 d . . . . .
H49A H 0.3663 0.3558 0.3476 0.032 Uiso 1 1 calc R U . . .
H49B H 0.3506 0.3885 0.3682 0.032 Uiso 1 1 calc R U . . .
C50 C 0.31081(10) 0.34869(10) 0.31271(11) 0.0226(6) Uani 1 1 d . . . . .
C51 C 0.31319(11) 0.32470(11) 0.27401(11) 0.0269(7) Uani 1 1 d . . . . .
H51 H 0.3340 0.3149 0.2745 0.032 Uiso 1 1 calc R U . . .
C52 C 0.28518(11) 0.31490(11) 0.23438(11) 0.0252(7) Uani 1 1 d . . . . .
H52 H 0.2866 0.2981 0.2082 0.030 Uiso 1 1 calc R U . . .
C53 C 0.25506(10) 0.32977(10) 0.23310(10) 0.0206(6) Uani 1 1 d . . . . .
C54 C 0.22485(10) 0.32001(10) 0.18963(11) 0.0212(6) Uani 1 1 d . . . . .
C55 C 0.25293(10) 0.35429(10) 0.27192(11) 0.0228(6) Uani 1 1 d . . . . .
H55 H 0.2325 0.3646 0.2711 0.027 Uiso 1 1 calc R U . . .
C56 C 0.28046(10) 0.36351(10) 0.31143(11) 0.0231(6) Uani 1 1 d . . . . .
H56 H 0.2788 0.3800 0.3379 0.028 Uiso 1 1 calc R U . . .
O71 O 0.42477(9) 0.20721(9) 1.22640(9) 0.0383(6) Uani 1 1 d . . . . .
O72 O 0.37601(9) 0.22892(9) 1.24340(8) 0.0374(6) Uani 1 1 d . . . . .
O73 O 0.40183(9) 0.23104(9) 0.97916(8) 0.0422(7) Uani 1 1 d . . . . .
O74 O 0.33890(10) 0.23023(10) 0.99284(9) 0.0439(7) Uani 1 1 d . . . . .
C71 C 0.39828(12) 0.22007(11) 1.21423(12) 0.0313(8) Uani 1 1 d . . . . .
C72 C 0.39318(12) 0.22583(11) 1.16031(12) 0.0310(7) Uani 1 1 d . . . . .
C73 C 0.42395(13) 0.22694(11) 1.12744(12) 0.0327(8) Uani 1 1 d . . . . .
H73 H 0.4492 0.2262 1.1387 0.039 Uiso 1 1 calc R U . . .
C74 C 0.41740(13) 0.22919(11) 1.07793(12) 0.0314(8) Uani 1 1 d . . . . .
H74 H 0.4384 0.2300 1.0555 0.038 Uiso 1 1 calc R U . . .
C75 C 0.38087(12) 0.23028(11) 1.06080(11) 0.0304(8) Uani 1 1 d . . . . .
C76 C 0.35094(13) 0.23068(13) 1.09384(12) 0.0386(9) Uani 1 1 d . . . . .
H76 H 0.3261 0.2322 1.0826 0.046 Uiso 1 1 calc R U . . .
C77 C 0.35758(13) 0.22888(13) 1.14331(12) 0.0381(9) Uani 1 1 d . . . . .
H77 H 0.3375 0.2298 1.1658 0.046 Uiso 1 1 calc R U . . .
C78 C 0.37309(13) 0.23067(11) 1.00681(12) 0.0319(8) Uani 1 1 d . . . . .
O1W O 0.38227(8) 0.18614(8) 0.89680(8) 0.0266(5) Uani 1 1 d . . . . .
H1WA H 0.3802 0.1618 0.9037 0.040 Uiso 1 1 d R U . . .
H1WB H 0.3840 0.1993 0.9229 0.040 Uiso 1 1 d R U . . .
O2W O 0.28505(7) 0.12488(7) 0.90067(7) 0.0245(5) Uani 1 1 d . . . . .
H2WA H 0.2945 0.1279 0.9292 0.037 Uiso 1 1 d R U . . .
H2WB H 0.2810 0.1006 0.8905 0.037 Uiso 1 1 d R U . . .
O3W O 0.32289(7) 0.22324(7) 0.89679(7) 0.0249(5) Uani 1 1 d . . . . .
H3WA H 0.3237 0.2191 0.9267 0.037 Uiso 1 1 d R U . . .
H3WB H 0.2990 0.2225 0.8910 0.037 Uiso 1 1 d R U . . .
O4W O 0.68261(9) 0.29298(9) 0.10084(9) 0.0387(6) Uani 1 1 d . . . . .
H4WA H 0.7052 0.2944 0.1132 0.058 Uiso 1 1 d R U . . .
H4WB H 0.6906 0.2995 0.0718 0.058 Uiso 1 1 d R U . . .
O5W O 0.41760(11) 0.16776(12) 1.31824(10) 0.0608(9) Uani 1 1 d G . . . .
H5WA H 0.3924 0.1459 1.3231 0.091 Uiso 1 1 d R U . . .
H5WB H 0.4175 0.1804 1.2924 0.091 Uiso 1 1 d R U . . .
O6W O 0.0843(4) 0.1623(4) 0.5585(4) 0.110(4) Uiso 0.5 1 d . . P D 1
O6W' O 0.0952(3) 0.1528(3) 0.5448(3) 0.084(3) Uiso 0.5 1 d . . P E 2
O7W O 0.09771(17) 0.07035(18) 0.52373(18) 0.0668(13) Uiso 0.75 1 d . . P F 1
O7W' O 0.0880(6) 0.0408(6) 0.5202(6) 0.079(4) Uiso 0.25 1 d . . P G 2
O8W O 0.26596(12) 0.02218(12) 0.99053(12) 0.0623(9) Uani 1 1 d . . . . .
H8WA H 0.2699 0.0365 1.0163 0.093 Uiso 1 1 d R U . . .
H8WB H 0.2458 -0.0040 0.9948 0.093 Uiso 1 1 d R U . . .
O9W O 0.30795(9) 0.11329(9) 0.99184(8) 0.0405(6) Uani 1 1 d . . . . .
H9WA H 0.3351 0.1313 0.9900 0.061 Uiso 1 1 d R U . . .
H9WB H 0.2996 0.1118 1.0207 0.061 Uiso 1 1 d R U . . .
O10W O 0.41166(11) 0.32043(10) 1.24273(10) 0.0535(8) Uani 1 1 d G . . . .
H10A H 0.4210 0.3325 1.2156 0.080 Uiso 1 1 d R U . . .
H10B H 0.3995 0.2929 1.2398 0.080 Uiso 1 1 d R U . . .
O11W O 0.26939(9) 0.19076(10) 0.33713(9) 0.0440(7) Uani 1 1 d G . . . .
H11A H 0.2519 0.1969 0.3513 0.066 Uiso 1 1 d R U . . .
H11B H 0.2575 0.1633 0.3343 0.066 Uiso 1 1 d R U . . .
O12W O 0.28978(10) 0.21929(9) 0.24522(9) 0.0431(7) Uani 1 1 d . . . . .
H12A H 0.2821 0.2098 0.2736 0.065 Uiso 1 1 d R U . . .
H12B H 0.3101 0.2148 0.2362 0.065 Uiso 1 1 d R U . . .
O13W O 0.23869(10) 0.19056(9) 0.16359(9) 0.0433(7) Uani 1 1 d . . . . .
H13A H 0.2375 0.1689 0.1492 0.065 Uiso 1 1 d R U . . .
H13B H 0.2484 0.2121 0.1446 0.065 Uiso 1 1 d R U . . .
O14W O 0.26961(9) 0.26349(9) 0.10488(10) 0.0423(6) Uani 1 1 d . . . . .
H14A H 0.2631 0.2622 0.0754 0.064 Uiso 1 1 d R U . . .
H14B H 0.2581 0.2758 0.1204 0.064 Uiso 1 1 d R U . . .
O15W O 0.7516(3) 0.3745(3) -0.0382(3) 0.181(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O31 2.016(2) . ?
Ni1 O34 2.047(2) 11_556 ?
Ni1 O1W 2.059(2) . ?
Ni1 O3W 2.071(2) . ?
Ni1 O1 2.083(2) . ?
Ni1 O2W 2.096(2) . ?
Ni2 O3 2.049(2) . ?
Ni2 O3 2.050(2) 2_655 ?
Ni2 O3 2.049(2) 3_665 ?
Ni2 O4W 2.093(3) . ?
Ni2 O4W 2.093(3) 2_655 ?
Ni2 O4W 2.093(3) 3_665 ?
N1 C9 1.344(5) . ?
N1 C13 1.345(4) . ?
N1 C8 1.489(4) . ?
N2 C16 1.346(4) . ?
N2 C17 1.347(4) . ?
N2 C19 1.494(4) . ?
O1 C1 1.246(4) . ?
O2 C1 1.270(4) . ?
O3 C24 1.253(4) . ?
O4 C24 1.260(4) . ?
C1 C2 1.513(4) . ?
C2 C3 1.386(5) . ?
C2 C7 1.391(5) . ?
C3 C4 1.387(5) . ?
C4 C5 1.394(5) . ?
C5 C6 1.390(5) . ?
C5 C8 1.515(4) . ?
C6 C7 1.391(4) . ?
C9 C10 1.369(5) . ?
C10 C11 1.397(4) . ?
C11 C12 1.386(5) . ?
C11 C14 1.487(4) . ?
C12 C13 1.376(5) . ?
C14 C18 1.397(4) . ?
C14 C15 1.399(4) . ?
C15 C16 1.370(5) . ?
C17 C18 1.375(5) . ?
C19 C20 1.511(5) . ?
C20 C21 1.394(5) . ?
C20 C26 1.396(5) . ?
C21 C22 1.387(5) . ?
C22 C23 1.392(5) . ?
C23 C25 1.389(5) . ?
C23 C24 1.515(5) . ?
C25 C26 1.392(5) . ?
N31 C43 1.335(4) . ?
N31 C39 1.343(4) . ?
N31 C38 1.502(4) . ?
N32 C46 1.341(4) . ?
N32 C47 1.344(4) . ?
N32 C49 1.497(4) . ?
O31 C31 1.255(4) . ?
O32 C31 1.253(4) . ?
O33 C54 1.256(4) . ?
O34 C54 1.250(4) . ?
O34 Ni1 2.047(2) 12_556 ?
C31 C32 1.515(4) . ?
C32 C37 1.385(4) . ?
C32 C33 1.397(4) . ?
C33 C34 1.385(4) . ?
C34 C35 1.395(5) . ?
C35 C36 1.388(5) . ?
C35 C38 1.510(4) . ?
C36 C37 1.388(5) . ?
C39 C40 1.371(5) . ?
C40 C41 1.396(4) . ?
C41 C42 1.399(4) . ?
C41 C44 1.480(4) . ?
C42 C43 1.380(5) . ?
C44 C48 1.393(5) . ?
C44 C45 1.394(4) . ?
C45 C46 1.387(5) . ?
C47 C48 1.372(5) . ?
C49 C50 1.517(4) . ?
C50 C51 1.386(4) . ?
C50 C56 1.398(4) . ?
C51 C52 1.392(4) . ?
C52 C53 1.391(4) . ?
C53 C55 1.397(4) . ?
C53 C54 1.520(4) . ?
C55 C56 1.382(4) . ?
O71 C71 1.263(4) . ?
O72 C71 1.262(4) . ?
O73 C78 1.258(4) . ?
O74 C78 1.251(5) . ?
C71 C72 1.522(5) . ?
C72 C77 1.386(5) . ?
C72 C73 1.394(5) . ?
C73 C74 1.393(5) . ?
C74 C75 1.383(5) . ?
C75 C76 1.394(5) . ?
C75 C78 1.514(4) . ?
C76 C77 1.390(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O31 Ni1 O34 87.53(9) . 11_556 ?
O31 Ni1 O1W 175.86(9) . . ?
O34 Ni1 O1W 88.35(9) 11_556 . ?
O31 Ni1 O3W 92.82(9) . . ?
O34 Ni1 O3W 174.09(9) 11_556 . ?
O1W Ni1 O3W 91.31(9) . . ?
O31 Ni1 O1 87.47(9) . . ?
O34 Ni1 O1 84.35(9) 11_556 . ?
O1W Ni1 O1 92.45(9) . . ?
O3W Ni1 O1 89.77(9) . . ?
O31 Ni1 O2W 88.05(9) . . ?
O34 Ni1 O2W 93.29(9) 11_556 . ?
O1W Ni1 O2W 91.86(9) . . ?
O3W Ni1 O2W 92.62(9) . . ?
O1 Ni1 O2W 175.02(9) . . ?
O3 Ni2 O3 87.03(10) . 2_655 ?
O3 Ni2 O3 87.02(10) . 3_665 ?
O3 Ni2 O3 87.03(10) 2_655 3_665 ?
O3 Ni2 O4W 88.17(10) . . ?
O3 Ni2 O4W 91.09(10) 2_655 . ?
O3 Ni2 O4W 174.92(10) 3_665 . ?
O3 Ni2 O4W 174.93(11) . 2_655 ?
O3 Ni2 O4W 88.17(10) 2_655 2_655 ?
O3 Ni2 O4W 91.09(10) 3_665 2_655 ?
O4W Ni2 O4W 93.56(10) . 2_655 ?
O3 Ni2 O4W 91.10(10) . 3_665 ?
O3 Ni2 O4W 174.93(10) 2_655 3_665 ?
O3 Ni2 O4W 88.17(10) 3_665 3_665 ?
O4W Ni2 O4W 93.56(10) . 3_665 ?
O4W Ni2 O4W 93.55(10) 2_655 3_665 ?
C9 N1 C13 119.8(3) . . ?
C9 N1 C8 120.4(3) . . ?
C13 N1 C8 119.8(3) . . ?
C16 N2 C17 120.4(3) . . ?
C16 N2 C19 120.1(3) . . ?
C17 N2 C19 119.4(3) . . ?
C1 O1 Ni1 126.3(2) . . ?
C24 O3 Ni2 127.8(2) . . ?
O1 C1 O2 125.6(3) . . ?
O1 C1 C2 117.6(3) . . ?
O2 C1 C2 116.9(3) . . ?
C3 C2 C7 119.5(3) . . ?
C3 C2 C1 119.7(3) . . ?
C7 C2 C1 120.8(3) . . ?
C2 C3 C4 120.6(3) . . ?
C3 C4 C5 120.1(3) . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 C8 120.8(3) . . ?
C4 C5 C8 119.8(3) . . ?
C5 C6 C7 120.3(3) . . ?
C2 C7 C6 120.2(3) . . ?
N1 C8 C5 111.5(3) . . ?
N1 C9 C10 121.5(3) . . ?
C9 C10 C11 119.8(3) . . ?
C12 C11 C10 117.7(3) . . ?
C12 C11 C14 120.8(3) . . ?
C10 C11 C14 121.5(3) . . ?
C13 C12 C11 120.2(3) . . ?
N1 C13 C12 121.0(3) . . ?
C18 C14 C15 117.2(3) . . ?
C18 C14 C11 121.7(3) . . ?
C15 C14 C11 121.1(3) . . ?
C16 C15 C14 120.3(3) . . ?
N2 C16 C15 121.0(3) . . ?
N2 C17 C18 120.6(3) . . ?
C17 C18 C14 120.5(3) . . ?
N2 C19 C20 110.8(3) . . ?
C21 C20 C26 119.4(3) . . ?
C21 C20 C19 120.8(3) . . ?
C26 C20 C19 119.9(3) . . ?
C22 C21 C20 120.4(3) . . ?
C21 C22 C23 120.1(3) . . ?
C25 C23 C22 119.7(3) . . ?
C25 C23 C24 119.7(3) . . ?
C22 C23 C24 120.5(3) . . ?
O3 C24 O4 126.4(3) . . ?
O3 C24 C23 116.2(3) . . ?
O4 C24 C23 117.3(3) . . ?
C23 C25 C26 120.2(3) . . ?
C25 C26 C20 120.1(3) . . ?
C43 N31 C39 120.4(3) . . ?
C43 N31 C38 119.4(3) . . ?
C39 N31 C38 120.2(3) . . ?
C46 N32 C47 120.5(3) . . ?
C46 N32 C49 119.5(3) . . ?
C47 N32 C49 120.0(3) . . ?
C31 O31 Ni1 131.3(2) . . ?
C54 O34 Ni1 129.1(2) . 12_556 ?
O32 C31 O31 126.4(3) . . ?
O32 C31 C32 118.7(3) . . ?
O31 C31 C32 114.9(3) . . ?
C37 C32 C33 119.2(3) . . ?
C37 C32 C31 121.1(3) . . ?
C33 C32 C31 119.7(3) . . ?
C34 C33 C32 120.6(3) . . ?
C33 C34 C35 120.1(3) . . ?
C36 C35 C34 119.0(3) . . ?
C36 C35 C38 120.7(3) . . ?
C34 C35 C38 120.3(3) . . ?
C37 C36 C35 120.9(3) . . ?
C32 C37 C36 120.2(3) . . ?
N31 C38 C35 111.2(3) . . ?
N31 C39 C40 121.1(3) . . ?
C39 C40 C41 120.4(3) . . ?
C40 C41 C42 117.0(3) . . ?
C40 C41 C44 121.7(3) . . ?
C42 C41 C44 121.2(3) . . ?
C43 C42 C41 120.1(3) . . ?
N31 C43 C42 121.0(3) . . ?
C48 C44 C45 117.6(3) . . ?
C48 C44 C41 121.1(3) . . ?
C45 C44 C41 121.3(3) . . ?
C46 C45 C44 119.7(3) . . ?
N32 C46 C45 121.0(3) . . ?
N32 C47 C48 120.7(3) . . ?
C47 C48 C44 120.6(3) . . ?
N32 C49 C50 110.7(3) . . ?
C51 C50 C56 119.6(3) . . ?
C51 C50 C49 120.5(3) . . ?
C56 C50 C49 119.9(3) . . ?
C50 C51 C52 120.3(3) . . ?
C53 C52 C51 120.1(3) . . ?
C52 C53 C55 119.6(3) . . ?
C52 C53 C54 120.6(3) . . ?
C55 C53 C54 119.8(3) . . ?
O34 C54 O33 126.1(3) . . ?
O34 C54 C53 116.2(3) . . ?
O33 C54 C53 117.7(3) . . ?
C56 C55 C53 120.1(3) . . ?
C55 C56 C50 120.3(3) . . ?
O72 C71 O71 125.0(3) . . ?
O72 C71 C72 117.5(3) . . ?
O71 C71 C72 117.6(3) . . ?
C77 C72 C73 119.5(3) . . ?
C77 C72 C71 120.7(3) . . ?
C73 C72 C71 119.8(3) . . ?
C74 C73 C72 119.4(4) . . ?
C75 C74 C73 121.1(3) . . ?
C74 C75 C76 119.3(3) . . ?
C74 C75 C78 120.6(3) . . ?
C76 C75 C78 120.1(3) . . ?
C77 C76 C75 119.8(4) . . ?
C72 C77 C76 120.8(3) . . ?
O74 C78 O73 124.8(3) . . ?
O74 C78 C75 118.5(3) . . ?
O73 C78 C75 116.7(3) . . ?

_refine_diff_density_max         1.962
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.092

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_da352
_database_code_depnum_ccdc_archive 'CCDC 1441127'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H52 Cd N3 O19'
_chemical_formula_sum            'C47 H52 Cd N3 O19'
_chemical_formula_weight         1075.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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

_cell_length_a                   12.1281(2)
_cell_length_b                   16.5109(3)
_cell_length_c                   23.7085(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.5049(10)
_cell_angle_gamma                90
_cell_volume                     4738.65(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    89372
_cell_measurement_theta_min      1.504
_cell_measurement_theta_max      28.332

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_F_000             2220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.543
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            89372
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.504
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11725
_reflns_number_gt                7823
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0466P)²+3.5887P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11725
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cd1 Cd 0.08976(2) -0.62325(2) 0.34928(2) 0.02852(7) Uani 1 1 d . . . . .
N1 N -0.1500(2) -0.93337(15) 0.62719(11) 0.0321(6) Uani 1 1 d . . . . .
N2 N -0.4724(2) -0.67663(16) 0.78240(11) 0.0329(6) Uani 1 1 d . . . . .
O1 O 0.0549(2) -0.70534(14) 0.41814(10) 0.0439(6) Uani 1 1 d . . . . .
O2 O 0.2139(2) -0.77246(16) 0.42067(10) 0.0462(6) Uani 1 1 d . . . . .
O3 O -0.88048(18) -0.42119(14) 0.64809(9) 0.0362(5) Uani 1 1 d . . . . .
O4 O -0.99331(17) -0.46591(14) 0.71071(9) 0.0358(5) Uani 1 1 d . . . . .
C1 C 0.1176(3) -0.7622(2) 0.43466(13) 0.0345(7) Uani 1 1 d . . . . .
C2 C 0.0690(3) -0.81952(19) 0.47597(13) 0.0324(7) Uani 1 1 d . . . . .
C3 C 0.1351(3) -0.8588(2) 0.51715(14) 0.0364(8) Uani 1 1 d . . . . .
H3 H 0.2126 -0.8502 0.5196 0.044 Uiso 1 1 calc R U . . .
C4 C 0.0875(3) -0.9109(2) 0.55478(14) 0.0377(8) Uani 1 1 d . . . . .
H4 H 0.1326 -0.9363 0.5838 0.045 Uiso 1 1 calc R U . . .
C5 C -0.0243(3) -0.92579(19) 0.55032(14) 0.0349(8) Uani 1 1 d . . . . .
C6 C -0.0898(3) -0.8874(2) 0.50858(15) 0.0413(8) Uani 1 1 d . . . . .
H6 H -0.1669 -0.8983 0.5049 0.050 Uiso 1 1 calc R U . . .
C7 C -0.0442(3) -0.8335(2) 0.47228(15) 0.0386(8) Uani 1 1 d . . . . .
H7 H -0.0902 -0.8058 0.4447 0.046 Uiso 1 1 calc R U . . .
C8 C -0.0769(3) -0.9822(2) 0.59130(15) 0.0403(8) Uani 1 1 d . . . . .
H8A H -0.1210 -1.0240 0.5702 0.048 Uiso 1 1 calc R U . . .
H8B H -0.0189 -1.0097 0.6155 0.048 Uiso 1 1 calc R U . . .
C9 C -0.1028(3) -0.88079(19) 0.66449(14) 0.0342(7) Uani 1 1 d . . . . .
H9 H -0.0246 -0.8777 0.6693 0.041 Uiso 1 1 calc R U . . .
C10 C -0.1667(3) -0.83161(19) 0.69558(13) 0.0311(7) Uani 1 1 d . . . . .
H10 H -0.1330 -0.7952 0.7224 0.037 Uiso 1 1 calc R U . . .
C11 C -0.2814(3) -0.83508(18) 0.68775(12) 0.0276(6) Uani 1 1 d . . . . .
C12 C -0.3278(3) -0.89225(18) 0.65012(13) 0.0315(7) Uani 1 1 d . . . . .
H12 H -0.4058 -0.8974 0.6449 0.038 Uiso 1 1 calc R U . . .
C13 C -0.2600(3) -0.94096(19) 0.62068(13) 0.0332(7) Uani 1 1 d . . . . .
H13 H -0.2914 -0.9805 0.5954 0.040 Uiso 1 1 calc R U . . .
C14 C -0.3507(2) -0.77967(18) 0.71961(12) 0.0276(6) Uani 1 1 d . . . . .
C15 C -0.3121(3) -0.70299(19) 0.73402(14) 0.0338(7) Uani 1 1 d . . . . .
H15 H -0.2428 -0.6853 0.7220 0.041 Uiso 1 1 calc R U . . .
C16 C -0.3739(3) -0.6522(2) 0.76576(14) 0.0366(8) Uani 1 1 d . . . . .
H16 H -0.3468 -0.5998 0.7759 0.044 Uiso 1 1 calc R U . . .
C17 C -0.5137(3) -0.7496(2) 0.76748(14) 0.0366(8) Uani 1 1 d . . . . .
H17 H -0.5845 -0.7651 0.7789 0.044 Uiso 1 1 calc R U . . .
C18 C -0.4547(3) -0.80184(19) 0.73596(14) 0.0330(7) Uani 1 1 d . . . . .
H18 H -0.4848 -0.8531 0.7253 0.040 Uiso 1 1 calc R U . . .
C19 C -0.5368(3) -0.6222(2) 0.81807(14) 0.0395(8) Uani 1 1 d . . . . .
H19A H -0.4874 -0.5800 0.8352 0.047 Uiso 1 1 calc R U . . .
H19B H -0.5668 -0.6539 0.8491 0.047 Uiso 1 1 calc R U . . .
C20 C -0.6304(3) -0.5826(2) 0.78357(13) 0.0323(7) Uani 1 1 d . . . . .
C21 C -0.6094(3) -0.5275(2) 0.74122(13) 0.0328(7) Uani 1 1 d . . . . .
H21 H -0.5353 -0.5159 0.7331 0.039 Uiso 1 1 calc R U . . .
C22 C -0.6954(3) -0.48943(19) 0.71078(13) 0.0302(7) Uani 1 1 d . . . . .
H22 H -0.6802 -0.4525 0.6815 0.036 Uiso 1 1 calc R U . . .
C23 C -0.8043(2) -0.50515(18) 0.72300(12) 0.0282(7) Uani 1 1 d . . . . .
C24 C -0.8983(3) -0.46171(18) 0.69139(13) 0.0289(7) Uani 1 1 d . . . . .
C25 C -0.8250(3) -0.55969(18) 0.76502(13) 0.0295(7) Uani 1 1 d . . . . .
H25 H -0.8991 -0.5705 0.7735 0.035 Uiso 1 1 calc R U . . .
C26 C -0.7389(3) -0.59922(19) 0.79512(13) 0.0319(7) Uani 1 1 d . . . . .
H26 H -0.7543 -0.6375 0.8235 0.038 Uiso 1 1 calc R U . . .
N31 N 0.2369(2) -0.92934(15) 0.02936(10) 0.0260(5) Uani 1 1 d . . . . .
O31 O 0.0550(2) -0.71811(14) 0.28051(9) 0.0413(6) Uani 1 1 d . . . . .
O32 O 0.2239(2) -0.67389(14) 0.26724(10) 0.0445(6) Uani 1 1 d . . . . .
C31 C 0.1405(3) -0.71429(19) 0.25164(13) 0.0340(7) Uani 1 1 d . . . . .
C32 C 0.1366(3) -0.76054(17) 0.19678(12) 0.0282(7) Uani 1 1 d . . . . .
C33 C 0.2228(3) -0.7546(2) 0.16112(13) 0.0345(7) Uani 1 1 d . . . . .
H33 H 0.2835 -0.7199 0.1708 0.041 Uiso 1 1 calc R U . . .
C34 C 0.2209(3) -0.79879(19) 0.11159(13) 0.0329(7) Uani 1 1 d . . . . .
H34 H 0.2804 -0.7942 0.0875 0.039 Uiso 1 1 calc R U . . .
C35 C 0.1330(2) -0.84994(18) 0.09663(12) 0.0262(6) Uani 1 1 d . . . . .
C36 C 0.0459(2) -0.85520(18) 0.13220(13) 0.0286(7) Uani 1 1 d . . . . .
H36 H -0.0151 -0.8896 0.1225 0.034 Uiso 1 1 calc R U . . .
C37 C 0.0479(3) -0.81062(18) 0.18146(13) 0.0296(7) Uani 1 1 d . . . . .
H37 H -0.0122 -0.8143 0.2052 0.036 Uiso 1 1 calc R U . . .
C38 C 0.1257(2) -0.89934(19) 0.04278(13) 0.0297(7) Uani 1 1 d . . . . .
H38A H 0.0756 -0.9459 0.0472 0.036 Uiso 1 1 calc R U . . .
H38B H 0.0946 -0.8655 0.0112 0.036 Uiso 1 1 calc R U . . .
C39 C 0.2969(3) -0.88847(19) -0.00698(12) 0.0298(7) Uani 1 1 d . . . . .
H39 H 0.2675 -0.8409 -0.0247 0.036 Uiso 1 1 calc R U . . .
C40 C 0.4007(3) -0.91507(18) -0.01870(12) 0.0289(7) Uani 1 1 d . . . . .
H40 H 0.4426 -0.8855 -0.0443 0.035 Uiso 1 1 calc R U . . .
C41 C 0.4449(2) -0.98502(18) 0.00664(12) 0.0259(6) Uani 1 1 d . . . . .
C42 C 0.3802(3) -1.0249(2) 0.04478(13) 0.0323(7) Uani 1 1 d . . . . .
H42 H 0.4077 -1.0722 0.0636 0.039 Uiso 1 1 calc R U . . .
C43 C 0.2772(3) -0.9962(2) 0.05527(13) 0.0320(7) Uani 1 1 d . . . . .
H43 H 0.2340 -1.0241 0.0812 0.038 Uiso 1 1 calc R U . . .
O51 O 0.11556(18) -0.50402(13) 0.41944(9) 0.0344(5) Uani 1 1 d . . . . .
O52 O 0.23616(18) -0.54091(13) 0.35853(10) 0.0367(5) Uani 1 1 d . . . . .
O53 O 0.5610(2) -0.20395(15) 0.42717(12) 0.0558(7) Uani 1 1 d . . . . .
O54 O 0.4602(2) -0.17741(14) 0.50055(10) 0.0420(6) Uani 1 1 d . . . . .
C51 C 0.2021(3) -0.49191(18) 0.39485(13) 0.0292(7) Uani 1 1 d . . . . .
C52 C 0.2709(3) -0.41842(18) 0.40871(12) 0.0276(6) Uani 1 1 d . . . . .
C53 C 0.3717(3) -0.40778(19) 0.38455(13) 0.0315(7) Uani 1 1 d . . . . .
H53 H 0.3952 -0.4458 0.3577 0.038 Uiso 1 1 calc R U . . .
C54 C 0.4378(3) -0.34199(19) 0.39959(13) 0.0321(7) Uani 1 1 d . . . . .
H54 H 0.5061 -0.3348 0.3826 0.038 Uiso 1 1 calc R U . . .
C55 C 0.4056(3) -0.28625(18) 0.43934(13) 0.0296(7) Uani 1 1 d . . . . .
C56 C 0.4821(3) -0.21713(19) 0.45697(15) 0.0361(8) Uani 1 1 d . . . . .
C57 C 0.3034(3) -0.29575(19) 0.46247(14) 0.0338(7) Uani 1 1 d . . . . .
H57 H 0.2796 -0.2574 0.4890 0.041 Uiso 1 1 calc R U . . .
C58 C 0.2368(3) -0.36085(19) 0.44683(14) 0.0331(7) Uani 1 1 d . . . . .
H58 H 0.1668 -0.3664 0.4623 0.040 Uiso 1 1 calc R U . . .
O1W O 0.6372(2) -0.09970(14) 0.55644(10) 0.0423(6) Uani 1 1 d G . . . .
H1WA H 0.5845 -0.1240 0.5392 0.063 Uiso 1 1 d R U . . .
H1WB H 0.6896 -0.1322 0.5634 0.063 Uiso 1 1 d R U . . .
O2W O 0.4496(2) -0.27621(15) 0.59777(10) 0.0457(6) Uani 1 1 d G . . . .
H0AA H 0.3852 -0.2746 0.6089 0.069 Uiso 1 1 d R U . . .
H0AB H 0.4527 -0.2482 0.5683 0.069 Uiso 1 1 d R U . . .
O3W O 0.3481(2) -0.03230(17) 0.51970(13) 0.0578(7) Uani 1 1 d G . . . .
H3WA H 0.3583 0.0078 0.4989 0.087 Uiso 1 1 d G U . . .
H3WB H 0.3901 -0.0702 0.5112 0.087 Uiso 1 1 d G U . . .
O4W O 0.5453(2) -0.40514(16) 0.66131(11) 0.0510(7) Uani 1 1 d G . . . .
H4WA H 0.5301 -0.3607 0.6455 0.077 Uiso 1 1 d R U . . .
H4WB H 0.6120 -0.4164 0.6576 0.077 Uiso 1 1 d R U . . .
O5W O 0.3167(2) -0.53589(15) 0.21595(11) 0.0518(7) Uani 1 1 d G . . . .
H5WA H 0.3008 -0.5791 0.2323 0.078 Uiso 1 1 d R U . . .
H5WB H 0.3402 -0.5467 0.1842 0.078 Uiso 1 1 d R U . . .
O6W O 0.5968(2) -0.05720(17) 0.38427(11) 0.0606(8) Uani 1 1 d G . . . .
H6WA H 0.5990 -0.1041 0.3981 0.091 Uiso 1 1 d R U . . .
H6WB H 0.6247 -0.0243 0.4081 0.091 Uiso 1 1 d R U . . .
O7W O 0.2422(2) -0.28143(18) 0.63357(13) 0.0679(9) Uani 1 1 d G . . . .
H7WA H 0.2049 -0.2462 0.6494 0.102 Uiso 1 1 d R U . . .
H7WB H 0.2080 -0.3257 0.6327 0.102 Uiso 1 1 d R U . . .
O8W O -1.1010(3) -0.5139(2) 0.80236(14) 0.0730(9) Uani 1 1 d G . . . .
H8WA H -1.0542 -0.4838 0.7883 0.110 Uiso 1 1 d R U . . .
H8WB H -1.1331 -0.5419 0.7767 0.110 Uiso 1 1 d R U . . .
O9W O -0.1006(3) -0.8240(2) 0.31942(16) 0.0883(12) Uani 1 1 d G . . . .
H9WA H -0.0731 -0.8693 0.3284 0.132 Uiso 1 1 d R U . . .
H9WB H -0.0502 -0.7925 0.3105 0.132 Uiso 1 1 d R U . . .


_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
Cd1 O1 2.183(2) . ?
Cd1 O52 2.236(2) . ?
Cd1 O31 2.282(2) . ?
Cd1 O4 2.314(2) 3_446 ?
Cd1 O51 2.584(2) . ?
Cd1 O3 2.646(2) 3_446 ?
Cd1 C51 2.747(3) . ?
N1 C13 1.340(4) . ?
N1 C9 1.342(4) . ?
N1 C8 1.501(4) . ?
N2 C17 1.343(4) . ?
N2 C16 1.343(4) . ?
N2 C19 1.488(4) . ?
O1 C1 1.255(4) . ?
O2 C1 1.245(4) . ?
O3 C24 1.255(4) . ?
O3 Cd1 2.646(2) 3_446 ?
O4 C24 1.268(4) . ?
O4 Cd1 2.314(2) 3_446 ?
C1 C2 1.507(4) . ?
C2 C3 1.385(5) . ?
C2 C7 1.390(5) . ?
C3 C4 1.389(5) . ?
C4 C5 1.377(5) . ?
C5 C6 1.384(5) . ?
C5 C8 1.515(4) . ?
C6 C7 1.377(5) . ?
C9 C10 1.369(4) . ?
C10 C11 1.393(4) . ?
C11 C12 1.393(4) . ?
C11 C14 1.480(4) . ?
C12 C13 1.371(4) . ?
C14 C15 1.385(4) . ?
C14 C18 1.392(4) . ?
C15 C16 1.378(4) . ?
C17 C18 1.372(4) . ?
C19 C20 1.508(4) . ?
C20 C26 1.387(4) . ?
C20 C21 1.389(5) . ?
C21 C22 1.382(4) . ?
C22 C23 1.394(4) . ?
C23 C25 1.377(4) . ?
C23 C24 1.507(4) . ?
C25 C26 1.391(4) . ?
N31 C43 1.341(4) . ?
N31 C39 1.343(4) . ?
N31 C38 1.489(4) . ?
O31 C31 1.278(4) . ?
O32 C31 1.249(4) . ?
C31 C32 1.506(4) . ?
C32 C37 1.387(4) . ?
C32 C33 1.388(4) . ?
C33 C34 1.382(4) . ?
C34 C35 1.389(4) . ?
C35 C36 1.394(4) . ?
C35 C38 1.513(4) . ?
C36 C37 1.380(4) . ?
C39 C40 1.378(4) . ?
C40 C41 1.394(4) . ?
C41 C42 1.397(4) . ?
C41 C41 1.477(6) 3_635 ?
C42 C43 1.373(4) . ?
O51 C51 1.248(4) . ?
O52 C51 1.269(4) . ?
O53 C56 1.243(4) . ?
O54 C56 1.266(4) . ?
C51 C52 1.498(4) . ?
C52 C58 1.392(4) . ?
C52 C53 1.393(4) . ?
C53 C54 1.384(4) . ?
C54 C55 1.390(4) . ?
C55 C57 1.394(4) . ?
C55 C56 1.514(4) . ?
C57 C58 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
O1 Cd1 O52 119.54(9) . . ?
O1 Cd1 O31 94.15(9) . . ?
O52 Cd1 O31 126.76(8) . . ?
O1 Cd1 O4 137.81(9) . 3_446 ?
O52 Cd1 O4 92.41(8) . 3_446 ?
O31 Cd1 O4 86.16(8) . 3_446 ?
O1 Cd1 O51 90.75(8) . . ?
O52 Cd1 O51 53.81(7) . . ?
O31 Cd1 O51 173.16(8) . . ?
O4 Cd1 O51 87.00(7) 3_446 . ?
O1 Cd1 O3 85.68(8) . 3_446 ?
O52 Cd1 O3 125.87(7) . 3_446 ?
O31 Cd1 O3 94.10(8) . 3_446 ?
O4 Cd1 O3 52.31(7) 3_446 3_446 ?
O51 Cd1 O3 81.50(7) . 3_446 ?
O1 Cd1 C51 108.07(9) . . ?
O52 Cd1 C51 27.10(8) . . ?
O31 Cd1 C51 152.69(9) . . ?
O4 Cd1 C51 87.68(8) 3_446 . ?
O51 Cd1 C51 26.85(8) . . ?
O3 Cd1 C51 103.02(8) 3_446 . ?
C13 N1 C9 121.2(3) . . ?
C13 N1 C8 120.2(3) . . ?
C9 N1 C8 118.5(3) . . ?
C17 N2 C16 121.1(3) . . ?
C17 N2 C19 119.4(3) . . ?
C16 N2 C19 119.5(3) . . ?
C1 O1 Cd1 123.8(2) . . ?
C24 O3 Cd1 85.16(18) . 3_446 ?
C24 O4 Cd1 100.35(19) . 3_446 ?
O2 C1 O1 125.3(3) . . ?
O2 C1 C2 119.8(3) . . ?
O1 C1 C2 114.8(3) . . ?
C3 C2 C7 119.5(3) . . ?
C3 C2 C1 121.3(3) . . ?
C7 C2 C1 119.1(3) . . ?
C2 C3 C4 119.8(3) . . ?
C5 C4 C3 120.5(3) . . ?
C4 C5 C6 119.5(3) . . ?
C4 C5 C8 120.8(3) . . ?
C6 C5 C8 119.6(3) . . ?
C7 C6 C5 120.5(3) . . ?
C6 C7 C2 120.1(3) . . ?
N1 C8 C5 108.7(3) . . ?
N1 C9 C10 120.4(3) . . ?
C9 C10 C11 119.8(3) . . ?
C12 C11 C10 118.3(3) . . ?
C12 C11 C14 121.7(3) . . ?
C10 C11 C14 120.0(3) . . ?
C13 C12 C11 119.5(3) . . ?
N1 C13 C12 120.7(3) . . ?
C15 C14 C18 118.0(3) . . ?
C15 C14 C11 119.8(3) . . ?
C18 C14 C11 122.1(3) . . ?
C16 C15 C14 120.3(3) . . ?
N2 C16 C15 120.0(3) . . ?
N2 C17 C18 120.6(3) . . ?
C17 C18 C14 119.9(3) . . ?
N2 C19 C20 111.0(3) . . ?
C26 C20 C21 119.4(3) . . ?
C26 C20 C19 119.9(3) . . ?
C21 C20 C19 120.7(3) . . ?
C22 C21 C20 120.6(3) . . ?
C21 C22 C23 120.0(3) . . ?
C25 C23 C22 119.3(3) . . ?
C25 C23 C24 120.3(3) . . ?
C22 C23 C24 120.4(3) . . ?
O3 C24 O4 122.0(3) . . ?
O3 C24 C23 119.9(3) . . ?
O4 C24 C23 118.1(3) . . ?
C23 C25 C26 120.9(3) . . ?
C20 C26 C25 119.8(3) . . ?
C43 N31 C39 120.7(3) . . ?
C43 N31 C38 119.0(3) . . ?
C39 N31 C38 120.2(3) . . ?
C31 O31 Cd1 103.2(2) . . ?
O32 C31 O31 122.5(3) . . ?
O32 C31 C32 120.6(3) . . ?
O31 C31 C32 117.0(3) . . ?
C37 C32 C33 118.9(3) . . ?
C37 C32 C31 120.7(3) . . ?
C33 C32 C31 120.3(3) . . ?
C34 C33 C32 120.4(3) . . ?
C33 C34 C35 120.7(3) . . ?
C34 C35 C36 118.8(3) . . ?
C34 C35 C38 123.2(3) . . ?
C36 C35 C38 118.0(3) . . ?
C37 C36 C35 120.3(3) . . ?
C36 C37 C32 120.9(3) . . ?
N31 C38 C35 110.6(2) . . ?
N31 C39 C40 120.5(3) . . ?
C39 C40 C41 120.6(3) . . ?
C40 C41 C42 116.9(3) . . ?
C40 C41 C41 121.0(3) . 3_635 ?
C42 C41 C41 122.1(3) . 3_635 ?
C43 C42 C41 120.5(3) . . ?
N31 C43 C42 120.7(3) . . ?
C51 O51 Cd1 83.89(18) . . ?
C51 O52 Cd1 99.49(19) . . ?
O51 C51 O52 122.2(3) . . ?
O51 C51 C52 120.0(3) . . ?
O52 C51 C52 117.7(3) . . ?
O51 C51 Cd1 69.26(17) . . ?
O52 C51 Cd1 53.41(15) . . ?
C52 C51 Cd1 169.2(2) . . ?
C58 C52 C53 119.0(3) . . ?
C58 C52 C51 120.8(3) . . ?
C53 C52 C51 120.2(3) . . ?
C54 C53 C52 120.2(3) . . ?
C53 C54 C55 120.8(3) . . ?
C54 C55 C57 119.1(3) . . ?
C54 C55 C56 119.5(3) . . ?
C57 C55 C56 121.4(3) . . ?
O53 C56 O54 125.5(3) . . ?
O53 C56 C55 117.1(3) . . ?
O54 C56 C55 117.4(3) . . ?
C58 C57 C55 120.1(3) . . ?
C57 C58 C52 120.9(3) . . ?

_refine_diff_density_max         0.927
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.082

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_da347
_database_code_depnum_ccdc_archive 'CCDC 1441128'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H52 N3 O19 Zn'
_chemical_formula_sum            'C47 H52 N3 O19 Zn'
_chemical_formula_weight         1028.28

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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

_cell_length_a                   12.4870(6)
_cell_length_b                   16.0350(8)
_cell_length_c                   23.5332(12)
_cell_angle_alpha                90
_cell_angle_beta                 94.8080(17)
_cell_angle_gamma                90
_cell_volume                     4695.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    65679
_cell_measurement_theta_min      1.538
_cell_measurement_theta_max      28.323

_exptl_crystal_description       plates
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_F_000             2148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.606
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            65679
_diffrn_reflns_av_unetI/netI     0.1564
_diffrn_reflns_av_R_equivalents  0.1546
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.538
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11676
_reflns_number_gt                5390
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0781P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11676
_refine_ls_number_parameters     634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1814
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.1848
_refine_ls_wR_factor_gt          0.1422
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Zn1 Zn 0.08279(4) -0.62793(3) 0.34475(2) 0.02852(15) Uani 1 1 d . . . . .
N1 N -0.1490(3) -0.9259(2) 0.62577(16) 0.0336(9) Uani 1 1 d . . . . .
N2 N -0.4734(3) -0.6734(2) 0.78076(15) 0.0350(9) Uani 1 1 d . . . . .
O1 O 0.0501(3) -0.7073(2) 0.40398(14) 0.0417(8) Uani 1 1 d . . . . .
O2 O 0.2085(3) -0.7710(2) 0.41777(14) 0.0457(9) Uani 1 1 d . . . . .
O3 O -0.8605(3) -0.4142(2) 0.63721(15) 0.0465(9) Uani 1 1 d . . . . .
O4 O -0.9759(2) -0.4460(2) 0.70094(14) 0.0391(8) Uani 1 1 d . . . . .
C1 C 0.1132(4) -0.7615(3) 0.42705(19) 0.0360(11) Uani 1 1 d . . . . .
C2 C 0.0642(4) -0.8166(3) 0.47051(19) 0.0325(11) Uani 1 1 d . . . . .
C3 C 0.1295(4) -0.8544(3) 0.5138(2) 0.0386(12) Uani 1 1 d . . . . .
H3 H 0.2050 -0.8459 0.5163 0.046 Uiso 1 1 calc R U . . .
C4 C 0.0841(4) -0.9050(3) 0.5537(2) 0.0379(12) Uani 1 1 d . . . . .
H4 H 0.1286 -0.9296 0.5838 0.046 Uiso 1 1 calc R U . . .
C5 C -0.0252(4) -0.9193(3) 0.5494(2) 0.0345(11) Uani 1 1 d . . . . .
C6 C -0.0897(4) -0.8813(3) 0.5054(2) 0.0421(12) Uani 1 1 d . . . . .
H6 H -0.1650 -0.8913 0.5019 0.051 Uiso 1 1 calc R U . . .
C7 C -0.0454(4) -0.8297(3) 0.4674(2) 0.0395(12) Uani 1 1 d . . . . .
H7 H -0.0906 -0.8027 0.4385 0.047 Uiso 1 1 calc R U . . .
C8 C -0.0754(4) -0.9755(3) 0.5917(2) 0.0413(12) Uani 1 1 d . . . . .
H8A H -0.1163 -1.0206 0.5710 0.050 Uiso 1 1 calc R U . . .
H8B H -0.0182 -1.0014 0.6176 0.050 Uiso 1 1 calc R U . . .
C9 C -0.1061(3) -0.8703(3) 0.6639(2) 0.0349(11) Uani 1 1 d . . . . .
H9 H -0.0302 -0.8649 0.6694 0.042 Uiso 1 1 calc R U . . .
C10 C -0.1697(3) -0.8213(3) 0.69487(19) 0.0319(11) Uani 1 1 d . . . . .
H10 H -0.1384 -0.7827 0.7221 0.038 Uiso 1 1 calc R U . . .
C11 C -0.2806(3) -0.8289(3) 0.68585(18) 0.0276(10) Uani 1 1 d . . . . .
C12 C -0.3243(4) -0.8880(3) 0.64754(18) 0.0297(10) Uani 1 1 d . . . . .
H12 H -0.3999 -0.8953 0.6418 0.036 Uiso 1 1 calc R U . . .
C13 C -0.2559(4) -0.9361(3) 0.61784(19) 0.0343(11) Uani 1 1 d . . . . .
H13 H -0.2850 -0.9767 0.5915 0.041 Uiso 1 1 calc R U . . .
C14 C -0.3512(3) -0.7735(3) 0.71783(18) 0.0289(10) Uani 1 1 d . . . . .
C15 C -0.3145(4) -0.6954(3) 0.7364(2) 0.0350(11) Uani 1 1 d . . . . .
H15 H -0.2461 -0.6760 0.7272 0.042 Uiso 1 1 calc R U . . .
C16 C -0.3767(4) -0.6467(3) 0.7677(2) 0.0420(13) Uani 1 1 d . . . . .
H16 H -0.3514 -0.5935 0.7804 0.050 Uiso 1 1 calc R U . . .
C17 C -0.5126(4) -0.7468(3) 0.7617(2) 0.0369(11) Uani 1 1 d . . . . .
H17 H -0.5824 -0.7636 0.7702 0.044 Uiso 1 1 calc R U . . .
C18 C -0.4532(3) -0.7979(3) 0.7299(2) 0.0348(11) Uani 1 1 d . . . . .
H18 H -0.4818 -0.8497 0.7162 0.042 Uiso 1 1 calc R U . . .
C19 C -0.5391(4) -0.6207(3) 0.8170(2) 0.0468(13) Uani 1 1 d . . . . .
H19A H -0.4924 -0.5783 0.8372 0.056 Uiso 1 1 calc R U . . .
H19B H -0.5700 -0.6561 0.8460 0.056 Uiso 1 1 calc R U . . .
C20 C -0.6289(4) -0.5774(3) 0.78107(19) 0.0335(11) Uani 1 1 d . . . . .
C21 C -0.6066(4) -0.5223(3) 0.7388(2) 0.0368(12) Uani 1 1 d . . . . .
H21 H -0.5341 -0.5123 0.7315 0.044 Uiso 1 1 calc R U . . .
C22 C -0.6885(3) -0.4811(3) 0.7069(2) 0.0341(11) Uani 1 1 d . . . . .
H22 H -0.6721 -0.4435 0.6777 0.041 Uiso 1 1 calc R U . . .
C23 C -0.7952(3) -0.4951(3) 0.71768(19) 0.0302(10) Uani 1 1 d . . . . .
C24 C -0.8830(4) -0.4481(3) 0.6821(2) 0.0358(12) Uani 1 1 d . . . . .
C25 C -0.8177(4) -0.5491(3) 0.75994(19) 0.0332(11) Uani 1 1 d . . . . .
H25 H -0.8902 -0.5576 0.7680 0.040 Uiso 1 1 calc R U . . .
C26 C -0.7356(4) -0.5923(3) 0.7915(2) 0.0370(12) Uani 1 1 d . . . . .
H26 H -0.7522 -0.6313 0.8199 0.044 Uiso 1 1 calc R U . . .
N31 N 0.2428(3) -0.9317(2) 0.02614(15) 0.0268(8) Uani 1 1 d . . . . .
O31 O 0.0838(2) -0.7072(2) 0.27868(14) 0.0437(9) Uani 1 1 d . . . . .
O32 O 0.2553(3) -0.6786(2) 0.26764(14) 0.0436(9) Uani 1 1 d . . . . .
C31 C 0.1678(4) -0.7113(3) 0.25155(19) 0.0326(11) Uani 1 1 d . . . . .
C32 C 0.1575(3) -0.7576(3) 0.19535(18) 0.0283(10) Uani 1 1 d . . . . .
C33 C 0.2403(4) -0.7570(3) 0.16009(19) 0.0360(11) Uani 1 1 d . . . . .
H33 H 0.3028 -0.7248 0.1705 0.043 Uiso 1 1 calc R U . . .
C34 C 0.2344(4) -0.8019(3) 0.11038(19) 0.0349(11) Uani 1 1 d . . . . .
H34 H 0.2925 -0.8002 0.0868 0.042 Uiso 1 1 calc R U . . .
C35 C 0.1446(3) -0.8498(3) 0.09403(18) 0.0275(10) Uani 1 1 d . . . . .
C36 C 0.0598(3) -0.8508(3) 0.12866(19) 0.0304(11) Uani 1 1 d . . . . .
H36 H -0.0023 -0.8835 0.1183 0.036 Uiso 1 1 calc R U . . .
C37 C 0.0660(3) -0.8038(3) 0.17846(19) 0.0327(11) Uani 1 1 d . . . . .
H37 H 0.0069 -0.8032 0.2013 0.039 Uiso 1 1 calc R U . . .
C38 C 0.1351(3) -0.9010(3) 0.04009(19) 0.0320(11) Uani 1 1 d . . . . .
H38A H 0.0871 -0.9491 0.0449 0.038 Uiso 1 1 calc R U . . .
H38B H 0.1029 -0.8666 0.0082 0.038 Uiso 1 1 calc R U . . .
C39 C 0.2985(4) -0.8902(3) -0.01059(18) 0.0309(11) Uani 1 1 d . . . . .
H39 H 0.2678 -0.8426 -0.0296 0.037 Uiso 1 1 calc R U . . .
C40 C 0.4001(3) -0.9157(3) -0.02117(19) 0.0308(10) Uani 1 1 d . . . . .
H40 H 0.4391 -0.8853 -0.0473 0.037 Uiso 1 1 calc R U . . .
C41 C 0.4461(3) -0.9851(3) 0.00567(18) 0.0271(10) Uani 1 1 d . . . . .
C42 C 0.3847(3) -1.0268(3) 0.04370(18) 0.0301(10) Uani 1 1 d . . . . .
H42 H 0.4132 -1.0749 0.0631 0.036 Uiso 1 1 calc R U . . .
C43 C 0.2841(3) -0.9993(3) 0.05325(19) 0.0328(11) Uani 1 1 d . . . . .
H43 H 0.2433 -1.0283 0.0793 0.039 Uiso 1 1 calc R U . . .
O51 O 0.0967(2) -0.5053(2) 0.42308(13) 0.0368(8) Uani 1 1 d . . . . .
O52 O 0.2024(2) -0.54823(19) 0.35739(14) 0.0384(8) Uani 1 1 d . . . . .
O53 O 0.5457(3) -0.2128(2) 0.42236(17) 0.0573(10) Uani 1 1 d . . . . .
O54 O 0.4596(3) -0.1834(2) 0.49975(15) 0.0467(9) Uani 1 1 d . . . . .
C51 C 0.1761(4) -0.4973(3) 0.39575(19) 0.0320(11) Uani 1 1 d . . . . .
C52 C 0.2510(3) -0.4233(3) 0.40853(19) 0.0317(11) Uani 1 1 d . . . . .
C53 C 0.2248(3) -0.3625(3) 0.44726(19) 0.0323(11) Uani 1 1 d . . . . .
H53 H 0.1576 -0.3648 0.4634 0.039 Uiso 1 1 calc R U . . .
C54 C 0.2963(3) -0.2986(3) 0.46242(19) 0.0334(11) Uani 1 1 d . . . . .
H54 H 0.2780 -0.2578 0.4893 0.040 Uiso 1 1 calc R U . . .
C55 C 0.3942(3) -0.2936(3) 0.43876(18) 0.0300(10) Uani 1 1 d . . . . .
C56 C 0.4735(4) -0.2247(3) 0.4548(2) 0.0349(11) Uani 1 1 d . . . . .
C57 C 0.4185(4) -0.3537(3) 0.39917(19) 0.0327(11) Uani 1 1 d . . . . .
H57 H 0.4846 -0.3501 0.3821 0.039 Uiso 1 1 calc R U . . .
C58 C 0.3494(3) -0.4183(3) 0.38411(19) 0.0312(11) Uani 1 1 d . . . . .
H58 H 0.3681 -0.4590 0.3574 0.037 Uiso 1 1 calc R U . . .
O1W O 0.6379(3) -0.1034(2) 0.55525(15) 0.0496(9) Uani 1 1 d . . . . .
H1WA H 0.6879 -0.1386 0.5580 0.074 Uiso 1 1 d R U . . .
H1WB H 0.5824 -0.1253 0.5390 0.074 Uiso 1 1 d R U . . .
O2W O 0.4409(3) -0.2727(2) 0.60068(14) 0.0498(9) Uani 1 1 d . . . . .
H2WA H 0.3802 -0.2752 0.6135 0.075 Uiso 1 1 d R U . . .
H2WB H 0.4303 -0.2515 0.5680 0.075 Uiso 1 1 d R U . . .
O3W O 0.3488(3) -0.0339(2) 0.51965(18) 0.0710(12) Uani 1 1 d . . . . .
H3WA H 0.3835 -0.0752 0.5092 0.107 Uiso 1 1 d R U . . .
H3WB H 0.3498 0.0061 0.4966 0.107 Uiso 1 1 d R U . . .
O4W O -1.2949(3) -0.4639(2) 0.79176(19) 0.0710(12) Uani 1 1 d G . . . .
H4WA H -1.3342 -0.4737 0.7618 0.107 Uiso 1 1 d R U . . .
H4WB H -1.3330 -0.4605 0.8194 0.107 Uiso 1 1 d R U . . .
O5W O 0.4403(3) -0.6012(2) 0.33924(16) 0.0632(11) Uani 1 1 d . . . . .
H5WA H 0.3728 -0.6020 0.3357 0.095 Uiso 1 1 d R U . . .
H5WB H 0.4631 -0.6441 0.3568 0.095 Uiso 1 1 d R U . . .
O6W O -1.4002(3) -0.4426(2) 0.87996(15) 0.0520(10) Uani 1 1 d . . . . .
H6WB H -1.4004 -0.3939 0.8930 0.078 Uiso 1 1 d R U . . .
H6WA H -1.3846 -0.4764 0.9066 0.078 Uiso 1 1 d R U . . .
O7W O 0.2365(3) -0.2627(2) 0.63290(16) 0.0628(11) Uani 1 1 d . . . . .
H7WB H 0.2086 -0.3099 0.6365 0.094 Uiso 1 1 d R U . . .
H7WA H 0.1977 -0.2249 0.6450 0.094 Uiso 1 1 d R U . . .
O8W O -1.0817(3) -0.5091(2) 0.79237(17) 0.0624(11) Uani 1 1 d . . . . .
H8WA H -1.0650 -0.5002 0.7591 0.094 Uiso 1 1 d R U . . .
H8WB H -1.1458 -0.4931 0.7919 0.094 Uiso 1 1 d R U . . .
O9W O -0.0883(3) -0.8210(2) 0.30398(16) 0.0590(11) Uani 1 1 d . . . . .
H9WA H -0.0952 -0.8731 0.3024 0.089 Uiso 1 1 d R U . . .
H9WB H -0.0382 -0.7870 0.3004 0.089 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.956(3) . ?
Zn1 O52 1.969(3) . ?
Zn1 O31 2.009(3) . ?
Zn1 O4 2.025(3) 3_446 ?
N1 C13 1.342(6) . ?
N1 C9 1.344(6) . ?
N1 C8 1.498(6) . ?
N2 C17 1.338(6) . ?
N2 C16 1.341(6) . ?
N2 C19 1.495(5) . ?
O1 C1 1.265(5) . ?
O2 C1 1.237(5) . ?
O3 C24 1.242(6) . ?
O4 C24 1.277(5) . ?
O4 Zn1 2.025(3) 3_446 ?
C1 C2 1.518(6) . ?
C2 C7 1.381(6) . ?
C2 C3 1.390(6) . ?
C3 C4 1.395(6) . ?
C4 C5 1.379(6) . ?
C5 C6 1.397(7) . ?
C5 C8 1.516(6) . ?
C6 C7 1.370(6) . ?
C9 C10 1.370(6) . ?
C10 C11 1.389(6) . ?
C11 C12 1.388(6) . ?
C11 C14 1.498(6) . ?
C12 C13 1.382(6) . ?
C14 C18 1.384(6) . ?
C14 C15 1.393(6) . ?
C15 C16 1.360(6) . ?
C17 C18 1.368(6) . ?
C19 C20 1.515(6) . ?
C20 C21 1.377(6) . ?
C20 C26 1.394(6) . ?
C21 C22 1.384(6) . ?
C22 C23 1.395(6) . ?
C23 C25 1.366(6) . ?
C23 C24 1.521(6) . ?
C25 C26 1.398(6) . ?
N31 C39 1.332(5) . ?
N31 C43 1.339(5) . ?
N31 C38 1.494(5) . ?
O31 C31 1.274(5) . ?
O32 C31 1.242(5) . ?
C31 C32 1.513(6) . ?
C32 C33 1.379(6) . ?
C32 C37 1.392(6) . ?
C33 C34 1.370(6) . ?
C34 C35 1.387(6) . ?
C35 C36 1.390(6) . ?
C35 C38 1.508(6) . ?
C36 C37 1.390(6) . ?
C39 C40 1.375(6) . ?
C40 C41 1.380(6) . ?
C41 C42 1.397(6) . ?
C41 C41 1.474(8) 3_635 ?
C42 C43 1.368(6) . ?
O51 C51 1.232(5) . ?
O52 C51 1.280(5) . ?
O53 C56 1.245(5) . ?
O54 C56 1.272(5) . ?
C51 C52 1.525(6) . ?
C52 C53 1.393(6) . ?
C52 C58 1.402(6) . ?
C53 C54 1.386(6) . ?
C54 C55 1.388(6) . ?
C55 C57 1.392(6) . ?
C55 C56 1.510(6) . ?
C57 C58 1.375(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O52 121.03(14) . . ?
O1 Zn1 O31 98.94(14) . . ?
O52 Zn1 O31 118.26(13) . . ?
O1 Zn1 O4 126.27(13) . 3_446 ?
O52 Zn1 O4 99.09(13) . 3_446 ?
O31 Zn1 O4 90.35(13) . 3_446 ?
C13 N1 C9 120.6(4) . . ?
C13 N1 C8 120.7(4) . . ?
C9 N1 C8 118.7(4) . . ?
C17 N2 C16 121.0(4) . . ?
C17 N2 C19 119.1(4) . . ?
C16 N2 C19 119.9(4) . . ?
C1 O1 Zn1 126.4(3) . . ?
C24 O4 Zn1 114.1(3) . 3_446 ?
O2 C1 O1 125.6(4) . . ?
O2 C1 C2 119.7(4) . . ?
O1 C1 C2 114.7(4) . . ?
C7 C2 C3 119.4(4) . . ?
C7 C2 C1 120.4(4) . . ?
C3 C2 C1 120.2(4) . . ?
C2 C3 C4 120.0(4) . . ?
C5 C4 C3 120.2(5) . . ?
C4 C5 C6 119.1(4) . . ?
C4 C5 C8 120.8(4) . . ?
C6 C5 C8 120.0(4) . . ?
C7 C6 C5 120.6(5) . . ?
C6 C7 C2 120.7(5) . . ?
N1 C8 C5 110.0(4) . . ?
N1 C9 C10 121.3(4) . . ?
C9 C10 C11 118.8(4) . . ?
C12 C11 C10 119.5(4) . . ?
C12 C11 C14 121.0(4) . . ?
C10 C11 C14 119.5(4) . . ?
C13 C12 C11 118.9(4) . . ?
N1 C13 C12 120.8(4) . . ?
C18 C14 C15 118.3(4) . . ?
C18 C14 C11 121.8(4) . . ?
C15 C14 C11 119.9(4) . . ?
C16 C15 C14 119.9(4) . . ?
N2 C16 C15 120.5(5) . . ?
N2 C17 C18 120.7(4) . . ?
C17 C18 C14 119.6(4) . . ?
N2 C19 C20 110.9(4) . . ?
C21 C20 C26 119.4(4) . . ?
C21 C20 C19 120.8(4) . . ?
C26 C20 C19 119.8(4) . . ?
C20 C21 C22 120.9(4) . . ?
C21 C22 C23 119.9(4) . . ?
C25 C23 C22 119.5(4) . . ?
C25 C23 C24 122.1(4) . . ?
C22 C23 C24 118.4(4) . . ?
O3 C24 O4 124.1(4) . . ?
O3 C24 C23 118.8(4) . . ?
O4 C24 C23 117.1(4) . . ?
C23 C25 C26 121.0(4) . . ?
C20 C26 C25 119.4(4) . . ?
C39 N31 C43 120.8(4) . . ?
C39 N31 C38 120.4(4) . . ?
C43 N31 C38 118.7(4) . . ?
C31 O31 Zn1 118.6(3) . . ?
O32 C31 O31 124.4(4) . . ?
O32 C31 C32 118.8(4) . . ?
O31 C31 C32 116.8(4) . . ?
C33 C32 C37 118.1(4) . . ?
C33 C32 C31 120.7(4) . . ?
C37 C32 C31 121.2(4) . . ?
C34 C33 C32 121.4(4) . . ?
C33 C34 C35 120.9(4) . . ?
C34 C35 C36 118.8(4) . . ?
C34 C35 C38 122.7(4) . . ?
C36 C35 C38 118.5(4) . . ?
C35 C36 C37 119.8(4) . . ?
C36 C37 C32 121.1(4) . . ?
N31 C38 C35 110.8(3) . . ?
N31 C39 C40 120.6(4) . . ?
C39 C40 C41 120.8(4) . . ?
C40 C41 C42 116.7(4) . . ?
C40 C41 C41 122.0(5) . 3_635 ?
C42 C41 C41 121.2(5) . 3_635 ?
C43 C42 C41 120.8(4) . . ?
N31 C43 C42 120.3(4) . . ?
C51 O52 Zn1 106.5(3) . . ?
O51 C51 O52 124.5(4) . . ?
O51 C51 C52 119.0(4) . . ?
O52 C51 C52 116.5(4) . . ?
C53 C52 C58 119.3(4) . . ?
C53 C52 C51 120.0(4) . . ?
C58 C52 C51 120.6(4) . . ?
C54 C53 C52 120.3(4) . . ?
C53 C54 C55 120.7(4) . . ?
C54 C55 C57 118.5(4) . . ?
C54 C55 C56 121.6(4) . . ?
C57 C55 C56 119.9(4) . . ?
O53 C56 O54 125.9(4) . . ?
O53 C56 C55 116.9(4) . . ?
O54 C56 C55 117.2(4) . . ?
C58 C57 C55 121.8(4) . . ?
C57 C58 C52 119.4(4) . . ?

_refine_diff_density_max         0.885
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.086

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_da459
_database_code_depnum_ccdc_archive 'CCDC 1441129'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 Cu2 N6 O15'
_chemical_formula_sum            'C34 H36 Cu2 N6 O15'
_chemical_formula_weight         895.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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

_cell_length_a                   11.9508(16)
_cell_length_b                   17.898(2)
_cell_length_c                   16.975(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.774(5)
_cell_angle_gamma                90
_cell_volume                     3623.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    43330
_cell_measurement_theta_min      2.321
_cell_measurement_theta_max      25.350

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_F_000             1840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.256
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43330
_diffrn_reflns_av_unetI/netI     0.1423
_diffrn_reflns_av_R_equivalents  0.1753
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.321
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6643
_reflns_number_gt                3510
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014/6 (Sheldrick, 2014)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0756P)²+31.7046P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6643
_refine_ls_number_parameters     522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.0900
_refine_ls_wR_factor_ref         0.2320
_refine_ls_wR_factor_gt          0.1969
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cu1 Cu 0.27885(9) 0.08070(7) 0.21608(7) 0.0270(3) Uani 1 1 d . . . . .
Cu2 Cu 0.53290(9) 0.07330(6) 0.37740(7) 0.0219(3) Uani 1 1 d . . . . .
N1 N 0.2762(6) 0.0644(4) 0.3305(5) 0.0260(19) Uani 1 1 d . . . . .
N2 N 0.3686(6) 0.0687(4) 0.3814(4) 0.0209(17) Uani 1 1 d . . . . .
O1 O 0.5246(5) 0.0825(3) 0.4928(4) 0.0231(14) Uani 1 1 d . . . . .
O2 O 0.4097(5) 0.0646(3) 0.5895(4) 0.0245(15) Uani 1 1 d . . . . .
C1 C 0.4288(7) 0.0691(5) 0.5193(6) 0.019(2) Uani 1 1 d . . . . .
C2 C 0.3354(7) 0.0617(4) 0.4554(5) 0.018(2) Uani 1 1 d . . . . .
C3 C 0.2220(8) 0.0498(5) 0.4530(6) 0.028(2) Uani 1 1 d . . . . .
H3 H 0.1773 0.0407 0.4962 0.034 Uiso 1 1 calc R U . . .
C4 C 0.1869(8) 0.0539(5) 0.3745(6) 0.027(2) Uani 1 1 d . . . . .
H4 H 0.1112 0.0499 0.3541 0.033 Uiso 1 1 calc R U . . .
N11 N 0.4445(6) 0.0750(4) 0.2122(5) 0.0263(18) Uani 1 1 d . . . . .
N12 N 0.5370(6) 0.0662(4) 0.2640(5) 0.0235(18) Uani 1 1 d . . . . .
O11 O 0.2895(6) 0.0940(4) 0.1008(4) 0.042(2) Uani 1 1 d . . . . .
O12 O 0.4100(6) 0.0990(5) 0.0066(4) 0.047(2) Uani 1 1 d . . . . .
C11 C 0.3877(9) 0.0920(6) 0.0760(6) 0.031(2) Uani 1 1 d . . . . .
C12 C 0.4772(8) 0.0768(5) 0.1392(6) 0.027(2) Uani 1 1 d . . . . .
C13 C 0.5941(8) 0.0717(6) 0.1412(6) 0.028(2) Uani 1 1 d . . . . .
H13 H 0.6406 0.0729 0.0979 0.033 Uiso 1 1 calc R U . . .
C14 C 0.6265(8) 0.0646(5) 0.2203(6) 0.028(2) Uani 1 1 d . . . . .
H14 H 0.7019 0.0592 0.2410 0.034 Uiso 1 1 calc R U . . .
O21 O 0.1209(5) 0.1149(4) 0.2063(4) 0.0351(18) Uani 1 1 d . . . . .
O22 O 0.2051(5) 0.2266(4) 0.2164(4) 0.0346(18) Uani 1 1 d . . . . .
O23 O -1.3789(5) 0.2081(4) 0.3761(4) 0.0298(16) Uani 1 1 d . . . . .
O24 O -1.3041(5) 0.0956(3) 0.3888(4) 0.0212(15) Uani 1 1 d . . . . .
N21 N -0.3836(6) 0.3325(5) 0.1558(5) 0.027(2) Uani 1 1 d . . . . .
N22 N -0.7904(6) 0.3117(4) 0.4323(5) 0.0235(18) Uani 1 1 d . . . . .
C21 C 0.1191(7) 0.1865(6) 0.2038(6) 0.028(2) Uani 1 1 d . . . . .
C22 C 0.0094(8) 0.2242(5) 0.1812(6) 0.026(2) Uani 1 1 d . . . . .
C23 C -0.0774(8) 0.1848(6) 0.1406(6) 0.031(2) Uani 1 1 d . . . . .
H23 H -0.0693 0.1329 0.1308 0.037 Uiso 1 1 calc R U . . .
C24 C -0.1756(8) 0.2213(6) 0.1144(6) 0.033(2) Uani 1 1 d . . . . .
H24 H -0.2334 0.1944 0.0857 0.039 Uiso 1 1 calc R U . . .
C25 C -0.1901(8) 0.2979(6) 0.1303(6) 0.028(2) Uani 1 1 d . . . . .
C26 C -0.1065(8) 0.3345(6) 0.1729(6) 0.031(2) Uani 1 1 d . . . . .
H26 H -0.1165 0.3856 0.1859 0.038 Uiso 1 1 calc R U . . .
C27 C -0.0069(8) 0.2991(6) 0.1980(6) 0.033(3) Uani 1 1 d . . . . .
H27 H 0.0503 0.3263 0.2268 0.040 Uiso 1 1 calc R U . . .
C28 C -0.2964(8) 0.3355(6) 0.0985(6) 0.030(2) Uani 1 1 d . . . . .
H28A H -0.2802 0.3883 0.0861 0.035 Uiso 1 1 calc R U . . .
H28B H -0.3243 0.3105 0.0490 0.035 Uiso 1 1 calc R U . . .
C29 C -0.4522(8) 0.2724(6) 0.1563(6) 0.032(2) Uani 1 1 d . . . . .
H29 H -0.4454 0.2338 0.1185 0.038 Uiso 1 1 calc R U . . .
C30 C -0.5308(9) 0.2667(6) 0.2103(6) 0.036(3) Uani 1 1 d . . . . .
H30 H -0.5770 0.2235 0.2107 0.043 Uiso 1 1 calc R U . . .
C31 C -0.5446(8) 0.3230(5) 0.2649(6) 0.023(2) Uani 1 1 d . . . . .
C32 C -0.4744(8) 0.3858(5) 0.2630(6) 0.025(2) Uani 1 1 d . . . . .
H32 H -0.4810 0.4257 0.2993 0.030 Uiso 1 1 calc R U . . .
C33 C -0.3958(9) 0.3881(5) 0.2074(6) 0.032(2) Uani 1 1 d . . . . .
H33 H -0.3485 0.4306 0.2056 0.038 Uiso 1 1 calc R U . . .
C34 C -0.6312(8) 0.3193(5) 0.3231(6) 0.023(2) Uani 1 1 d . . . . .
C35 C -0.6402(8) 0.2572(5) 0.3714(6) 0.029(2) Uani 1 1 d . . . . .
H35 H -0.5911 0.2159 0.3664 0.035 Uiso 1 1 calc R U . . .
C36 C -0.7185(8) 0.2550(5) 0.4257(6) 0.029(2) Uani 1 1 d . . . . .
H36 H -0.7224 0.2128 0.4594 0.034 Uiso 1 1 calc R U . . .
C37 C -0.7854(8) 0.3727(5) 0.3852(6) 0.028(2) Uani 1 1 d . . . . .
H37 H -0.8367 0.4127 0.3903 0.034 Uiso 1 1 calc R U . . .
C38 C -0.7074(8) 0.3767(5) 0.3309(6) 0.026(2) Uani 1 1 d . . . . .
H38 H -0.7049 0.4194 0.2978 0.031 Uiso 1 1 calc R U . . .
C39 C -0.8764(8) 0.3073(5) 0.4921(6) 0.029(2) Uani 1 1 d . . . . .
H39A H -0.8955 0.3584 0.5091 0.035 Uiso 1 1 calc R U . . .
H39B H -0.8451 0.2796 0.5390 0.035 Uiso 1 1 calc R U . . .
C40 C -0.9808(8) 0.2688(6) 0.4589(5) 0.028(2) Uani 1 1 d . . . . .
C41 C -1.0006(7) 0.1945(5) 0.4767(5) 0.022(2) Uani 1 1 d . . . . .
H41 H -0.9455 0.1671 0.5075 0.027 Uiso 1 1 calc R U . . .
C42 C -1.0993(8) 0.1598(6) 0.4504(6) 0.028(2) Uani 1 1 d . . . . .
H42 H -1.1108 0.1085 0.4618 0.034 Uiso 1 1 calc R U . . .
C43 C -1.1810(7) 0.1997(5) 0.4077(5) 0.019(2) Uani 1 1 d . . . . .
C44 C -1.1618(8) 0.2733(6) 0.3870(6) 0.030(2) Uani 1 1 d . . . . .
H44 H -1.2171 0.3005 0.3561 0.036 Uiso 1 1 calc R U . . .
C45 C -1.0610(8) 0.3069(5) 0.4118(6) 0.030(2) Uani 1 1 d . . . . .
H45 H -1.0467 0.3568 0.3964 0.036 Uiso 1 1 calc R U . . .
C46 C -1.2956(8) 0.1666(6) 0.3880(6) 0.025(2) Uani 1 1 d . . . . .
O1W O 0.2079(6) -0.0395(4) 0.1887(4) 0.0417(19) Uani 1 1 d . . . . .
H1WA H 0.2312 -0.0567 0.1468 0.063 Uiso 1 1 d R U . . .
H1WB H 0.1375 -0.0391 0.1835 0.063 Uiso 1 1 d R U . . .
O2W O 0.6106(7) 0.1657(5) -0.0252(5) 0.065(3) Uani 1 1 d . . . . .
H2WA H 0.5457 0.1488 -0.0207 0.098 Uiso 1 1 d R U . . .
H2WB H 0.6001 0.2092 -0.0429 0.098 Uiso 1 1 d R U . . .
O3W O 0.7655(10) 0.0538(5) -0.0265(6) 0.092(4) Uani 1 1 d G . . A 1
H3WA H 0.7131 0.0801 -0.0468 0.138 Uiso 1 1 d R U . A 1
H3WB H 0.7432 0.0096 -0.0220 0.138 Uiso 1 1 d R U . A 1
O4W O 0.2245(6) 0.3479(4) 0.1156(4) 0.0408(19) Uani 1 1 d G . . B 1
H4WA H 0.2316 0.3133 0.1490 0.061 Uiso 1 1 d R U . B 1
H4WB H 0.2879 0.3652 0.1072 0.061 Uiso 1 1 d R U . B 1
O5W O -0.0230(6) -0.0060(5) 0.2086(5) 0.054(2) Uani 1 1 d G . . C 1
H5WA H -0.0773 -0.0077 0.2376 0.082 Uiso 1 1 d R U . C 1
H5WB H -0.0465 -0.0117 0.1613 0.082 Uiso 1 1 d R U . C 1
O6W O -0.1347(6) -0.0130(4) 0.3444(5) 0.047(2) Uani 1 1 d G . . D 1
H6WA H -0.1547 -0.0557 0.3585 0.071 Uiso 1 1 d R U . D 1
H6WB H -0.1898 0.0162 0.3436 0.071 Uiso 1 1 d R U . D 1
O7W O 0.936(2) 0.0047(17) 0.0405(17) 0.308(14) Uiso 1 1 d . . . E 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
Cu1 N1 1.966(8) . ?
Cu1 O21 1.981(7) . ?
Cu1 O11 1.984(7) . ?
Cu1 N11 1.988(8) . ?
Cu1 O1W 2.348(7) . ?
Cu2 N12 1.933(8) . ?
Cu2 N2 1.971(7) . ?
Cu2 O1 1.974(6) . ?
Cu2 O24 1.986(6) 1_755 ?
N1 C4 1.356(12) . ?
N1 N2 1.360(10) . ?
N2 C2 1.347(11) . ?
O1 C1 1.280(10) . ?
O2 C1 1.231(10) . ?
C1 C2 1.511(12) . ?
C2 C3 1.370(13) . ?
C3 C4 1.371(13) . ?
N11 C12 1.325(12) . ?
N11 N12 1.376(10) . ?
N12 C14 1.341(11) . ?
O11 C11 1.274(12) . ?
O12 C11 1.230(12) . ?
C11 C12 1.490(13) . ?
C12 C13 1.398(13) . ?
C13 C14 1.379(13) . ?
O21 C21 1.283(12) . ?
O22 C21 1.261(11) . ?
O23 C46 1.247(11) . ?
O24 C46 1.274(11) . ?
O24 Cu2 1.986(6) 1_355 ?
N21 C33 1.340(12) . ?
N21 C29 1.354(12) . ?
N21 C28 1.472(11) . ?
N22 C36 1.339(12) . ?
N22 C37 1.357(12) . ?
N22 C39 1.492(11) . ?
C21 C22 1.502(13) . ?
C22 C27 1.387(14) . ?
C22 C23 1.398(14) . ?
C23 C24 1.390(13) . ?
C24 C25 1.410(14) . ?
C25 C26 1.364(14) . ?
C25 C28 1.505(13) . ?
C26 C27 1.390(13) . ?
C29 C30 1.360(14) . ?
C30 C31 1.385(14) . ?
C31 C32 1.403(13) . ?
C31 C34 1.480(12) . ?
C32 C33 1.375(13) . ?
C34 C38 1.385(13) . ?
C34 C35 1.390(13) . ?
C35 C36 1.356(13) . ?
C37 C38 1.356(13) . ?
C39 C40 1.502(13) . ?
C40 C45 1.387(13) . ?
C40 C41 1.387(13) . ?
C41 C42 1.381(13) . ?
C42 C43 1.377(12) . ?
C43 C44 1.387(13) . ?
C43 C46 1.510(12) . ?
C44 C45 1.386(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 O21 92.9(3) . . ?
N1 Cu1 O11 176.8(3) . . ?
O21 Cu1 O11 90.2(3) . . ?
N1 Cu1 N11 96.1(3) . . ?
O21 Cu1 N11 163.5(3) . . ?
O11 Cu1 N11 81.1(3) . . ?
N1 Cu1 O1W 91.7(3) . . ?
O21 Cu1 O1W 86.4(3) . . ?
O11 Cu1 O1W 87.8(3) . . ?
N11 Cu1 O1W 107.1(3) . . ?
N12 Cu2 N2 97.1(3) . . ?
N12 Cu2 O1 178.3(3) . . ?
N2 Cu2 O1 81.6(3) . . ?
N12 Cu2 O24 91.2(3) . 1_755 ?
N2 Cu2 O24 168.0(3) . 1_755 ?
O1 Cu2 O24 90.0(3) . 1_755 ?
C4 N1 N2 107.0(7) . . ?
C4 N1 Cu1 129.0(7) . . ?
N2 N1 Cu1 123.7(6) . . ?
C2 N2 N1 108.1(7) . . ?
C2 N2 Cu2 113.1(6) . . ?
N1 N2 Cu2 138.5(6) . . ?
C1 O1 Cu2 116.0(6) . . ?
O2 C1 O1 125.5(8) . . ?
O2 C1 C2 121.0(8) . . ?
O1 C1 C2 113.5(8) . . ?
N2 C2 C3 109.8(8) . . ?
N2 C2 C1 114.3(8) . . ?
C3 C2 C1 135.9(9) . . ?
C2 C3 C4 105.0(9) . . ?
N1 C4 C3 110.0(9) . . ?
C12 N11 N12 109.0(7) . . ?
C12 N11 Cu1 112.7(6) . . ?
N12 N11 Cu1 138.2(6) . . ?
C14 N12 N11 106.6(8) . . ?
C14 N12 Cu2 128.8(7) . . ?
N11 N12 Cu2 123.8(6) . . ?
C11 O11 Cu1 116.3(7) . . ?
O12 C11 O11 125.2(10) . . ?
O12 C11 C12 121.2(9) . . ?
O11 C11 C12 113.6(9) . . ?
N11 C12 C13 109.4(8) . . ?
N11 C12 C11 115.9(9) . . ?
C13 C12 C11 134.3(9) . . ?
C14 C13 C12 104.2(8) . . ?
N12 C14 C13 110.7(9) . . ?
C21 O21 Cu1 109.0(6) . . ?
C46 O24 Cu2 106.1(6) . 1_355 ?
C33 N21 C29 119.6(8) . . ?
C33 N21 C28 121.2(8) . . ?
C29 N21 C28 119.2(9) . . ?
C36 N22 C37 120.4(8) . . ?
C36 N22 C39 119.4(8) . . ?
C37 N22 C39 120.2(8) . . ?
O22 C21 O21 123.6(9) . . ?
O22 C21 C22 118.4(9) . . ?
O21 C21 C22 118.0(8) . . ?
C27 C22 C23 118.6(9) . . ?
C27 C22 C21 121.0(9) . . ?
C23 C22 C21 120.4(9) . . ?
C24 C23 C22 120.3(10) . . ?
C23 C24 C25 120.5(10) . . ?
C26 C25 C24 118.3(9) . . ?
C26 C25 C28 123.1(10) . . ?
C24 C25 C28 118.6(9) . . ?
C25 C26 C27 121.7(10) . . ?
C22 C27 C26 120.5(10) . . ?
N21 C28 C25 111.4(7) . . ?
N21 C29 C30 120.6(10) . . ?
C29 C30 C31 121.0(10) . . ?
C30 C31 C32 118.0(9) . . ?
C30 C31 C34 122.2(9) . . ?
C32 C31 C34 119.8(8) . . ?
C33 C32 C31 118.4(9) . . ?
N21 C33 C32 122.4(9) . . ?
C38 C34 C35 117.4(9) . . ?
C38 C34 C31 121.5(9) . . ?
C35 C34 C31 121.0(8) . . ?
C36 C35 C34 120.5(9) . . ?
N22 C36 C35 120.7(9) . . ?
C38 C37 N22 120.2(9) . . ?
C37 C38 C34 120.7(9) . . ?
N22 C39 C40 111.2(8) . . ?
C45 C40 C41 118.4(9) . . ?
C45 C40 C39 121.0(9) . . ?
C41 C40 C39 120.5(9) . . ?
C42 C41 C40 121.0(9) . . ?
C43 C42 C41 119.8(9) . . ?
C42 C43 C44 120.2(9) . . ?
C42 C43 C46 120.9(8) . . ?
C44 C43 C46 118.7(8) . . ?
C45 C44 C43 119.3(9) . . ?
C44 C45 C40 121.0(9) . . ?
O23 C46 O24 122.2(9) . . ?
O23 C46 C43 120.3(8) . . ?
O24 C46 C43 117.4(8) . . ?

_refine_diff_density_max         1.879
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.135

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_da325
_database_code_depnum_ccdc_archive 'CCDC 1441130'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H10 Cl2 N O2.17 Zn'
_chemical_formula_sum            'C13 H10 Cl2 N O2.17 Zn'
_chemical_formula_weight         351.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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

_cell_length_a                   12.7183(4)
_cell_length_b                   14.0183(5)
_cell_length_c                   16.7134(6)
_cell_angle_alpha                90
_cell_angle_beta                 110.7756(18)
_cell_angle_gamma                90
_cell_volume                     2786.06(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    25073
_cell_measurement_theta_min      2.246
_cell_measurement_theta_max      28.259

_exptl_crystal_description       plates
_exptl_crystal_colour            'clear white'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             1411
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    2.143
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25073
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.246
_diffrn_reflns_theta_max         28.259
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3451
_reflns_number_gt                2628
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014/6 (Sheldrick, 2014)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1037P)²+7.5637P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3451
_refine_ls_number_parameters     177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1778
_refine_ls_wR_factor_gt          0.1601
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Zn1 Zn 0.14837(4) 0.15043(4) 0.47061(3) 0.0411(2) Uani 1 1 d . . . . .
Cl1 Cl 0.06883(10) 0.03113(9) 0.37825(8) 0.0518(3) Uani 1 1 d . . . . .
Cl2 Cl 0.10258(9) 0.16916(8) 0.58946(6) 0.0424(3) Uani 1 1 d . . . . .
N1 N 0.7558(4) -0.1511(3) 0.8095(3) 0.0515(10) Uani 1 1 d . . . . .
O1 O 0.3978(3) 0.2350(2) 0.6009(2) 0.0545(8) Uani 1 1 d . . . . .
O2 O 0.3078(3) 0.1186(3) 0.5119(2) 0.0589(9) Uani 1 1 d . . . . .
C1 C 0.3888(4) 0.1507(3) 0.5739(3) 0.0445(10) Uani 1 1 d . . . . .
C2 C 0.4819(4) 0.0835(3) 0.6174(3) 0.0419(9) Uani 1 1 d . . . . .
C3 C 0.4749(4) -0.0108(4) 0.5904(3) 0.0506(11) Uani 1 1 d . . . . .
H3 H 0.4088 -0.0330 0.5466 0.061 Uiso 1 1 calc R U . . .
C4 C 0.5651(5) -0.0731(4) 0.6278(3) 0.0544(12) Uani 1 1 d . . . . .
H4 H 0.5600 -0.1376 0.6094 0.065 Uiso 1 1 calc R U . . .
C5 C 0.6608(4) -0.0414(4) 0.6909(3) 0.0489(11) Uani 1 1 d . . . . .
C6 C 0.6675(4) 0.0516(4) 0.7190(3) 0.0584(13) Uani 1 1 d . . . . .
H6 H 0.7334 0.0729 0.7635 0.070 Uiso 1 1 calc R U . . .
C7 C 0.5788(4) 0.1146(4) 0.6829(3) 0.0535(11) Uani 1 1 d . . . . .
H7 H 0.5841 0.1786 0.7027 0.064 Uiso 1 1 calc R U . . .
C8 C 0.7590(5) -0.1089(5) 0.7291(3) 0.0603(14) Uani 1 1 d . . . . .
H8A H 0.7556 -0.1603 0.6877 0.072 Uiso 1 1 calc R U . . .
H8B H 0.8305 -0.0738 0.7410 0.072 Uiso 1 1 calc R U . . .
C9 C 0.6939(6) -0.2282(5) 0.8072(3) 0.0716(17) Uani 1 1 d . . . . .
H9 H 0.6519 -0.2558 0.7534 0.086 Uiso 1 1 calc R U . . .
C10 C 0.6892(6) -0.2691(4) 0.8810(3) 0.0685(15) Uani 1 1 d . . . . .
H10 H 0.6446 -0.3243 0.8780 0.082 Uiso 1 1 calc R U . . .
C11 C 0.7507(4) -0.2284(4) 0.9602(3) 0.0460(10) Uani 1 1 d . . . . .
C12 C 0.8113(5) -0.1479(5) 0.9605(4) 0.0670(16) Uani 1 1 d . . . . .
H12 H 0.8523 -0.1177 1.0132 0.080 Uiso 1 1 calc R U . . .
C13 C 0.8135(5) -0.1099(5) 0.8842(3) 0.0681(16) Uani 1 1 d . . . . .
H13 H 0.8564 -0.0541 0.8853 0.082 Uiso 1 1 calc R U . . .
O1W O 0.5000 -0.3620(13) 0.7500 0.077(5) Uani 0.3333 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O2 1.948(4) . ?
Zn1 O1 1.963(3) 7_556 ?
Zn1 Cl1 2.2572(12) . ?
Zn1 Cl2 2.2748(11) . ?
N1 C9 1.329(8) . ?
N1 C13 1.335(8) . ?
N1 C8 1.481(6) . ?
O1 C1 1.255(6) . ?
O1 Zn1 1.963(3) 7_556 ?
O2 C1 1.257(6) . ?
C1 C2 1.485(6) . ?
C2 C3 1.389(7) . ?
C2 C7 1.397(7) . ?
C3 C4 1.401(7) . ?
C4 C5 1.372(7) . ?
C5 C6 1.378(8) . ?
C5 C8 1.516(6) . ?
C6 C7 1.390(7) . ?
C9 C10 1.381(8) . ?
C10 C11 1.398(7) . ?
C11 C12 1.365(8) . ?
C11 C11 1.468(9) 7_647 ?
C12 C13 1.391(8) . ?

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 Zn1 O1 116.85(17) . 7_556 ?
O2 Zn1 Cl1 103.32(12) . . ?
O1 Zn1 Cl1 103.03(11) 7_556 . ?
O2 Zn1 Cl2 105.90(12) . . ?
O1 Zn1 Cl2 108.85(11) 7_556 . ?
Cl1 Zn1 Cl2 119.42(4) . . ?
C9 N1 C13 120.2(4) . . ?
C9 N1 C8 120.3(5) . . ?
C13 N1 C8 119.5(5) . . ?
C1 O1 Zn1 125.6(3) . 7_556 ?
C1 O2 Zn1 131.0(3) . . ?
O1 C1 O2 125.1(4) . . ?
O1 C1 C2 117.8(4) . . ?
O2 C1 C2 117.0(4) . . ?
C3 C2 C7 119.2(4) . . ?
C3 C2 C1 119.8(4) . . ?
C7 C2 C1 120.9(4) . . ?
C2 C3 C4 120.0(5) . . ?
C5 C4 C3 120.3(5) . . ?
C4 C5 C6 120.0(4) . . ?
C4 C5 C8 119.7(5) . . ?
C6 C5 C8 120.4(5) . . ?
C5 C6 C7 120.7(5) . . ?
C6 C7 C2 119.8(5) . . ?
N1 C8 C5 110.4(4) . . ?
N1 C9 C10 121.6(6) . . ?
C9 C10 C11 119.3(6) . . ?
C12 C11 C10 117.8(5) . . ?
C12 C11 C11 121.8(6) . 7_647 ?
C10 C11 C11 120.5(6) . 7_647 ?
C11 C12 C13 120.6(6) . . ?
N1 C13 C12 120.5(6) . . ?

_refine_diff_density_max         1.406
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.113

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_an94
_database_code_depnum_ccdc_archive 'CCDC 1441131'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H26 Br2 N4 O10 Pd'
_chemical_formula_sum            'C26 H26 Br2 N4 O10 Pd'
_chemical_formula_weight         820.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1476(17)
_cell_length_b                   8.2521(18)
_cell_length_c                   12.398(3)
_cell_angle_alpha                80.843(8)
_cell_angle_beta                 72.380(7)
_cell_angle_gamma                67.642(7)
_cell_volume                     733.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9915
_cell_measurement_theta_min      2.672
_cell_measurement_theta_max      28.362

_exptl_crystal_description       plates
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_F_000             406
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    3.418
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_T_max  0.599
_exptl_absorpt_process_details   'SADABS (Sheldrick 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9915
_diffrn_reflns_av_unetI/netI     0.0967
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.672
_diffrn_reflns_theta_max         28.362
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             3495
_reflns_number_gt                2234
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'APEX2 (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014/6 (Sheldrick, 2014)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3495
_refine_ls_number_parameters     197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1058
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pd1 Pd 0.0000 0.0000 0.5000 0.02760(15) Uani 1 2 d S . P . .
Br1 Br 0.03617(7) 0.13580(6) 0.30845(4) 0.03582(17) Uani 1 1 d . . . . .
N1 N 0.1009(5) 0.2131(4) -0.2691(3) 0.0224(8) Uani 1 1 d . . . . .
N2 N 0.2869(7) -0.1755(6) 0.4589(3) 0.0363(12) Uani 1 1 d . . . . .
O1 O 0.7295(5) 0.2644(4) 0.0131(3) 0.0287(7) Uani 1 1 d . . . . .
O2 O 0.4683(5) 0.3721(4) 0.1473(3) 0.0325(8) Uani 1 1 d . . . . .
H2 H 0.5384 0.3883 0.1787 0.049 Uiso 1 1 calc R U . . .
O21 O 0.3723(8) -0.1123(7) 0.4663(5) 0.0832(16) Uani 1 1 d . . . . .
O22 O 0.3085(7) -0.3030(6) 0.4262(5) 0.0802(16) Uani 1 1 d . . . . .
C1 C 0.5671(7) 0.2967(5) 0.0486(4) 0.0234(10) Uani 1 1 d . . . . .
C2 C 0.4522(6) 0.2543(5) -0.0094(4) 0.0215(9) Uani 1 1 d . . . . .
C3 C 0.2646(6) 0.2948(6) 0.0358(4) 0.0244(10) Uani 1 1 d . . . . .
H3 H 0.2038 0.3568 0.1034 0.029 Uiso 1 1 calc R U . . .
C4 C 0.1653(7) 0.2450(6) -0.0174(4) 0.0275(10) Uani 1 1 d . . . . .
H4 H 0.0360 0.2754 0.0128 0.033 Uiso 1 1 calc R U . . .
C5 C 0.2548(6) 0.1506(5) -0.1150(4) 0.0214(9) Uani 1 1 d . . . . .
C6 C 0.4411(7) 0.1116(6) -0.1597(4) 0.0253(10) Uani 1 1 d . . . . .
H6 H 0.5019 0.0488 -0.2270 0.030 Uiso 1 1 calc R U . . .
C7 C 0.5416(6) 0.1626(5) -0.1080(4) 0.0224(9) Uani 1 1 d . . . . .
H7 H 0.6703 0.1352 -0.1396 0.027 Uiso 1 1 calc R U . . .
C8 C 0.1469(7) 0.0910(6) -0.1709(4) 0.0269(10) Uani 1 1 d . . . . .
H8A H 0.2206 -0.0289 -0.1975 0.032 Uiso 1 1 calc R U . . .
H8B H 0.0319 0.0875 -0.1150 0.032 Uiso 1 1 calc R U . . .
C9 C -0.0569(7) 0.3501(6) -0.2543(4) 0.0298(11) Uani 1 1 d . . . . .
H9 H -0.1414 0.3685 -0.1814 0.036 Uiso 1 1 calc R U . . .
C10 C -0.0977(7) 0.4641(6) -0.3432(4) 0.0313(12) Uani 1 1 d . . . . .
H10 H -0.2104 0.5611 -0.3312 0.038 Uiso 1 1 calc R U . . .
C11 C 0.0230(7) 0.4405(5) -0.4509(4) 0.0234(10) Uani 1 1 d . . . . .
C12 C 0.1821(7) 0.2968(7) -0.4617(4) 0.0361(13) Uani 1 1 d . . . . .
H12 H 0.2686 0.2743 -0.5339 0.043 Uiso 1 1 calc R U . . .
C13 C 0.2191(7) 0.1851(6) -0.3706(4) 0.0382(13) Uani 1 1 d . . . . .
H13 H 0.3305 0.0866 -0.3804 0.046 Uiso 1 1 calc R U . . .
O1W O 0.6247(6) 0.4440(5) 0.2807(4) 0.0691(14) Uani 1 1 d . . . . .
H1WA H 0.5639 0.4911 0.3428 0.104 Uiso 1 1 d R U . . .
H1WB H 0.7172 0.3779 0.3029 0.104 Uiso 1 1 d R U . . .


_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
Pd1 N2 2.181(5) 2_556 ?
Pd1 N2 2.181(5) . ?
Pd1 Br1 2.4419(7) 2_556 ?
Pd1 Br1 2.4419(7) . ?
N1 C13 1.324(6) . ?
N1 C9 1.335(6) . ?
N1 C8 1.495(5) . ?
N2 O21 1.046(6) . ?
N2 O22 1.120(5) . ?
O1 C1 1.196(6) . ?
O2 C1 1.340(5) . ?
C1 C2 1.501(6) . ?
C2 C3 1.384(6) . ?
C2 C7 1.390(6) . ?
C3 C4 1.386(6) . ?
C4 C5 1.392(6) . ?
C5 C6 1.375(7) . ?
C5 C8 1.518(6) . ?
C6 C7 1.387(6) . ?
C9 C10 1.365(6) . ?
C10 C11 1.389(6) . ?
C11 C12 1.371(6) . ?
C11 C11 1.485(9) 2_564 ?
C12 C13 1.371(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 N2 180.0 2_556 . ?
N2 Pd1 Br1 91.72(10) 2_556 2_556 ?
N2 Pd1 Br1 88.28(10) . 2_556 ?
N2 Pd1 Br1 88.28(10) 2_556 . ?
N2 Pd1 Br1 91.72(10) . . ?
Br1 Pd1 Br1 180.000(12) 2_556 . ?
C13 N1 C9 120.3(4) . . ?
C13 N1 C8 119.4(4) . . ?
C9 N1 C8 120.3(4) . . ?
O21 N2 O22 135.5(7) . . ?
O21 N2 Pd1 110.5(5) . . ?
O22 N2 Pd1 113.5(4) . . ?
O1 C1 O2 123.0(4) . . ?
O1 C1 C2 124.5(4) . . ?
O2 C1 C2 112.4(4) . . ?
C3 C2 C7 120.0(4) . . ?
C3 C2 C1 122.0(4) . . ?
C7 C2 C1 117.9(4) . . ?
C2 C3 C4 120.2(4) . . ?
C3 C4 C5 120.0(4) . . ?
C6 C5 C4 119.5(4) . . ?
C6 C5 C8 120.5(4) . . ?
C4 C5 C8 120.0(4) . . ?
C5 C6 C7 121.0(4) . . ?
C6 C7 C2 119.3(4) . . ?
N1 C8 C5 110.6(3) . . ?
N1 C9 C10 120.5(4) . . ?
C9 C10 C11 121.1(4) . . ?
C12 C11 C10 116.1(4) . . ?
C12 C11 C11 122.3(5) . 2_564 ?
C10 C11 C11 121.6(5) . 2_564 ?
C11 C12 C13 121.4(5) . . ?
N1 C13 C12 120.6(5) . . ?

_refine_diff_density_max         0.837
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.119

_shelxl_version_number           2013-3

