# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Compound1
_database_code_depnum_ccdc_archive 'CCDC 1417516'
_audit_update_record             
;
2015-09-23 deposited with the CCDC.
2015-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H32 Ni2 O18'
_chemical_formula_weight         653.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0132 0.0074 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Ni Ni 0.3262 1.3024 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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'

_cell_length_a                   15.4414(15)
_cell_length_b                   10.9156(11)
_cell_length_c                   14.5960(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2460.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9998
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      33.60

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    2.040
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6735
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_process_details   'SADABS, G. M. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light source station 11.3.1'
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34124
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.876
_diffrn_reflns_theta_max         33.610
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7435
_reflns_number_gt                6938
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.997

_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.
;
_vrf_PLAT420_Compound1           
;
PROBLEM: D-H Without Acceptor        O10W   -   H10A   ..     Please Check 
RESPONSE: After locating the two hydrogen atoms bound to O10w, only one was found to be directed towards a suitable hydrogen bond acceptor.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (beta)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0589P)²] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.481(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7435
_refine_ls_number_parameters     397
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.086
_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
C1 C 0.2042(2) 0.5085(3) 0.3683(2) 0.0138(6) Uani 1 1 d . . . . .
C2 C 0.2913(2) 0.5705(3) 0.3603(3) 0.0137(6) Uani 1 1 d . . . . .
C3 C 0.3659(2) 0.5016(3) 0.3739(3) 0.0152(7) Uani 1 1 d . . . . .
H3 H 0.3618 0.4166 0.3874 0.018 Uiso 1 1 calc R U . . .
C4 C 0.4470(2) 0.5579(3) 0.3675(3) 0.0147(6) Uani 1 1 d . . . . .
C5 C 0.5284(2) 0.4826(3) 0.3758(2) 0.0142(6) Uani 1 1 d . . . . .
C6 C 0.4527(2) 0.6823(3) 0.3476(3) 0.0183(7) Uani 1 1 d . . . . .
H6 H 0.5080 0.7204 0.3444 0.022 Uiso 1 1 calc R U . . .
C7 C 0.3778(3) 0.7525(3) 0.3321(4) 0.0192(10) Uani 1 1 d . . . . .
C8 C 0.2974(2) 0.6958(3) 0.3395(3) 0.0162(6) Uani 1 1 d . . . . .
H8 H 0.2461 0.7423 0.3304 0.019 Uiso 1 1 calc R U . . .
C9 C 0.3850(3) 0.8860(3) 0.3054(4) 0.0281(9) Uani 1 1 d . . . . .
H9A H 0.3939 0.8923 0.2391 0.042 Uiso 1 1 calc R U . . .
H9B H 0.4341 0.9232 0.3374 0.042 Uiso 1 1 calc R U . . .
H9C H 0.3315 0.9288 0.3223 0.042 Uiso 1 1 calc R U . . .
C10 C 0.5499(2) 0.5143(3) 0.6239(2) 0.0138(6) Uani 1 1 d . . . . .
C11 C 0.4678(2) 0.4407(3) 0.6242(2) 0.0128(6) Uani 1 1 d . . . . .
C12 C 0.3881(2) 0.5000(3) 0.6164(3) 0.0136(7) Uani 1 1 d . . . . .
H12 H 0.3862 0.5863 0.6079 0.016 Uiso 1 1 calc R U . . .
C13 C 0.3115(2) 0.4333(3) 0.6212(2) 0.0133(6) Uani 1 1 d . . . . .
C14 C 0.2266(2) 0.4982(3) 0.6128(2) 0.0149(6) Uani 1 1 d . . . . .
C15 C 0.3148(2) 0.3070(3) 0.6359(3) 0.0175(6) Uani 1 1 d . . . . .
H15 H 0.2625 0.2614 0.6402 0.021 Uiso 1 1 calc R U . . .
C16 C 0.3944(3) 0.2469(3) 0.6445(4) 0.0204(9) Uani 1 1 d . . . . .
C17 C 0.4703(2) 0.3144(3) 0.6371(3) 0.0168(6) Uani 1 1 d . . . . .
H17 H 0.5246 0.2739 0.6408 0.020 Uiso 1 1 calc R U . . .
C18 C 0.3980(3) 0.1122(4) 0.6644(5) 0.0367(12) Uani 1 1 d . . . . .
H18A H 0.4121 0.0675 0.6081 0.055 Uiso 1 1 calc R U . . .
H18B H 0.3416 0.0847 0.6874 0.055 Uiso 1 1 calc R U . . .
H18C H 0.4425 0.0962 0.7107 0.055 Uiso 1 1 calc R U . . .
O1 O 0.20437(16) 0.3954(2) 0.34568(19) 0.0156(5) Uani 1 1 d . . . . .
O2 O 0.13970(17) 0.5685(2) 0.3931(2) 0.0197(5) Uani 1 1 d . . . . .
O1W O 0.20531(17) 0.1346(2) 0.31414(19) 0.0170(5) Uani 1 1 d D . . . .
O3 O 0.51810(16) 0.3667(2) 0.3667(2) 0.0181(5) Uani 1 1 d . . . . .
O2W O 0.07822(19) 0.2870(2) 0.2262(2) 0.0225(5) Uani 1 1 d D . . . .
O4 O 0.59970(18) 0.5340(2) 0.3871(2) 0.0194(6) Uani 1 1 d . . . . .
O3W O 0.02831(17) 0.3844(2) 0.4135(3) 0.0286(7) Uani 1 1 d D . . . .
O5 O 0.62046(16) 0.4617(2) 0.6105(2) 0.0176(5) Uani 1 1 d . . . . .
O4W O 0.16382(19) 0.2257(2) 0.48957(19) 0.0177(5) Uani 1 1 d D . . . .
O6 O 0.54159(16) 0.6289(2) 0.6392(2) 0.0161(5) Uani 1 1 d . . . . .
O5W O 0.65973(18) 0.7239(2) 0.49698(19) 0.0174(5) Uani 1 1 d D . . . .
O7 O 0.16167(16) 0.4415(2) 0.5837(2) 0.0198(5) Uani 1 1 d . . . . .
O6W O 0.73265(17) 0.6302(2) 0.66453(18) 0.0156(5) Uani 1 1 d D . . . .
O8 O 0.22703(16) 0.6106(2) 0.6376(2) 0.0159(5) Uani 1 1 d . . . . .
O7W O 0.61259(17) 0.7853(3) 0.7740(2) 0.0207(5) Uani 1 1 d D . . . .
O8W O 0.54179(17) 0.8859(2) 0.6008(2) 0.0197(5) Uani 1 1 d D . . . .
O9W O -0.1512(3) 0.3870(4) 0.4521(3) 0.0502(10) Uani 1 1 d D . . . .
O10W O 0.8685(2) 0.6392(4) 0.5285(3) 0.0499(11) Uani 1 1 d D . . . .
Ni1 Ni 0.11446(3) 0.25981(4) 0.36162(3) 0.01230(13) Uani 1 1 d . . . . .
Ni2 Ni 0.63588(3) 0.75673(3) 0.63267(3) 0.01182(12) Uani 1 1 d . . . . .
H10B H 0.846(3) 0.682(4) 0.5772(18) 0.018 Uiso 1 1 d D U . . .
H2B H 0.069(3) 0.353(2) 0.191(2) 0.018 Uiso 1 1 d D U . . .
H7B H 0.654(2) 0.803(4) 0.814(2) 0.018 Uiso 1 1 d D U . . .
H9W H -0.2005(18) 0.338(3) 0.456(3) 0.018 Uiso 1 1 d D U . . .
H1A H 0.220(3) 0.125(3) 0.2563(12) 0.018 Uiso 1 1 d D U . . .
H1B H 0.176(3) 0.067(2) 0.333(3) 0.018 Uiso 1 1 d D U . . .
H2A H 0.047(3) 0.224(2) 0.205(3) 0.018 Uiso 1 1 d D U . . .
H3A H -0.0268(12) 0.372(4) 0.428(3) 0.018 Uiso 1 1 d D U . . .
H3B H 0.040(2) 0.4624(17) 0.401(3) 0.018 Uiso 1 1 d D U . . .
H4A H 0.127(2) 0.178(3) 0.520(3) 0.018 Uiso 1 1 d D U . . .
H4B H 0.170(3) 0.297(2) 0.520(3) 0.018 Uiso 1 1 d D U . . .
H5A H 0.653(3) 0.6515(19) 0.469(3) 0.018 Uiso 1 1 d D U . . .
H5B H 0.651(3) 0.781(3) 0.454(2) 0.018 Uiso 1 1 d D U . . .
H6A H 0.704(3) 0.561(2) 0.656(3) 0.018 Uiso 1 1 d D U . . .
H7A H 0.585(3) 0.723(3) 0.804(3) 0.018 Uiso 1 1 d D U . . .
H8A H 0.567(3) 0.950(3) 0.576(3) 0.018 Uiso 1 1 d D U . . .
H10A H 0.836(2) 0.656(4) 0.4769(16) 0.018 Uiso 1 1 d D 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
C1 O2 1.246(4) . ?
C1 O1 1.278(4) . ?
C1 C2 1.511(4) . ?
C2 C3 1.390(4) . ?
C2 C8 1.404(4) . ?
C3 C4 1.398(5) . ?
C3 H3 0.9500 . ?
C4 C6 1.392(5) . ?
C4 C5 1.506(5) . ?
C5 O4 1.247(4) . ?
C5 O3 1.282(4) . ?
C6 C7 1.405(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.393(5) . ?
C7 C9 1.512(5) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 O5 1.247(4) . ?
C10 O6 1.278(4) . ?
C10 C11 1.500(4) . ?
C11 C17 1.392(4) . ?
C11 C12 1.395(4) . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C15 1.396(4) . ?
C13 C14 1.495(5) . ?
C14 O7 1.252(4) . ?
C14 O8 1.279(4) . ?
C15 C16 1.399(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(5) . ?
C16 C18 1.500(5) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O1 Ni1 2.043(2) . ?
O1W Ni1 2.078(2) . ?
O1W H1A 0.881(14) . ?
O1W H1B 0.905(13) . ?
O3 Ni1 2.031(2) 3 ?
O2W Ni1 2.076(3) . ?
O2W H2B 0.894(14) . ?
O2W H2A 0.899(14) . ?
O3W Ni1 2.047(3) . ?
O3W H3A 0.888(14) . ?
O3W H3B 0.889(14) . ?
O4W Ni1 2.051(3) . ?
O4W H4A 0.893(14) . ?
O4W H4B 0.898(14) . ?
O6 Ni2 2.019(2) . ?
O5W Ni2 2.046(3) . ?
O5W H5A 0.896(14) . ?
O5W H5B 0.894(14) . ?
O6W Ni2 2.087(2) . ?
O6W H6A 0.884(14) . ?
O8 Ni2 2.021(2) 3_465 ?
O7W Ni2 2.117(3) . ?
O7W H7B 0.887(14) . ?
O7W H7A 0.908(14) . ?
O8W Ni2 2.077(3) . ?
O8W H8A 0.886(14) . ?
O9W H9W 0.934(14) . ?
O10W H10B 0.916(14) . ?
O10W H10A 0.922(14) . ?
Ni1 O3 2.031(2) 3_455 ?
Ni2 O8 2.021(2) 3_565 ?

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 C1 O1 125.8(3) . . ?
O2 C1 C2 119.9(3) . . ?
O1 C1 C2 114.2(3) . . ?
C3 C2 C8 120.2(3) . . ?
C3 C2 C1 119.0(3) . . ?
C8 C2 C1 120.8(3) . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C6 C4 C3 120.0(3) . . ?
C6 C4 C5 119.8(3) . . ?
C3 C4 C5 120.1(3) . . ?
O4 C5 O3 124.5(3) . . ?
O4 C5 C4 120.1(3) . . ?
O3 C5 C4 115.3(3) . . ?
C4 C6 C7 120.9(3) . . ?
C4 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 118.6(3) . . ?
C8 C7 C9 120.9(4) . . ?
C6 C7 C9 120.5(4) . . ?
C7 C8 C2 120.6(3) . . ?
C7 C8 H8 119.7 . . ?
C2 C8 H8 119.7 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5 C10 O6 124.4(3) . . ?
O5 C10 C11 119.5(3) . . ?
O6 C10 C11 116.0(3) . . ?
C17 C11 C12 119.6(3) . . ?
C17 C11 C10 120.5(3) . . ?
C12 C11 C10 119.8(3) . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C15 119.6(3) . . ?
C12 C13 C14 119.5(3) . . ?
C15 C13 C14 120.9(3) . . ?
O7 C14 O8 125.1(3) . . ?
O7 C14 C13 119.7(3) . . ?
O8 C14 C13 115.3(3) . . ?
C13 C15 C16 120.5(3) . . ?
C13 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 119.1(3) . . ?
C17 C16 C18 120.3(4) . . ?
C15 C16 C18 120.6(4) . . ?
C16 C17 C11 120.9(3) . . ?
C16 C17 H17 119.6 . . ?
C11 C17 H17 119.6 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C1 O1 Ni1 132.0(2) . . ?
Ni1 O1W H1A 125(3) . . ?
Ni1 O1W H1B 96(3) . . ?
H1A O1W H1B 109(3) . . ?
C5 O3 Ni1 125.7(2) . 3 ?
Ni1 O2W H2B 134(3) . . ?
Ni1 O2W H2A 112(3) . . ?
H2B O2W H2A 110(3) . . ?
Ni1 O3W H3A 128(3) . . ?
Ni1 O3W H3B 116(3) . . ?
H3A O3W H3B 112(3) . . ?
Ni1 O4W H4A 109(3) . . ?
Ni1 O4W H4B 110(3) . . ?
H4A O4W H4B 109(3) . . ?
C10 O6 Ni2 126.6(2) . . ?
Ni2 O5W H5A 125(3) . . ?
Ni2 O5W H5B 122(3) . . ?
H5A O5W H5B 106(3) . . ?
Ni2 O6W H6A 100(3) . . ?
C14 O8 Ni2 132.3(2) . 3_465 ?
Ni2 O7W H7B 124(3) . . ?
Ni2 O7W H7A 116(3) . . ?
H7B O7W H7A 100(4) . . ?
Ni2 O8W H8A 109(3) . . ?
H10B O10W H10A 109(3) . . ?
O3 Ni1 O1 174.04(12) 3_455 . ?
O3 Ni1 O3W 87.82(11) 3_455 . ?
O1 Ni1 O3W 90.15(11) . . ?
O3 Ni1 O4W 96.64(12) 3_455 . ?
O1 Ni1 O4W 89.01(11) . . ?
O3W Ni1 O4W 91.46(14) . . ?
O3 Ni1 O2W 86.23(12) 3_455 . ?
O1 Ni1 O2W 88.35(11) . . ?
O3W Ni1 O2W 94.70(14) . . ?
O4W Ni1 O2W 173.30(12) . . ?
O3 Ni1 O1W 93.41(10) 3_455 . ?
O1 Ni1 O1W 88.84(10) . . ?
O3W Ni1 O1W 177.45(13) . . ?
O4W Ni1 O1W 86.18(11) . . ?
O2W Ni1 O1W 87.61(12) . . ?
O6 Ni2 O8 174.84(14) . 3_565 ?
O6 Ni2 O5W 93.12(12) . . ?
O8 Ni2 O5W 91.97(11) 3_565 . ?
O6 Ni2 O8W 88.57(10) . . ?
O8 Ni2 O8W 90.50(10) 3_565 . ?
O5W Ni2 O8W 91.62(12) . . ?
O6 Ni2 O6W 92.80(10) . . ?
O8 Ni2 O6W 88.14(10) 3_565 . ?
O5W Ni2 O6W 88.34(11) . . ?
O8W Ni2 O6W 178.64(10) . . ?
O6 Ni2 O7W 86.17(12) . . ?
O8 Ni2 O7W 88.76(12) 3_565 . ?
O5W Ni2 O7W 178.26(11) . . ?
O8W Ni2 O7W 89.95(12) . . ?
O6W Ni2 O7W 90.11(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3W H3A O9W 0.888(14) 1.959(18) 2.829(5) 166(4) .
O3W H3B O2 0.889(14) 1.94(3) 2.662(4) 138(3) .
O4W H4B O7 0.898(14) 1.840(17) 2.727(4) 169(4) .
O5W H5A O4 0.896(14) 1.93(2) 2.780(4) 157(4) .
O6W H6A O5 0.884(14) 1.81(2) 2.647(4) 156(4) .
O1W H1B O4 0.905(13) 1.800(17) 2.679(4) 164(4) 3_455
O4W H4A O5 0.893(14) 2.02(3) 2.784(4) 143(4) 3_455
O1W H1A O8 0.881(14) 1.921(15) 2.793(4) 170(4) 4_544
O2W H2A O6 0.899(14) 1.96(2) 2.830(4) 162(4) 4_544
O2W H2B O8W 0.894(14) 2.19(3) 2.819(4) 127(3) 4_544
O5W H5B O2 0.894(14) 1.874(16) 2.744(4) 164(4) 3_565
O8W H8A O7 0.886(14) 1.88(3) 2.653(4) 145(4) 3_565
O7W H7A O3 0.908(14) 2.09(2) 2.942(4) 156(4) 2_665
O7W H7B O1W 0.887(14) 2.28(3) 3.002(4) 139(4) 2_665
O10W H10B O6W 0.916(14) 2.24(4) 2.890(5) 128(4) .

_refine_diff_density_max         0.681
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.111

####################################################################### 
# 
# 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_Compound2
_database_code_depnum_ccdc_archive 'CCDC 1417517'
_audit_update_record             
;
2015-09-23 deposited with the CCDC.
2015-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H54.75 O33.50 Zn6'
_chemical_formula_weight         1523.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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'
O O 0.0132 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2282 1.6718 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_H-M_alt        'P n n 2'
_space_group_name_Hall           'P 2 -2n'

_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'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   20.775(3)
_cell_length_b                   27.566(3)
_cell_length_c                   10.8460(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6211.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9911
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      33.21

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_F_000             3091
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    2.992
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_process_details   'SADABS, G. M. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            90099
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.643
_diffrn_reflns_theta_max         33.601
_diffrn_reflns_theta_full        27.706
_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 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             18933
_reflns_number_gt                16548
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.908
_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.
 
 _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.
;
_vrf_PLAT201_Compound2           
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         17 Report
RESPONSE: There is some rotational disorder of four of the five methylisophthlate ligands, so the affected atoms have been modelled over two sites with complementary site occupancy factors. These partial occupancy atoms have been refined with isotropic thermal displacement parameters.
;
_vrf_PLAT430_Compound2           
;
PROBLEM: Short Inter D...A Contact  O3WA   ..  O115    ..       1.48 Ang.  
RESPONSE: All D...A contacts of less than 2.6 A involve two partial occupancy oxygen atoms whose site occupancy factors sum to less than 1, so they will not both be present at the same time. The D...A contacts between 2.62 and 2.9 A also always involve at least one partial occupancy water molecule, however these contacts are long enough to be hydrogen bonds. No hydrogen atoms have been included on the water molecules because they could not be located during the refinement process.
;
_vrf_PLAT043_Compound2           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      25.89 Check 
RESPONSE: This is due to hydrogen atoms belonging to water molecules and hydroxide anions being included in the molecular formula but not in the model, as they could not be located.
;
_vrf_PLAT306_Compound2           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......       O100 Check 
RESPONSE: These atoms are the oxygen atoms of water molecules, and hydrogen atoms could not be located durng the refinement.
;
_vrf_PLAT934_Compound2           
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          2 Check 
RESPONSE: This refers to (1 4 0) and (1 1 7). As there are only two reflections, it is not likely that this is a systematic error.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (beta)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0699P)²+15.1807P] 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   0.491(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         18933
_refine_ls_number_parameters     767
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1432
_refine_ls_wR_factor_gt          0.1378
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
C1 C 0.5528(3) 0.3143(2) 0.7289(5) 0.0222(12) Uani 1 1 d . . . . .
C2 C 0.5735(4) 0.2951(2) 0.6074(5) 0.0251(13) Uani 1 1 d . . . . .
C3 C 0.5400(3) 0.3072(2) 0.5014(6) 0.0241(11) Uani 1 1 d . . . . .
H3 H 0.5043 0.3287 0.5059 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5587(3) 0.2878(2) 0.3882(5) 0.0245(13) Uani 1 1 d . . . . .
C5 C 0.5205(3) 0.2990(2) 0.2768(6) 0.0244(12) Uani 1 1 d . . . . .
C6 C 0.6133(4) 0.2581(3) 0.3814(6) 0.0331(15) Uani 1 1 d . . . . .
H6 H 0.6261 0.2453 0.3039 0.040 Uiso 1 1 calc R U . . .
C7 C 0.6490(5) 0.2468(3) 0.4862(7) 0.043(2) Uani 1 1 d . . . . .
C8 C 0.6278(4) 0.2650(3) 0.5985(6) 0.0339(16) Uani 1 1 d . . . . .
H8 H 0.6508 0.2570 0.6713 0.041 Uiso 1 1 calc R U . . .
C9A C 0.7169(13) 0.2231(11) 0.4715(18) 0.053(6) Uiso 0.61(6) 1 d . . P A 1
H9A1 H 0.7228 0.2125 0.3860 0.079 Uiso 0.61(6) 1 calc R U P A 1
H9A2 H 0.7502 0.2468 0.4928 0.079 Uiso 0.61(6) 1 calc R U P A 1
H9A3 H 0.7203 0.1950 0.5266 0.079 Uiso 0.61(6) 1 calc R U P A 1
C9B C 0.6994(13) 0.2085(10) 0.4761(17) 0.027(7) Uiso 0.39(6) 1 d . . P A 2
H9B1 H 0.7070 0.2010 0.3890 0.041 Uiso 0.39(6) 1 calc R U P A 2
H9B2 H 0.7394 0.2202 0.5136 0.041 Uiso 0.39(6) 1 calc R U P A 2
H9B3 H 0.6850 0.1792 0.5191 0.041 Uiso 0.39(6) 1 calc R U P A 2
C10 C 0.3901(5) 0.4369(3) 0.2482(8) 0.042(2) Uani 1 1 d . . . . .
C11 C 0.3793(5) 0.4909(3) 0.2568(8) 0.0397(19) Uani 1 1 d . . . . .
C12 C 0.4014(4) 0.5212(2) 0.1640(6) 0.0285(14) Uani 1 1 d . . . . .
H12 H 0.4224 0.5079 0.0939 0.034 Uiso 1 1 calc R U . . .
C13 C 0.3926(4) 0.5715(2) 0.1739(6) 0.0273(14) Uani 1 1 d . . . . .
C14 C 0.4167(3) 0.6032(2) 0.0729(6) 0.0231(12) Uani 1 1 d . . . . .
C15A C 0.3562(8) 0.5914(5) 0.2703(14) 0.025(3) Uiso 0.57(3) 1 d . . P B 1
H15A H 0.3483 0.6254 0.2735 0.030 Uiso 0.57(3) 1 calc R U P B 1
C16A C 0.3317(8) 0.5606(5) 0.3619(14) 0.030(3) Uiso 0.57(3) 1 d . . P B 1
C17A C 0.3382(8) 0.5110(5) 0.3484(14) 0.029(3) Uiso 0.57(3) 1 d . . P B 1
H17A H 0.3149 0.4900 0.4013 0.035 Uiso 0.57(3) 1 calc R U P B 1
C18A C 0.3005(9) 0.5819(6) 0.4759(16) 0.041(4) Uiso 0.57(3) 1 d . . P B 1
H18A H 0.3000 0.6173 0.4695 0.062 Uiso 0.57(3) 1 calc R U P B 1
H18B H 0.2563 0.5698 0.4829 0.062 Uiso 0.57(3) 1 calc R U P B 1
H18C H 0.3251 0.5722 0.5490 0.062 Uiso 0.57(3) 1 calc R U P B 1
C15B C 0.3746(10) 0.5911(6) 0.2914(17) 0.023(4) Uiso 0.43(3) 1 d . . P B 2
H15B H 0.3763 0.6252 0.3037 0.028 Uiso 0.43(3) 1 calc R U P B 2
C16B C 0.3553(9) 0.5622(5) 0.3849(15) 0.022(3) Uiso 0.43(3) 1 d . . P B 2
C17B C 0.3604(9) 0.5121(5) 0.3725(15) 0.020(3) Uiso 0.43(3) 1 d . . P B 2
H17B H 0.3514 0.4917 0.4409 0.024 Uiso 0.43(3) 1 calc R U P B 2
C18B C 0.3280(10) 0.5854(6) 0.5010(18) 0.031(4) Uiso 0.43(3) 1 d . . P B 2
H18D H 0.3162 0.5599 0.5600 0.047 Uiso 0.43(3) 1 calc R U P B 2
H18E H 0.3604 0.6067 0.5380 0.047 Uiso 0.43(3) 1 calc R U P B 2
H18F H 0.2897 0.6044 0.4798 0.047 Uiso 0.43(3) 1 calc R U P B 2
C19 C 0.3490(3) 0.2714(2) 0.1712(7) 0.0287(14) Uani 1 1 d . . . . .
C20 C 0.3022(3) 0.2437(2) 0.2470(7) 0.0253(13) Uani 1 1 d . . . . .
C21 C 0.2604(3) 0.2687(2) 0.3261(8) 0.0255(11) Uani 1 1 d . . . . .
H21 H 0.2603 0.3032 0.3264 0.031 Uiso 1 1 calc R U . . .
C22 C 0.2197(3) 0.2440(2) 0.4031(6) 0.0245(12) Uani 1 1 d . . . . .
C23 C 0.1727(3) 0.2717(2) 0.4791(6) 0.0259(13) Uani 1 1 d . . . . .
C24 C 0.2200(3) 0.1931(2) 0.4053(6) 0.0250(12) Uani 1 1 d . . . . .
H24 H 0.1928 0.1762 0.4608 0.030 Uiso 1 1 calc R U . . .
C25 C 0.2608(4) 0.1672(2) 0.3252(8) 0.0275(11) Uani 1 1 d . . . . .
C26 C 0.3009(3) 0.1930(2) 0.2467(7) 0.0269(13) Uani 1 1 d . . . . .
H26 H 0.3282 0.1758 0.1915 0.032 Uiso 1 1 calc R U . . .
C27 C 0.2611(5) 0.1126(2) 0.3282(9) 0.0397(16) Uani 1 1 d . . . . .
H27A H 0.2297 0.1012 0.3890 0.060 Uiso 1 1 calc R U . . .
H27B H 0.2497 0.1000 0.2465 0.060 Uiso 1 1 calc R U . . .
H27C H 0.3041 0.1011 0.3509 0.060 Uiso 1 1 calc R U . . .
C28 C 0.0013(3) 0.3020(2) 0.3758(5) 0.0253(13) Uani 1 1 d . . . . .
C29 C -0.0380(4) 0.2913(3) 0.2641(6) 0.0291(14) Uani 1 1 d . . . . .
C30 C -0.0211(4) 0.3109(3) 0.1489(7) 0.0326(14) Uani 1 1 d . . . . .
H30 H 0.0142 0.3327 0.1427 0.039 Uiso 1 1 calc R U . . .
C31 C -0.0556(4) 0.2985(3) 0.0450(6) 0.0335(16) Uani 1 1 d . . . . .
C32 C -0.0345(4) 0.3188(3) -0.0783(6) 0.0345(16) Uani 1 1 d . . . . .
C33 C -0.1071(4) 0.2670(4) 0.0530(6) 0.042(2) Uani 1 1 d . . . . .
H33 H -0.1299 0.2579 -0.0195 0.050 Uiso 1 1 calc R U . . .
C34 C -0.1260(5) 0.2481(4) 0.1680(7) 0.048(2) Uani 1 1 d D . . . .
C35 C -0.0911(4) 0.2606(3) 0.2717(7) 0.0380(17) Uani 1 1 d . . . . .
H35 H -0.1035 0.2480 0.3496 0.046 Uiso 1 1 calc R U . . .
C36A C -0.1751(16) 0.2032(14) 0.167(2) 0.049(8) Uiso 0.43(7) 1 d D . P C 1
H36A H -0.1949 0.2004 0.0852 0.073 Uiso 0.43(7) 1 calc R U P C 1
H36B H -0.1518 0.1732 0.1860 0.073 Uiso 0.43(7) 1 calc R U P C 1
H36C H -0.2087 0.2084 0.2289 0.073 Uiso 0.43(7) 1 calc R U P C 1
C36B C -0.1885(9) 0.2199(10) 0.1762(15) 0.039(5) Uiso 0.57(7) 1 d D . P C 2
H36D H -0.2057 0.2147 0.0931 0.058 Uiso 0.57(7) 1 calc R U P C 2
H36E H -0.1805 0.1885 0.2156 0.058 Uiso 0.57(7) 1 calc R U P C 2
H36F H -0.2197 0.2383 0.2252 0.058 Uiso 0.57(7) 1 calc R U P C 2
C37 C 0.1310(6) 0.4409(3) 0.4092(11) 0.067(4) Uani 1 1 d . . . . .
C38 C 0.1330(6) 0.4947(3) 0.4036(9) 0.052(3) Uani 1 1 d . . . . .
C39 C 0.1030(4) 0.5221(2) 0.4954(8) 0.0357(17) Uani 1 1 d . . . . .
H39 H 0.0833 0.5068 0.5641 0.043 Uiso 1 1 calc R U . . .
C40 C 0.1025(4) 0.5729(2) 0.4838(6) 0.0296(15) Uani 1 1 d . . . . .
C41 C 0.0688(4) 0.6028(2) 0.5804(6) 0.0252(13) Uani 1 1 d . . . . .
C42A C 0.1397(7) 0.5945(4) 0.3899(11) 0.024(3) Uiso 0.61(2) 1 d . . P D 1
H42A H 0.1427 0.6289 0.3870 0.029 Uiso 0.61(2) 1 calc R U P D 1
C43A C 0.1717(8) 0.5676(4) 0.3022(12) 0.030(3) Uiso 0.61(2) 1 d . . P D 1
C44A C 0.1723(8) 0.5169(5) 0.3179(14) 0.033(3) Uiso 0.61(2) 1 d . . P D 1
H44A H 0.2001 0.4976 0.2687 0.040 Uiso 0.61(2) 1 calc R U P D 1
C45A C 0.2046(9) 0.5915(6) 0.1959(15) 0.045(4) Uiso 0.61(2) 1 d . . P D 1
H45A H 0.2247 0.5667 0.1436 0.067 Uiso 0.61(2) 1 calc R U P D 1
H45B H 0.1730 0.6098 0.1476 0.067 Uiso 0.61(2) 1 calc R U P D 1
H45C H 0.2378 0.6137 0.2268 0.067 Uiso 0.61(2) 1 calc R U P D 1
C42B C 0.1195(12) 0.5965(7) 0.374(2) 0.027(4) Uiso 0.39(2) 1 d . . P D 2
H42B H 0.1125 0.6304 0.3648 0.033 Uiso 0.39(2) 1 calc R U P D 2
C43B C 0.1458(11) 0.5705(6) 0.2816(18) 0.028(4) Uiso 0.39(2) 1 d . . P D 2
C44B C 0.1495(10) 0.5204(6) 0.2842(19) 0.027(4) Uiso 0.39(2) 1 d . . P D 2
H44B H 0.1621 0.5027 0.2131 0.033 Uiso 0.39(2) 1 calc R U P D 2
C45B C 0.1743(12) 0.5946(8) 0.166(2) 0.040(5) Uiso 0.39(2) 1 d . . P D 2
H45D H 0.1909 0.5696 0.1102 0.060 Uiso 0.39(2) 1 calc R U P D 2
H45E H 0.1407 0.6133 0.1237 0.060 Uiso 0.39(2) 1 calc R U P D 2
H45F H 0.2094 0.6164 0.1900 0.060 Uiso 0.39(2) 1 calc R U P D 2
O1 O 0.5762(2) 0.29532(18) 0.8246(4) 0.0251(9) Uani 1 1 d . . . . .
O1H O 0.4658(2) 0.33418(17) -0.0144(4) 0.0220(9) Uani 1 1 d . . . . .
O2A O 0.5206(12) 0.3502(4) 0.7265(8) 0.017(3) Uiso 0.54(7) 1 d . . P . .
O2B O 0.5024(13) 0.3466(4) 0.7266(9) 0.015(3) Uiso 0.46(7) 1 d . . P . .
O1W O 0.5214(3) 0.4497(2) 0.7447(5) 0.0443(14) Uani 1 1 d . . . . .
O2H O 0.0557(2) 0.33692(17) 0.6664(4) 0.0249(9) Uani 1 1 d . . . . .
O3 O 0.5246(2) 0.27032(17) 0.1833(4) 0.0224(9) Uani 1 1 d . . . . .
O2WA O 0.4096(6) 0.4267(5) 0.8917(12) 0.050(4) Uiso 0.63(3) 1 d . . P . .
O2WB O 0.3952(9) 0.4073(7) 0.8420(19) 0.048(6) Uiso 0.37(3) 1 d . . P . .
O4 O 0.4850(3) 0.33530(19) 0.2785(5) 0.0325(11) Uani 1 1 d . . . . .
O3WA O 0.0173(6) 0.5503(4) 0.9104(11) 0.057(3) Uiso 0.712(12) 1 d . . P . .
O3WB O -0.0130(16) 0.5421(11) 0.875(3) 0.023(6) Uiso 0.144(6) 1 d . . P . .
O5 O 0.4066(3) 0.42064(17) 0.1447(5) 0.0330(11) Uani 1 1 d . . . . .
O4WA O -0.1029(6) 0.5714(5) 0.7699(13) 0.070(4) Uiso 0.712(12) 1 d . . P . .
O4WB O -0.0698(14) 0.5379(10) 0.786(3) 0.021(6) Uiso 0.144(6) 1 d . . P . .
O6 O 0.3857(4) 0.4117(2) 0.3455(7) 0.059(2) Uani 1 1 d . . . . .
O5W O -0.1127(13) 0.6284(10) 0.897(3) 0.061(7) Uiso 0.288(12) 1 d . . P . .
O7 O 0.4471(3) 0.58274(18) -0.0143(5) 0.0357(12) Uani 1 1 d . . . . .
O8 O 0.4047(2) 0.64770(16) 0.0814(5) 0.0262(10) Uani 1 1 d . . . . .
O9 O 0.3923(2) 0.25045(17) 0.1118(5) 0.0275(10) Uani 1 1 d . . . . .
O10 O 0.3428(2) 0.31789(18) 0.1718(6) 0.0342(12) Uani 1 1 d . . . . .
O11 O 0.1304(2) 0.25040(19) 0.5405(4) 0.0276(10) Uani 1 1 d . . . . .
O12 O 0.1781(3) 0.31799(17) 0.4785(6) 0.0372(13) Uani 1 1 d . . . . .
O13 O -0.0033(2) 0.27253(17) 0.4656(4) 0.0233(9) Uani 1 1 d . . . . .
O14 O 0.0362(3) 0.33961(19) 0.3742(5) 0.0311(10) Uani 1 1 d . . . . .
O15 O -0.0541(3) 0.2972(2) -0.1711(4) 0.0344(12) Uani 1 1 d . . . . .
O16A O 0.0061(4) 0.3519(3) -0.0773(8) 0.0330(18) Uiso 0.712(12) 1 d . . P . .
O16B O -0.0213(9) 0.3666(6) -0.0810(15) 0.024(4) Uiso 0.288(12) 1 d . . P . .
O17 O 0.1134(3) 0.42248(18) 0.5133(6) 0.0378(12) Uani 1 1 d . . . . .
O18A O 0.1670(7) 0.4126(5) 0.3497(14) 0.056(4) Uiso 0.513(12) 1 d . . P . .
O18B O 0.1283(5) 0.4175(4) 0.3008(10) 0.032(2) Uiso 0.513(12) 1 d . . P . .
O19 O 0.0362(3) 0.58024(19) 0.6607(6) 0.0418(14) Uani 1 1 d . . . . .
O20 O 0.0759(2) 0.64803(16) 0.5720(5) 0.0279(10) Uani 1 1 d . . . . .
O100 O 0.2477(5) 0.3995(4) 0.1562(10) 0.087(3) Uani 1 1 d . . . . .
O101 O 0.2782(5) 0.3971(4) 0.4987(11) 0.080 Uiso 0.95(2) 1 d . U . . .
O102 O 0.5024(7) 0.4412(5) 0.4807(14) 0.080 Uiso 0.73(2) 1 d . U . . .
O103 O -0.0053(10) 0.5613(7) 1.174(2) 0.043(5) Uiso 0.306(15) 1 d . . P . .
O104 O -0.1345(8) 0.5063(6) 0.9549(16) 0.080 Uiso 0.589(19) 1 d . U . . .
O105 O -0.0412(11) 0.5396(8) 1.138(2) 0.097(7) Uiso 0.513(12) 1 d . . P . .
O106 O 0.3573(18) 0.4440(14) 0.636(4) 0.080 Uiso 0.243(19) 1 d . U . . .
O107 O 0.3553(10) 0.5098(8) 0.822(2) 0.080 Uiso 0.462(19) 1 d . U . . .
O108 O 0.2710(14) 0.4660(12) -0.009(3) 0.080 Uiso 0.35(2) 1 d . U . . .
O109 O 0.2512(11) 0.4734(9) 0.644(3) 0.080 Uiso 0.39(2) 1 d . U . . .
O110 O 0.3626(15) 0.4879(12) 0.722(3) 0.080 Uiso 0.307(19) 1 d . U . . .
O111 O 0.4620(13) 0.4584(9) 0.525(3) 0.080 Uiso 0.38(2) 1 d . U . . .
O112 O -0.0882(14) 0.5823(10) 1.127(3) 0.034(8) Uiso 0.187(18) 1 d . . P . .
O113 O -0.1172(13) 0.5946(9) 1.076(3) 0.060 Uiso 0.306(15) 1 d . U P . .
O114 O 0.734(2) 0.1014(14) 0.341(4) 0.080 Uiso 0.22(2) 1 d . U . . .
O115 O 0.0731(14) 0.5404(11) 0.992(3) 0.024(6) Uiso 0.144(6) 1 d . . P . .
O116 O 0.2537(15) 0.4947(13) -0.001(3) 0.080 Uiso 0.33(2) 1 d . U . . .
Zn1 Zn 0.55189(3) 0.29388(2) 1.00454(6) 0.01717(13) Uani 1 1 d . . . . .
Zn2 Zn 0.49201(4) 0.39043(3) 0.86661(7) 0.02533(16) Uani 1 1 d . . . . .
Zn3 Zn 0.42485(4) 0.35115(2) 0.14517(7) 0.02311(15) Uani 1 1 d . . . . .
Zn4 Zn 0.09719(4) 0.35249(3) 0.50746(8) 0.02814(17) Uani 1 1 d . . . . .
Zn5 Zn -0.02608(5) 0.60669(3) 0.77999(8) 0.0367(2) Uani 1 1 d . . . . .
Zn6 Zn 0.02982(3) 0.70474(2) 0.64698(6) 0.01851(14) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2A 1.194(14) . ?
C1 O1 1.260(7) . ?
C1 O2B 1.374(19) . ?
C1 C2 1.485(8) . ?
C2 C3 1.385(9) . ?
C2 C8 1.402(11) . ?
C3 C4 1.394(9) . ?
C3 H3 0.9500 . ?
C4 C6 1.402(10) . ?
C4 C5 1.477(10) . ?
C5 O4 1.245(9) . ?
C5 O3 1.288(7) . ?
C6 C7 1.392(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(10) . ?
C7 C9B 1.49(2) . ?
C7 C9A 1.56(2) . ?
C8 H8 0.9500 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10 O5 1.257(10) . ?
C10 O6 1.266(10) . ?
C10 C11 1.510(10) . ?
C11 C12 1.385(9) . ?
C11 C17A 1.422(15) . ?
C11 C17B 1.438(17) . ?
C12 C13 1.403(9) . ?
C12 H12 0.9500 . ?
C13 C15A 1.402(15) . ?
C13 C15B 1.434(18) . ?
C13 C14 1.489(9) . ?
C14 O8 1.255(8) . ?
C14 O7 1.269(8) . ?
C15A C16A 1.404(19) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.381(18) . ?
C16A C18A 1.51(2) . ?
C17A H17A 0.9500 . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C15B C16B 1.35(2) . ?
C15B H15B 0.9500 . ?
C16B C17B 1.392(19) . ?
C16B C18B 1.52(2) . ?
C17B H17B 0.9500 . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C19 O9 1.248(8) . ?
C19 O10 1.288(8) . ?
C19 C20 1.484(9) . ?
C20 C26 1.398(9) . ?
C20 C21 1.402(9) . ?
C21 C22 1.369(9) . ?
C21 H21 0.9500 . ?
C22 C24 1.403(9) . ?
C22 C23 1.487(9) . ?
C23 O11 1.248(8) . ?
C23 O12 1.282(8) . ?
C24 C25 1.407(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(10) . ?
C25 C27 1.506(8) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 O14 1.265(9) . ?
C28 O13 1.272(7) . ?
C28 C29 1.490(9) . ?
C29 C35 1.393(12) . ?
C29 C30 1.406(10) . ?
C30 C31 1.379(11) . ?
C30 H30 0.9500 . ?
C31 C33 1.382(13) . ?
C31 C32 1.514(10) . ?
C32 O15 1.238(9) . ?
C32 O16A 1.243(12) . ?
C32 O16B 1.346(19) . ?
C33 C34 1.408(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(11) . ?
C34 C36B 1.516(17) . ?
C34 C36A 1.60(2) . ?
C35 H35 0.9500 . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
C37 O18A 1.259(17) . ?
C37 O17 1.290(11) . ?
C37 O18B 1.343(15) . ?
C37 C38 1.486(11) . ?
C38 C44A 1.378(15) . ?
C38 C39 1.397(10) . ?
C38 C44B 1.52(2) . ?
C39 C40 1.405(9) . ?
C39 H39 0.9500 . ?
C40 C42B 1.40(2) . ?
C40 C42A 1.410(14) . ?
C40 C41 1.506(9) . ?
C41 O20 1.260(8) . ?
C41 O19 1.266(9) . ?
C42A C43A 1.378(17) . ?
C42A H42A 0.9500 . ?
C43A C44A 1.409(17) . ?
C43A C45A 1.49(2) . ?
C44A H44A 0.9500 . ?
C45A H45A 0.9800 . ?
C45A H45B 0.9800 . ?
C45A H45C 0.9800 . ?
C42B C43B 1.35(3) . ?
C42B H42B 0.9500 . ?
C43B C44B 1.38(2) . ?
C43B C45B 1.54(3) . ?
C44B H44B 0.9500 . ?
C45B H45D 0.9800 . ?
C45B H45E 0.9800 . ?
C45B H45F 0.9800 . ?
O1 Zn1 2.016(4) . ?
O1H Zn3 1.985(4) . ?
O1H Zn2 2.089(5) 1_554 ?
O1H Zn1 2.115(5) 1_554 ?
O2A Zn2 1.973(10) . ?
O2B Zn2 1.952(10) . ?
O1W Zn2 2.189(6) . ?
O2H Zn4 1.974(5) . ?
O2H Zn5 2.077(5) 2_565 ?
O2H Zn6 2.126(5) 2_565 ?
O3 Zn1 2.122(4) 1_554 ?
O3 Zn6 2.168(4) 4_544 ?
O2WA O2WB 0.82(2) . ?
O2WA Zn2 2.002(11) . ?
O2WB Zn2 2.082(19) . ?
O4 Zn3 1.960(6) . ?
O3WA O3WB 0.77(3) . ?
O3WA O115 1.48(3) . ?
O3WA Zn5 2.286(11) . ?
O3WB O4WB 1.52(4) . ?
O3WB Zn5 2.07(3) . ?
O5 Zn3 1.953(5) . ?
O4WA O4WB 1.17(3) . ?
O4WA Zn5 1.871(13) . ?
O4WB Zn5 2.10(3) . ?
O5W Zn5 2.28(3) . ?
O7 Zn2 1.953(5) 2_664 ?
O8 Zn1 2.025(5) 2_664 ?
O9 Zn6 2.086(5) 4_544 ?
O10 Zn3 1.957(5) . ?
O11 Zn1 2.074(5) 3_454 ?
O12 Zn4 1.956(5) . ?
O13 Zn6 2.137(4) 2_565 ?
O13 Zn1 2.201(4) 3_454 ?
O14 Zn4 1.954(6) . ?
O15 Zn6 2.037(5) 2_564 ?
O16A O16B 0.699(16) . ?
O16A Zn5 1.968(8) 2_564 ?
O16B Zn5 1.945(16) 2_564 ?
O17 Zn4 1.960(5) . ?
O18A O18B 0.972(17) . ?
O19 Zn5 1.969(6) . ?
O20 Zn6 2.006(5) . ?
O102 O111 1.08(3) . ?
O103 O105 1.03(3) . ?
O105 O112 1.53(4) . ?
O106 O110 1.53(5) . ?
O107 O110 1.25(4) . ?
O108 O116 0.87(3) . ?
O112 O113 0.89(3) . ?
Zn1 O8 2.025(5) 2_666 ?
Zn1 O11 2.074(5) 3 ?
Zn1 O1H 2.115(5) 1_556 ?
Zn1 O3 2.122(4) 1_556 ?
Zn1 O13 2.201(4) 3 ?
Zn2 O7 1.953(5) 2_666 ?
Zn2 O1H 2.089(5) 1_556 ?
Zn5 O16B 1.945(16) 2_566 ?
Zn5 O16A 1.968(8) 2_566 ?
Zn5 O2H 2.077(5) 2_565 ?
Zn6 O15 2.037(5) 2_566 ?
Zn6 O9 2.086(5) 4 ?
Zn6 O2H 2.126(5) 2_565 ?
Zn6 O13 2.137(4) 2_565 ?
Zn6 O3 2.168(4) 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
O2A C1 O1 125.3(7) . . ?
O2A C1 O2B 15.6(6) . . ?
O1 C1 O2B 125.3(7) . . ?
O2A C1 C2 116.1(7) . . ?
O1 C1 C2 118.1(6) . . ?
O2B C1 C2 115.9(7) . . ?
C3 C2 C8 119.3(6) . . ?
C3 C2 C1 120.3(6) . . ?
C8 C2 C1 120.4(6) . . ?
C2 C3 C4 119.9(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C6 119.7(6) . . ?
C3 C4 C5 119.5(6) . . ?
C6 C4 C5 120.8(6) . . ?
O4 C5 O3 122.9(7) . . ?
O4 C5 C4 118.3(6) . . ?
O3 C5 C4 118.8(6) . . ?
C7 C6 C4 121.3(6) . . ?
C7 C6 H6 119.4 . . ?
C4 C6 H6 119.4 . . ?
C8 C7 C6 117.8(7) . . ?
C8 C7 C9B 122.9(9) . . ?
C6 C7 C9B 118.2(9) . . ?
C8 C7 C9A 121.8(10) . . ?
C6 C7 C9A 119.4(9) . . ?
C7 C8 C2 121.9(7) . . ?
C7 C8 H8 119.0 . . ?
C2 C8 H8 119.0 . . ?
C7 C9A H9A1 109.5 . . ?
C7 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C7 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C7 C9B H9B1 109.5 . . ?
C7 C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C7 C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
O5 C10 O6 124.7(7) . . ?
O5 C10 C11 116.5(7) . . ?
O6 C10 C11 118.6(7) . . ?
C12 C11 C17A 118.1(8) . . ?
C12 C11 C17B 118.6(8) . . ?
C12 C11 C10 120.1(6) . . ?
C17A C11 C10 121.1(8) . . ?
C17B C11 C10 119.7(8) . . ?
C11 C12 C13 119.8(6) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C15A C13 C12 121.0(7) . . ?
C12 C13 C15B 118.4(8) . . ?
C15A C13 C14 120.0(7) . . ?
C12 C13 C14 118.7(6) . . ?
C15B C13 C14 121.4(8) . . ?
O8 C14 O7 126.0(6) . . ?
O8 C14 C13 116.9(6) . . ?
O7 C14 C13 117.1(6) . . ?
C13 C15A C16A 119.1(11) . . ?
C13 C15A H15A 120.5 . . ?
C16A C15A H15A 120.5 . . ?
C17A C16A C15A 119.2(12) . . ?
C17A C16A C18A 120.8(13) . . ?
C15A C16A C18A 119.9(12) . . ?
C16A C17A C11 121.3(12) . . ?
C16A C17A H17A 119.4 . . ?
C11 C17A H17A 119.4 . . ?
C16A C18A H18A 109.5 . . ?
C16A C18A H18B 109.5 . . ?
H18A C18A H18B 109.5 . . ?
C16A C18A H18C 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C16B C15B C13 121.5(13) . . ?
C16B C15B H15B 119.3 . . ?
C13 C15B H15B 119.3 . . ?
C15B C16B C17B 119.3(14) . . ?
C15B C16B C18B 119.0(14) . . ?
C17B C16B C18B 121.7(13) . . ?
C16B C17B C11 120.6(12) . . ?
C16B C17B H17B 119.7 . . ?
C11 C17B H17B 119.7 . . ?
C16B C18B H18D 109.5 . . ?
C16B C18B H18E 109.5 . . ?
H18D C18B H18E 109.5 . . ?
C16B C18B H18F 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
O9 C19 O10 122.4(6) . . ?
O9 C19 C20 121.4(6) . . ?
O10 C19 C20 116.3(6) . . ?
C26 C20 C21 118.8(6) . . ?
C26 C20 C19 121.6(6) . . ?
C21 C20 C19 119.5(6) . . ?
C22 C21 C20 120.8(5) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C24 120.3(6) . . ?
C21 C22 C23 119.3(6) . . ?
C24 C22 C23 120.4(6) . . ?
O11 C23 O12 122.2(6) . . ?
O11 C23 C22 121.1(6) . . ?
O12 C23 C22 116.7(6) . . ?
C22 C24 C25 120.0(6) . . ?
C22 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 118.7(5) . . ?
C26 C25 C27 121.5(7) . . ?
C24 C25 C27 119.8(7) . . ?
C25 C26 C20 121.5(6) . . ?
C25 C26 H26 119.3 . . ?
C20 C26 H26 119.3 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O14 C28 O13 125.2(6) . . ?
O14 C28 C29 117.7(6) . . ?
O13 C28 C29 117.0(6) . . ?
C35 C29 C30 118.9(7) . . ?
C35 C29 C28 120.4(6) . . ?
C30 C29 C28 120.6(7) . . ?
C31 C30 C29 120.1(7) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C33 120.4(7) . . ?
C30 C31 C32 118.7(7) . . ?
C33 C31 C32 120.8(7) . . ?
O15 C32 O16A 125.7(7) . . ?
O15 C32 O16B 121.3(9) . . ?
O16A C32 O16B 31.0(7) . . ?
O15 C32 C31 116.5(7) . . ?
O16A C32 C31 117.4(7) . . ?
O16B C32 C31 116.0(9) . . ?
C31 C33 C34 120.3(7) . . ?
C31 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C35 C34 C33 118.8(8) . . ?
C35 C34 C36B 122.0(9) . . ?
C33 C34 C36B 118.7(9) . . ?
C35 C34 C36A 122.2(11) . . ?
C33 C34 C36A 117.1(12) . . ?
C34 C35 C29 121.3(7) . . ?
C34 C35 H35 119.3 . . ?
C29 C35 H35 119.3 . . ?
C34 C36A H36A 109.5 . . ?
C34 C36A H36B 109.5 . . ?
H36A C36A H36B 109.5 . . ?
C34 C36A H36C 109.5 . . ?
H36A C36A H36C 109.5 . . ?
H36B C36A H36C 109.5 . . ?
C34 C36B H36D 109.5 . . ?
C34 C36B H36E 109.5 . . ?
H36D C36B H36E 109.5 . . ?
C34 C36B H36F 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
O18A C37 O17 111.8(11) . . ?
O18A C37 O18B 43.7(8) . . ?
O17 C37 O18B 124.4(8) . . ?
O18A C37 C38 125.5(10) . . ?
O17 C37 C38 115.9(8) . . ?
O18B C37 C38 116.5(10) . . ?
C44A C38 C39 120.4(8) . . ?
C44A C38 C37 119.1(9) . . ?
C39 C38 C37 119.8(7) . . ?
C39 C38 C44B 117.2(9) . . ?
C37 C38 C44B 120.6(10) . . ?
C38 C39 C40 118.5(7) . . ?
C38 C39 H39 120.7 . . ?
C40 C39 H39 120.7 . . ?
C42B C40 C39 122.4(10) . . ?
C39 C40 C42A 118.8(7) . . ?
C42B C40 C41 117.0(10) . . ?
C39 C40 C41 119.1(6) . . ?
C42A C40 C41 121.8(7) . . ?
O20 C41 O19 126.8(6) . . ?
O20 C41 C40 115.9(6) . . ?
O19 C41 C40 117.3(6) . . ?
C43A C42A C40 122.4(10) . . ?
C43A C42A H42A 118.8 . . ?
C40 C42A H42A 118.8 . . ?
C42A C43A C44A 117.0(11) . . ?
C42A C43A C45A 121.1(12) . . ?
C44A C43A C45A 121.9(12) . . ?
C38 C44A C43A 121.1(12) . . ?
C38 C44A H44A 119.5 . . ?
C43A C44A H44A 119.5 . . ?
C43A C45A H45A 109.5 . . ?
C43A C45A H45B 109.5 . . ?
H45A C45A H45B 109.5 . . ?
C43A C45A H45C 109.5 . . ?
H45A C45A H45C 109.5 . . ?
H45B C45A H45C 109.5 . . ?
C43B C42B C40 119.1(16) . . ?
C43B C42B H42B 120.5 . . ?
C40 C42B H42B 120.5 . . ?
C42B C43B C44B 122.6(18) . . ?
C42B C43B C45B 122.2(17) . . ?
C44B C43B C45B 115.3(17) . . ?
C43B C44B C38 118.2(15) . . ?
C43B C44B H44B 120.9 . . ?
C38 C44B H44B 120.9 . . ?
C43B C45B H45D 109.5 . . ?
C43B C45B H45E 109.5 . . ?
H45D C45B H45E 109.5 . . ?
C43B C45B H45F 109.5 . . ?
H45D C45B H45F 109.5 . . ?
H45E C45B H45F 109.5 . . ?
C1 O1 Zn1 135.1(4) . . ?
Zn3 O1H Zn2 118.4(2) . 1_554 ?
Zn3 O1H Zn1 113.7(2) . 1_554 ?
Zn2 O1H Zn1 103.26(19) 1_554 1_554 ?
C1 O2A Zn2 128.2(7) . . ?
C1 O2B Zn2 118.1(11) . . ?
Zn4 O2H Zn5 119.0(2) . 2_565 ?
Zn4 O2H Zn6 113.3(2) . 2_565 ?
Zn5 O2H Zn6 102.4(2) 2_565 2_565 ?
C5 O3 Zn1 123.3(4) . 1_554 ?
C5 O3 Zn6 128.3(4) . 4_544 ?
Zn1 O3 Zn6 103.22(17) 1_554 4_544 ?
O2WB O2WA Zn2 84.1(17) . . ?
O2WA O2WB Zn2 73.0(16) . . ?
C5 O4 Zn3 123.1(5) . . ?
O3WB O3WA O115 152(3) . . ?
O3WB O3WA Zn5 64(2) . . ?
O115 O3WA Zn5 143.2(14) . . ?
O3WA O3WB O4WB 165(4) . . ?
O3WA O3WB Zn5 96(3) . . ?
O4WB O3WB Zn5 69.7(16) . . ?
C10 O5 Zn3 113.5(5) . . ?
O4WB O4WA Zn5 84.3(16) . . ?
O4WA O4WB O3WB 119(3) . . ?
O4WA O4WB Zn5 62.3(14) . . ?
O3WB O4WB Zn5 67.5(16) . . ?
C14 O7 Zn2 130.3(4) . 2_664 ?
C14 O8 Zn1 131.2(5) . 2_664 ?
C19 O9 Zn6 138.1(5) . 4_544 ?
C19 O10 Zn3 112.2(4) . . ?
C23 O11 Zn1 136.8(5) . 3_454 ?
C23 O12 Zn4 114.1(4) . . ?
C28 O13 Zn6 122.4(4) . 2_565 ?
C28 O13 Zn1 129.8(4) . 3_454 ?
Zn6 O13 Zn1 101.62(17) 2_565 3_454 ?
C28 O14 Zn4 120.7(4) . . ?
C32 O15 Zn6 136.0(6) . 2_564 ?
O16B O16A C32 82.7(17) . . ?
O16B O16A Zn5 77.9(16) . 2_564 ?
C32 O16A Zn5 124.2(7) . 2_564 ?
O16A O16B C32 66.3(16) . . ?
O16A O16B Zn5 81.5(16) . 2_564 ?
C32 O16B Zn5 119.4(11) . 2_564 ?
C37 O17 Zn4 114.1(5) . . ?
O18B O18A C37 72.7(13) . . ?
O18A O18B C37 63.5(12) . . ?
C41 O19 Zn5 128.4(5) . . ?
C41 O20 Zn6 133.3(5) . . ?
O103 O105 O112 92(2) . . ?
O107 O110 O106 154(3) . . ?
O113 O112 O105 141(4) . . ?
O1 Zn1 O8 105.8(2) . 2_666 ?
O1 Zn1 O11 89.81(19) . 3 ?
O8 Zn1 O11 92.3(2) 2_666 3 ?
O1 Zn1 O1H 96.15(19) . 1_556 ?
O8 Zn1 O1H 89.91(19) 2_666 1_556 ?
O11 Zn1 O1H 172.80(18) 3 1_556 ?
O1 Zn1 O3 163.20(19) . 1_556 ?
O8 Zn1 O3 89.21(19) 2_666 1_556 ?
O11 Zn1 O3 81.86(19) 3 1_556 ?
O1H Zn1 O3 91.35(18) 1_556 1_556 ?
O1 Zn1 O13 87.76(18) . 3 ?
O8 Zn1 O13 166.48(18) 2_666 3 ?
O11 Zn1 O13 87.5(2) 3 3 ?
O1H Zn1 O13 88.72(18) 1_556 3 ?
O3 Zn1 O13 77.38(16) 1_556 3 ?
O2B Zn2 O7 132.6(8) . 2_666 ?
O2B Zn2 O2A 11.4(4) . . ?
O7 Zn2 O2A 121.8(7) 2_666 . ?
O2B Zn2 O2WA 120.6(8) . . ?
O7 Zn2 O2WA 106.0(5) 2_666 . ?
O2A Zn2 O2WA 130.0(7) . . ?
O2B Zn2 O2WB 98.4(10) . . ?
O7 Zn2 O2WB 128.7(7) 2_666 . ?
O2A Zn2 O2WB 108.6(9) . . ?
O2WA Zn2 O2WB 22.9(5) . . ?
O2B Zn2 O1H 92.9(5) . 1_556 ?
O7 Zn2 O1H 92.4(2) 2_666 1_556 ?
O2A Zn2 O1H 97.9(4) . 1_556 ?
O2WA Zn2 O1H 93.7(4) . 1_556 ?
O2WB Zn2 O1H 89.6(5) . 1_556 ?
O2B Zn2 O1W 87.8(5) . . ?
O7 Zn2 O1W 86.3(2) 2_666 . ?
O2A Zn2 O1W 82.6(4) . . ?
O2WA Zn2 O1W 87.0(4) . . ?
O2WB Zn2 O1W 91.4(5) . . ?
O1H Zn2 O1W 178.7(2) 1_556 . ?
O5 Zn3 O10 106.9(2) . . ?
O5 Zn3 O4 110.2(2) . . ?
O10 Zn3 O4 110.0(2) . . ?
O5 Zn3 O1H 108.2(2) . . ?
O10 Zn3 O1H 113.1(2) . . ?
O4 Zn3 O1H 108.5(2) . . ?
O14 Zn4 O12 110.5(2) . . ?
O14 Zn4 O17 108.3(3) . . ?
O12 Zn4 O17 109.6(2) . . ?
O14 Zn4 O2H 108.8(2) . . ?
O12 Zn4 O2H 114.2(2) . . ?
O17 Zn4 O2H 105.1(2) . . ?
O4WA Zn5 O16B 132.3(7) . 2_566 ?
O4WA Zn5 O16A 121.8(5) . 2_566 ?
O16B Zn5 O16A 20.6(5) 2_566 2_566 ?
O4WA Zn5 O19 109.2(5) . . ?
O16B Zn5 O19 108.5(6) 2_566 . ?
O16A Zn5 O19 126.4(3) 2_566 . ?
O4WA Zn5 O3WB 72.2(10) . . ?
O16B Zn5 O3WB 82.8(11) 2_566 . ?
O16A Zn5 O3WB 94.6(10) 2_566 . ?
O19 Zn5 O3WB 85.5(9) . . ?
O4WA Zn5 O2H 95.8(4) . 2_565 ?
O16B Zn5 O2H 109.0(5) 2_566 2_565 ?
O16A Zn5 O2H 95.5(3) 2_566 2_565 ?
O19 Zn5 O2H 94.7(2) . 2_565 ?
O3WB Zn5 O2H 167.3(10) . 2_565 ?
O4WA Zn5 O4WB 33.5(9) . . ?
O16B Zn5 O4WB 122.3(10) 2_566 . ?
O16A Zn5 O4WB 126.0(9) 2_566 . ?
O19 Zn5 O4WB 88.3(8) . . ?
O3WB Zn5 O4WB 42.8(12) . . ?
O2H Zn5 O4WB 124.5(8) 2_565 . ?
O4WA Zn5 O5W 59.7(8) . . ?
O16B Zn5 O5W 82.5(9) 2_566 . ?
O16A Zn5 O5W 65.0(7) 2_566 . ?
O19 Zn5 O5W 168.6(7) . . ?
O3WB Zn5 O5W 93.0(11) . . ?
O2H Zn5 O5W 84.2(7) 2_565 . ?
O4WB Zn5 O5W 83.0(11) . . ?
O4WA Zn5 O3WA 91.1(5) . . ?
O16B Zn5 O3WA 65.1(6) 2_566 . ?
O16A Zn5 O3WA 79.9(4) 2_566 . ?
O19 Zn5 O3WA 84.0(3) . . ?
O3WB Zn5 O3WA 19.7(9) . . ?
O2H Zn5 O3WA 173.0(3) 2_565 . ?
O4WB Zn5 O3WA 62.4(9) . . ?
O5W Zn5 O3WA 98.4(8) . . ?
O20 Zn6 O15 104.7(2) . 2_566 ?
O20 Zn6 O9 91.5(2) . 4 ?
O15 Zn6 O9 90.1(2) 2_566 4 ?
O20 Zn6 O2H 91.04(19) . 2_565 ?
O15 Zn6 O2H 95.5(2) 2_566 2_565 ?
O9 Zn6 O2H 173.06(18) 4 2_565 ?
O20 Zn6 O13 88.7(2) . 2_565 ?
O15 Zn6 O13 164.4(2) 2_566 2_565 ?
O9 Zn6 O13 81.64(19) 4 2_565 ?
O2H Zn6 O13 91.96(19) 2_565 2_565 ?
O20 Zn6 O3 166.53(19) . 4 ?
O15 Zn6 O3 88.56(18) 2_566 4 ?
O9 Zn6 O3 86.21(19) 4 4 ?
O2H Zn6 O3 89.82(18) 2_565 4 ?
O13 Zn6 O3 77.79(16) 2_565 4 ?

_refine_diff_density_max         1.506
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.125

####################################################################### 
# 
# 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_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1417518'
_audit_update_record             
;
2015-09-23 deposited with the CCDC.
2015-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H44 O28 Zn6'
_chemical_formula_weight         1425.02

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'
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      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

_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'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   17.382(4)
_cell_length_b                   10.4516(15)
_cell_length_c                   15.970(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2901.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5672
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       platelet
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_F_000             1436
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    2.524
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Rigaku Mercury2 (2x2 bin mode) SCXMini: Fixed Chi 2 circle
;
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            30286
_diffrn_reflns_av_unetI/netI     0.0976
_diffrn_reflns_av_R_equivalents  0.1248
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.274
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6666
_reflns_number_gt                4455
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    1.000

_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.
;
_vrf_PLAT601_Compound3           
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        230 Ang3  
RESPONSE: This is correct, there are large spaces between parallel 2D frameworks. Two full occupancy water molecules have been located in these voids, however the largest peak of electron density remaining in the voids is only 1 e/A3 so no attempts have been made to model disordered solvent in these regions.
;
_vrf_PLAT306_Compound3           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O2W Check 
RESPONSE: These hydrogen atoms belonging to these two guest water molecules could not be located, so have not been included in the final model.
;
_vrf_PLAT341_Compound3           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0165 Ang.  
RESPONSE: Crystal diffracted fairly weakly at higher angles, most likely due to the solvent-filled voids, it is possible that this has lead to low bond [recision. The atoms belonging to the framework refined satisfactorily.
;
_vrf_PLAT430_Compound3           
;
PROBLEM: Short Inter D...A Contact  O1W    ..  O2W     ..       2.84 Ang.  
RESPONSE: This is most likely a hydrogen bond, however the hydrogen atoms belonging to the water molecules could not be located so they have not been included in the final model.
;
_vrf_PLAT934_Compound3           
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          2 Check 
RESPONSE: These are the (1 0 2) and (4 0 0) reflections. They occur at low theta values and appear not to be systematic error.
;
_vrf_PLAT987_Compound3           
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: The Flack parameter is 0.033, this indicates that the crystal has been solved in the correct orientation.
;

_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0627P)²+5.2699P] 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 
;
 Flack x determined using 1515 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6666
_refine_ls_number_parameters     358
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1517
_refine_ls_wR_factor_gt          0.1285
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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
C1 C 0.1434(7) 1.0398(11) -0.0632(7) 0.029(3) Uani 1 1 d . . . . .
C2 C 0.0677(7) 1.0203(10) -0.1084(7) 0.026(2) Uani 1 1 d . . . . .
C3 C 0.0000 1.0000 -0.0637(10) 0.029(4) Uani 1 2 d S T P . .
H3 H 0.0000 1.0000 -0.0042 0.035 Uiso 1 2 calc R U P . .
C4 C 0.0665(7) 1.0218(11) -0.1953(7) 0.028(3) Uani 1 1 d . . . . .
H4 H 0.1129 1.0383 -0.2249 0.033 Uiso 1 1 calc R U . . .
C5 C 0.0000 1.0000 -0.2400(10) 0.028(3) Uani 1 2 d S T P . .
C6 C 0.0000 1.0000 -0.3351(10) 0.041(5) Uani 1 2 d S T P . .
H6A H -0.0522 0.9829 -0.3555 0.062 Uiso 0.5 1 calc R U P . .
H6B H 0.0172 1.0837 -0.3555 0.062 Uiso 0.5 1 calc R U P . .
H6C H 0.0350 0.9334 -0.3555 0.062 Uiso 0.5 1 calc R U P . .
C7 C 0.4206(7) 1.1575(11) 0.1289(7) 0.025(2) Uani 1 1 d . . . . .
C8 C 0.5020(7) 1.1504(10) 0.1265(7) 0.026(2) Uani 1 1 d . . . . .
H8 H 0.5277 1.1402 0.0745 0.031 Uiso 1 1 calc R U . . .
C9 C 0.5441(6) 1.1585(10) 0.2002(7) 0.024(2) Uani 1 1 d . . . . .
C10 C 0.5077(7) 1.1732(12) 0.2768(7) 0.031(3) Uani 1 1 d . . . . .
H10 H 0.5375 1.1799 0.3265 0.038 Uiso 1 1 calc R U . . .
C11 C 0.4266(7) 1.1783(12) 0.2813(7) 0.032(3) Uani 1 1 d . . . . .
C12 C 0.3849(7) 1.1711(11) 0.2068(7) 0.027(3) Uani 1 1 d . . . . .
H12 H 0.3304 1.1757 0.2091 0.033 Uiso 1 1 calc R U . . .
C13 C 0.3762(6) 1.1376(11) 0.0514(7) 0.024(2) Uani 1 1 d . . . . .
C14 C 0.3685(7) 0.8486(10) 0.1947(7) 0.026(3) Uani 1 1 d . . . . .
C15 C 0.3865(9) 1.1866(19) 0.3644(9) 0.059(5) Uani 1 1 d . . . . .
H15A H 0.4248 1.1909 0.4093 0.089 Uiso 1 1 calc R U . . .
H15B H 0.3543 1.2636 0.3658 0.089 Uiso 1 1 calc R U . . .
H15C H 0.3541 1.1108 0.3723 0.089 Uiso 1 1 calc R U . . .
C16 C 0.1793(7) 1.1719(10) 0.3162(7) 0.024(2) Uani 1 1 d . . . . .
C17 C 0.1763(7) 1.2869(11) 0.2725(7) 0.027(3) Uani 1 1 d . . . . .
H17 H 0.1744 1.2861 0.2130 0.032 Uiso 1 1 calc R U . . .
C18 C 0.1759(7) 1.4024(11) 0.3148(7) 0.030(3) Uani 1 1 d . . . . .
C19 C 0.1792(8) 1.4016(12) 0.4029(8) 0.037(3) Uani 1 1 d . . . . .
H19 H 0.1803 1.4806 0.4323 0.045 Uiso 1 1 calc R U . . .
C20 C 0.1807(9) 1.2889(12) 0.4473(7) 0.038(3) Uani 1 1 d . . . . .
C21 C 0.1796(7) 1.1734(11) 0.4024(7) 0.030(3) Uani 1 1 d . . . . .
H21 H 0.1789 1.0947 0.4321 0.036 Uiso 1 1 calc R U . . .
C22 C 0.1870(6) 1.0499(11) 0.2673(7) 0.025(2) Uani 1 1 d . . . . .
C23 C 0.1758(7) 0.5256(11) 0.2651(7) 0.031(3) Uani 1 1 d . . . . .
C24 C 0.1824(12) 1.2891(15) 0.5418(8) 0.060(5) Uani 1 1 d . . . . .
H24A H 0.1834 1.2007 0.5623 0.089 Uiso 1 1 calc R U . . .
H24B H 0.2285 1.3342 0.5613 0.089 Uiso 1 1 calc R U . . .
H24C H 0.1364 1.3325 0.5632 0.089 Uiso 1 1 calc R U . . .
O1 O 0.1472(4) 1.0069(8) 0.0127(5) 0.0298(19) Uani 1 1 d . . . . .
O1H O 0.1818(4) 0.7936(7) 0.1308(4) 0.0229(16) Uani 1 1 d . . . . .
H1H H 0.1255 0.8129 0.1322 0.028 Uiso 1 1 calc R U . . .
O2 O 0.1977(5) 1.0885(8) -0.1068(5) 0.035(2) Uani 1 1 d . . . . .
O1W O 0.2878(5) 0.8734(8) -0.0313(5) 0.0319(19) Uani 1 1 d . . . . .
O3 O 0.4103(4) 1.1125(8) -0.0177(5) 0.0286(18) Uani 1 1 d . . . . .
O2W O 0.5597(5) 1.1676(9) -0.0890(7) 0.055(3) Uani 1 1 d . . . . .
O4 O 0.3028(4) 1.1391(7) 0.0521(5) 0.0289(18) Uani 1 1 d . . . . .
O3W O 0.0261(6) 0.8677(11) 0.1621(8) 0.068(3) Uani 1 1 d . . . . .
O5 O 0.3310(4) 0.8059(8) 0.2566(5) 0.0280(17) Uani 1 1 d . . . . .
O6 O 0.3402(4) 0.8958(8) 0.1293(5) 0.0288(18) Uani 1 1 d . . . . .
O7 O 0.1836(5) 0.9447(7) 0.3080(5) 0.0335(19) Uani 1 1 d . . . . .
O8 O 0.1983(5) 1.0584(7) 0.1904(5) 0.0302(18) Uani 1 1 d . . . . .
O9 O 0.1981(5) 0.6257(7) 0.3023(5) 0.036(2) Uani 1 1 d . . . . .
O10 O 0.1532(5) 0.5199(8) 0.1894(5) 0.037(2) Uani 1 1 d . . . . .
Zn1 Zn 0.21793(8) 0.79048(12) 0.24904(8) 0.0258(3) Uani 1 1 d . . . . .
Zn2 Zn 0.23690(7) 0.95759(12) 0.08659(8) 0.0240(3) Uani 1 1 d . . . . .
Zn3 Zn 0.19303(7) 0.61284(12) 0.08731(8) 0.0246(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.262(13) . ?
C1 O2 1.278(13) . ?
C1 C2 1.515(16) . ?
C2 C4 1.389(15) . ?
C2 C3 1.392(14) . ?
C3 C2 1.392(14) 2_575 ?
C4 C5 1.377(14) . ?
C5 C4 1.377(14) 2_575 ?
C5 C6 1.52(2) . ?
C7 C12 1.397(16) . ?
C7 C8 1.416(17) . ?
C7 C13 1.473(15) . ?
C8 C9 1.388(16) . ?
C9 C10 1.385(16) . ?
C9 C14 1.524(16) 2_675 ?
C10 C11 1.413(17) . ?
C11 C12 1.395(16) . ?
C11 C15 1.502(18) . ?
C13 O4 1.277(13) . ?
C13 O3 1.279(13) . ?
C13 Zn3 2.535(11) 4 ?
C14 O6 1.257(14) . ?
C14 O5 1.265(13) . ?
C14 C9 1.524(16) 2_675 ?
C16 C21 1.376(15) . ?
C16 C17 1.391(15) . ?
C16 C22 1.501(15) . ?
C17 C18 1.384(16) . ?
C18 C19 1.408(16) . ?
C18 C23 1.513(16) 1_565 ?
C19 C20 1.375(17) . ?
C20 C21 1.404(17) . ?
C20 C24 1.510(17) . ?
C22 O8 1.246(13) . ?
C22 O7 1.278(13) . ?
C23 O9 1.265(13) . ?
C23 O10 1.272(14) . ?
C23 C18 1.513(16) 1_545 ?
O1 Zn2 2.021(8) . ?
O1H Zn1 1.990(7) . ?
O1H Zn3 2.023(7) . ?
O1H Zn2 2.087(7) . ?
O2 Zn3 1.941(8) 4 ?
O1W Zn2 2.259(8) . ?
O3 Zn3 2.113(7) 4 ?
O4 Zn3 2.244(8) 4 ?
O4 Zn2 2.283(7) . ?
O5 Zn1 1.976(7) . ?
O6 Zn2 2.025(8) . ?
O7 Zn1 1.960(8) . ?
O8 Zn2 2.076(8) . ?
O9 Zn1 1.952(8) . ?
O10 Zn3 2.021(8) . ?
Zn1 Zn2 3.1449(17) . ?
Zn3 O2 1.941(8) 4_545 ?
Zn3 O3 2.113(7) 4_545 ?
Zn3 O4 2.244(8) 4_545 ?
Zn3 C13 2.535(11) 4_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 126.3(11) . . ?
O1 C1 C2 117.8(10) . . ?
O2 C1 C2 115.9(10) . . ?
C4 C2 C3 120.1(11) . . ?
C4 C2 C1 119.1(10) . . ?
C3 C2 C1 120.7(10) . . ?
C2 C3 C2 118.3(15) . 2_575 ?
C5 C4 C2 121.8(11) . . ?
C4 C5 C4 117.7(15) . 2_575 ?
C4 C5 C6 121.2(8) . . ?
C4 C5 C6 121.2(8) 2_575 . ?
C12 C7 C8 118.2(10) . . ?
C12 C7 C13 122.0(10) . . ?
C8 C7 C13 119.5(10) . . ?
C9 C8 C7 120.0(10) . . ?
C10 C9 C8 121.0(10) . . ?
C10 C9 C14 120.7(10) . 2_675 ?
C8 C9 C14 118.3(10) . 2_675 ?
C9 C10 C11 120.3(11) . . ?
C12 C11 C10 118.2(11) . . ?
C12 C11 C15 121.0(11) . . ?
C10 C11 C15 120.7(11) . . ?
C11 C12 C7 122.3(11) . . ?
O4 C13 O3 118.2(10) . . ?
O4 C13 C7 121.0(10) . . ?
O3 C13 C7 120.7(10) . . ?
O4 C13 Zn3 62.2(5) . 4 ?
O3 C13 Zn3 56.3(5) . 4 ?
C7 C13 Zn3 175.9(8) . 4 ?
O6 C14 O5 125.9(11) . . ?
O6 C14 C9 117.2(10) . 2_675 ?
O5 C14 C9 116.9(10) . 2_675 ?
C21 C16 C17 119.5(10) . . ?
C21 C16 C22 122.0(10) . . ?
C17 C16 C22 118.4(10) . . ?
C18 C17 C16 120.6(10) . . ?
C17 C18 C19 118.9(11) . . ?
C17 C18 C23 119.1(10) . 1_565 ?
C19 C18 C23 122.0(10) . 1_565 ?
C20 C19 C18 121.4(11) . . ?
C19 C20 C21 118.2(10) . . ?
C19 C20 C24 121.0(12) . . ?
C21 C20 C24 120.8(12) . . ?
C16 C21 C20 121.4(10) . . ?
O8 C22 O7 124.7(10) . . ?
O8 C22 C16 117.8(10) . . ?
O7 C22 C16 117.5(9) . . ?
O9 C23 O10 125.5(10) . . ?
O9 C23 C18 117.2(10) . 1_545 ?
O10 C23 C18 117.3(10) . 1_545 ?
C1 O1 Zn2 132.1(8) . . ?
Zn1 O1H Zn3 106.3(3) . . ?
Zn1 O1H Zn2 100.9(3) . . ?
Zn3 O1H Zn2 127.3(4) . . ?
C1 O2 Zn3 133.4(7) . 4 ?
C13 O3 Zn3 93.5(6) . 4 ?
C13 O4 Zn3 87.6(6) . 4 ?
C13 O4 Zn2 119.6(7) . . ?
Zn3 O4 Zn2 98.9(3) 4 . ?
C14 O5 Zn1 119.6(7) . . ?
C14 O6 Zn2 138.8(8) . . ?
C22 O7 Zn1 116.7(7) . . ?
C22 O8 Zn2 143.3(8) . . ?
C23 O9 Zn1 125.4(7) . . ?
C23 O10 Zn3 129.6(8) . . ?
O9 Zn1 O7 117.6(3) . . ?
O9 Zn1 O5 102.7(4) . . ?
O7 Zn1 O5 101.9(4) . . ?
O9 Zn1 O1H 111.9(3) . . ?
O7 Zn1 O1H 110.3(3) . . ?
O5 Zn1 O1H 111.7(3) . . ?
O9 Zn1 Zn2 150.3(2) . . ?
O7 Zn1 Zn2 88.4(2) . . ?
O5 Zn1 Zn2 84.3(2) . . ?
O1H Zn1 Zn2 40.7(2) . . ?
O1 Zn2 O6 163.9(3) . . ?
O1 Zn2 O8 95.0(3) . . ?
O6 Zn2 O8 100.3(3) . . ?
O1 Zn2 O1H 93.0(3) . . ?
O6 Zn2 O1H 91.8(3) . . ?
O8 Zn2 O1H 89.9(3) . . ?
O1 Zn2 O1W 85.1(3) . . ?
O6 Zn2 O1W 79.0(3) . . ?
O8 Zn2 O1W 171.9(3) . . ?
O1H Zn2 O1W 98.2(3) . . ?
O1 Zn2 O4 92.0(3) . . ?
O6 Zn2 O4 84.3(3) . . ?
O8 Zn2 O4 86.2(3) . . ?
O1H Zn2 O4 173.9(3) . . ?
O1W Zn2 O4 85.8(3) . . ?
O1 Zn2 Zn1 122.8(2) . . ?
O6 Zn2 Zn1 68.8(2) . . ?
O8 Zn2 Zn1 65.7(2) . . ?
O1H Zn2 Zn1 38.4(2) . . ?
O1W Zn2 Zn1 120.8(2) . . ?
O4 Zn2 Zn1 135.49(19) . . ?
O2 Zn3 O10 98.2(4) 4_545 . ?
O2 Zn3 O1H 99.3(3) 4_545 . ?
O10 Zn3 O1H 98.0(3) . . ?
O2 Zn3 O3 156.3(3) 4_545 4_545 ?
O10 Zn3 O3 97.6(3) . 4_545 ?
O1H Zn3 O3 95.8(3) . 4_545 ?
O2 Zn3 O4 98.2(3) 4_545 4_545 ?
O10 Zn3 O4 150.5(3) . 4_545 ?
O1H Zn3 O4 103.3(3) . 4_545 ?
O3 Zn3 O4 60.4(3) 4_545 4_545 ?
O2 Zn3 C13 128.2(3) 4_545 4_545 ?
O10 Zn3 C13 126.3(4) . 4_545 ?
O1H Zn3 C13 99.2(3) . 4_545 ?
O3 Zn3 C13 30.2(3) 4_545 4_545 ?
O4 Zn3 C13 30.2(3) 4_545 4_545 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1H H1H O3W 1.00 1.88 2.858(13) 165.1 .

_refine_diff_density_max         1.016
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.149

####################################################################### 
# 
# 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_Compound4
_database_code_depnum_ccdc_archive 'CCDC 1417519'
_audit_update_record             
;
2015-09-23 deposited with the CCDC.
2015-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H14 Mn O10'
_chemical_formula_weight         445.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   4.5131(8)
_cell_length_b                   14.483(3)
_cell_length_c                   12.622(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.792(9)
_cell_angle_gamma                90
_cell_volume                     817.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1650
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      27.8

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_F_000             454
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    0.871
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  
;
Rigaku Mercury2 (2x2 bin mode) SCXMini: Fixed Chi 2 circle
;
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            8512
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.152
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1877
_reflns_number_gt                1398
_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       
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;

_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0378P)²+0.5014P] 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         1877
_refine_ls_number_parameters     135
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0829
_refine_ls_wR_factor_gt          0.0737
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
C1 C 0.1497(5) 0.63984(15) -0.17169(17) 0.0140(4) Uani 1 1 d . . . . .
C2 C 0.3271(5) 0.66214(15) -0.25818(17) 0.0136(5) Uani 1 1 d . . . . .
C3 C 0.3383(5) 0.75014(15) -0.30079(17) 0.0140(5) Uani 1 1 d . . . . .
H3 H 0.2312 0.7995 -0.2742 0.017 Uiso 1 1 calc R U . . .
C4 C 0.5094(5) 0.76491(15) -0.38325(17) 0.0126(4) Uani 1 1 d . . . . .
C5 C 0.4737(5) 0.35961(15) -0.06932(17) 0.0123(4) Uani 1 1 d . . . . .
C6 C 0.6612(5) 0.69158(15) -0.42164(18) 0.0150(5) Uani 1 1 d . . . . .
H6 H 0.7779 0.7017 -0.4778 0.018 Uiso 1 1 calc R U . . .
C7 C 0.6452(5) 0.60316(16) -0.37915(18) 0.0151(5) Uani 1 1 d . . . . .
C8 C 0.4798(5) 0.58832(15) -0.29651(18) 0.0148(5) Uani 1 1 d . . . . .
H8 H 0.4702 0.5286 -0.2661 0.018 Uiso 1 1 calc R U . . .
C9 C 0.8036(6) 0.44665(16) -0.3781(2) 0.0237(6) Uani 1 1 d . . . . .
H9A H 0.8879 0.4494 -0.3024 0.036 Uiso 1 1 calc R U . . .
H9B H 0.9251 0.4054 -0.4161 0.036 Uiso 1 1 calc R U . . .
H9C H 0.5983 0.4232 -0.3845 0.036 Uiso 1 1 calc R U . . .
Mn1 Mn 0.0000 0.5000 0.0000 0.01210(13) Uani 1 2 d S . P . .
O1 O 0.1143(3) 0.56000(11) -0.14448(12) 0.0158(3) Uani 1 1 d . . . . .
O2 O 0.0335(4) 0.71096(11) -0.12632(13) 0.0202(4) Uani 1 1 d . . . . .
H2 H -0.0748 0.6918 -0.0818 0.030 Uiso 1 1 calc R U . . .
O3 O 0.2773(4) 0.37422(10) -0.00797(13) 0.0156(3) Uani 1 1 d . . . . .
O4 O 0.6538(3) 0.41943(10) -0.09253(12) 0.0156(3) Uani 1 1 d . . . . .
O5 O 0.8026(4) 0.53714(11) -0.42358(14) 0.0219(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.223(3) . ?
C1 O2 1.321(3) . ?
C1 C2 1.474(3) . ?
C2 C3 1.387(3) . ?
C2 C8 1.394(3) . ?
C3 C4 1.394(3) . ?
C4 C6 1.386(3) . ?
C4 C5 1.503(3) 2_654 ?
C5 O4 1.250(3) . ?
C5 O3 1.271(3) . ?
C5 C4 1.503(3) 2_644 ?
C6 C7 1.394(3) . ?
C7 O5 1.357(3) . ?
C7 C8 1.379(3) . ?
C9 O5 1.431(3) . ?
Mn1 O1 2.1451(15) 3_565 ?
Mn1 O1 2.1452(15) . ?
Mn1 O4 2.1616(15) 3_665 ?
Mn1 O4 2.1616(15) 1_455 ?
Mn1 O3 2.2201(15) 3_565 ?
Mn1 O3 2.2201(15) . ?
O4 Mn1 2.1615(15) 1_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 122.7(2) . . ?
O1 C1 C2 121.3(2) . . ?
O2 C1 C2 115.94(19) . . ?
C3 C2 C8 121.6(2) . . ?
C3 C2 C1 122.7(2) . . ?
C8 C2 C1 115.6(2) . . ?
C2 C3 C4 118.9(2) . . ?
C6 C4 C3 119.6(2) . . ?
C6 C4 C5 120.38(19) . 2_654 ?
C3 C4 C5 120.05(19) . 2_654 ?
O4 C5 O3 123.8(2) . . ?
O4 C5 C4 118.01(19) . 2_644 ?
O3 C5 C4 118.15(18) . 2_644 ?
C4 C6 C7 121.0(2) . . ?
O5 C7 C8 124.7(2) . . ?
O5 C7 C6 115.54(19) . . ?
C8 C7 C6 119.7(2) . . ?
C7 C8 C2 119.1(2) . . ?
O1 Mn1 O1 180.00(8) 3_565 . ?
O1 Mn1 O4 89.94(6) 3_565 3_665 ?
O1 Mn1 O4 90.06(6) . 3_665 ?
O1 Mn1 O4 90.06(6) 3_565 1_455 ?
O1 Mn1 O4 89.94(6) . 1_455 ?
O4 Mn1 O4 180.0 3_665 1_455 ?
O1 Mn1 O3 95.27(6) 3_565 3_565 ?
O1 Mn1 O3 84.73(6) . 3_565 ?
O4 Mn1 O3 84.44(6) 3_665 3_565 ?
O4 Mn1 O3 95.56(6) 1_455 3_565 ?
O1 Mn1 O3 84.73(6) 3_565 . ?
O1 Mn1 O3 95.27(6) . . ?
O4 Mn1 O3 95.56(6) 3_665 . ?
O4 Mn1 O3 84.44(6) 1_455 . ?
O3 Mn1 O3 180.0 3_565 . ?
C1 O1 Mn1 132.64(15) . . ?
C5 O3 Mn1 127.44(14) . . ?
C5 O4 Mn1 133.88(14) . 1_655 ?
C7 O5 C9 116.92(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O3 0.84 1.82 2.647(2) 167.5 3_565

_refine_diff_density_max         0.441
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_Compound5
_database_code_depnum_ccdc_archive 'CCDC 1417520'
_audit_update_record             
;
2015-09-23 deposited with the CCDC.
2015-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H62 Mn3 O18'
_chemical_formula_weight         1139.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0132 0.0074 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Mn Mn 0.3529 0.8587 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_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                   9.1496(12)
_cell_length_b                   9.7908(12)
_cell_length_c                   16.078(2)
_cell_angle_alpha                89.207(2)
_cell_angle_beta                 76.087(2)
_cell_angle_gamma                74.643(2)
_cell_volume                     1346.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7803
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      33.60

_exptl_crystal_description       'trapezoidal plate'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_F_000             593
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.960
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6788
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_process_details   'SADABS, G. M. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20014
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.596
_diffrn_reflns_theta_max         33.615
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8056
_reflns_number_gt                6684
_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.
;
_vrf_PLAT201_Compound5           
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: One of the tert-butyl groups is rotationally disordered over two sites. The partial occupancy carbon atoms of this disordered tert-butyl group have been refined with isotropic thermal displacement parameters.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (beta)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0598P)²+0.2452P] 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         8056
_refine_ls_number_parameters     343
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1260
_refine_ls_wR_factor_gt          0.1204
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
C1 C 0.26240(19) 1.32466(16) 0.45579(11) 0.0129(3) Uani 1 1 d . . . . .
C1E C -0.2152(3) 1.4352(2) 0.73079(14) 0.0300(4) Uani 1 1 d . . . . .
H1E1 H -0.2996 1.5245 0.7366 0.036 Uiso 1 1 calc R U . . .
H1E2 H -0.1601 1.4372 0.7765 0.036 Uiso 1 1 calc R U . . .
C2 C 0.34480(19) 1.17459(16) 0.42648(11) 0.0135(3) Uani 1 1 d . . . . .
C2E C -0.2839(3) 1.3107(3) 0.74000(16) 0.0401(6) Uani 1 1 d . . . . .
H2E1 H -0.3504 1.3166 0.6998 0.060 Uiso 1 1 calc R U . . .
H2E2 H -0.3467 1.3120 0.7988 0.060 Uiso 1 1 calc R U . . .
H2E3 H -0.1995 1.2225 0.7274 0.060 Uiso 1 1 calc R U . . .
C3 C 0.26621(19) 1.06948(17) 0.44933(11) 0.0150(3) Uani 1 1 d . . . . .
H3 H 0.1586 1.0939 0.4784 0.018 Uiso 1 1 calc R U . . .
C4 C 0.3498(2) 0.92866(17) 0.42838(11) 0.0156(3) Uani 1 1 d . . . . .
C5 C 0.2731(2) 0.81379(17) 0.45684(11) 0.0162(3) Uani 1 1 d . . . . .
C6 C 0.5051(2) 0.89385(17) 0.38003(12) 0.0171(3) Uani 1 1 d . . . . .
H6 H 0.5608 0.7969 0.3673 0.021 Uiso 1 1 calc R U . . .
C7 C 0.57961(19) 0.99813(18) 0.35020(11) 0.0161(3) Uani 1 1 d . . . . .
C8 C 0.4987(2) 1.13921(17) 0.37704(11) 0.0157(3) Uani 1 1 d . . . . .
H8 H 0.5495 1.2120 0.3613 0.019 Uiso 1 1 calc R U . . .
C9 C 0.7426(2) 0.96489(19) 0.28744(12) 0.0201(3) Uani 1 1 d . . . . .
C10 C 0.7250(2) 1.0381(2) 0.20380(13) 0.0293(4) Uani 1 1 d . . . . .
H10A H 0.6533 1.0020 0.1793 0.044 Uiso 1 1 calc R U . . .
H10B H 0.8274 1.0182 0.1628 0.044 Uiso 1 1 calc R U . . .
H10C H 0.6830 1.1407 0.2160 0.044 Uiso 1 1 calc R U . . .
C11 C 0.8556(2) 1.0211(2) 0.32521(13) 0.0258(4) Uani 1 1 d . . . . .
H11A H 0.9539 1.0105 0.2816 0.039 Uiso 1 1 calc R U . . .
H11B H 0.8764 0.9671 0.3748 0.039 Uiso 1 1 calc R U . . .
H11C H 0.8088 1.1215 0.3433 0.039 Uiso 1 1 calc R U . . .
C12 C 0.8120(3) 0.8050(2) 0.26632(17) 0.0349(5) Uani 1 1 d . . . . .
H12A H 0.8210 0.7564 0.3193 0.052 Uiso 1 1 calc R U . . .
H12B H 0.9158 0.7878 0.2269 0.052 Uiso 1 1 calc R U . . .
H12C H 0.7436 0.7688 0.2393 0.052 Uiso 1 1 calc R U . . .
C13 C 0.7928(2) 0.42726(18) 0.34048(11) 0.0165(3) Uani 1 1 d . . . . .
C14 C 0.8430(2) 0.38893(19) 0.24565(11) 0.0178(3) Uani 1 1 d . . . . .
C15 C 0.7345(2) 0.4275(2) 0.19664(12) 0.0210(3) Uani 1 1 d . . . . .
H15 H 0.6309 0.4825 0.2218 0.025 Uiso 1 1 calc R U . . .
C16 C 0.7796(2) 0.3844(2) 0.10991(12) 0.0241(4) Uani 1 1 d . . . . .
C17 C 0.6584(3) 0.4281(2) 0.05978(13) 0.0290(4) Uani 1 1 d . . . . .
C18 C 0.9299(2) 0.3019(2) 0.07301(13) 0.0261(4) Uani 1 1 d . . . . .
H18 H 0.9578 0.2724 0.0139 0.031 Uiso 1 1 calc R U . . .
C19 C 1.0408(2) 0.2614(2) 0.12176(13) 0.0240(4) Uani 1 1 d . . . . .
C20 C 0.9944(2) 0.3066(2) 0.20818(12) 0.0203(3) Uani 1 1 d . . . . .
H20 H 1.0676 0.2807 0.2426 0.024 Uiso 1 1 calc R U . . .
C21 C 1.2046(2) 0.1653(3) 0.08014(14) 0.0324(5) Uani 1 1 d . . . . .
C22A C 1.3053(6) 0.1222(7) 0.1476(3) 0.0362(14) Uiso 0.560(15) 1 d . . P A 1
H22A H 1.4083 0.0605 0.1192 0.054 Uiso 0.560(15) 1 calc R U P A 1
H22B H 1.2524 0.0715 0.1930 0.054 Uiso 0.560(15) 1 calc R U P A 1
H22C H 1.3180 0.2077 0.1727 0.054 Uiso 0.560(15) 1 calc R U P A 1
C23A C 1.2884(8) 0.2334(6) 0.0090(5) 0.0435(14) Uiso 0.560(15) 1 d . . P A 1
H23A H 1.3091 0.3170 0.0314 0.065 Uiso 0.560(15) 1 calc R U P A 1
H23B H 1.2241 0.2624 -0.0323 0.065 Uiso 0.560(15) 1 calc R U P A 1
H23C H 1.3876 0.1661 -0.0197 0.065 Uiso 0.560(15) 1 calc R U P A 1
C24A C 1.1876(7) 0.0238(6) 0.0462(4) 0.0338(13) Uiso 0.560(15) 1 d . . P A 1
H24A H 1.1231 0.0439 0.0045 0.051 Uiso 0.560(15) 1 calc R U P A 1
H24B H 1.1376 -0.0242 0.0942 0.051 Uiso 0.560(15) 1 calc R U P A 1
H24C H 1.2912 -0.0374 0.0184 0.051 Uiso 0.560(15) 1 calc R U P A 1
C22B C 1.3226(9) 0.1715(11) 0.1305(5) 0.047(2) Uiso 0.440(15) 1 d . . P A 2
H22D H 1.4260 0.1130 0.1001 0.070 Uiso 0.440(15) 1 calc R U P A 2
H22E H 1.2920 0.1355 0.1874 0.070 Uiso 0.440(15) 1 calc R U P A 2
H22F H 1.3262 0.2699 0.1367 0.070 Uiso 0.440(15) 1 calc R U P A 2
C23B C 1.2647(10) 0.2238(8) -0.0122(6) 0.0457(19) Uiso 0.440(15) 1 d . . P A 2
H23D H 1.2672 0.3224 -0.0051 0.069 Uiso 0.440(15) 1 calc R U P A 2
H23E H 1.1935 0.2194 -0.0483 0.069 Uiso 0.440(15) 1 calc R U P A 2
H23F H 1.3700 0.1654 -0.0397 0.069 Uiso 0.440(15) 1 calc R U P A 2
C24B C 1.1911(11) 0.0119(10) 0.0678(7) 0.050(2) Uiso 0.440(15) 1 d . . P A 2
H24D H 1.1162 0.0132 0.0331 0.075 Uiso 0.440(15) 1 calc R U P A 2
H24E H 1.1551 -0.0244 0.1240 0.075 Uiso 0.440(15) 1 calc R U P A 2
H24F H 1.2937 -0.0496 0.0386 0.075 Uiso 0.440(15) 1 calc R U P A 2
O1 O 0.33951(14) 1.41699(12) 0.44718(8) 0.0165(2) Uani 1 1 d . . . . .
O1E O -0.10758(16) 1.42322(15) 0.64813(9) 0.0214(3) Uani 1 1 d D . . . .
O2 O 0.11700(14) 1.36162(13) 0.48759(8) 0.0172(2) Uani 1 1 d . . . . .
O3 O 0.12836(15) 0.83494(13) 0.46844(9) 0.0216(3) Uani 1 1 d . . . . .
O4 O 0.35826(16) 0.69177(13) 0.46618(10) 0.0238(3) Uani 1 1 d . . . . .
O5 O 0.89926(14) 0.40657(14) 0.38094(8) 0.0181(2) Uani 1 1 d . . . . .
O6 O 0.64967(15) 0.47477(16) 0.37302(9) 0.0234(3) Uani 1 1 d . . . . .
O7 O 0.7073(2) 0.3896(2) -0.02245(10) 0.0395(4) Uani 1 1 d . . . . .
H7 H 0.6359 0.4252 -0.0471 0.059 Uiso 1 1 calc R U . . .
O8 O 0.5246(2) 0.4946(2) 0.09364(10) 0.0449(5) Uani 1 1 d . . . . .
Mn1 Mn -0.12873(3) 1.38762(2) 0.51640(2) 0.01281(8) Uani 1 1 d . . . . .
Mn2 Mn 0.5000 0.5000 0.5000 0.01242(9) Uani 1 2 d S . P . .
H1E H -0.046(2) 1.480(2) 0.6469(14) 0.019 Uiso 1 1 d D 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
C1 O2 1.259(2) . ?
C1 O1 1.2734(19) . ?
C1 C2 1.487(2) . ?
C1E O1E 1.436(2) . ?
C1E C2E 1.503(3) . ?
C1E H1E1 0.9900 . ?
C1E H1E2 0.9900 . ?
C2 C8 1.395(2) . ?
C2 C3 1.402(2) . ?
C2E H2E1 0.9800 . ?
C2E H2E2 0.9800 . ?
C2E H2E3 0.9800 . ?
C3 C4 1.389(2) . ?
C3 H3 0.9500 . ?
C4 C6 1.399(2) . ?
C4 C5 1.489(2) . ?
C5 O3 1.253(2) . ?
C5 O4 1.271(2) . ?
C5 Mn1 2.6272(17) 2_576 ?
C6 C7 1.391(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.401(2) . ?
C7 C9 1.541(2) . ?
C8 H8 0.9500 . ?
C9 C12 1.534(3) . ?
C9 C11 1.534(3) . ?
C9 C10 1.537(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O6 1.249(2) . ?
C13 O5 1.268(2) . ?
C13 C14 1.505(2) . ?
C14 C15 1.385(2) . ?
C14 C20 1.397(2) . ?
C15 C16 1.393(3) . ?
C15 H15 0.9500 . ?
C16 C18 1.389(3) . ?
C16 C17 1.494(3) . ?
C17 O8 1.219(3) . ?
C17 O7 1.315(3) . ?
C18 C19 1.401(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.393(3) . ?
C19 C21 1.539(3) . ?
C20 H20 0.9500 . ?
C21 C23A 1.472(6) . ?
C21 C22B 1.510(7) . ?
C21 C24A 1.555(6) . ?
C21 C24B 1.559(9) . ?
C21 C22A 1.570(5) . ?
C21 C23B 1.608(8) . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
O1 Mn2 2.1883(12) 1_565 ?
O1 Mn1 2.2925(12) 2_586 ?
O1E Mn1 2.2132(14) . ?
O1E H1E 0.886(16) . ?
O2 Mn1 2.1292(13) . ?
O2 Mn1 2.4850(13) 2_586 ?
O3 Mn1 2.1885(13) 2_576 ?
O4 Mn2 2.1270(13) . ?
O4 Mn1 2.3809(14) 2_576 ?
O5 Mn1 2.1422(13) 1_645 ?
O6 Mn2 2.1435(13) . ?
O7 H7 0.8400 . ?
Mn1 O5 2.1422(13) 1_465 ?
Mn1 O3 2.1885(13) 2_576 ?
Mn1 O1 2.2925(12) 2_586 ?
Mn1 O4 2.3809(14) 2_576 ?
Mn1 O2 2.4850(13) 2_586 ?
Mn1 C5 2.6271(17) 2_576 ?
Mn2 O4 2.1269(13) 2_666 ?
Mn2 O6 2.1435(13) 2_666 ?
Mn2 O1 2.1884(12) 1_545 ?
Mn2 O1 2.1884(12) 2_676 ?

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 C1 O1 119.78(15) . . ?
O2 C1 C2 120.67(14) . . ?
O1 C1 C2 119.53(15) . . ?
O1E C1E C2E 109.29(18) . . ?
O1E C1E H1E1 109.8 . . ?
C2E C1E H1E1 109.8 . . ?
O1E C1E H1E2 109.8 . . ?
C2E C1E H1E2 109.8 . . ?
H1E1 C1E H1E2 108.3 . . ?
C8 C2 C3 120.57(15) . . ?
C8 C2 C1 120.19(14) . . ?
C3 C2 C1 119.24(15) . . ?
C1E C2E H2E1 109.5 . . ?
C1E C2E H2E2 109.5 . . ?
H2E1 C2E H2E2 109.5 . . ?
C1E C2E H2E3 109.5 . . ?
H2E1 C2E H2E3 109.5 . . ?
H2E2 C2E H2E3 109.5 . . ?
C4 C3 C2 118.27(15) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C3 C4 C6 120.60(15) . . ?
C3 C4 C5 119.71(15) . . ?
C6 C4 C5 119.69(15) . . ?
O3 C5 O4 120.37(15) . . ?
O3 C5 C4 120.97(15) . . ?
O4 C5 C4 118.61(16) . . ?
O3 C5 Mn1 55.99(8) . 2_576 ?
O4 C5 Mn1 64.75(9) . 2_576 ?
C4 C5 Mn1 171.18(13) . 2_576 ?
C7 C6 C4 121.46(15) . . ?
C7 C6 H6 119.3 . . ?
C4 C6 H6 119.3 . . ?
C6 C7 C8 117.53(16) . . ?
C6 C7 C9 122.85(15) . . ?
C8 C7 C9 119.59(15) . . ?
C2 C8 C7 121.13(15) . . ?
C2 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C12 C9 C11 108.67(17) . . ?
C12 C9 C10 108.45(18) . . ?
C11 C9 C10 109.27(16) . . ?
C12 C9 C7 111.69(15) . . ?
C11 C9 C7 110.68(15) . . ?
C10 C9 C7 108.03(15) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O6 C13 O5 125.44(17) . . ?
O6 C13 C14 117.26(15) . . ?
O5 C13 C14 117.29(15) . . ?
C15 C14 C20 119.99(17) . . ?
C15 C14 C13 119.37(16) . . ?
C20 C14 C13 120.48(16) . . ?
C14 C15 C16 118.95(18) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C18 C16 C15 120.89(18) . . ?
C18 C16 C17 122.10(18) . . ?
C15 C16 C17 117.00(18) . . ?
O8 C17 O7 123.3(2) . . ?
O8 C17 C16 121.65(19) . . ?
O7 C17 C16 115.04(19) . . ?
C16 C18 C19 120.86(18) . . ?
C16 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C20 C19 C18 117.57(18) . . ?
C20 C19 C21 122.56(18) . . ?
C18 C19 C21 119.82(18) . . ?
C19 C20 C14 121.73(17) . . ?
C19 C20 H20 119.1 . . ?
C14 C20 H20 119.1 . . ?
C23A C21 C19 111.6(3) . . ?
C22B C21 C19 112.3(3) . . ?
C23A C21 C24A 109.6(4) . . ?
C19 C21 C24A 108.8(3) . . ?
C22B C21 C24B 112.7(5) . . ?
C19 C21 C24B 108.5(4) . . ?
C23A C21 C22A 109.7(3) . . ?
C19 C21 C22A 111.6(2) . . ?
C24A C21 C22A 105.4(3) . . ?
C22B C21 C23B 106.2(4) . . ?
C19 C21 C23B 107.9(3) . . ?
C24B C21 C23B 109.2(5) . . ?
C21 C22A H22A 109.5 . . ?
C21 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C21 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C21 C23A H23A 109.5 . . ?
C21 C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C21 C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C21 C24A H24A 109.5 . . ?
C21 C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C21 C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C21 C22B H22D 109.5 . . ?
C21 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C21 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C21 C23B H23D 109.5 . . ?
C21 C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C21 C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C21 C24B H24D 109.5 . . ?
C21 C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C21 C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C1 O1 Mn2 144.23(11) . 1_565 ?
C1 O1 Mn1 96.90(10) . 2_586 ?
Mn2 O1 Mn1 96.97(5) 1_565 2_586 ?
C1E O1E Mn1 132.57(13) . . ?
C1E O1E H1E 110.7(15) . . ?
Mn1 O1E H1E 109.1(15) . . ?
C1 O2 Mn1 165.41(12) . . ?
C1 O2 Mn1 88.33(9) . 2_586 ?
Mn1 O2 Mn1 101.32(5) . 2_586 ?
C5 O3 Mn1 95.69(10) . 2_576 ?
C5 O4 Mn2 171.48(14) . . ?
C5 O4 Mn1 86.38(10) . 2_576 ?
Mn2 O4 Mn1 96.06(5) . 2_576 ?
C13 O5 Mn1 126.94(11) . 1_645 ?
C13 O6 Mn2 135.88(12) . . ?
C17 O7 H7 109.5 . . ?
O2 Mn1 O5 84.57(5) . 1_465 ?
O2 Mn1 O3 98.69(5) . 2_576 ?
O5 Mn1 O3 102.35(5) 1_465 2_576 ?
O2 Mn1 O1E 81.78(5) . . ?
O5 Mn1 O1E 159.52(5) 1_465 . ?
O3 Mn1 O1E 94.78(5) 2_576 . ?
O2 Mn1 O1 132.67(5) . 2_586 ?
O5 Mn1 O1 94.55(5) 1_465 2_586 ?
O3 Mn1 O1 127.32(5) 2_576 2_586 ?
O1E Mn1 O1 83.69(5) . 2_586 ?
O2 Mn1 O4 154.76(5) . 2_576 ?
O5 Mn1 O4 93.45(5) 1_465 2_576 ?
O3 Mn1 O4 57.08(5) 2_576 2_576 ?
O1E Mn1 O4 105.36(5) . 2_576 ?
O1 Mn1 O4 72.56(4) 2_586 2_576 ?
O2 Mn1 O2 78.68(5) . 2_586 ?
O5 Mn1 O2 82.88(5) 1_465 2_586 ?
O3 Mn1 O2 173.98(5) 2_576 2_586 ?
O1E Mn1 O2 79.52(5) . 2_586 ?
O1 Mn1 O2 54.41(4) 2_586 2_586 ?
O4 Mn1 O2 126.14(4) 2_576 2_586 ?
O2 Mn1 C5 126.94(5) . 2_576 ?
O5 Mn1 C5 100.87(5) 1_465 2_576 ?
O3 Mn1 C5 28.32(5) 2_576 2_576 ?
O1E Mn1 C5 99.54(5) . 2_576 ?
O1 Mn1 C5 99.80(5) 2_586 2_576 ?
O4 Mn1 C5 28.87(5) 2_576 2_576 ?
O2 Mn1 C5 154.21(5) 2_586 2_576 ?
O4 Mn2 O4 180.0 2_666 . ?
O4 Mn2 O6 89.47(5) 2_666 2_666 ?
O4 Mn2 O6 90.53(5) . 2_666 ?
O4 Mn2 O6 90.53(5) 2_666 . ?
O4 Mn2 O6 89.47(5) . . ?
O6 Mn2 O6 180.0 2_666 . ?
O4 Mn2 O1 100.27(5) 2_666 1_545 ?
O4 Mn2 O1 79.73(5) . 1_545 ?
O6 Mn2 O1 92.34(5) 2_666 1_545 ?
O6 Mn2 O1 87.66(5) . 1_545 ?
O4 Mn2 O1 79.73(5) 2_666 2_676 ?
O4 Mn2 O1 100.27(5) . 2_676 ?
O6 Mn2 O1 87.66(5) 2_666 2_676 ?
O6 Mn2 O1 92.34(5) . 2_676 ?
O1 Mn2 O1 180.0 1_545 2_676 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1E H1E O5 0.886(16) 1.931(16) 2.8038(19) 168(2) 2_676
O7 H7 O8 0.84 1.80 2.637(2) 176.5 2_665

_refine_diff_density_max         0.875
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.087

