data_1
_audit_creation_date              2016-11-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          '0.25(C92 H80 O64 Zn12), C5 H9 N O, 2(H2 O)'
_chemical_formula_sum             'C28 H33 N O19 Zn3'
_chemical_formula_weight          883.66
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system       'orthorhombic'
_space_group_IT_number            62
_space_group_name_H-M_alt         'P n m a'
_space_group_name_Hall            '-P 2ac 2n'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'

_cell_length_a                    8.6370(10)
_cell_length_b                    20.398(2)
_cell_length_c                    18.307(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      3225.3(7)
_cell_formula_units_Z             4
_cell_measurement_reflns_used     9359
_cell_measurement_temperature     296(2)
_cell_measurement_theta_max       28.43
_cell_measurement_theta_min       2.36
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     2.302
_exptl_absorpt_correction_T_max   0.7457
_exptl_absorpt_correction_T_min   0.5202
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0972 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.6976.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             colourless
_exptl_crystal_colour_primary     colourless
_exptl_crystal_density_diffrn     1.820
_exptl_crystal_density_meas       .
_exptl_crystal_density_method     ?
_exptl_crystal_description        block
_exptl_crystal_F_000              1800
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0317
_diffrn_reflns_av_unetI/netI      0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_k_max        24
_diffrn_reflns_limit_k_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_number             15434
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          25.347
_diffrn_reflns_theta_min          1.997
_diffrn_ambient_temperature       296.15
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_radiation_monochromator   'graphite'
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    ?
_diffrn_standards_number          0
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 2923
_reflns_number_total              3037
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        'SAINT V8.18C (?, 2016)'
_computing_data_collection        ?
_computing_data_reduction         'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     ?
_refine_diff_density_max          1.190
_refine_diff_density_min          -1.434
_refine_diff_density_rms          0.139
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.164
_refine_ls_hydrogen_treatment     mixed
_refine_ls_matrix_type            full
_refine_ls_number_parameters      303
_refine_ls_number_reflns          3037
_refine_ls_number_restraints      55
_refine_ls_R_factor_all           0.0540
_refine_ls_R_factor_gt            0.0521
_refine_ls_restrained_S_all       1.183
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0470P)²+25.5976P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1351
_refine_ls_wR_factor_ref          0.1371
_refine_special_details           ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Zn1A) \\sim Ueq, Uanis(Zn1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O12, C14, N2, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, Zn1A, Zn1, O7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Zn1A)=1-FVAR(1)
 Sof(Zn1)=FVAR(1)
 Sof(O7A)=1-FVAR(2)
 Sof(O7)=FVAR(2)
 Fixed Sof: O12(0.5) C14(0.5) N2(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) O13(0.5) H13A(0.5) H13B(0.5) O14(0.5) H14A(0.5) H14B(0.5)
6.a Riding coordinates:
 O8(H8), O9(H9A,H9B), O7(H7A,H7B), O13(H13A,H13B), O14(H14A,H14B)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C6(H6), C3(H3), C5(H5)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens    mixed
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.46879(18) 0.32910(4) 0.52787(6) 0.0128(3) Uani 0.928(6) 1 d . U . A
 1
 Zn2 Zn 0.21529(10) 0.7500 0.45032(4) 0.0183(2) Uani 1 2 d S T P . .
 O1 O 0.5507(5) 0.2500 0.5796(2) 0.0127(9) Uani 1 2 d DS T P . .
 O2 O 0.3087(4) 0.67472(17) 0.52108(18) 0.0189(8) Uani 1 1 d . . . . .
 O3 O 0.1070(4) 0.65706(19) 0.5943(2) 0.0244(8) Uani 1 1 d . . . . .
 O4 O 0.1465(4) 0.80501(15) 0.93974(17) 0.0146(7) Uani 1 1 d . . . . .
 O8 O 0.0067(6) 0.7500 0.5043(3) 0.0235(11) Uani 1 2 d S T P . .
 H8 H 0.0035 0.7184 0.5369 0.035 Uiso 1 1 d R . . . .
 O5 O 0.4634(5) 0.42065(18) 0.55503(19) 0.0278(9) Uani 1 1 d . U . . .
 O9 O 0.1591(5) 0.67623(19) 0.3769(2) 0.0290(9) Uani 1 1 d . . . . .
 H9A H 0.2051 0.6873 0.3363 0.044 Uiso 1 1 d R . . . .
 H9B H 0.1891 0.6386 0.3851 0.044 Uiso 1 1 d R . . . .
 O6 O 0.5876(6) 0.39753(19) 0.6580(2) 0.0345(10) Uani 1 1 d . . . . .
 C10 C 0.2807(5) 0.6908(2) 0.8025(2) 0.0093(9) Uani 1 1 d . . . . .
 H10 H 0.2636 0.6514 0.8267 0.011 Uiso 1 1 calc R . . . .
 C2 C 0.3435(5) 0.6074(2) 0.6276(2) 0.0107(9) Uani 1 1 d . . . . .
 C9 C 0.3638(7) 0.7500 0.6962(3) 0.0082(12) Uani 1 2 d S T P . .
 H9 H 0.3972 0.7500 0.6479 0.010 Uiso 1 2 calc RS T P . .
 C6 C 0.4733(5) 0.5837(2) 0.7406(2) 0.0124(9) Uani 1 1 d . . . . .
 H6 H 0.5046 0.5968 0.7870 0.015 Uiso 1 1 calc R . . . .
 C3 C 0.3876(6) 0.5459(2) 0.6017(2) 0.0141(10) Uani 1 1 d . . . . .
 H3 H 0.3610 0.5336 0.5545 0.017 Uiso 1 1 calc R . . . .
 C8 C 0.3392(5) 0.6905(2) 0.7318(2) 0.0092(9) Uani 1 1 d . . . . .
 C5 C 0.5168(6) 0.5227(2) 0.7152(3) 0.0157(10) Uani 1 1 d . . . . .
 H5 H 0.5764 0.4952 0.7444 0.019 Uiso 1 1 calc R . . . .
 C7 C 0.3833(5) 0.6264(2) 0.6985(2) 0.0088(8) Uani 1 1 d . . . . .
 C1 C 0.2434(5) 0.6497(2) 0.5789(2) 0.0108(9) Uani 1 1 d . . . . .
 C13 C 0.5110(7) 0.4358(2) 0.6183(3) 0.0238(12) Uani 1 1 d . . . . .
 C11 C 0.2473(7) 0.7500 0.8374(3) 0.0084(12) Uani 1 2 d S T P . .
 C4 C 0.4709(6) 0.5026(2) 0.6454(2) 0.0151(10) Uani 1 1 d . . . . .
 C12 C 0.1773(7) 0.7500 0.9118(3) 0.0074(12) Uani 1 2 d S T P . .
 O7 O 0.230(3) 0.3010(15) 0.5871(10) 0.032(5) Uani 0.36(6) 1 d . U . A 1
 H7A H 0.1522 0.3230 0.5668 0.048 Uiso 1 1 d R . . . .
 H7B H 0.2387 0.3152 0.6330 0.048 Uiso 1 1 d R . . . .
 O12 O 0.0482(9) 0.4128(4) 0.5728(5) 0.0264(16) Uani 0.5 1 d . U . B -1
 C14 C 0.0486(19) 0.4542(9) 0.5215(9) 0.020(3) Uani 0.5 1 d . U . B -1
 N2 N -0.0425(10) 0.5064(5) 0.5185(5) 0.0212(18) Uani 0.5 1 d . U . B -1
 C15 C 0.1484(15) 0.4514(6) 0.4546(7) 0.020(2) Uani 0.5 1 d . U . B -1
 H15A H 0.2571 0.4550 0.4673 0.024 Uiso 0.5 1 calc R . . B -1
 H15B H 0.1320 0.4108 0.4280 0.024 Uiso 0.5 1 calc R . . B -1
 C16 C 0.099(3) 0.5073(10) 0.4118(9) 0.092(9) Uani 0.5 1 d . U . B -1
 H16A H 0.0533 0.4923 0.3663 0.111 Uiso 0.5 1 calc R . . B -1
 H16B H 0.1874 0.5346 0.4001 0.111 Uiso 0.5 1 calc R . . B -1
 C17 C -0.018(2) 0.5466(8) 0.4536(8) 0.022(3) Uani 0.5 1 d . . . B -1
 H17A H 0.0228 0.5895 0.4663 0.026 Uiso 0.5 1 calc R . . B -1
 H17B H -0.1128 0.5520 0.4260 0.026 Uiso 0.5 1 calc R . . B -1
 C18 C -0.1506(15) 0.5263(8) 0.5742(8) 0.026(3) Uani 0.5 1 d . . . B -1
 H18A H -0.2537 0.5256 0.5547 0.038 Uiso 0.5 1 calc GR . . B -1
 H18B H -0.1259 0.5698 0.5904 0.038 Uiso 0.5 1 calc GR . . B -1
 H18C H -0.1442 0.4965 0.6148 0.038 Uiso 0.5 1 calc GR . . B -1
 Zn1A Zn 0.411(2) 0.3212(5) 0.5443(7) 0.010(3) Uani 0.072(6) 1 d . U . A 2
 O7A O 0.264(2) 0.3239(12) 0.5929(9) 0.044(5) Uani 0.64(6) 1 d . U . A 2
 O13 O 0.0922(18) 0.3380(10) 0.7116(7) 0.109(7) Uani 0.5 1 d . . . C -1
 H13A H 0.0868 0.3432 0.7581 0.164 Uiso 0.5 1 d R . . C -1
 H13B H 0.0503 0.3683 0.6899 0.164 Uiso 0.5 1 d R . . C -1
 O14 O -0.027(3) 0.2159(8) 0.7680(7) 0.147(10) Uani 0.5 1 d . . . D -1
 H14A H -0.0266 0.1761 0.7823 0.220 Uiso 0.5 1 d R . . D -1
 H14B H -0.0077 0.2342 0.7273 0.220 Uiso 0.5 1 d R . . D -1
 H1 H 0.51(3) 0.2500 0.620(6) 0.220 Uiso 1 2 d DRS T P . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 2.000(3) . ?
 Zn1 O2 2.122(4) 5_666 ?
 Zn1 O4 1.959(3) 8_655 ?
 Zn1 O5 1.933(4) . ?
 Zn1 O7 2.40(3) . ?
 Zn2 O1 2.094(5) 5_666 ?
 Zn2 O2 2.165(3) 7_575 ?
 Zn2 O2 2.165(3) . ?
 Zn2 O8 2.055(5) . ?
 Zn2 O9 2.075(4) 7_575 ?
 Zn2 O9 2.075(4) . ?
 O1 Zn1 2.000(3) 7_565 ?
 O1 Zn2 2.094(5) 5_666 ?
 O1 Zn1A 1.998(10) . ?
 O1 Zn1A 1.998(10) 7_565 ?
 O1 H1 0.81(2) . ?
 O2 Zn1 2.122(4) 5_666 ?
 O2 C1 1.302(6) . ?
 O3 C1 1.220(6) . ?
 O4 Zn1 1.959(3) 8_666 ?
 O4 C12 1.261(4) . ?
 O4 Zn1A 2.003(10) 8_666 ?
 O8 H8 0.8790 . ?
 O5 C13 1.267(6) . ?
 O5 Zn1A 2.089(12) . ?
 O9 H9A 0.8730 . ?
 O9 H9B 0.8232 . ?
 O6 C13 1.254(7) . ?
 C10 H10 0.9300 . ?
 C10 C8 1.389(6) . ?
 C10 C11 1.396(5) . ?
 C2 C3 1.393(6) . ?
 C2 C7 1.398(6) . ?
 C2 C1 1.513(6) . ?
 C9 H9 0.9300 . ?
 C9 C8 1.394(5) . ?
 C9 C8 1.394(5) 7_575 ?
 C6 H6 0.9300 . ?
 C6 C5 1.380(6) . ?
 C6 C7 1.399(6) . ?
 C3 H3 0.9300 . ?
 C3 C4 1.393(7) . ?
 C8 C7 1.492(6) . ?
 C5 H5 0.9300 . ?
 C5 C4 1.399(7) . ?
 C13 C4 1.491(6) . ?
 C11 C10 1.396(5) 7_575 ?
 C11 C12 1.490(8) . ?
 C12 O4 1.261(4) 7_575 ?
 O7 H7A 0.8902 . ?
 O7 H7B 0.8913 . ?
 O12 C14 1.265(19) . ?
 C14 N2 1.32(2) . ?
 C14 C15 1.50(2) . ?
 N2 C17 1.460(17) . ?
 N2 C18 1.440(15) . ?
 C15 H15A 0.9700 . ?
 C15 H15B 0.9700 . ?
 C15 C16 1.448(19) . ?
 C16 H16A 0.9700 . ?
 C16 H16B 0.9700 . ?
 C16 C17 1.50(2) . ?
 C17 H17A 0.9700 . ?
 C17 H17B 0.9700 . ?
 C18 H18A 0.9600 . ?
 C18 H18B 0.9600 . ?
 C18 H18C 0.9600 . ?
 Zn1A O4 2.003(10) 8_655 ?
 Zn1A Zn1A 2.90(2) 7_565 ?
 Zn1A O7A 1.55(2) . ?
 O7A H7A 1.0748 . ?
 O7A H7B 0.7852 . ?
 O13 H13A 0.8579 . ?
 O13 H13B 0.8191 . ?
 O14 H14A 0.8525 . ?
 O14 H14B 0.8508 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O2 81.37(17) . 5_666 ?
 O1 Zn1 O7 84.1(6) . . ?
 O2 Zn1 O7 163.8(7) 5_666 . ?
 O4 Zn1 O1 111.56(14) 8_655 . ?
 O4 Zn1 O2 95.94(15) 8_655 5_666 ?
 O4 Zn1 O7 82.8(4) 8_655 . ?
 O5 Zn1 O1 131.76(15) . . ?
 O5 Zn1 O2 99.56(18) . 5_666 ?
 O5 Zn1 O4 116.23(15) . 8_655 ?
 O5 Zn1 O7 95.4(6) . . ?
 O1 Zn2 O2 78.29(13) 5_666 7_575 ?
 O1 Zn2 O2 78.29(13) 5_666 . ?
 O2 Zn2 O2 90.35(19) 7_575 . ?
 O8 Zn2 O1 166.4(2) . 5_666 ?
 O8 Zn2 O2 92.22(14) . 7_575 ?
 O8 Zn2 O2 92.22(14) . . ?
 O8 Zn2 O9 96.11(16) . 7_575 ?
 O8 Zn2 O9 96.11(16) . . ?
 O9 Zn2 O1 93.23(15) 7_575 5_666 ?
 O9 Zn2 O1 93.23(15) . 5_666 ?
 O9 Zn2 O2 171.52(16) . 7_575 ?
 O9 Zn2 O2 171.52(16) 7_575 . ?
 O9 Zn2 O2 87.73(15) . . ?
 O9 Zn2 O2 87.74(15) 7_575 7_575 ?
 O9 Zn2 O9 93.0(2) 7_575 . ?
 Zn1 O1 Zn1 107.5(2) . 7_565 ?
 Zn1 O1 Zn2 102.57(16) 7_565 5_666 ?
 Zn1 O1 Zn2 102.57(16) . 5_666 ?
 Zn1 O1 H1 106(10) 7_565 . ?
 Zn1 O1 H1 106(10) . . ?
 Zn2 O1 H1 131(10) 5_666 . ?
 Zn1A O1 Zn2 120.0(6) 7_565 5_666 ?
 Zn1A O1 Zn2 120.0(6) . 5_666 ?
 Zn1A O1 Zn1A 93.2(8) 7_565 . ?
 Zn1A O1 H1 92(10) 7_565 . ?
 Zn1A O1 H1 92(10) . . ?
 Zn1 O2 Zn2 96.36(14) 5_666 . ?
 C1 O2 Zn1 136.1(3) . 5_666 ?
 C1 O2 Zn2 127.0(3) . . ?
 C12 O4 Zn1 131.6(3) . 8_666 ?
 C12 O4 Zn1A 125.8(5) . 8_666 ?
 Zn2 O8 H8 110.7 . . ?
 C13 O5 Zn1 117.5(3) . . ?
 C13 O5 Zn1A 113.2(4) . . ?
 Zn2 O9 H9A 105.0 . . ?
 Zn2 O9 H9B 119.0 . . ?
 H9A O9 H9B 104.6 . . ?
 C8 C10 H10 119.8 . . ?
 C8 C10 C11 120.4(4) . . ?
 C11 C10 H10 119.8 . . ?
 C3 C2 C7 119.9(4) . . ?
 C3 C2 C1 118.1(4) . . ?
 C7 C2 C1 121.9(4) . . ?
 C8 C9 H9 119.5 7_575 . ?
 C8 C9 H9 119.5 . . ?
 C8 C9 C8 121.0(5) . 7_575 ?
 C5 C6 H6 119.1 . . ?
 C5 C6 C7 121.7(4) . . ?
 C7 C6 H6 119.1 . . ?
 C2 C3 H3 119.4 . . ?
 C2 C3 C4 121.2(4) . . ?
 C4 C3 H3 119.4 . . ?
 C10 C8 C9 119.2(4) . . ?
 C10 C8 C7 118.6(4) . . ?
 C9 C8 C7 122.1(4) . . ?
 C6 C5 H5 120.1 . . ?
 C6 C5 C4 119.7(4) . . ?
 C4 C5 H5 120.1 . . ?
 C2 C7 C6 118.4(4) . . ?
 C2 C7 C8 124.1(4) . . ?
 C6 C7 C8 117.5(4) . . ?
 O2 C1 C2 117.0(4) . . ?
 O3 C1 O2 123.9(4) . . ?
 O3 C1 C2 119.0(4) . . ?
 O5 C13 C4 116.8(5) . . ?
 O6 C13 O5 123.3(5) . . ?
 O6 C13 C4 119.8(4) . . ?
 C10 C11 C10 119.7(5) . 7_575 ?
 C10 C11 C12 120.1(3) . . ?
 C10 C11 C12 120.1(3) 7_575 . ?
 C3 C4 C5 118.9(4) . . ?
 C3 C4 C13 120.6(4) . . ?
 C5 C4 C13 120.5(4) . . ?
 O4 C12 O4 125.6(5) 7_575 . ?
 O4 C12 C11 117.1(3) . . ?
 O4 C12 C11 117.1(3) 7_575 . ?
 Zn1 O7 H7A 109.9 . . ?
 Zn1 O7 H7B 106.0 . . ?
 H7A O7 H7B 106.9 . . ?
 O12 C14 N2 124.5(14) . . ?
 O12 C14 C15 125.7(15) . . ?
 N2 C14 C15 109.8(14) . . ?
 C14 N2 C17 113.4(9) . . ?
 C14 N2 C18 125.5(12) . . ?
 C18 N2 C17 120.9(11) . . ?
 C14 C15 H15A 111.0 . . ?
 C14 C15 H15B 111.0 . . ?
 H15A C15 H15B 109.0 . . ?
 C16 C15 C14 104.0(12) . . ?
 C16 C15 H15A 111.0 . . ?
 C16 C15 H15B 111.0 . . ?
 C15 C16 H16A 109.6 . . ?
 C15 C16 H16B 109.6 . . ?
 C15 C16 C17 110.1(12) . . ?
 H16A C16 H16B 108.1 . . ?
 C17 C16 H16A 109.6 . . ?
 C17 C16 H16B 109.6 . . ?
 N2 C17 C16 102.3(12) . . ?
 N2 C17 H17A 111.3 . . ?
 N2 C17 H17B 111.3 . . ?
 C16 C17 H17A 111.3 . . ?
 C16 C17 H17B 111.3 . . ?
 H17A C17 H17B 109.2 . . ?
 N2 C18 H18A 109.5 . . ?
 N2 C18 H18B 109.5 . . ?
 N2 C18 H18C 109.5 . . ?
 H18A C18 H18B 109.5 . . ?
 H18A C18 H18C 109.5 . . ?
 H18B C18 H18C 109.5 . . ?
 O1 Zn1A O4 109.8(5) . 8_655 ?
 O1 Zn1A O5 122.9(7) . . ?
 O1 Zn1A Zn1A 43.4(4) . 7_565 ?
 O4 Zn1A O5 107.7(6) 8_655 . ?
 O4 Zn1A Zn1A 80.5(3) 8_655 7_565 ?
 O5 Zn1A Zn1A 166.2(3) . 7_565 ?
 O7A Zn1A O1 109.6(9) . . ?
 O7A Zn1A O4 110.7(12) . 8_655 ?
 O7A Zn1A O5 95.2(11) . . ?
 O7A Zn1A Zn1A 92.0(10) . 7_565 ?
 H7A O7A H7B 99.5 . . ?
 Zn1A O7A H7A 118.6 . . ?
 Zn1A O7A H7B 138.9 . . ?
 H13A O13 H13B 111.2 . . ?
 H14A O14 H14B 133.3 . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
 O8 H8 O3 0.88 1.86 2.656(5) 149.4 .
 O9 H9A O14 0.87 2.52 2.998(13) 115.3 3_556
 O9 H9B O6 0.82 2.21 2.731(6) 121.4 5_666
 O7 H7A O8 0.89 2.41 2.84(2) 110.1 5_566
 O7A H7A O8 1.07 2.41 3.30(3) 139.5 5_566
 O13 H13A O6 0.86 1.89 2.679(12) 151.2 6_557
 O14 H14A O6 0.85 2.10 2.858(16) 147.4 4_456
 O14 H14B O9 0.85 2.60 2.998(13) 110.1 3_546
 O1 H1 O14 0.81(2) 2.19(7) 2.953(13) 155(16) 6_657
 O1 H1 O14 0.81(2) 2.19(7) 2.953(13) 155(16) 4_556

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O2 C1 O3 -176.5(4) 5_666 . . . ?
 Zn1 O2 C1 C2 1.3(6) 5_666 . . . ?
 Zn1 O4 C12 O4 -5.4(10) 8_666 . . 7_575 ?
 Zn1 O4 C12 C11 170.5(4) 8_666 . . . ?
 Zn1 O5 C13 O6 14.2(8) . . . . ?
 Zn1 O5 C13 C4 -165.3(4) . . . . ?
 Zn2 O2 C1 O3 13.7(7) . . . . ?
 Zn2 O2 C1 C2 -168.5(3) . . . . ?
 O5 C13 C4 C3 -1.3(8) . . . . ?
 O5 C13 C4 C5 178.9(5) . . . . ?
 O6 C13 C4 C3 179.2(5) . . . . ?
 O6 C13 C4 C5 -0.6(8) . . . . ?
 C10 C8 C7 C2 134.4(5) . . . . ?
 C10 C8 C7 C6 -47.2(6) . . . . ?
 C10 C11 C12 O4 -2.1(8) . . . 7_575 ?
 C10 C11 C12 O4 178.4(5) 7_575 . . 7_575 ?
 C10 C11 C12 O4 2.1(8) 7_575 . . . ?
 C10 C11 C12 O4 -178.4(5) . . . . ?
 C2 C3 C4 C5 -3.0(7) . . . . ?
 C2 C3 C4 C13 177.1(5) . . . . ?
 C9 C8 C7 C2 -49.7(7) . . . . ?
 C9 C8 C7 C6 128.7(5) . . . . ?
 C6 C5 C4 C3 2.8(7) . . . . ?
 C6 C5 C4 C13 -177.3(5) . . . . ?
 C3 C2 C7 C6 2.8(6) . . . . ?
 C3 C2 C7 C8 -178.8(4) . . . . ?
 C3 C2 C1 O2 -71.0(6) . . . . ?
 C3 C2 C1 O3 106.9(5) . . . . ?
 C8 C10 C11 C10 -3.4(9) . . . 7_575 ?
 C8 C10 C11 C12 177.0(5) . . . . ?
 C8 C9 C8 C10 3.8(9) 7_575 . . . ?
 C8 C9 C8 C7 -172.1(3) 7_575 . . . ?
 C5 C6 C7 C2 -3.0(7) . . . . ?
 C5 C6 C7 C8 178.4(4) . . . . ?
 C7 C2 C3 C4 0.2(7) . . . . ?
 C7 C2 C1 O2 113.2(5) . . . . ?
 C7 C2 C1 O3 -68.9(6) . . . . ?
 C7 C6 C5 C4 0.2(7) . . . . ?
 C1 C2 C3 C4 -175.7(4) . . . . ?
 C1 C2 C7 C6 178.5(4) . . . . ?
 C1 C2 C7 C8 -3.1(7) . . . . ?
 C11 C10 C8 C9 -0.1(7) . . . . ?
 C11 C10 C8 C7 175.9(5) . . . . ?
 O12 C14 N2 C17 179.5(10) . . . . ?
 O12 C14 N2 C18 3(2) . . . . ?
 O12 C14 C15 C16 176.8(18) . . . . ?
 C14 N2 C17 C16 4(2) . . . . ?
 C14 C15 C16 C17 5(2) . . . . ?
 N2 C14 C15 C16 -2(2) . . . . ?
 C15 C14 N2 C17 -2(2) . . . . ?
 C15 C14 N2 C18 -178.0(12) . . . . ?
 C15 C16 C17 N2 -6(2) . . . . ?
 C18 N2 C17 C16 -179.1(15) . . . . ?
 Zn1A O4 C12 O4 16.0(11) 8_666 . . 7_575 ?
 Zn1A O4 C12 C11 -168.1(7) 8_666 . . . ?
 Zn1A O5 C13 O6 32.2(9) . . . . ?
 Zn1A O5 C13 C4 -147.3(7) . . . . ?

_shelx_SHELXL_version_number      '2014/7'
_olex2_submission_special_instructions 'No special instructions were received'
data_2
_audit_creation_date              2016-12-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          'C23 H11 O11 Zn2, C2 H8 N'
_chemical_formula_sum             'C25 H19 N O11 Zn2'
_chemical_formula_weight          640.15
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                    12.252(5)
_cell_length_b                    12.820(5)
_cell_length_c                    13.635(6)
_cell_angle_alpha                 65.009(7)
_cell_angle_beta                  79.056(7)
_cell_angle_gamma                 79.551(7)
_cell_volume                      1893.6(14)
_cell_formula_units_Z             2
_cell_measurement_reflns_used     4146
_cell_measurement_temperature     173
_cell_measurement_theta_max       28.253
_cell_measurement_theta_min       2.526
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     1.309
_exptl_absorpt_correction_T_max   0.7457
_exptl_absorpt_correction_T_min   0.5966
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0662 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.8001.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             colourless
_exptl_crystal_colour_primary     colourless
_exptl_crystal_density_diffrn     1.123
_exptl_crystal_density_meas       .
_exptl_crystal_density_method     ?
_exptl_crystal_description        block
_exptl_crystal_F_000              648
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0332
_diffrn_reflns_av_unetI/netI      0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_number             10198
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          26.370
_diffrn_reflns_theta_min          6.822
_diffrn_ambient_temperature       173
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_radiation_monochromator   graphite
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    ?
_diffrn_special_details           ?
_diffrn_standards_number          0
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 5713
_reflns_number_total              7377
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        'SAINT V8.18C (?, 2016)'
_computing_data_collection        ?
_computing_data_reduction         'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     ?
_refine_diff_density_max          1.629
_refine_diff_density_min          -1.560
_refine_diff_density_rms          0.234
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.226
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      354
_refine_ls_number_reflns          7377
_refine_ls_number_restraints      51
_refine_ls_R_factor_all           0.1015
_refine_ls_R_factor_gt            0.0791
_refine_ls_restrained_S_all       1.232
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.2428
_refine_ls_wR_factor_ref          0.3037
_refine_special_details           ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C5)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 N1, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 O11(H11A,H11B)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C10(H10), C12(H12), C14(H14), C17(H17), C18(H18),
 C20(H20)
4.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens    mixed
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 1.54116(5) 0.92546(6) -0.11370(5) 0.0153(3) Uani 1 1 d . . . . .
 Zn2 Zn 1.08889(5) 0.53397(5) 0.53935(5) 0.0133(3) Uani 1 1 d . . . . .
 O1 O 1.4042(3) 0.8556(4) -0.0813(4) 0.0217(9) Uani 1 1 d . . . . .
 O2 O 1.4417(4) 0.6880(4) 0.0581(5) 0.0392(14) Uani 1 1 d . . . . .
 O3 O 1.1215(4) 0.6190(4) 0.3740(3) 0.0249(10) Uani 1 1 d . . . . .
 O4 O 0.9888(4) 0.5713(4) 0.3151(4) 0.0230(10) Uani 1 1 d . . . . .
 O5 O 0.6488(3) 0.8784(3) -0.0123(3) 0.0190(9) Uani 1 1 d . U . . .
 O6 O 0.5227(3) 0.9167(4) 0.1127(3) 0.0178(9) Uani 1 1 d . . . . .
 O7 O 0.5890(4) 0.9753(4) 0.7275(4) 0.0248(10) Uani 1 1 d . . . . .
 O8 O 0.6703(5) 0.7999(5) 0.8057(4) 0.0478(16) Uani 1 1 d . . . . .
 O9 O 0.8337(4) 0.6131(4) 0.4775(4) 0.0332(12) Uani 1 1 d . . . . .
 O10 O 0.9649(4) 0.6648(4) 0.5366(4) 0.0288(11) Uani 1 1 d . . . . .
 O11 O 1.2081(5) 0.5793(5) 0.5855(5) 0.0490(16) Uani 1 1 d . . . . .
 H11A H 1.2265 0.6236 0.5167 0.074 Uiso 1 1 d R . . . .
 H11B H 1.2296 0.5055 0.6137 0.074 Uiso 1 1 d R . . . .
 C1 C 1.3777(5) 0.7710(6) 0.0022(6) 0.0236(14) Uani 1 1 d . . . . .
 C2 C 1.2534(5) 0.7710(5) 0.0430(5) 0.0157(12) Uani 1 1 d . . . . .
 C3 C 1.1798(5) 0.8561(5) -0.0271(5) 0.0180(12) Uani 1 1 d . . . . .
 H3 H 1.2060 0.9068 -0.0988 0.022 Uiso 1 1 calc R . . . .
 C4 C 1.0658(5) 0.8614(5) 0.0152(5) 0.0183(12) Uani 1 1 d . . . . .
 H4 H 1.0133 0.9130 -0.0315 0.022 Uiso 1 1 calc R . . . .
 C5 C 1.0273(4) 0.7945(4) 0.1218(4) 0.0099(10) Uani 1 1 d . U . . .
 C6 C 1.1029(5) 0.7088(5) 0.1879(5) 0.0154(12) Uani 1 1 d . . . . .
 C7 C 1.2149(5) 0.6993(5) 0.1462(5) 0.0188(13) Uani 1 1 d . . . . .
 H7 H 1.2660 0.6416 0.1905 0.023 Uiso 1 1 calc R . . . .
 C8 C 1.0666(5) 0.6268(5) 0.3023(5) 0.0193(13) Uani 1 1 d . . . . .
 C9 C 0.9082(5) 0.8178(5) 0.1670(5) 0.0148(12) Uani 1 1 d . . . . .
 C10 C 0.8226(5) 0.8377(5) 0.1045(5) 0.0162(12) Uani 1 1 d . . . . .
 H10 H 0.8385 0.8314 0.0361 0.019 Uiso 1 1 calc R . . . .
 C11 C 0.7146(5) 0.8667(5) 0.1441(5) 0.0138(11) Uani 1 1 d . . . . .
 C12 C 0.6901(5) 0.8743(5) 0.2440(5) 0.0172(12) Uani 1 1 d . . . . .
 H12 H 0.6148 0.8934 0.2699 0.021 Uiso 1 1 calc R . . . .
 C13 C 0.7743(5) 0.8541(5) 0.3072(5) 0.0143(12) Uani 1 1 d . . . . .
 C14 C 0.8832(5) 0.8287(5) 0.2648(5) 0.0159(12) Uani 1 1 d . . . . .
 H14 H 0.9425 0.8185 0.3050 0.019 Uiso 1 1 calc R . . . .
 C15 C 0.6207(5) 0.8902(5) 0.0798(5) 0.0151(12) Uani 1 1 d . . . . .
 C16 C 0.7487(5) 0.8659(5) 0.4125(5) 0.0154(12) Uani 1 1 d . . . . .
 C17 C 0.6747(5) 0.9565(6) 0.4206(5) 0.0197(13) Uani 1 1 d . . . . .
 H17 H 0.6442 1.0134 0.3576 0.024 Uiso 1 1 calc R . . . .
 C18 C 0.6434(5) 0.9660(5) 0.5213(5) 0.0166(12) Uani 1 1 d . U . . .
 H18 H 0.5914 1.0288 0.5262 0.020 Uiso 1 1 calc R . . . .
 C19 C 0.6880(5) 0.8842(5) 0.6135(5) 0.0220(13) Uani 1 1 d . U . . .
 C20 C 0.7668(6) 0.7947(6) 0.6041(5) 0.0286(16) Uani 1 1 d . . . . .
 H20 H 0.8007 0.7406 0.6662 0.034 Uiso 1 1 calc R . . . .
 C21 C 0.7962(5) 0.7835(6) 0.5056(5) 0.0230(14) Uani 1 1 d . . . . .
 C22 C 0.8700(6) 0.6789(6) 0.5059(5) 0.0242(14) Uani 1 1 d . . . . .
 C23 C 0.6475(6) 0.8872(6) 0.7249(5) 0.0218(13) Uani 1 1 d . . . . .
 N1 N 1.6625(15) 0.6148(16) 0.0208(16) 0.145(5) Uani 1 1 d . U . . .
 H1A H 1.7062 0.6671 -0.0316 0.174 Uiso 1 1 calc R . . . .
 H1B H 1.5913 0.6499 0.0259 0.174 Uiso 1 1 calc R . . . .
 C24 C 1.706(3) 0.568(3) 0.126(3) 0.216(11) Uani 1 1 d . U . . .
 H24A H 1.7321 0.4850 0.1473 0.325 Uiso 1 1 calc GR . . . .
 H24B H 1.6470 0.5776 0.1821 0.325 Uiso 1 1 calc GR . . . .
 H24C H 1.7691 0.6088 0.1201 0.325 Uiso 1 1 calc GR . . . .
 C25 C 1.6654(17) 0.5120(18) -0.004(2) 0.137(6) Uani 1 1 d . U . . .
 H25A H 1.6705 0.5366 -0.0834 0.206 Uiso 1 1 calc GR . . . .
 H25B H 1.5970 0.4748 0.0312 0.206 Uiso 1 1 calc GR . . . .
 H25C H 1.7306 0.4568 0.0226 0.206 Uiso 1 1 calc GR . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.934(4) . ?
 Zn1 O5 1.927(4) 1_655 ?
 Zn1 O6 2.038(4) 2_775 ?
 Zn1 O7 1.982(4) 1_654 ?
 Zn1 C23 2.524(6) 1_654 ?
 Zn2 Zn2 3.0032(15) 2_766 ?
 Zn2 O3 2.042(4) . ?
 Zn2 O4 2.037(4) 2_766 ?
 Zn2 O9 2.035(5) 2_766 ?
 Zn2 O10 2.041(4) . ?
 Zn2 O11 1.958(5) . ?
 Zn2 H11A 2.1126 . ?
 Zn2 H11B 2.0626 . ?
 O1 C1 1.234(8) . ?
 O2 C1 1.252(8) . ?
 O3 C8 1.249(8) . ?
 O4 Zn2 2.037(4) 2_766 ?
 O4 C8 1.234(8) . ?
 O5 Zn1 1.927(4) 1_455 ?
 O5 C15 1.302(7) . ?
 O6 Zn1 2.038(4) 2_775 ?
 O6 C15 1.239(7) . ?
 O7 Zn1 1.982(4) 1_456 ?
 O7 C23 1.233(8) . ?
 O8 C23 1.227(8) . ?
 O9 Zn2 2.035(5) 2_766 ?
 O9 C22 1.240(9) . ?
 O10 C22 1.266(8) . ?
 O11 H11A 0.8775 . ?
 O11 H11B 0.8686 . ?
 C1 C2 1.518(8) . ?
 C2 C3 1.417(8) . ?
 C2 C7 1.363(8) . ?
 C3 H3 0.9500 . ?
 C3 C4 1.408(8) . ?
 C4 H4 0.9500 . ?
 C4 C5 1.379(8) . ?
 C5 C6 1.410(7) . ?
 C5 C9 1.501(7) . ?
 C6 C7 1.387(8) . ?
 C6 C8 1.502(9) . ?
 C7 H7 0.9500 . ?
 C9 C10 1.396(8) . ?
 C9 C14 1.371(8) . ?
 C10 H10 0.9500 . ?
 C10 C11 1.379(8) . ?
 C11 C12 1.379(8) . ?
 C11 C15 1.488(8) . ?
 C12 H12 0.9500 . ?
 C12 C13 1.388(8) . ?
 C13 C14 1.389(8) . ?
 C13 C16 1.475(8) . ?
 C14 H14 0.9500 . ?
 C16 C17 1.368(8) . ?
 C16 C21 1.411(8) . ?
 C17 H17 0.9500 . ?
 C17 C18 1.404(8) . ?
 C18 H18 0.9500 . ?
 C18 C19 1.386(9) . ?
 C19 C20 1.392(9) . ?
 C19 C23 1.520(9) . ?
 C20 H20 0.9500 . ?
 C20 C21 1.384(9) . ?
 C21 C22 1.474(9) . ?
 C23 Zn1 2.524(6) 1_456 ?
 N1 H1A 0.9100 . ?
 N1 H1B 0.9100 . ?
 N1 C24 1.47(3) . ?
 N1 C25 1.49(2) . ?
 C24 H24A 0.9800 . ?
 C24 H24B 0.9800 . ?
 C24 H24C 0.9800 . ?
 C25 H25A 0.9800 . ?
 C25 H25B 0.9800 . ?
 C25 H25C 0.9800 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O6 99.92(18) . 2_775 ?
 O1 Zn1 O7 107.08(19) . 1_654 ?
 O1 Zn1 C23 104.6(2) . 1_654 ?
 O5 Zn1 O1 123.52(18) 1_655 . ?
 O5 Zn1 O6 100.06(17) 1_655 2_775 ?
 O5 Zn1 O7 121.22(18) 1_655 1_654 ?
 O5 Zn1 C23 104.6(2) 1_655 1_654 ?
 O6 Zn1 C23 126.35(19) 2_775 1_654 ?
 O7 Zn1 O6 98.49(18) 1_654 2_775 ?
 O7 Zn1 C23 28.66(19) 1_654 1_654 ?
 Zn2 Zn2 H11A 153.6 2_766 . ?
 Zn2 Zn2 H11B 155.3 2_766 . ?
 O3 Zn2 Zn2 77.83(14) . 2_766 ?
 O3 Zn2 H11A 75.8 . . ?
 O3 Zn2 H11B 111.3 . . ?
 O4 Zn2 Zn2 80.03(14) 2_766 2_766 ?
 O4 Zn2 O3 157.9(2) 2_766 . ?
 O4 Zn2 O10 89.29(19) 2_766 . ?
 O4 Zn2 H11A 126.3 2_766 . ?
 O4 Zn2 H11B 88.8 2_766 . ?
 O9 Zn2 Zn2 78.12(16) 2_766 2_766 ?
 O9 Zn2 O3 87.8(2) 2_766 . ?
 O9 Zn2 O4 86.8(2) 2_766 2_766 ?
 O9 Zn2 O10 158.3(2) 2_766 . ?
 O9 Zn2 H11A 101.7 2_766 . ?
 O9 Zn2 H11B 79.4 2_766 . ?
 O10 Zn2 Zn2 80.19(15) . 2_766 ?
 O10 Zn2 O3 87.8(2) . . ?
 O10 Zn2 H11A 97.8 . . ?
 O10 Zn2 H11B 121.9 . . ?
 O11 Zn2 Zn2 177.9(2) . 2_766 ?
 O11 Zn2 O3 100.3(2) . . ?
 O11 Zn2 O4 101.9(2) . 2_766 ?
 O11 Zn2 O9 101.0(3) . 2_766 ?
 O11 Zn2 O10 100.6(2) . . ?
 O11 Zn2 H11A 24.5 . . ?
 O11 Zn2 H11B 24.8 . . ?
 H11A Zn2 H11B 43.1 . . ?
 C1 O1 Zn1 125.3(4) . . ?
 C8 O3 Zn2 128.5(4) . . ?
 C8 O4 Zn2 126.2(4) . 2_766 ?
 C15 O5 Zn1 120.1(4) . 1_455 ?
 C15 O6 Zn1 125.3(4) . 2_775 ?
 C23 O7 Zn1 100.9(4) . 1_456 ?
 C22 O9 Zn2 129.5(4) . 2_766 ?
 C22 O10 Zn2 125.8(4) . . ?
 Zn2 O11 H11A 87.6 . . ?
 Zn2 O11 H11B 84.3 . . ?
 H11A O11 H11B 122.8 . . ?
 O1 C1 O2 127.3(6) . . ?
 O1 C1 C2 115.6(5) . . ?
 O2 C1 C2 117.0(6) . . ?
 C3 C2 C1 117.0(5) . . ?
 C7 C2 C1 121.6(5) . . ?
 C7 C2 C3 121.2(5) . . ?
 C2 C3 H3 121.8 . . ?
 C4 C3 C2 116.5(5) . . ?
 C4 C3 H3 121.8 . . ?
 C3 C4 H4 118.7 . . ?
 C5 C4 C3 122.6(5) . . ?
 C5 C4 H4 118.7 . . ?
 C4 C5 C6 118.9(5) . . ?
 C4 C5 C9 119.9(5) . . ?
 C6 C5 C9 121.2(5) . . ?
 C5 C6 C8 122.4(5) . . ?
 C7 C6 C5 119.1(5) . . ?
 C7 C6 C8 118.5(5) . . ?
 C2 C7 C6 121.5(5) . . ?
 C2 C7 H7 119.2 . . ?
 C6 C7 H7 119.2 . . ?
 O3 C8 C6 116.2(6) . . ?
 O4 C8 O3 126.8(6) . . ?
 O4 C8 C6 116.9(6) . . ?
 C10 C9 C5 119.4(5) . . ?
 C14 C9 C5 120.9(5) . . ?
 C14 C9 C10 119.5(5) . . ?
 C9 C10 H10 120.7 . . ?
 C11 C10 C9 118.6(5) . . ?
 C11 C10 H10 120.7 . . ?
 C10 C11 C12 121.3(5) . . ?
 C10 C11 C15 120.6(5) . . ?
 C12 C11 C15 118.1(5) . . ?
 C11 C12 H12 119.7 . . ?
 C11 C12 C13 120.7(5) . . ?
 C13 C12 H12 119.7 . . ?
 C12 C13 C14 117.4(5) . . ?
 C12 C13 C16 120.7(5) . . ?
 C14 C13 C16 121.8(5) . . ?
 C9 C14 C13 122.4(5) . . ?
 C9 C14 H14 118.8 . . ?
 C13 C14 H14 118.8 . . ?
 O5 C15 C11 115.1(5) . . ?
 O6 C15 O5 122.5(5) . . ?
 O6 C15 C11 122.4(5) . . ?
 C17 C16 C13 119.3(5) . . ?
 C17 C16 C21 119.5(5) . . ?
 C21 C16 C13 121.2(5) . . ?
 C16 C17 H17 119.7 . . ?
 C16 C17 C18 120.5(5) . . ?
 C18 C17 H17 119.7 . . ?
 C17 C18 H18 119.8 . . ?
 C19 C18 C17 120.3(5) . . ?
 C19 C18 H18 119.8 . . ?
 C18 C19 C20 119.0(6) . . ?
 C18 C19 C23 120.9(5) . . ?
 C20 C19 C23 119.9(6) . . ?
 C19 C20 H20 119.6 . . ?
 C21 C20 C19 120.8(6) . . ?
 C21 C20 H20 119.6 . . ?
 C16 C21 C22 123.0(5) . . ?
 C20 C21 C16 119.7(6) . . ?
 C20 C21 C22 117.1(5) . . ?
 O9 C22 O10 126.3(6) . . ?
 O9 C22 C21 117.6(6) . . ?
 O10 C22 C21 116.0(6) . . ?
 O7 C23 Zn1 50.4(3) . 1_456 ?
 O7 C23 C19 117.4(5) . . ?
 O8 C23 Zn1 74.4(4) . 1_456 ?
 O8 C23 O7 124.7(6) . . ?
 O8 C23 C19 117.8(6) . . ?
 C19 C23 Zn1 165.9(5) . 1_456 ?
 H1A N1 H1B 108.9 . . ?
 C24 N1 H1A 110.8 . . ?
 C24 N1 H1B 110.9 . . ?
 C24 N1 C25 104.5(19) . . ?
 C25 N1 H1A 110.9 . . ?
 C25 N1 H1B 110.9 . . ?
 N1 C24 H24A 109.5 . . ?
 N1 C24 H24B 109.5 . . ?
 N1 C24 H24C 109.5 . . ?
 H24A C24 H24B 109.5 . . ?
 H24A C24 H24C 109.5 . . ?
 H24B C24 H24C 109.5 . . ?
 N1 C25 H25A 109.5 . . ?
 N1 C25 H25B 109.5 . . ?
 N1 C25 H25C 109.5 . . ?
 H25A C25 H25B 109.5 . . ?
 H25A C25 H25C 109.5 . . ?
 H25B C25 H25C 109.5 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 O2 -31.3(10) . . . . ?
 Zn1 O1 C1 C2 146.3(4) . . . . ?
 Zn1 O5 C15 O6 9.6(8) 1_455 . . . ?
 Zn1 O5 C15 C11 -171.7(4) 1_455 . . . ?
 Zn1 O6 C15 O5 -106.1(6) 2_775 . . . ?
 Zn1 O6 C15 C11 75.3(7) 2_775 . . . ?
 Zn1 O7 C23 O8 -4.4(8) 1_456 . . . ?
 Zn1 O7 C23 C19 171.6(5) 1_456 . . . ?
 Zn2 O3 C8 O4 -10.8(9) . . . . ?
 Zn2 O3 C8 C6 172.0(4) . . . . ?
 Zn2 O4 C8 O3 9.1(9) 2_766 . . . ?
 Zn2 O4 C8 C6 -173.7(3) 2_766 . . . ?
 Zn2 O9 C22 O10 -3.7(10) 2_766 . . . ?
 Zn2 O9 C22 C21 177.0(4) 2_766 . . . ?
 Zn2 O10 C22 O9 3.8(10) . . . . ?
 Zn2 O10 C22 C21 -176.9(4) . . . . ?
 O1 C1 C2 C3 10.3(8) . . . . ?
 O1 C1 C2 C7 -164.0(6) . . . . ?
 O2 C1 C2 C3 -171.9(6) . . . . ?
 O2 C1 C2 C7 13.8(9) . . . . ?
 C1 C2 C3 C4 -174.9(5) . . . . ?
 C1 C2 C7 C6 172.2(6) . . . . ?
 C2 C3 C4 C5 5.1(9) . . . . ?
 C3 C2 C7 C6 -1.9(9) . . . . ?
 C3 C4 C5 C6 -7.0(9) . . . . ?
 C3 C4 C5 C9 170.1(5) . . . . ?
 C4 C5 C6 C7 4.3(8) . . . . ?
 C4 C5 C6 C8 -175.7(5) . . . . ?
 C4 C5 C9 C10 44.3(8) . . . . ?
 C4 C5 C9 C14 -130.5(6) . . . . ?
 C5 C6 C7 C2 0.0(9) . . . . ?
 C5 C6 C8 O3 -129.0(6) . . . . ?
 C5 C6 C8 O4 53.5(8) . . . . ?
 C5 C9 C10 C11 -175.6(5) . . . . ?
 C5 C9 C14 C13 177.7(5) . . . . ?
 C6 C5 C9 C10 -138.7(6) . . . . ?
 C6 C5 C9 C14 46.5(8) . . . . ?
 C7 C2 C3 C4 -0.6(9) . . . . ?
 C7 C6 C8 O3 51.0(8) . . . . ?
 C7 C6 C8 O4 -126.5(6) . . . . ?
 C8 C6 C7 C2 -179.9(6) . . . . ?
 C9 C5 C6 C7 -172.7(5) . . . . ?
 C9 C5 C6 C8 7.2(8) . . . . ?
 C9 C10 C11 C12 -1.1(9) . . . . ?
 C9 C10 C11 C15 179.3(5) . . . . ?
 C10 C9 C14 C13 2.9(9) . . . . ?
 C10 C11 C12 C13 0.8(9) . . . . ?
 C10 C11 C15 O5 1.5(8) . . . . ?
 C10 C11 C15 O6 -179.9(6) . . . . ?
 C11 C12 C13 C14 1.3(9) . . . . ?
 C11 C12 C13 C16 178.0(5) . . . . ?
 C12 C11 C15 O5 -178.1(5) . . . . ?
 C12 C11 C15 O6 0.5(9) . . . . ?
 C12 C13 C14 C9 -3.2(9) . . . . ?
 C12 C13 C16 C17 -41.4(9) . . . . ?
 C12 C13 C16 C21 136.5(6) . . . . ?
 C13 C16 C17 C18 176.1(6) . . . . ?
 C13 C16 C21 C20 -177.4(6) . . . . ?
 C13 C16 C21 C22 -2.5(10) . . . . ?
 C14 C9 C10 C11 -0.7(9) . . . . ?
 C14 C13 C16 C17 135.2(6) . . . . ?
 C14 C13 C16 C21 -46.9(9) . . . . ?
 C15 C11 C12 C13 -179.5(6) . . . . ?
 C16 C13 C14 C9 -179.9(5) . . . . ?
 C16 C17 C18 C19 0.6(10) . . . . ?
 C16 C21 C22 O9 -55.6(9) . . . . ?
 C16 C21 C22 O10 125.0(7) . . . . ?
 C17 C16 C21 C20 0.5(10) . . . . ?
 C17 C16 C21 C22 175.4(6) . . . . ?
 C17 C18 C19 C20 2.0(10) . . . . ?
 C17 C18 C19 C23 -174.6(6) . . . . ?
 C18 C19 C20 C21 -3.4(11) . . . . ?
 C18 C19 C23 Zn1 15(2) . . . 1_456 ?
 C18 C19 C23 O7 -12.5(9) . . . . ?
 C18 C19 C23 O8 163.8(7) . . . . ?
 C19 C20 C21 C16 2.1(11) . . . . ?
 C19 C20 C21 C22 -173.0(7) . . . . ?
 C20 C19 C23 Zn1 -161.4(16) . . . 1_456 ?
 C20 C19 C23 O7 171.0(6) . . . . ?
 C20 C19 C23 O8 -12.7(10) . . . . ?
 C20 C21 C22 O9 119.4(7) . . . . ?
 C20 C21 C22 O10 -60.0(9) . . . . ?
 C21 C16 C17 C18 -1.8(9) . . . . ?
 C23 C19 C20 C21 173.3(7) . . . . ?

# SQUEEZE RESULTS (Version = 191016)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.027  0.031  0.442       840       233 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
  _platon_missing_refln_index_h
  _platon_missing_refln_index_k
  _platon_missing_refln_index_l
  _platon_missing_refln_theta
   -2    1    0     4.014
    0    2    0     3.530
    4    3    0     8.166
    1    5    0     8.824
   -1   -4    1     7.953
    0   -4    1     7.896
    1   -4    1     8.205
    2   -4    1     8.843
   -3   -3    1     7.767
   -1   -3    1     6.289
   -2   -2    1     5.506
   -1   -1    1     3.343
    2    0    1     3.598
    0    1    1     1.875
   -3    2    1     6.562
    3    2    1     5.518
    0    3    1     4.873
    4    3    1     7.708
    0    4    1     6.580
    3    4    1     7.696
   -3   -3    2     8.835
   -2   -2    2     6.697
    1    0    2     3.538
    2    1    2     4.103
   -3    2    2     6.988
   -2    2    2     5.602
    3    2    2     5.646
   -4    3    2     9.276
    4    3    2     7.598
    5    3    2     8.983
   -2    4    2     7.894
    0    4    2     6.492
    3    5    2     8.799
   -3   -3    3    10.075
   -2   -3    3     9.306
    2   -3    3     9.282
   -2   -2    3     8.064
   -1   -1    3     6.288
   -1    0    3     5.475
    2    1    3     5.185
    4    2    3     7.470
   -2    3    3     7.206
    5    3    3     9.158
   -2    4    3     8.259
    0    4    3     6.824
    3    5    3     8.791
   -2   -1    4     8.556
   -3    1    4     8.672
    2    1    4     6.520
    3    2    4     7.170
    4    2    4     8.227
   -2    3    4     8.110
   -3    4    4    10.010
   -2    0    5     9.411
    2    0    5     8.599
   -1    4    5     9.031
    2    0    6    10.168
    2    5    6    10.183
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details
;
TITL 1_sq      P -1         R = 0.11
CELL   12.2520   12.8200   13.6350     65.01     79.06     79.55
SPGR P-1
# Solvent Accessible Volume =       836
# Electrons Found in S.A.V. =       233
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.466 0.324 0.348 !       3.83 eA-3
Q102 0.607 0.533 0.372 !       3.71 eA-3
C103 0.144 0.879 0.411 !       3.57 eA-3
C104 0.415 0.669 0.328 !       3.57 eA-3
C105 0.486 0.671 0.406 !       3.52 eA-3
C106 0.160 0.963 0.217 !       3.40 eA-3
C107 0.100 0.967 0.325 !       3.37 eA-3
C108 0.383 0.421 0.278 !       3.18 eA-3
C109 0.467 0.318 0.438 !       3.14 eA-3
C110 0.285 0.817 0.317 !       2.95 eA-3
C111 0.455 0.753 0.454 !       2.94 eA-3
Q112 0.667 0.625 0.013 !       2.94 eA-3
C113 0.525 0.237 0.506 !       2.79 eA-3
C114 0.578 0.590 0.425 !       2.50 eA-3
C115 0.551 0.284 0.283 !       2.42 eA-3
C116 0.192 0.894 0.313 !       2.38 eA-3
Q117 0.690 0.471 0.377 !       2.29 eA-3
Q118 0.097 0.372 0.012 !       2.15 eA-3
C119 0.984 0.424 0.113 !       2.13 eA-3
C120 0.019 0.402 0.185 !       2.04 eA-3
C121 0.328 0.746 0.406 !       2.03 eA-3
C122 0.401 0.784 0.308 !       1.99 eA-3
C123 0.996 0.323 0.232 !       1.99 eA-3
Q124 0.671 0.476 0.298 !       1.93 eA-3
Q125 0.748 0.520 0.328 !       1.91 eA-3
Q126 0.469 0.134 0.112 !       1.87 eA-3
C127 0.965 0.386 0.041 !       1.83 eA-3
C128 0.186 0.830 0.474 !       1.79 eA-3
C129 0.953 0.543 0.063 !       1.67 eA-3
Q130 0.437 0.084 0.079 !       1.56 eA-3
Q131 0.934 0.499 0.472 !       1.55 eA-3
C132 0.535 0.294 0.368 !       1.54 eA-3
C133 0.971 0.371 0.140 !       1.53 eA-3
Q134 0.455 0.058 0.198 !       1.50 eA-3
C135 0.952 0.365 0.107 !       1.47 eA-3
C136 0.437 0.394 0.215 !       1.43 eA-3
C137 0.391 0.448 0.351 !       1.42 eA-3
C138 0.027 0.494 0.093 !       1.35 eA-3
C139 1.001 0.220 0.220 !       1.35 eA-3
C140 0.530 0.466 0.393 !       1.33 eA-3
C141 0.061 0.140 0.233 !       1.31 eA-3
Q142 0.621 0.609 0.487 !       1.30 eA-3
C143 0.855 0.203 0.268 !       1.30 eA-3
C144 0.416 0.355 0.482 !       1.29 eA-3
C145 0.030 0.553 0.009 !       1.28 eA-3
C146 0.935 0.304 0.184 !       1.26 eA-3
C147 0.799 0.274 0.305 !       1.25 eA-3
C148 0.980 0.197 0.280 !       1.24 eA-3
Q149 0.896 0.466 0.430 !       1.23 eA-3
C150 0.913 0.321 0.097 !       1.22 eA-3
Q151 0.432 0.996 0.280 !       1.21 eA-3
Q152 0.454 0.823 0.043 !       1.19 eA-3
Q153 0.500 1.000 0.000 !       1.19 eA-3
Q154 0.512 0.939 0.058 !       1.19 eA-3
Q155 0.876 0.406 0.486 !       1.17 eA-3
C156 0.033 0.071 0.301 !       1.16 eA-3
C157 0.487 0.522 0.373 !       1.16 eA-3
C158 0.513 0.360 0.237 !       1.16 eA-3
C159 0.059 0.262 0.225 !       1.16 eA-3
C160 0.943 0.062 0.405 !       1.15 eA-3
C161 1.002 0.030 0.344 !       1.14 eA-3
C162 0.975 0.082 0.422 !       1.12 eA-3
Q163 0.112 0.627 0.402 !       1.12 eA-3
C164 0.707 0.249 0.270 !       1.12 eA-3
Q165 0.968 0.455 0.245 !       1.10 eA-3
Q166 0.465 0.765 0.297 !       1.10 eA-3
Q167 0.143 0.668 0.378 !       1.10 eA-3
Q168 0.331 0.301 0.471 !       1.09 eA-3
C169 0.098 0.369 0.112 !       1.08 eA-3
C170 0.606 0.208 0.334 !       1.08 eA-3
Q171 0.752 0.608 0.039 !       1.07 eA-3
Q172 0.327 0.908 0.227 !       1.07 eA-3
Q173 0.861 0.222 0.467 !       1.05 eA-3
Q174 0.575 0.927 0.096 !       1.05 eA-3
Q175 0.311 0.089 0.416 !       1.05 eA-3
Q176 0.108 0.554 0.442 !       1.05 eA-3
Q177 0.985 0.345 0.377 !       1.05 eA-3
Q178 0.705 0.217 0.068 !       1.05 eA-3
Q179 0.099 0.563 0.482 !       1.04 eA-3
Q180 0.659 0.571 0.081 !       1.03 eA-3
C181 0.834 0.314 0.135 !       1.01 eA-3
Q182 0.358 0.083 0.155 !       1.00 eA-3
Q183 0.891 0.831 0.222 !       0.99 eA-3
C184 0.909 0.099 0.470 !       0.99 eA-3
Q185 0.908 0.811 0.262 !       0.98 eA-3
C186 0.061 0.251 0.167 !       0.98 eA-3
Q187 0.135 0.335 0.156 !       0.97 eA-3
Q188 0.514 0.578 0.062 !       0.97 eA-3
Q189 0.715 0.883 0.168 !       0.96 eA-3
C190 0.123 0.897 0.484 !       0.96 eA-3
C191 0.541 0.329 0.465 !       0.96 eA-3
Q192 0.278 0.107 0.346 !       0.95 eA-3
Q193 0.189 0.083 0.297 !       0.95 eA-3
C194 0.886 0.175 0.453 !       0.95 eA-3
Q195 0.473 0.703 0.060 !       0.94 eA-3
C196 0.920 0.061 0.328 !       0.94 eA-3
Q197 0.732 0.455 0.431 !       0.93 eA-3
Q198 0.441 0.295 0.256 !       0.93 eA-3
Q199 0.788 0.220 0.407 !       0.93 eA-3

;
_shelx_SHELXL_version_number      '2014/7'

_olex2_submission_special_instructions 'No special instructions were received'
data_3
_audit_creation_date              2016-12-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          '0.25(C184 H160 Co20 O124), 2(H2 O)'
_chemical_formula_sum             'C46 H44 Co5 O33'
_chemical_formula_weight          1419.46
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0030 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'
 'Co' 'Co' 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system       'monoclinic'
_space_group_IT_number            15
_space_group_name_H-M_alt         'C 1 2/c 1'
_space_group_name_Hall            '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                    35.966(6)
_cell_length_b                    7.1675(12)
_cell_length_c                    22.077(4)
_cell_angle_alpha                 90
_cell_angle_beta                  115.480(2)
_cell_angle_gamma                 90
_cell_volume                      5137.6(15)
_cell_formula_units_Z             4
_cell_measurement_reflns_used     1674
_cell_measurement_temperature     100
_cell_measurement_theta_max       25.331
_cell_measurement_theta_min       2.821
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     1.688
_exptl_absorpt_correction_T_max   0.7457
_exptl_absorpt_correction_T_min   0.5979
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0791 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.8018.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             colourless
_exptl_crystal_colour_primary     colourless
_exptl_crystal_density_diffrn     1.835
_exptl_crystal_density_meas       .
_exptl_crystal_density_method     ?
_exptl_crystal_description        block
_exptl_crystal_F_000              2876
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0738
_diffrn_reflns_av_unetI/netI      0.0981
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max        41
_diffrn_reflns_limit_h_min        -44
_diffrn_reflns_limit_k_max        4
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_limit_l_min        -27
_diffrn_reflns_number             13569
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          26.372
_diffrn_reflns_theta_min          1.254
_diffrn_ambient_temperature       100
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_radiation_monochromator   'graphite'
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    ?
_diffrn_standards_number          0
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 3225
_reflns_number_total              5189
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        'SAINT V8.18C (?, 2016)'
_computing_data_collection        ?
_computing_data_reduction         'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max          1.481
_refine_diff_density_min          -1.165
_refine_diff_density_rms          0.197
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.062
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      399
_refine_ls_number_reflns          5189
_refine_ls_number_restraints      129
_refine_ls_R_factor_all           0.1346
_refine_ls_R_factor_gt            0.0812
_refine_ls_restrained_S_all       1.064
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1592P)²+27.2704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.2305
_refine_ls_wR_factor_ref          0.2784
_refine_special_details           ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 Co1A, Co1, O1, O2, O16A, O16, C1, C2, C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Co1A)=Sof(O16)=Sof(H16C)=Sof(H16D)=0.5*(1-FVAR(2))
 Sof(Co1)=Sof(O16A)=Sof(H16A)=Sof(H16B)=0.5*FVAR(2)
5.a Riding coordinates:
 O6(H6A,H6B), O11(H11A,H11B), O13(H13A,H13B), O14(H14A,H14B), O16A(H16A,H16B),
 O16(H16C,H16D), O17(H17A,H17B)
5.b Rotating group:
 O10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C10(H10), C13(H13), C18(H18), C21(H21), C22(H22),
 C23(H23)
;
_atom_sites_solution_hydrogens    mixed
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Co1A Co 0.5000 0.3900(11) 0.7500 0.0266(18) Uani 0.388(11) 2 d S TU P A 2
 Co1 Co 0.5000 0.2542(11) 0.7500 0.049(2) Uani 0.612(11) 2 d S TU P A 1
 Co4 Co 0.7500 1.2500 0.5000 0.0183(4) Uani 1 2 d S T P . .
 Co3 Co 0.85772(3) 0.27201(18) 0.53664(5) 0.0260(4) Uani 1 1 d . . . . .
 Co2 Co 1.0000 0.5000 1.0000 0.0238(4) Uani 1 2 d S T P . .
 O1 O 0.5586(2) 0.4195(15) 0.7799(3) 0.064(2) Uani 1 1 d . U . . .
 O2 O 0.5198(2) 0.3484(14) 0.6750(3) 0.062(2) Uani 1 1 d . U . . .
 O3 O 0.63438(17) 0.3467(9) 0.5408(3) 0.0284(14) Uani 1 1 d . . . . .
 O4 O 0.5755(2) 0.5031(11) 0.4991(3) 0.0445(19) Uani 1 1 d . . . . .
 O5 O 0.74040(19) 1.0203(9) 0.5463(3) 0.0390(17) Uani 1 1 d . . . . .
 O6 O 0.80189(17) 1.0960(9) 0.4996(3) 0.0275(14) Uani 1 1 d . . . . .
 H6A H 0.8015 1.0575 0.4642 0.041 Uiso 1 1 d R . . . .
 H6B H 0.8065 1.0164 0.5310 0.041 Uiso 1 1 d R . . . .
 O7 O 0.67371(18) 1.0139(10) 0.5222(4) 0.0436(19) Uani 1 1 d . . . . .
 O8 O 0.78348(18) 0.3592(10) 0.5945(3) 0.0352(16) Uani 1 1 d . . . . .
 O9 O 0.8497(2) 0.3568(14) 0.6164(3) 0.058(3) Uani 1 1 d . . . . .
 O10 O 0.8983(3) 0.0587(13) 0.5961(4) 0.062(2) Uani 1 1 d . U . . .
 H10A H 0.9191 0.0462 0.5859 0.094 Uiso 1 1 d GR . . . .
 H10B H 0.8856 -0.0492 0.5895 0.094 Uiso 1 1 d GR . . . .
 O11 O 0.9089(3) 0.4611(15) 0.5668(5) 0.082(3) Uani 1 1 d . U . . .
 H11A H 0.9117 0.5583 0.5969 0.124 Uiso 1 1 d R . . . .
 H11B H 0.9335 0.4072 0.5702 0.124 Uiso 1 1 d R . . . .
 O12 O 0.94342(18) 0.4856(10) 0.9212(3) 0.0342(15) Uani 1 1 d . . . . .
 O13 O 0.97525(18) 0.6750(10) 1.0536(3) 0.0354(15) Uani 1 1 d . . . . .
 H13A H 0.9969 0.6920 1.0881 0.053 Uiso 1 1 d R . . . .
 H13B H 0.9760 0.7793 1.0320 0.053 Uiso 1 1 d R . . . .
 O14 O 0.9849(2) 0.2672(11) 1.0425(3) 0.050(2) Uani 1 1 d . . . . .
 H14A H 0.9954 0.2786 1.0855 0.075 Uiso 1 1 d R . . . .
 H14B H 0.9656 0.1857 1.0312 0.075 Uiso 1 1 d R . . . .
 O15 O 0.95751(19) 0.3851(15) 0.8389(3) 0.062(3) Uani 1 1 d . . . . .
 O16A O 0.5423(7) 0.046(4) 0.7913(14) 0.061(6) Uani 0.306(5) 1 d . U . A 1
 H16A H 0.5444 -0.0161 0.7601 0.092 Uiso 0.306(5) 1 d R . . A 1
 H16B H 0.5348 -0.0256 0.8146 0.092 Uiso 0.306(5) 1 d R . . A 1
 O16 O 0.5000 0.692(6) 0.7500 0.107(10) Uani 0.388(11) 2 d S TU P A 2
 H16C H 0.5115 0.7319 0.7259 0.161 Uiso 0.194(5) 1 d R . . A 2
 H16D H 0.5132 0.7319 0.7899 0.161 Uiso 0.194(5) 1 d R . . A 2
 C1 C 0.5538(3) 0.4014(16) 0.7186(4) 0.039(2) Uani 1 1 d . U . . .
 C2 C 0.5894(3) 0.4473(15) 0.7035(4) 0.033(2) Uani 1 1 d . U . . .
 C3 C 0.5821(3) 0.4509(13) 0.6337(4) 0.0256(18) Uani 1 1 d . U . . .
 H3 H 0.5553 0.4314 0.5989 0.031 Uiso 1 1 calc R . . . .
 C4 C 0.6156(2) 0.4838(12) 0.6191(3) 0.0199(16) Uani 1 1 d . U . . .
 C5 C 0.6079(3) 0.4458(13) 0.5479(4) 0.0246(19) Uani 1 1 d . U . . .
 C6 C 0.6547(2) 0.5217(11) 0.6687(4) 0.0204(16) Uani 1 1 d . U . . .
 C7 C 0.6604(3) 0.5137(12) 0.7362(4) 0.0238(18) Uani 1 1 d . U . . .
 H7 H 0.6869 0.5350 0.7716 0.029 Uiso 1 1 calc R . . . .
 C8 C 0.6275(3) 0.4753(14) 0.7507(4) 0.032(2) Uani 1 1 d . U . . .
 H8 H 0.6323 0.4683 0.7964 0.039 Uiso 1 1 calc R . . . .
 C9 C 0.6897(2) 0.5819(11) 0.6543(4) 0.0186(16) Uani 1 1 d . . . . .
 C10 C 0.6837(2) 0.7190(11) 0.6075(4) 0.0201(17) Uani 1 1 d . . . . .
 H10 H 0.6567 0.7656 0.5819 0.024 Uiso 1 1 calc R . . . .
 C11 C 0.7164(2) 0.7916(11) 0.5967(4) 0.0205(17) Uani 1 1 d . . . . .
 C12 C 0.7100(3) 0.9542(12) 0.5528(4) 0.0231(18) Uani 1 1 d . . . . .
 C13 C 0.7561(2) 0.7224(12) 0.6352(4) 0.0224(18) Uani 1 1 d . . . . .
 H13 H 0.7787 0.7721 0.6292 0.027 Uiso 1 1 calc R . . . .
 C14 C 0.7626(2) 0.5827(12) 0.6817(4) 0.0196(17) Uani 1 1 d . . . . .
 C15 C 0.8055(2) 0.5247(12) 0.7257(4) 0.0193(17) Uani 1 1 d . . . . .
 C16 C 0.8336(2) 0.4524(11) 0.7016(3) 0.0178(16) Uani 1 1 d . . . . .
 C17 C 0.8207(2) 0.3847(13) 0.6312(3) 0.0222(18) Uani 1 1 d . . . . .
 C18 C 0.8744(2) 0.4306(13) 0.7474(4) 0.0240(18) Uani 1 1 d . . . . .
 H18 H 0.8934 0.3862 0.7313 0.029 Uiso 1 1 calc R . . . .
 C19 C 0.8888(2) 0.4692(12) 0.8141(4) 0.0243(18) Uani 1 1 d . . . . .
 C20 C 0.9329(3) 0.4435(14) 0.8604(4) 0.030(2) Uani 1 1 d . . . . .
 C21 C 0.8606(2) 0.5328(12) 0.8386(4) 0.0230(18) Uani 1 1 d . . . . .
 H21 H 0.8695 0.5579 0.8850 0.028 Uiso 1 1 calc R . . . .
 C22 C 0.8210(2) 0.5571(12) 0.7951(4) 0.0210(17) Uani 1 1 d . . . . .
 H22 H 0.8023 0.5986 0.8123 0.025 Uiso 1 1 calc R . . . .
 C23 C 0.7296(3) 0.5138(12) 0.6924(4) 0.0233(18) Uani 1 1 d . . . . .
 H23 H 0.7342 0.4208 0.7255 0.028 Uiso 1 1 calc R . . . .
 O17 O 0.3362(4) 0.2951(14) 0.5795(5) 0.105(4) Uani 1 1 d . . . . .
 H17A H 0.3291 0.2361 0.5443 0.158 Uiso 1 1 d R . . . .
 H17B H 0.3461 0.1849 0.6115 0.158 Uiso 1 1 d R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Co1A O1 1.928(7) 2_656 ?
 Co1A O1 1.929(7) . ?
 Co1A O2 2.086(6) . ?
 Co1A O2 2.086(6) 2_656 ?
 Co1A O16 2.17(4) . ?
 Co1A C1 2.320(9) . ?
 Co1A C1 2.320(9) 2_656 ?
 Co1 O1 2.254(9) . ?
 Co1 O1 2.254(9) 2_656 ?
 Co1 O2 2.172(7) 2_656 ?
 Co1 O2 2.173(7) . ?
 Co1 O16A 2.04(3) 2_656 ?
 Co1 O16A 2.04(3) . ?
 Co4 O5 2.044(6) 7_676 ?
 Co4 O5 2.044(6) . ?
 Co4 O6 2.172(6) . ?
 Co4 O6 2.172(6) 7_676 ?
 Co4 O8 2.063(6) 7_666 ?
 Co4 O8 2.063(6) 1_565 ?
 Co3 O3 2.036(5) 7_656 ?
 Co3 O6 2.209(6) 1_545 ?
 Co3 O7 2.015(6) 7_666 ?
 Co3 O9 1.997(6) . ?
 Co3 O10 2.131(8) . ?
 Co3 O11 2.148(10) . ?
 Co2 O12 2.033(6) . ?
 Co2 O12 2.033(6) 5_767 ?
 Co2 O13 2.162(6) . ?
 Co2 O13 2.162(6) 5_767 ?
 Co2 O14 2.097(7) 5_767 ?
 Co2 O14 2.097(7) . ?
 O1 C1 1.295(10) . ?
 O2 C1 1.247(11) . ?
 O3 Co3 2.036(5) 7_656 ?
 O3 C5 1.251(10) . ?
 O4 C5 1.269(10) . ?
 O5 C12 1.256(10) . ?
 O6 Co3 2.209(6) 1_565 ?
 O6 H6A 0.8217 . ?
 O6 H6B 0.8567 . ?
 O7 Co3 2.015(6) 7_666 ?
 O7 C12 1.259(10) . ?
 O8 Co4 2.063(6) 1_545 ?
 O8 C17 1.243(10) . ?
 O9 C17 1.236(10) . ?
 O10 H10A 0.8757 . ?
 O10 H10B 0.8769 . ?
 O11 H11A 0.9392 . ?
 O11 H11B 0.9372 . ?
 O12 C20 1.264(10) . ?
 O13 H13A 0.8308 . ?
 O13 H13B 0.8941 . ?
 O14 H14A 0.8616 . ?
 O14 H14B 0.8575 . ?
 O15 C20 1.245(11) . ?
 O16A H16A 0.8498 . ?
 O16A H16B 0.8502 . ?
 O16 H16C 0.8499 . ?
 O16 H16D 0.8500 . ?
 C1 C2 1.492(12) . ?
 C2 C3 1.447(11) . ?
 C2 C8 1.334(12) . ?
 C3 H3 0.9500 . ?
 C3 C4 1.395(11) . ?
 C4 C5 1.499(9) . ?
 C4 C6 1.388(11) . ?
 C6 C7 1.417(10) . ?
 C6 C9 1.487(11) . ?
 C7 H7 0.9500 . ?
 C7 C8 1.378(12) . ?
 C8 H8 0.9500 . ?
 C9 C10 1.374(11) . ?
 C9 C23 1.403(11) . ?
 C10 H10 0.9500 . ?
 C10 C11 1.395(11) . ?
 C11 C12 1.469(11) . ?
 C11 C13 1.401(11) . ?
 C13 H13 0.9500 . ?
 C13 C14 1.380(11) . ?
 C14 C15 1.486(11) . ?
 C14 C23 1.398(11) . ?
 C15 C16 1.424(11) . ?
 C15 C22 1.407(10) . ?
 C16 C17 1.500(10) . ?
 C16 C18 1.387(11) . ?
 C18 H18 0.9500 . ?
 C18 C19 1.363(11) . ?
 C19 C20 1.482(11) . ?
 C19 C21 1.415(11) . ?
 C21 H21 0.9500 . ?
 C21 C22 1.342(11) . ?
 C22 H22 0.9500 . ?
 C23 H23 0.9500 . ?
 O17 H17A 0.8219 . ?
 O17 H17B 1.0172 . ?

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 Co1A O1 167.4(8) 2_656 . ?
 O1 Co1A O2 66.0(3) 2_656 2_656 ?
 O1 Co1A O2 116.0(3) . 2_656 ?
 O1 Co1A O2 116.0(3) 2_656 . ?
 O1 Co1A O2 66.0(3) . . ?
 O1 Co1A O16 83.7(4) . . ?
 O1 Co1A O16 83.7(4) 2_656 . ?
 O1 Co1A C1 33.9(3) . . ?
 O1 Co1A C1 145.3(3) 2_656 . ?
 O1 Co1A C1 145.3(3) . 2_656 ?
 O1 Co1A C1 33.9(3) 2_656 2_656 ?
 O2 Co1A O2 163.6(7) . 2_656 ?
 O2 Co1A O16 98.2(4) . . ?
 O2 Co1A O16 98.2(4) 2_656 . ?
 O2 Co1A C1 148.8(3) 2_656 . ?
 O2 Co1A C1 32.3(3) . . ?
 O2 Co1A C1 32.3(3) 2_656 2_656 ?
 O2 Co1A C1 148.8(3) . 2_656 ?
 O16 Co1A C1 88.0(4) . 2_656 ?
 O16 Co1A C1 88.0(4) . . ?
 C1 Co1A C1 175.9(7) 2_656 . ?
 O1 Co1 O1 116.6(6) 2_656 . ?
 O2 Co1 O1 59.3(3) . . ?
 O2 Co1 O1 100.6(4) . 2_656 ?
 O2 Co1 O1 100.6(4) 2_656 . ?
 O2 Co1 O1 59.3(3) 2_656 2_656 ?
 O2 Co1 O2 143.8(7) 2_656 . ?
 O16A Co1 O1 80.2(8) 2_656 2_656 ?
 O16A Co1 O1 80.2(8) . . ?
 O16A Co1 O1 159.6(7) . 2_656 ?
 O16A Co1 O1 159.6(7) 2_656 . ?
 O16A Co1 O2 108.2(8) 2_656 . ?
 O16A Co1 O2 98.1(7) 2_656 2_656 ?
 O16A Co1 O2 108.2(8) . 2_656 ?
 O16A Co1 O2 98.1(7) . . ?
 O16A Co1 O16A 86.4(16) . 2_656 ?
 O5 Co4 O5 180.0 7_676 . ?
 O5 Co4 O6 85.6(2) . . ?
 O5 Co4 O6 94.4(2) . 7_676 ?
 O5 Co4 O6 85.6(2) 7_676 7_676 ?
 O5 Co4 O6 94.4(2) 7_676 . ?
 O5 Co4 O8 87.2(3) 7_676 7_666 ?
 O5 Co4 O8 92.8(3) 7_676 1_565 ?
 O5 Co4 O8 92.8(3) . 7_666 ?
 O5 Co4 O8 87.2(3) . 1_565 ?
 O6 Co4 O6 180.0 7_676 . ?
 O8 Co4 O6 93.9(2) 1_565 . ?
 O8 Co4 O6 93.9(2) 7_666 7_676 ?
 O8 Co4 O6 86.1(2) 7_666 . ?
 O8 Co4 O6 86.1(2) 1_565 7_676 ?
 O8 Co4 O8 180.0 7_666 1_565 ?
 O3 Co3 O6 83.3(2) 7_656 1_545 ?
 O3 Co3 O10 84.9(3) 7_656 . ?
 O3 Co3 O11 96.5(3) 7_656 . ?
 O7 Co3 O3 91.1(3) 7_666 7_656 ?
 O7 Co3 O6 91.6(2) 7_666 1_545 ?
 O7 Co3 O10 171.7(3) 7_666 . ?
 O7 Co3 O11 83.5(3) 7_666 . ?
 O9 Co3 O3 173.0(4) . 7_656 ?
 O9 Co3 O6 92.7(3) . 1_545 ?
 O9 Co3 O7 94.8(3) . 7_666 ?
 O9 Co3 O10 89.7(3) . . ?
 O9 Co3 O11 88.0(4) . . ?
 O10 Co3 O6 95.2(3) . 1_545 ?
 O10 Co3 O11 89.6(4) . . ?
 O11 Co3 O6 175.1(3) . 1_545 ?
 O12 Co2 O12 180.0 . 5_767 ?
 O12 Co2 O13 89.9(2) . 5_767 ?
 O12 Co2 O13 89.9(2) 5_767 . ?
 O12 Co2 O13 90.1(2) . . ?
 O12 Co2 O13 90.1(2) 5_767 5_767 ?
 O12 Co2 O14 90.8(3) . 5_767 ?
 O12 Co2 O14 89.2(3) . . ?
 O12 Co2 O14 89.2(3) 5_767 5_767 ?
 O12 Co2 O14 90.8(3) 5_767 . ?
 O13 Co2 O13 180.0(2) 5_767 . ?
 O14 Co2 O13 91.7(3) 5_767 . ?
 O14 Co2 O13 88.3(3) 5_767 5_767 ?
 O14 Co2 O13 91.7(3) . 5_767 ?
 O14 Co2 O13 88.3(3) . . ?
 O14 Co2 O14 180.0 5_767 . ?
 C1 O1 Co1A 89.8(6) . . ?
 C1 O1 Co1 87.4(6) . . ?
 C1 O2 Co1A 84.2(5) . . ?
 C1 O2 Co1 92.2(5) . . ?
 C5 O3 Co3 137.0(5) . 7_656 ?
 C12 O5 Co4 134.8(6) . . ?
 Co4 O6 Co3 110.7(3) . 1_565 ?
 Co4 O6 H6A 120.7 . . ?
 Co4 O6 H6B 101.7 . . ?
 Co3 O6 H6A 100.8 1_565 . ?
 Co3 O6 H6B 104.5 1_565 . ?
 H6A O6 H6B 117.5 . . ?
 C12 O7 Co3 140.3(6) . 7_666 ?
 C17 O8 Co4 135.3(5) . 1_545 ?
 C17 O9 Co3 137.8(6) . . ?
 Co3 O10 H10A 110.4 . . ?
 Co3 O10 H10B 111.3 . . ?
 H10A O10 H10B 107.9 . . ?
 Co3 O11 H11A 120.2 . . ?
 Co3 O11 H11B 114.7 . . ?
 H11A O11 H11B 116.1 . . ?
 C20 O12 Co2 130.8(6) . . ?
 Co2 O13 H13A 98.2 . . ?
 Co2 O13 H13B 94.5 . . ?
 H13A O13 H13B 97.8 . . ?
 Co2 O14 H14A 110.1 . . ?
 Co2 O14 H14B 138.1 . . ?
 H14A O14 H14B 107.6 . . ?
 Co1 O16A H16A 109.2 . . ?
 Co1 O16A H16B 110.0 . . ?
 H16A O16A H16B 109.5 . . ?
 Co1A O16 H16C 109.5 . . ?
 Co1A O16 H16D 109.5 . . ?
 H16C O16 H16D 109.5 . . ?
 O1 C1 Co1A 56.2(5) . . ?
 O1 C1 C2 118.1(8) . . ?
 O2 C1 Co1A 63.5(5) . . ?
 O2 C1 O1 118.9(8) . . ?
 O2 C1 C2 123.0(7) . . ?
 C2 C1 Co1A 168.7(8) . . ?
 C3 C2 C1 117.5(8) . . ?
 C8 C2 C1 123.5(7) . . ?
 C8 C2 C3 118.9(8) . . ?
 C2 C3 H3 121.0 . . ?
 C4 C3 C2 118.1(8) . . ?
 C4 C3 H3 121.0 . . ?
 C3 C4 C5 115.1(7) . . ?
 C6 C4 C3 122.2(7) . . ?
 C6 C4 C5 122.0(7) . . ?
 O3 C5 O4 123.3(7) . . ?
 O3 C5 C4 115.4(7) . . ?
 O4 C5 C4 121.3(7) . . ?
 C4 C6 C7 117.5(7) . . ?
 C4 C6 C9 123.5(7) . . ?
 C7 C6 C9 118.8(7) . . ?
 C6 C7 H7 120.0 . . ?
 C8 C7 C6 120.1(8) . . ?
 C8 C7 H7 120.0 . . ?
 C2 C8 C7 123.1(8) . . ?
 C2 C8 H8 118.4 . . ?
 C7 C8 H8 118.4 . . ?
 C10 C9 C6 119.7(7) . . ?
 C10 C9 C23 119.2(7) . . ?
 C23 C9 C6 120.9(7) . . ?
 C9 C10 H10 119.2 . . ?
 C9 C10 C11 121.7(7) . . ?
 C11 C10 H10 119.2 . . ?
 C10 C11 C12 120.3(7) . . ?
 C10 C11 C13 118.5(7) . . ?
 C13 C11 C12 120.6(7) . . ?
 O5 C12 O7 124.3(8) . . ?
 O5 C12 C11 118.7(7) . . ?
 O7 C12 C11 117.0(7) . . ?
 C11 C13 H13 119.6 . . ?
 C14 C13 C11 120.7(8) . . ?
 C14 C13 H13 119.6 . . ?
 C13 C14 C15 119.1(7) . . ?
 C13 C14 C23 119.8(7) . . ?
 C23 C14 C15 120.7(7) . . ?
 C16 C15 C14 124.1(6) . . ?
 C22 C15 C14 118.6(7) . . ?
 C22 C15 C16 117.0(7) . . ?
 C15 C16 C17 123.5(7) . . ?
 C18 C16 C15 117.8(6) . . ?
 C18 C16 C17 118.5(7) . . ?
 O8 C17 C16 119.2(7) . . ?
 O9 C17 O8 126.7(7) . . ?
 O9 C17 C16 114.0(7) . . ?
 C16 C18 H18 118.1 . . ?
 C19 C18 C16 123.8(8) . . ?
 C19 C18 H18 118.1 . . ?
 C18 C19 C20 121.1(8) . . ?
 C18 C19 C21 118.4(7) . . ?
 C21 C19 C20 120.4(7) . . ?
 O12 C20 C19 116.5(8) . . ?
 O15 C20 O12 123.2(8) . . ?
 O15 C20 C19 120.3(7) . . ?
 C19 C21 H21 120.6 . . ?
 C22 C21 C19 118.8(7) . . ?
 C22 C21 H21 120.6 . . ?
 C15 C22 H22 118.0 . . ?
 C21 C22 C15 124.0(7) . . ?
 C21 C22 H22 118.0 . . ?
 C9 C23 H23 120.0 . . ?
 C14 C23 C9 120.1(7) . . ?
 C14 C23 H23 120.0 . . ?
 H17A O17 H17B 97.5 . . ?

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
 O6 H6B O17 0.86 1.95 2.723(12) 148.7 3
 O10 H10A O4 0.88 2.00 2.686(10) 134.4 7_656
 O10 H10B O17 0.88 2.03 2.825(16) 150.5 3_545
 O11 H11A O16A 0.94 2.31 2.92(3) 122.6 4_656
 O11 H11B O13 0.94 1.79 2.707(11) 164.5 6_565
 O13 H13A O15 0.83 1.82 2.594(9) 153.9 5_767
 O13 H13B O4 0.89 2.32 2.896(11) 122.2 4_656
 O13 H13B O14 0.89 2.60 3.057(9) 112.2 5_767
 O14 H14A O2 0.86 2.00 2.766(9) 147.4 8_556
 O14 H14B O4 0.86 1.87 2.725(9) 175.6 4_646
 O16A H16A O15 0.85 2.27 3.10(3) 165.1 4_646
 O16 H16C O15 0.85 2.42 3.268(18) 172.5 4_656
 O17 H17A O7 0.82 2.29 3.064(13) 156.6 5_666
 O17 H17B O9 1.02 2.35 3.229(14) 143.4 3_445

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Co1A O1 C1 O2 -10.8(13) . . . . ?
 Co1A O1 C1 C2 168.6(10) . . . . ?
 Co1A O2 C1 O1 10.0(12) . . . . ?
 Co1A O2 C1 C2 -169.3(11) . . . . ?
 Co1A C1 C2 C3 -115(3) . . . . ?
 Co1A C1 C2 C8 69(4) . . . . ?
 Co1 O1 C1 O2 14.5(12) . . . . ?
 Co1 O1 C1 C2 -166.1(10) . . . . ?
 Co1 O2 C1 O1 -15.0(12) . . . . ?
 Co1 O2 C1 C2 165.6(10) . . . . ?
 Co4 O5 C12 O7 8.9(15) . . . . ?
 Co4 O5 C12 C11 -173.7(6) . . . . ?
 Co4 O8 C17 O9 4.9(16) 1_545 . . . ?
 Co4 O8 C17 C16 -173.7(6) 1_545 . . . ?
 Co3 O3 C5 O4 -1.3(15) 7_656 . . . ?
 Co3 O3 C5 C4 175.0(6) 7_656 . . . ?
 Co3 O7 C12 O5 -9.3(16) 7_666 . . . ?
 Co3 O7 C12 C11 173.3(7) 7_666 . . . ?
 Co3 O9 C17 O8 1.8(19) . . . . ?
 Co3 O9 C17 C16 -179.5(8) . . . . ?
 Co2 O12 C20 O15 6.4(15) . . . . ?
 Co2 O12 C20 C19 -172.8(6) . . . . ?
 O1 C1 C2 C3 -171.9(10) . . . . ?
 O1 C1 C2 C8 11.7(17) . . . . ?
 O2 C1 C2 C3 7.5(17) . . . . ?
 O2 C1 C2 C8 -168.9(12) . . . . ?
 C1 C2 C3 C4 -176.7(9) . . . . ?
 C1 C2 C8 C7 178.6(10) . . . . ?
 C2 C3 C4 C5 167.6(8) . . . . ?
 C2 C3 C4 C6 -3.2(13) . . . . ?
 C3 C2 C8 C7 2.2(16) . . . . ?
 C3 C4 C5 O3 -130.5(9) . . . . ?
 C3 C4 C5 O4 45.9(12) . . . . ?
 C3 C4 C6 C7 4.1(13) . . . . ?
 C3 C4 C6 C9 -171.6(8) . . . . ?
 C4 C6 C7 C8 -2.0(13) . . . . ?
 C4 C6 C9 C10 45.9(11) . . . . ?
 C4 C6 C9 C23 -140.2(8) . . . . ?
 C5 C4 C6 C7 -166.0(8) . . . . ?
 C5 C4 C6 C9 18.3(13) . . . . ?
 C6 C4 C5 O3 40.2(12) . . . . ?
 C6 C4 C5 O4 -143.3(9) . . . . ?
 C6 C7 C8 C2 -1.2(15) . . . . ?
 C6 C9 C10 C11 174.2(7) . . . . ?
 C6 C9 C23 C14 -175.1(7) . . . . ?
 C7 C6 C9 C10 -129.7(8) . . . . ?
 C7 C6 C9 C23 44.1(11) . . . . ?
 C8 C2 C3 C4 0.0(14) . . . . ?
 C9 C6 C7 C8 174.0(8) . . . . ?
 C9 C10 C11 C12 -172.1(7) . . . . ?
 C9 C10 C11 C13 -0.4(12) . . . . ?
 C10 C9 C23 C14 -1.2(12) . . . . ?
 C10 C11 C12 O5 177.2(8) . . . . ?
 C10 C11 C12 O7 -5.2(12) . . . . ?
 C10 C11 C13 C14 1.4(12) . . . . ?
 C11 C13 C14 C15 -174.7(7) . . . . ?
 C11 C13 C14 C23 -2.3(12) . . . . ?
 C12 C11 C13 C14 173.1(7) . . . . ?
 C13 C11 C12 O5 5.7(12) . . . . ?
 C13 C11 C12 O7 -176.7(8) . . . . ?
 C13 C14 C15 C16 -59.7(11) . . . . ?
 C13 C14 C15 C22 114.6(9) . . . . ?
 C13 C14 C23 C9 2.2(12) . . . . ?
 C14 C15 C16 C17 -14.7(13) . . . . ?
 C14 C15 C16 C18 170.4(8) . . . . ?
 C14 C15 C22 C21 -171.3(8) . . . . ?
 C15 C14 C23 C9 174.4(7) . . . . ?
 C15 C16 C17 O8 -12.8(13) . . . . ?
 C15 C16 C17 O9 168.4(9) . . . . ?
 C15 C16 C18 C19 2.0(13) . . . . ?
 C16 C15 C22 C21 3.5(13) . . . . ?
 C16 C18 C19 C20 -179.8(8) . . . . ?
 C16 C18 C19 C21 0.9(14) . . . . ?
 C17 C16 C18 C19 -173.2(8) . . . . ?
 C18 C16 C17 O8 162.0(8) . . . . ?
 C18 C16 C17 O9 -16.7(12) . . . . ?
 C18 C19 C20 O12 179.0(9) . . . . ?
 C18 C19 C20 O15 -0.3(15) . . . . ?
 C18 C19 C21 C22 -1.6(13) . . . . ?
 C19 C21 C22 C15 -0.6(13) . . . . ?
 C20 C19 C21 C22 179.0(8) . . . . ?
 C21 C19 C20 O12 -1.7(13) . . . . ?
 C21 C19 C20 O15 179.0(9) . . . . ?
 C22 C15 C16 C17 170.9(8) . . . . ?
 C22 C15 C16 C18 -4.0(12) . . . . ?
 C23 C9 C10 C11 0.3(12) . . . . ?
 C23 C14 C15 C16 128.0(9) . . . . ?
 C23 C14 C15 C22 -57.7(11) . . . . ?

_shelx_SHELXL_version_number      '2014/7'
_olex2_submission_special_instructions 'No special instructions were received'
data_4
_audit_creation_date              2017-04-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number      '2014/7'
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic
;
 ? 
;
_chemical_formula_moiety          'C46 H42 Mn5 O32, 6(H2 O)'
_chemical_formula_sum             'C46 H54 Mn5 O38'
_chemical_formula_weight          1489.59
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 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'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system       'monoclinic'
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 1 21/c 1'
_space_group_name_Hall            '-P 2ybc'
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                    17.715(8)
_cell_length_b                    21.652(10)
_cell_length_c                    7.406(4)
_cell_angle_alpha                 90
_cell_angle_beta                  95.535(8)
_cell_angle_gamma                 90
_cell_volume                      2827(2)
_cell_formula_units_Z             2
_cell_measurement_reflns_used     2581
_cell_measurement_temperature     100
_cell_measurement_theta_max       23.797
_cell_measurement_theta_min       2.208
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     1.195
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_type    none
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             colourless
_exptl_crystal_colour_primary     colourless
_exptl_crystal_density_diffrn     1.750
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        block
_exptl_crystal_F_000              1518
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_special_details
;
 ? 
;
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0464
_diffrn_reflns_av_unetI/netI      0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max        21
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_k_min        -26
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_number             15114
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          26.000
_diffrn_reflns_theta_min          1.489
_diffrn_ambient_temperature       100
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type   'Bruker P4'
_diffrn_measurement_method        ?
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    ?
_diffrn_special_details           ?
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 4071
_reflns_number_total              5497
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection        ?
_computing_data_reduction         'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max          1.040
_refine_diff_density_min          -0.438
_refine_diff_density_rms          0.086
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.028
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      432
_refine_ls_number_reflns          5497
_refine_ls_number_restraints      24
_refine_ls_R_factor_all           0.0661
_refine_ls_R_factor_gt            0.0452
_refine_ls_restrained_S_all       1.035
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0520P)²+2.3743P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1069
_refine_ls_wR_factor_ref          0.1203
_refine_special_details           ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O18A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq, Uanis(O19A) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(O19A)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(O19)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(O8A)=Sof(O18A)=Sof(H18A)=Sof(H18B)=1-FVAR(2)
 Sof(O8)=Sof(O18)=Sof(H18C)=Sof(H18D)=FVAR(2)
4.a Riding coordinates:
 O7(H7A,H7B), O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B),
 O16(H16A,H16B), O18A(H18A,H18B), O17(H17A,H17B), O18(H18C,H18D), O19(H19A,
 H19B), O19A(H19C,H19D)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C11(H11), C13(H13), C15(H15), C16(H16),
 C18(H18)
;
_atom_sites_solution_hydrogens    mixed
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Mn1 Mn 0.5000 0.5000 1.0000 0.01816(17) Uani 1 2 d S T P . .
 Mn2 Mn 0.70988(3) 0.49611(2) 0.08878(7) 0.02265(15) Uani 1 1 d . . . . .
 Mn3 Mn 0.10253(3) 0.16372(2) 0.87193(8) 0.02650(16) Uani 1 1 d . . . . .
 O1 O 0.46063(14) 0.41667(11) 0.8700(4) 0.0332(6) Uani 1 1 d . . . . .
 O2 O 0.33480(16) 0.41823(12) 0.8501(5) 0.0458(8) Uani 1 1 d . . . . .
 O3 O 0.53253(14) 0.44180(13) 0.2345(4) 0.0387(7) Uani 1 1 d . . . . .
 O4 O 0.65680(15) 0.45205(14) 0.2935(4) 0.0423(7) Uani 1 1 d . . . . .
 O5 O 0.23955(15) 0.14214(12) 0.8265(4) 0.0386(7) Uani 1 1 d . . . . .
 O6 O 0.18801(14) 0.23447(12) 0.8402(4) 0.0351(6) Uani 1 1 d . . . . .
 O7 O 0.39052(13) 0.51778(11) 1.1357(3) 0.0270(6) Uani 1 1 d . . . . .
 H7A H 0.3828 0.5003 1.2369 0.040 Uiso 1 1 d R . . . .
 H7B H 0.3867 0.5550 1.1667 0.040 Uiso 1 1 d R . . . .
 O8 O 0.8480(4) 0.4333(4) 0.8448(13) 0.0376(19) Uani 0.618(14) 1 d . . . A 1
 O8A O 0.8236(10) 0.4369(7) 0.764(3) 0.066(5) Uani 0.382(14) 1 d . . . A 2
 O9 O 1.02173(14) 0.24870(14) 0.8796(4) 0.0444(8) Uani 1 1 d . . . . .
 O10 O 0.97305(15) 0.15597(13) 0.8796(5) 0.0480(8) Uani 1 1 d . . . . .
 O11 O 0.74365(14) 0.41097(12) 0.9711(4) 0.0338(6) Uani 1 1 d . . . . .
 O12 O 0.8080(2) 0.5046(2) 0.3009(7) 0.1017(16) Uani 1 1 d . . . . .
 H12A H 0.8114 0.4873 0.4040 0.153 Uiso 1 1 d R . . . .
 H12B H 0.8500 0.4950 0.2677 0.153 Uiso 1 1 d R . . . .
 O13 O 0.78850(16) 0.54565(13) -0.0729(5) 0.0528(9) Uani 1 1 d . . . . .
 H13A H 0.8148 0.5185 -0.1198 0.079 Uiso 1 1 d R . . . .
 H13B H 0.7875 0.5820 -0.1223 0.079 Uiso 1 1 d R . . . .
 O14 O 0.08027(18) 0.15395(15) 0.5776(4) 0.0540(8) Uani 1 1 d . . . . .
 H14A H 0.0564 0.1816 0.5166 0.081 Uiso 1 1 d R . . . .
 H14B H 0.0789 0.1179 0.5234 0.081 Uiso 1 1 d R . . . .
 O15 O 0.1326(2) 0.16085(17) 1.1656(4) 0.0661(10) Uani 1 1 d . . . . .
 H15A H 0.1627 0.1893 1.2123 0.099 Uiso 1 1 d R . . . .
 H15B H 0.0947 0.1674 1.2328 0.099 Uiso 1 1 d R . . . .
 O16 O 0.0970(2) 0.06299(15) 0.8851(6) 0.0773(12) Uani 1 1 d . . . . .
 H16A H 0.0535 0.0507 0.8385 0.116 Uiso 1 1 d R . . . .
 H16B H 0.0996 0.0484 0.9890 0.116 Uiso 1 1 d R . . . .
 O18A O 0.9595(11) 0.4415(6) 0.634(3) 0.128(8) Uani 0.382(14) 1 d . U . A 2
 H18A H 0.9671 0.4084 0.5802 0.192 Uiso 0.382(14) 1 d R . . A 2
 H18B H 0.9242 0.4369 0.6960 0.192 Uiso 0.382(14) 1 d R . . A 2
 C1 C 0.39776(19) 0.39207(15) 0.8351(5) 0.0215(7) Uani 1 1 d . . . . .
 C2 C 0.39315(17) 0.32480(14) 0.7814(4) 0.0168(7) Uani 1 1 d . . . . .
 C3 C 0.32614(18) 0.29424(15) 0.8076(4) 0.0197(7) Uani 1 1 d . . . . .
 H3 H 0.2842 0.3175 0.8409 0.024 Uiso 1 1 calc R . . . .
 C4 C 0.31855(18) 0.23095(15) 0.7870(4) 0.0198(7) Uani 1 1 d . . . . .
 C5 C 0.38011(18) 0.19661(16) 0.7381(5) 0.0215(7) Uani 1 1 d . . . . .
 H5 H 0.3764 0.1530 0.7268 0.026 Uiso 1 1 calc R . . . .
 C6 C 0.44693(18) 0.22667(15) 0.7060(4) 0.0187(7) Uani 1 1 d . . . . .
 H6 H 0.4881 0.2031 0.6697 0.022 Uiso 1 1 calc R . . . .
 C7 C 0.45499(17) 0.29078(14) 0.7258(4) 0.0160(7) Uani 1 1 d . . . . .
 C8 C 0.52755(17) 0.31898(15) 0.6766(4) 0.0169(7) Uani 1 1 d . . . . .
 C9 C 0.59739(18) 0.29561(15) 0.7525(5) 0.0202(7) Uani 1 1 d . . . . .
 H9 H 0.5983 0.2639 0.8413 0.024 Uiso 1 1 calc R . . . .
 C10 C 0.66598(18) 0.31853(15) 0.6989(4) 0.0185(7) Uani 1 1 d . . . . .
 C11 C 0.66332(18) 0.36353(15) 0.5632(4) 0.0191(7) Uani 1 1 d . . . . .
 H11 H 0.7093 0.3792 0.5253 0.023 Uiso 1 1 calc R . . . .
 C12 C 0.59392(18) 0.38586(15) 0.4821(4) 0.0175(7) Uani 1 1 d . . . . .
 C13 C 0.52626(18) 0.36421(15) 0.5415(4) 0.0174(7) Uani 1 1 d . . . . .
 H13 H 0.4791 0.3803 0.4900 0.021 Uiso 1 1 calc R . . . .
 C14 C 0.74075(18) 0.29207(15) 0.7674(4) 0.0196(7) Uani 1 1 d . . . . .
 C15 C 0.75231(19) 0.22844(16) 0.7547(5) 0.0236(8) Uani 1 1 d . . . . .
 H15 H 0.7106 0.2023 0.7171 0.028 Uiso 1 1 calc R . . . .
 C16 C 0.8240(2) 0.20271(17) 0.7962(5) 0.0268(8) Uani 1 1 d . . . . .
 H16 H 0.8305 0.1592 0.7913 0.032 Uiso 1 1 calc R . . . .
 C17 C 0.88588(18) 0.24050(17) 0.8447(5) 0.0247(8) Uani 1 1 d . . . . .
 C18 C 0.87530(19) 0.30342(17) 0.8594(5) 0.0259(8) Uani 1 1 d . . . . .
 H18 H 0.9178 0.3292 0.8924 0.031 Uiso 1 1 calc R . . . .
 C19 C 0.80336(18) 0.32987(16) 0.8267(5) 0.0226(7) Uani 1 1 d . . . . .
 C20 C 0.7946(2) 0.39698(17) 0.8723(6) 0.0333(9) Uani 1 1 d . . . . .
 C21 C 0.9647(2) 0.21360(18) 0.8714(5) 0.0311(9) Uani 1 1 d . . . . .
 C22 C 0.59337(19) 0.43012(15) 0.3233(5) 0.0221(7) Uani 1 1 d . . . . .
 C23 C 0.2453(2) 0.20022(16) 0.8199(5) 0.0259(8) Uani 1 1 d . . . . .
 O17 O 0.34845(19) 0.45163(15) 1.4178(4) 0.0566(9) Uani 1 1 d . . . . .
 H17A H 0.3217 0.4197 1.4040 0.085 Uiso 1 1 d R . . . .
 H17B H 0.3492 0.4726 1.5185 0.085 Uiso 1 1 d R . . . .
 O18 O 0.8984(5) 0.4387(3) 0.5114(10) 0.073(3) Uani 0.618(14) 1 d . U . A 1
 H18C H 0.8816 0.4395 0.6198 0.110 Uiso 0.618(14) 1 d R . . A 1
 H18D H 0.9131 0.4036 0.4694 0.110 Uiso 0.618(14) 1 d R . . A 1
 O19 O 0.9642(8) 0.5511(7) 0.130(2) 0.220(8) Uani 0.562(11) 1 d . U . B 1
 H19A H 0.9752 0.5267 0.0489 0.330 Uiso 0.562(11) 1 d R . . B 1
 H19B H 1.0070 0.5720 0.1484 0.330 Uiso 0.562(11) 1 d R . . B 1
 O19A O 0.9364(6) 0.4547(5) 0.1718(17) 0.119(6) Uani 0.438(11) 1 d . U . B 2
 H19C H 0.9246 0.4196 0.1260 0.178 Uiso 0.438(11) 1 d R . . B 2
 H19D H 0.9697 0.4783 0.1301 0.178 Uiso 0.438(11) 1 d R . . B 2


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Mn1 O1 2.130(2) 3_667 ?
 Mn1 O1 2.131(2) . ?
 Mn1 O3 2.178(3) 1_556 ?
 Mn1 O3 2.178(3) 3_666 ?
 Mn1 O7 2.301(2) 3_667 ?
 Mn1 O7 2.301(2) . ?
 Mn2 O2 2.083(3) 3_666 ?
 Mn2 O4 2.090(3) . ?
 Mn2 O7 2.334(3) 3_666 ?
 Mn2 O11 2.149(3) 1_554 ?
 Mn2 O12 2.236(4) . ?
 Mn2 O13 2.201(3) . ?
 Mn3 O5 2.526(3) . ?
 Mn3 O6 2.183(3) . ?
 Mn3 O9 2.335(3) 1_455 ?
 Mn3 O10 2.306(3) 1_455 ?
 Mn3 O14 2.187(3) . ?
 Mn3 O15 2.190(3) . ?
 Mn3 O16 2.186(3) . ?
 O1 C1 1.239(4) . ?
 O2 Mn2 2.083(3) 3_666 ?
 O2 C1 1.265(4) . ?
 O3 Mn1 2.178(3) 1_554 ?
 O3 C22 1.234(4) . ?
 O4 C22 1.259(4) . ?
 O5 C23 1.263(4) . ?
 O6 C23 1.277(4) . ?
 O7 Mn2 2.334(3) 3_666 ?
 O8 C20 1.260(10) . ?
 O8A C20 1.317(18) . ?
 O9 Mn3 2.335(3) 1_655 ?
 O9 C21 1.261(5) . ?
 O10 Mn3 2.306(3) 1_655 ?
 O10 C21 1.257(5) . ?
 O11 Mn2 2.149(3) 1_556 ?
 O11 C20 1.253(4) . ?
 C1 C2 1.510(4) . ?
 C2 C3 1.389(4) . ?
 C2 C7 1.414(4) . ?
 C3 C4 1.384(5) . ?
 C4 C5 1.396(5) . ?
 C4 C23 1.499(5) . ?
 C5 C6 1.391(5) . ?
 C6 C7 1.402(4) . ?
 C7 C8 1.499(4) . ?
 C8 C9 1.403(4) . ?
 C8 C13 1.399(4) . ?
 C9 C10 1.405(4) . ?
 C10 C11 1.397(5) . ?
 C10 C14 1.487(4) . ?
 C11 C12 1.401(4) . ?
 C12 C13 1.397(4) . ?
 C12 C22 1.516(4) . ?
 C14 C15 1.397(5) . ?
 C14 C19 1.414(5) . ?
 C15 C16 1.393(5) . ?
 C16 C17 1.388(5) . ?
 C17 C18 1.381(5) . ?
 C17 C21 1.508(5) . ?
 C18 C19 1.397(5) . ?
 C19 C20 1.503(5) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Mn1 O1 180.0 3_667 . ?
 O1 Mn1 O3 94.58(11) . 3_666 ?
 O1 Mn1 O3 85.42(11) . 1_556 ?
 O1 Mn1 O3 85.42(11) 3_667 3_666 ?
 O1 Mn1 O3 94.58(11) 3_667 1_556 ?
 O1 Mn1 O7 85.06(9) 3_667 . ?
 O1 Mn1 O7 94.94(9) 3_667 3_667 ?
 O1 Mn1 O7 94.94(9) . . ?
 O1 Mn1 O7 85.06(9) . 3_667 ?
 O3 Mn1 O3 180.00(12) 3_666 1_556 ?
 O3 Mn1 O7 94.71(10) 3_666 . ?
 O3 Mn1 O7 85.29(10) 1_556 . ?
 O3 Mn1 O7 85.29(10) 3_666 3_667 ?
 O3 Mn1 O7 94.71(10) 1_556 3_667 ?
 O7 Mn1 O7 180.0 . 3_667 ?
 O2 Mn2 O4 92.39(13) 3_666 . ?
 O2 Mn2 O7 89.44(11) 3_666 3_666 ?
 O2 Mn2 O11 168.09(12) 3_666 1_554 ?
 O2 Mn2 O12 93.43(16) 3_666 . ?
 O2 Mn2 O13 87.60(12) 3_666 . ?
 O4 Mn2 O7 95.32(11) . 3_666 ?
 O4 Mn2 O11 93.72(12) . 1_554 ?
 O4 Mn2 O12 84.35(17) . . ?
 O4 Mn2 O13 165.82(12) . . ?
 O11 Mn2 O7 79.83(10) 1_554 3_666 ?
 O11 Mn2 O12 97.33(15) 1_554 . ?
 O11 Mn2 O13 88.96(11) 1_554 . ?
 O12 Mn2 O7 177.12(14) . 3_666 ?
 O13 Mn2 O7 98.86(12) . 3_666 ?
 O13 Mn2 O12 81.49(17) . . ?
 O6 Mn3 O5 55.25(9) . . ?
 O6 Mn3 O9 83.27(11) . 1_455 ?
 O6 Mn3 O10 139.09(10) . 1_455 ?
 O6 Mn3 O14 91.19(12) . . ?
 O6 Mn3 O15 91.25(12) . . ?
 O6 Mn3 O16 137.70(12) . . ?
 O9 Mn3 O5 138.43(10) 1_455 . ?
 O10 Mn3 O5 163.87(10) 1_455 . ?
 O10 Mn3 O9 56.17(10) 1_455 1_455 ?
 O14 Mn3 O5 86.14(11) . . ?
 O14 Mn3 O9 92.77(12) . 1_455 ?
 O14 Mn3 O10 86.17(12) . 1_455 ?
 O14 Mn3 O15 171.95(14) . . ?
 O15 Mn3 O5 88.96(12) . . ?
 O15 Mn3 O9 95.13(13) . 1_455 ?
 O15 Mn3 O10 96.96(13) . 1_455 ?
 O16 Mn3 O5 82.47(11) . . ?
 O16 Mn3 O9 139.03(12) . 1_455 ?
 O16 Mn3 O10 82.96(12) . 1_455 ?
 O16 Mn3 O14 86.75(15) . . ?
 O16 Mn3 O15 86.28(15) . . ?
 C1 O1 Mn1 135.0(2) . . ?
 C1 O2 Mn2 140.7(2) . 3_666 ?
 C22 O3 Mn1 134.0(2) . 1_554 ?
 C22 O4 Mn2 140.4(2) . . ?
 C23 O5 Mn3 84.4(2) . . ?
 C23 O6 Mn3 99.9(2) . . ?
 Mn1 O7 Mn2 106.49(10) . 3_666 ?
 C21 O9 Mn3 90.8(2) . 1_655 ?
 C21 O10 Mn3 92.3(2) . 1_655 ?
 C20 O11 Mn2 133.5(2) . 1_556 ?
 O1 C1 O2 124.8(3) . . ?
 O1 C1 C2 119.6(3) . . ?
 O2 C1 C2 115.4(3) . . ?
 C3 C2 C1 116.6(3) . . ?
 C3 C2 C7 119.3(3) . . ?
 C7 C2 C1 123.8(3) . . ?
 C4 C3 C2 122.1(3) . . ?
 C3 C4 C5 119.1(3) . . ?
 C3 C4 C23 119.9(3) . . ?
 C5 C4 C23 121.1(3) . . ?
 C6 C5 C4 119.6(3) . . ?
 C5 C6 C7 121.7(3) . . ?
 C2 C7 C8 124.4(3) . . ?
 C6 C7 C2 118.2(3) . . ?
 C6 C7 C8 117.3(3) . . ?
 C9 C8 C7 120.0(3) . . ?
 C13 C8 C7 120.2(3) . . ?
 C13 C8 C9 119.5(3) . . ?
 C8 C9 C10 120.9(3) . . ?
 C9 C10 C14 122.3(3) . . ?
 C11 C10 C9 118.6(3) . . ?
 C11 C10 C14 118.8(3) . . ?
 C10 C11 C12 121.1(3) . . ?
 C11 C12 C22 119.4(3) . . ?
 C13 C12 C11 119.5(3) . . ?
 C13 C12 C22 121.0(3) . . ?
 C12 C13 C8 120.3(3) . . ?
 C15 C14 C10 119.2(3) . . ?
 C15 C14 C19 118.4(3) . . ?
 C19 C14 C10 122.0(3) . . ?
 C16 C15 C14 121.0(3) . . ?
 C17 C16 C15 120.1(3) . . ?
 C16 C17 C21 120.3(3) . . ?
 C18 C17 C16 119.5(3) . . ?
 C18 C17 C21 120.1(3) . . ?
 C17 C18 C19 121.3(3) . . ?
 C14 C19 C20 122.3(3) . . ?
 C18 C19 C14 119.5(3) . . ?
 C18 C19 C20 118.0(3) . . ?
 O8 C20 C19 118.1(5) . . ?
 O8A C20 C19 116.3(8) . . ?
 O11 C20 O8 122.5(5) . . ?
 O11 C20 O8A 122.8(8) . . ?
 O11 C20 C19 117.4(3) . . ?
 O9 C21 C17 120.1(3) . . ?
 O10 C21 O9 120.3(3) . . ?
 O10 C21 C17 119.5(3) . . ?
 O3 C22 O4 125.3(3) . . ?
 O3 C22 C12 118.9(3) . . ?
 O4 C22 C12 115.8(3) . . ?
 O5 C23 O6 120.4(3) . . ?
 O5 C23 C4 121.5(3) . . ?
 O6 C23 C4 118.1(3) . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
 O7 H7A O17 0.86 1.85 2.697(4) 165.7 .
 O12 H12A O18 0.85 1.97 2.559(9) 125.8 .
 O12 H12B O19 0.83 2.65 3.309(17) 137.4 .
 O12 H12B O19A 0.83 1.95 2.770(13) 166.8 .
 O13 H13A O8 0.85 1.96 2.743(10) 153.2 1_554
 O13 H13A O8A 0.85 1.98 2.744(17) 150.4 1_554
 O13 H13B O5 0.87 2.02 2.821(4) 153.5 2_655
 O14 H14A O9 0.84 1.89 2.716(4) 168.7 4_465
 O14 H14B O19 0.88 1.95 2.777(12) 156.8 2_645
 O15 H15A O6 0.86 1.93 2.743(4) 155.4 4_566
 O15 H15B O9 0.89 2.54 3.287(5) 143.3 4_466
 O15 H15B O14 0.89 2.61 3.277(5) 133.2 1_556
 O16 H16A O18A 0.86 2.39 2.814(14) 111.4 2_646
 O16 H16A O19A 0.86 2.31 3.141(10) 163.2 4_466
 O16 H16B O12 0.83 2.35 3.013(6) 137.9 2_646
 O16 H16B O18 0.83 2.37 2.797(7) 112.3 2_646
 O18A H18A O10 0.84 2.05 2.855(17) 161.9 4_565
 O18A H18B O8A 0.82 1.90 2.68(2) 159.9 .
 O17 H17A O5 0.84 2.02 2.837(4) 164.5 4_566
 O17 H17B O4 0.87 2.15 2.995(5) 161.7 3_667
 O18 H18C O8 0.88 1.83 2.709(13) 174.6 .
 O18 H18D O10 0.87 1.84 2.674(7) 161.1 4_565
 O19 H19A O19 0.84 2.45 3.27(3) 164.8 3_765
 O19 H19B O8 0.88 2.57 3.331(17) 145.4 3_766

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Mn1 O1 C1 O2 11.1(6) . . . . ?
 Mn1 O1 C1 C2 -164.9(2) . . . . ?
 Mn1 O3 C22 O4 0.1(6) 1_554 . . . ?
 Mn1 O3 C22 C12 -179.8(2) 1_554 . . . ?
 Mn2 O2 C1 O1 4.7(7) 3_666 . . . ?
 Mn2 O2 C1 C2 -179.2(3) 3_666 . . . ?
 Mn2 O4 C22 O3 -17.7(6) . . . . ?
 Mn2 O4 C22 C12 162.2(3) . . . . ?
 Mn2 O11 C20 O8 12.4(8) 1_556 . . . ?
 Mn2 O11 C20 O8A -25.5(13) 1_556 . . . ?
 Mn2 O11 C20 C19 176.2(2) 1_556 . . . ?
 Mn3 O5 C23 O6 1.3(3) . . . . ?
 Mn3 O5 C23 C4 -178.3(3) . . . . ?
 Mn3 O6 C23 O5 -1.5(4) . . . . ?
 Mn3 O6 C23 C4 178.1(3) . . . . ?
 Mn3 O9 C21 O10 6.2(4) 1_655 . . . ?
 Mn3 O9 C21 C17 -171.5(3) 1_655 . . . ?
 Mn3 O10 C21 O9 -6.3(4) 1_655 . . . ?
 Mn3 O10 C21 C17 171.4(3) 1_655 . . . ?
 O1 C1 C2 C3 157.3(3) . . . . ?
 O1 C1 C2 C7 -15.7(5) . . . . ?
 O2 C1 C2 C3 -19.0(4) . . . . ?
 O2 C1 C2 C7 168.0(3) . . . . ?
 C1 C2 C3 C4 -171.2(3) . . . . ?
 C1 C2 C7 C6 170.5(3) . . . . ?
 C1 C2 C7 C8 -13.0(5) . . . . ?
 C2 C3 C4 C5 0.0(5) . . . . ?
 C2 C3 C4 C23 179.1(3) . . . . ?
 C2 C7 C8 C9 130.8(3) . . . . ?
 C2 C7 C8 C13 -55.8(4) . . . . ?
 C3 C2 C7 C6 -2.4(5) . . . . ?
 C3 C2 C7 C8 174.2(3) . . . . ?
 C3 C4 C5 C6 -1.9(5) . . . . ?
 C3 C4 C23 O5 -170.3(3) . . . . ?
 C3 C4 C23 O6 10.2(5) . . . . ?
 C4 C5 C6 C7 1.6(5) . . . . ?
 C5 C4 C23 O5 8.8(5) . . . . ?
 C5 C4 C23 O6 -170.8(3) . . . . ?
 C5 C6 C7 C2 0.5(5) . . . . ?
 C5 C6 C7 C8 -176.3(3) . . . . ?
 C6 C7 C8 C9 -52.6(4) . . . . ?
 C6 C7 C8 C13 120.8(3) . . . . ?
 C7 C2 C3 C4 2.2(5) . . . . ?
 C7 C8 C9 C10 175.6(3) . . . . ?
 C7 C8 C13 C12 -173.2(3) . . . . ?
 C8 C9 C10 C11 -2.4(5) . . . . ?
 C8 C9 C10 C14 -175.9(3) . . . . ?
 C9 C8 C13 C12 0.2(5) . . . . ?
 C9 C10 C11 C12 0.3(5) . . . . ?
 C9 C10 C14 C15 52.1(5) . . . . ?
 C9 C10 C14 C19 -135.1(4) . . . . ?
 C10 C11 C12 C13 2.0(5) . . . . ?
 C10 C11 C12 C22 -174.2(3) . . . . ?
 C10 C14 C15 C16 172.0(3) . . . . ?
 C10 C14 C19 C18 -168.8(3) . . . . ?
 C10 C14 C19 C20 16.8(5) . . . . ?
 C11 C10 C14 C15 -121.4(4) . . . . ?
 C11 C10 C14 C19 51.4(5) . . . . ?
 C11 C12 C13 C8 -2.2(5) . . . . ?
 C11 C12 C22 O3 168.5(3) . . . . ?
 C11 C12 C22 O4 -11.4(5) . . . . ?
 C13 C8 C9 C10 2.2(5) . . . . ?
 C13 C12 C22 O3 -7.7(5) . . . . ?
 C13 C12 C22 O4 172.5(3) . . . . ?
 C14 C10 C11 C12 174.1(3) . . . . ?
 C14 C15 C16 C17 -2.4(5) . . . . ?
 C14 C19 C20 O8 -148.7(6) . . . . ?
 C14 C19 C20 O8A -112.8(11) . . . . ?
 C14 C19 C20 O11 46.8(5) . . . . ?
 C15 C14 C19 C18 4.0(5) . . . . ?
 C15 C14 C19 C20 -170.3(3) . . . . ?
 C15 C16 C17 C18 2.9(5) . . . . ?
 C15 C16 C17 C21 -173.8(3) . . . . ?
 C16 C17 C18 C19 0.1(6) . . . . ?
 C16 C17 C21 O9 165.9(4) . . . . ?
 C16 C17 C21 O10 -11.8(6) . . . . ?
 C17 C18 C19 C14 -3.6(5) . . . . ?
 C17 C18 C19 C20 171.0(3) . . . . ?
 C18 C17 C21 O9 -10.9(6) . . . . ?
 C18 C17 C21 O10 171.4(4) . . . . ?
 C18 C19 C20 O8 36.9(7) . . . . ?
 C18 C19 C20 O8A 72.7(11) . . . . ?
 C18 C19 C20 O11 -127.6(4) . . . . ?
 C19 C14 C15 C16 -1.1(5) . . . . ?
 C21 C17 C18 C19 176.9(3) . . . . ?
 C22 C12 C13 C8 173.9(3) . . . . ?
 C23 C4 C5 C6 179.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
