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

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

data_13dab11b
_database_code_depnum_ccdc_archive 'CCDC 1474449'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H12 K N O7'
_chemical_formula_weight         321.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.6083(7)
_cell_length_b                   12.3265(7)
_cell_length_c                   8.9860(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.5060(10)
_cell_angle_gamma                90
_cell_volume                     1352.05(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5289
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      28.09

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_F_000             664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.427
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9045
_exptl_absorpt_correction_T_max  0.9748
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20803
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.668
_diffrn_reflns_theta_max         28.387
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3381
_reflns_number_gt                2791
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0327P)²+0.5478P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3381
_refine_ls_number_parameters     201
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.53533(2) 0.97470(2) 0.19995(3) 0.01428(8) Uani 1 1 d . . . . .
N N 0.77443(9) 1.02068(9) 0.29750(12) 0.0129(2) Uani 1 1 d . . . . .
O1 O 0.70035(8) 0.82662(8) 0.34538(11) 0.0162(2) Uani 1 1 d . . . . .
O2 O 0.53116(10) 0.84590(8) 0.45369(13) 0.0242(2) Uani 1 1 d D . . . .
H2 H 0.478(3) 0.854(4) 0.493(5) 0.047(13) Uiso 0.5 1 d D . P A 1
O3 O 0.50488(8) 0.66738(8) 0.46745(12) 0.0190(2) Uani 1 1 d . . . . .
O4 O 0.61972(9) 1.11395(8) 0.42866(11) 0.0188(2) Uani 1 1 d D . . . .
H4 H 0.572(2) 1.134(3) 0.473(4) 0.029(10) Uiso 0.5 1 d D . P B 2
O5 O 0.73133(12) 1.10911(11) 0.66422(13) 0.0397(3) Uani 1 1 d . . . . .
O6 O 0.67305(8) 1.02380(8) -0.01448(11) 0.0146(2) Uani 1 1 d . . . . .
O7 O 0.78018(9) 1.16227(9) -0.04722(11) 0.0195(2) Uani 1 1 d D . . . .
H1 H 0.7582(15) 1.1437(15) -0.1395(12) 0.029 Uiso 1 1 d D U . . .
C1 C 0.78910(11) 0.82450(11) 0.28234(15) 0.0144(3) Uani 1 1 d . . . . .
C2 C 0.82998(11) 0.92765(11) 0.25805(15) 0.0140(3) Uani 1 1 d . . . . .
C3 C 0.91787(12) 0.93308(12) 0.19045(16) 0.0180(3) Uani 1 1 d . . . . .
H3A H 0.9470 1.0019 0.1739 0.022 Uiso 1 1 calc R U . . .
C4 C 0.96385(12) 0.83932(13) 0.14672(17) 0.0204(3) Uani 1 1 d . . . . .
H4A H 1.0232 0.8443 0.0995 0.025 Uiso 1 1 calc R U . . .
C5 C 0.92274(12) 0.73877(12) 0.17235(17) 0.0191(3) Uani 1 1 d . . . . .
H5A H 0.9542 0.6748 0.1428 0.023 Uiso 1 1 calc R U . . .
C6 C 0.83549(12) 0.73072(12) 0.24111(16) 0.0174(3) Uani 1 1 d . . . . .
H6A H 0.8080 0.6616 0.2596 0.021 Uiso 1 1 calc R U . . .
C7 C 0.65280(12) 0.72560(11) 0.37053(16) 0.0155(3) Uani 1 1 d . . . . .
H7A H 0.7075 0.6810 0.4432 0.019 Uiso 1 1 calc R U . . .
H7B H 0.6294 0.6855 0.2723 0.019 Uiso 1 1 calc R U . . .
C8 C 0.55476(12) 0.74637(11) 0.43590(15) 0.0154(3) Uani 1 1 d . . . . .
C9 C 0.80128(12) 1.04172(12) 0.46328(15) 0.0180(3) Uani 1 1 d . . . . .
H9A H 0.8660 1.0900 0.4893 0.022 Uiso 1 1 calc R U . . .
H9B H 0.8226 0.9722 0.5176 0.022 Uiso 1 1 calc R U . . .
C10 C 0.71126(13) 1.09261(12) 0.52499(16) 0.0199(3) Uani 1 1 d . . . . .
C11 C 0.77975(11) 1.11829(11) 0.20752(15) 0.0137(3) Uani 1 1 d . . . . .
H11A H 0.8565 1.1441 0.2290 0.016 Uiso 1 1 calc R U . . .
H11B H 0.7350 1.1763 0.2377 0.016 Uiso 1 1 calc R U . . .
C12 C 0.73786(11) 1.09507(11) 0.03762(15) 0.0123(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K O3 2.6791(10) 4_575 ?
K O4 2.6845(10) . ?
K O6 2.7363(10) 3_675 ?
K O3 2.7890(10) 2_655 ?
K O2 2.7897(11) . ?
K O1 2.8296(10) . ?
K O6 2.9615(10) . ?
K N 2.9756(12) . ?
K C8 3.4953(14) . ?
K K 3.5345(6) 3_675 ?
K H4 3.09(3) . ?
N C2 1.4337(17) . ?
N C11 1.4605(17) . ?
N C9 1.4657(17) . ?
O1 C1 1.3753(16) . ?
O1 C7 1.4244(16) . ?
O2 C8 1.2819(17) . ?
O2 H2 0.840(10) . ?
O3 C8 1.2301(17) . ?
O3 K 2.6791(10) 4_576 ?
O3 K 2.7890(10) 2_645 ?
O4 C10 1.2845(19) . ?
O4 H4 0.838(10) . ?
O5 C10 1.2297(17) . ?
O6 C12 1.2112(16) . ?
O6 K 2.7363(10) 3_675 ?
O7 C12 1.3252(16) . ?
O7 H1 0.837(9) . ?
C1 C6 1.387(2) . ?
C1 C2 1.4094(19) . ?
C2 C3 1.3924(19) . ?
C3 C4 1.393(2) . ?
C3 H3A 0.9500 . ?
C4 C5 1.385(2) . ?
C4 H4A 0.9500 . ?
C5 C6 1.394(2) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 C8 1.5174(19) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 C10 1.518(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 C12 1.5126(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?

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
O3 K O4 165.21(3) 4_575 . ?
O3 K O6 66.50(3) 4_575 3_675 ?
O4 K O6 126.72(3) . 3_675 ?
O3 K O3 99.49(3) 4_575 2_655 ?
O4 K O3 81.49(3) . 2_655 ?
O6 K O3 69.43(3) 3_675 2_655 ?
O3 K O2 103.71(3) 4_575 . ?
O4 K O2 79.82(3) . . ?
O6 K O2 106.85(3) 3_675 . ?
O3 K O2 152.55(3) 2_655 . ?
O3 K O1 83.32(3) 4_575 . ?
O4 K O1 87.38(3) . . ?
O6 K O1 140.21(3) 3_675 . ?
O3 K O1 144.27(3) 2_655 . ?
O2 K O1 54.38(3) . . ?
O3 K O6 67.61(3) 4_575 . ?
O4 K O6 100.54(3) . . ?
O6 K O6 103.43(3) 3_675 . ?
O3 K O6 62.10(3) 2_655 . ?
O2 K O6 141.47(3) . . ?
O1 K O6 87.09(3) . . ?
O3 K N 106.91(3) 4_575 . ?
O4 K N 58.31(3) . . ?
O6 K N 157.75(3) 3_675 . ?
O3 K N 91.75(3) 2_655 . ?
O2 K N 95.32(3) . . ?
O1 K N 54.08(3) . . ?
O6 K N 55.73(3) . . ?
O3 K C8 85.48(3) 4_575 . ?
O4 K C8 95.53(3) . . ?
O6 K C8 106.60(3) 3_675 . ?
O3 K C8 171.32(3) 2_655 . ?
O2 K C8 19.73(3) . . ?
O1 K C8 43.00(3) . . ?
O6 K C8 126.57(3) . . ?
N K C8 93.60(3) . . ?
O3 K K 51.10(2) 4_575 3_675 ?
O4 K K 128.04(3) . 3_675 ?
O6 K K 54.58(2) 3_675 3_675 ?
O3 K K 48.38(2) 2_655 3_675 ?
O2 K K 151.63(3) . 3_675 ?
O1 K K 123.53(2) . 3_675 ?
O6 K K 48.85(2) . 3_675 ?
N K K 104.16(2) . 3_675 ?
C8 K K 136.08(3) . 3_675 ?
O3 K H4 178.8(8) 4_575 . ?
O4 K H4 14.7(5) . . ?
O6 K H4 114.2(6) 3_675 . ?
O3 K H4 81.7(8) 2_655 . ?
O2 K H4 75.1(7) . . ?
O1 K H4 95.6(7) . . ?
O6 K H4 113.0(6) . . ?
N K H4 72.9(5) . . ?
C8 K H4 93.3(8) . . ?
K K H4 130.1(8) 3_675 . ?
C2 N C11 115.40(10) . . ?
C2 N C9 112.96(11) . . ?
C11 N C9 112.71(11) . . ?
C2 N K 107.24(8) . . ?
C11 N K 100.22(8) . . ?
C9 N K 106.99(8) . . ?
C1 O1 C7 117.84(10) . . ?
C1 O1 K 113.71(8) . . ?
C7 O1 K 110.32(8) . . ?
C8 O2 K 112.97(9) . . ?
C8 O2 H2 113(3) . . ?
K O2 H2 118(3) . . ?
C8 O3 K 135.68(9) . 4_576 ?
C8 O3 K 125.74(9) . 2_645 ?
K O3 K 80.51(3) 4_576 2_645 ?
C10 O4 K 120.12(9) . . ?
C10 O4 H4 112(3) . . ?
K O4 H4 111(3) . . ?
C12 O6 K 133.04(9) . 3_675 ?
C12 O6 K 110.21(8) . . ?
K O6 K 76.57(3) 3_675 . ?
C12 O7 H1 108.5(13) . . ?
O1 C1 C6 124.53(13) . . ?
O1 C1 C2 114.42(12) . . ?
C6 C1 C2 121.03(13) . . ?
C3 C2 C1 118.22(13) . . ?
C3 C2 N 124.12(12) . . ?
C1 C2 N 117.59(12) . . ?
C2 C3 C4 121.07(14) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 119.74(13) . . ?
C5 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
C4 C5 C6 120.49(14) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C1 C6 C5 119.44(13) . . ?
C1 C6 H6A 120.3 . . ?
C5 C6 H6A 120.3 . . ?
O1 C7 C8 109.27(11) . . ?
O1 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
O1 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
O3 C8 O2 125.51(13) . . ?
O3 C8 C7 117.95(12) . . ?
O2 C8 C7 116.54(12) . . ?
O3 C8 K 144.59(10) . . ?
O2 C8 K 47.29(7) . . ?
C7 C8 K 80.86(7) . . ?
N C9 C10 116.16(12) . . ?
N C9 H9A 108.2 . . ?
C10 C9 H9A 108.2 . . ?
N C9 H9B 108.2 . . ?
C10 C9 H9B 108.2 . . ?
H9A C9 H9B 107.4 . . ?
O5 C10 O4 124.95(15) . . ?
O5 C10 C9 117.25(14) . . ?
O4 C10 C9 117.80(12) . . ?
N C11 C12 110.49(11) . . ?
N C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
O6 C12 O7 124.12(12) . . ?
O6 C12 C11 123.96(12) . . ?
O7 C12 C11 111.92(11) . . ?

_refine_diff_density_max         0.312
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.054

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

data_15dab1h_twin5
_database_code_depnum_ccdc_archive 'CCDC 1474450'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H52 Mg3 N2 O28'
_chemical_formula_weight         937.64

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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   24.2955(12)
_cell_length_b                   9.4801(4)
_cell_length_c                   18.5395(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.9470(10)
_cell_angle_gamma                90
_cell_volume                     4144.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9992
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.19

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_F_000             1976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.174
_shelx_estimated_absorpt_T_min   0.932
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.712319
_exptl_absorpt_correction_T_max  0.745686
_exptl_absorpt_process_details   TWINABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9928
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.727
_diffrn_reflns_theta_max         28.287
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9928
_reflns_number_gt                8476
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0415P)²+3.0187P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9928
_refine_ls_number_parameters     314
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0953
_refine_ls_wR_factor_gt          0.0911
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg1 Mg 0.26440(2) 0.60674(6) 0.30378(3) 0.01077(13) Uani 1 1 d . . . . .
O1 O 0.29604(5) 0.72482(12) 0.40358(6) 0.0139(2) Uani 1 1 d . . . . .
O4 O 0.34531(5) 0.56834(12) 0.29606(6) 0.0134(2) Uani 1 1 d . . . . .
O3 O 0.26877(5) 1.04181(12) 0.30306(6) 0.0137(2) Uani 1 1 d . . . . .
O6 O 0.19247(5) 0.54963(12) 0.33441(6) 0.0133(2) Uani 1 1 d . . . . .
O2 O 0.25276(5) 0.81420(12) 0.27451(6) 0.0135(2) Uani 1 1 d . . . . .
O5 O 0.40916(5) 0.39870(13) 0.29752(7) 0.0159(3) Uani 1 1 d . . . . .
O7 O 0.15165(5) 0.40445(13) 0.40132(7) 0.0179(3) Uani 1 1 d . . . . .
N1 N 0.29648(6) 0.44004(14) 0.39489(7) 0.0104(3) Uani 1 1 d . . . . .
C1 C 0.31331(7) 0.65668(17) 0.47115(9) 0.0120(3) Uani 1 1 d . . . . .
C2 C 0.31426(7) 0.50969(17) 0.46716(9) 0.0109(3) Uani 1 1 d . . . . .
C3 C 0.33049(7) 0.43321(17) 0.53314(9) 0.0127(3) Uani 1 1 d . . . . .
H3 H 0.3319 0.3332 0.5315 0.015 Uiso 1 1 calc R U . . .
C4 C 0.34457(7) 0.50209(19) 0.60143(9) 0.0146(3) Uani 1 1 d . . . . .
H4 H 0.3548 0.4492 0.6462 0.017 Uiso 1 1 calc R U . . .
C5 C 0.34355(7) 0.64802(18) 0.60392(9) 0.0145(3) Uani 1 1 d . . . . .
H5 H 0.3534 0.6948 0.6506 0.017 Uiso 1 1 calc R U . . .
C6 C 0.32824(7) 0.72692(17) 0.53881(9) 0.0133(3) Uani 1 1 d . . . . .
H6 H 0.3280 0.8271 0.5406 0.016 Uiso 1 1 calc R U . . .
C7 C 0.29661(7) 0.87569(16) 0.39996(9) 0.0123(3) Uani 1 1 d . . . . .
H7A H 0.3359 0.9118 0.4157 0.015 Uiso 1 1 calc R U . . .
H7B H 0.2740 0.9168 0.4326 0.015 Uiso 1 1 calc R U . . .
C8 C 0.27065(7) 0.91326(17) 0.31920(9) 0.0111(3) Uani 1 1 d . . . . .
C9 C 0.34385(7) 0.36504(17) 0.37328(9) 0.0119(3) Uani 1 1 d . . . . .
H9A H 0.3301 0.2729 0.3509 0.014 Uiso 1 1 calc R U . . .
H9B H 0.3744 0.3467 0.4183 0.014 Uiso 1 1 calc R U . . .
C10 C 0.36794(7) 0.44996(17) 0.31779(9) 0.0126(3) Uani 1 1 d . . . . .
C11 C 0.24585(7) 0.35179(17) 0.39299(9) 0.0120(3) Uani 1 1 d . . . . .
H11A H 0.2498 0.3049 0.4417 0.014 Uiso 1 1 calc R U . . .
H11B H 0.2429 0.2777 0.3546 0.014 Uiso 1 1 calc R U . . .
C12 C 0.19230(7) 0.44196(17) 0.37560(9) 0.0126(3) Uani 1 1 d . . . . .
Mg2 Mg 0.5000 0.75025(8) 0.2500 0.01365(17) Uani 1 2 d S T P . .
O8 O 0.43197(6) 0.75563(14) 0.29656(8) 0.0197(3) Uani 1 1 d D . . . .
H8A H 0.4048(8) 0.699(2) 0.2925(12) 0.030 Uiso 1 1 d D U . . .
H8B H 0.4337(10) 0.806(2) 0.3343(9) 0.030 Uiso 1 1 d D U . . .
O9 O 0.44562(6) 0.74671(14) 0.14697(7) 0.0213(3) Uani 1 1 d D . . . .
H9C H 0.4153(7) 0.793(2) 0.1324(12) 0.032 Uiso 1 1 d D U . . .
H9D H 0.4486(10) 0.693(2) 0.1129(10) 0.032 Uiso 1 1 d D U . . .
O10 O 0.5000 0.53144(18) 0.2500 0.0219(4) Uani 1 2 d DS T P . .
H10 H 0.4748(6) 0.481(2) 0.2598(13) 0.033 Uiso 1 1 d D U . . .
O11 O 0.5000 0.96716(18) 0.2500 0.0221(4) Uani 1 2 d DS T P . .
H11 H 0.4740(6) 1.020(2) 0.2560(13) 0.033 Uiso 1 1 d D U . . .
O12 O 0.44440(6) 0.96029(14) 0.40165(8) 0.0228(3) Uani 1 1 d D . . . .
H12A H 0.4373(10) 0.973(2) 0.4430(8) 0.034 Uiso 1 1 d D U . . .
H12B H 0.4281(9) 1.021(2) 0.3713(10) 0.034 Uiso 1 1 d D U . . .
O13 O 0.40851(6) 1.11516(13) 0.27392(8) 0.0192(3) Uani 1 1 d D . . . .
H13A H 0.3782(7) 1.096(2) 0.2434(10) 0.029 Uiso 1 1 d D U . . .
H13B H 0.4093(10) 1.2027(13) 0.2779(12) 0.029 Uiso 1 1 d D U . . .
O14 O 0.43745(6) 0.96784(17) 0.54489(8) 0.0294(3) Uani 1 1 d D . . . .
H14A H 0.4691(6) 0.998(3) 0.5688(12) 0.044 Uiso 1 1 d D U . . .
H14B H 0.4128(8) 0.999(3) 0.5656(13) 0.044 Uiso 1 1 d D U . . .
O15 O 0.46580(6) 0.41782(15) 0.53534(8) 0.0253(3) Uani 1 1 d . . . . .
C13 C 0.47516(9) 0.5657(2) 0.55136(12) 0.0273(4) Uani 1 1 d . . . . .
H13C H 0.5084 0.5778 0.5939 0.033 Uiso 1 1 calc R U . . .
H13D H 0.4417 0.6065 0.5653 0.033 Uiso 1 1 calc R U . . .
C14 C 0.51478(9) 0.3591(2) 0.51488(12) 0.0292(5) Uani 1 1 d . . . . .
H14C H 0.5085 0.2575 0.5035 0.035 Uiso 1 1 calc R U . . .
H14D H 0.5485 0.3685 0.5569 0.035 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 O6 2.0367(13) . ?
Mg1 O4 2.0380(13) . ?
Mg1 O2 2.0417(13) . ?
Mg1 O3 2.0452(12) 4_545 ?
Mg1 O1 2.1404(13) . ?
Mg1 N1 2.3072(14) . ?
O1 C1 1.3818(19) . ?
O1 C7 1.4321(18) . ?
O4 C10 1.272(2) . ?
O3 C8 1.2530(19) . ?
O3 Mg1 2.0452(12) 4 ?
O6 C12 1.275(2) . ?
O2 C8 1.2583(19) . ?
O5 C10 1.250(2) . ?
O7 C12 1.247(2) . ?
N1 C2 1.463(2) . ?
N1 C11 1.481(2) . ?
N1 C9 1.488(2) . ?
C1 C6 1.389(2) . ?
C1 C2 1.396(2) . ?
C2 C3 1.395(2) . ?
C3 C4 1.392(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.520(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 C10 1.529(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 C12 1.525(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
Mg2 O8 2.0414(13) 2_655 ?
Mg2 O8 2.0414(13) . ?
Mg2 O9 2.0442(13) 2_655 ?
Mg2 O9 2.0442(13) . ?
Mg2 O11 2.0563(19) . ?
Mg2 O10 2.0744(19) . ?
O8 H8A 0.838(12) . ?
O8 H8B 0.838(12) . ?
O9 H9C 0.845(12) . ?
O9 H9D 0.828(12) . ?
O10 H10 0.830(11) . ?
O11 H11 0.837(11) . ?
O12 H12A 0.834(12) . ?
O12 H12B 0.833(12) . ?
O13 H13A 0.834(12) . ?
O13 H13B 0.833(12) . ?
O14 H14A 0.838(12) . ?
O14 H14B 0.838(12) . ?
O15 C13 1.439(2) . ?
O15 C14 1.445(2) . ?
C13 C14 1.490(3) 5_666 ?
C13 H13C 0.9900 . ?
C13 H13D 0.9900 . ?
C14 C13 1.490(3) 5_666 ?
C14 H14C 0.9900 . ?
C14 H14D 0.9900 . ?

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
O6 Mg1 O4 151.54(5) . . ?
O6 Mg1 O2 104.90(5) . . ?
O4 Mg1 O2 103.15(5) . . ?
O6 Mg1 O3 91.48(5) . 4_545 ?
O4 Mg1 O3 92.27(5) . 4_545 ?
O2 Mg1 O3 92.04(5) . 4_545 ?
O6 Mg1 O1 92.96(5) . . ?
O4 Mg1 O1 90.15(5) . . ?
O2 Mg1 O1 73.97(5) . . ?
O3 Mg1 O1 165.98(5) 4_545 . ?
O6 Mg1 N1 77.00(5) . . ?
O4 Mg1 N1 76.57(5) . . ?
O2 Mg1 N1 148.77(5) . . ?
O3 Mg1 N1 119.18(5) 4_545 . ?
O1 Mg1 N1 74.80(5) . . ?
C1 O1 C7 120.34(12) . . ?
C1 O1 Mg1 120.43(10) . . ?
C7 O1 Mg1 119.16(9) . . ?
C10 O4 Mg1 119.08(11) . . ?
C8 O3 Mg1 120.47(11) . 4 ?
C12 O6 Mg1 120.43(11) . . ?
C8 O2 Mg1 122.70(11) . . ?
C2 N1 C11 109.69(12) . . ?
C2 N1 C9 112.69(13) . . ?
C11 N1 C9 114.56(12) . . ?
C2 N1 Mg1 109.54(10) . . ?
C11 N1 Mg1 103.73(10) . . ?
C9 N1 Mg1 106.08(9) . . ?
O1 C1 C6 123.42(14) . . ?
O1 C1 C2 115.09(14) . . ?
C6 C1 C2 121.49(15) . . ?
C3 C2 C1 118.51(15) . . ?
C3 C2 N1 121.84(14) . . ?
C1 C2 N1 119.62(14) . . ?
C4 C3 C2 120.63(15) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 119.78(15) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.73(15) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 118.85(15) . . ?
C1 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?
O1 C7 C8 105.88(12) . . ?
O1 C7 H7A 110.6 . . ?
C8 C7 H7A 110.6 . . ?
O1 C7 H7B 110.6 . . ?
C8 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
O3 C8 O2 125.57(15) . . ?
O3 C8 C7 116.46(14) . . ?
O2 C8 C7 117.97(14) . . ?
N1 C9 C10 112.08(13) . . ?
N1 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
O5 C10 O4 124.36(15) . . ?
O5 C10 C9 117.51(14) . . ?
O4 C10 C9 118.12(14) . . ?
N1 C11 C12 110.47(13) . . ?
N1 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N1 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
O7 C12 O6 125.03(16) . . ?
O7 C12 C11 118.24(14) . . ?
O6 C12 C11 116.72(15) . . ?
O8 Mg2 O8 177.14(9) 2_655 . ?
O8 Mg2 O9 89.35(6) 2_655 2_655 ?
O8 Mg2 O9 90.70(6) . 2_655 ?
O8 Mg2 O9 90.70(6) 2_655 . ?
O8 Mg2 O9 89.35(6) . . ?
O9 Mg2 O9 178.12(9) 2_655 . ?
O8 Mg2 O11 88.57(4) 2_655 . ?
O8 Mg2 O11 88.57(4) . . ?
O9 Mg2 O11 90.94(4) 2_655 . ?
O9 Mg2 O11 90.94(4) . . ?
O8 Mg2 O10 91.43(4) 2_655 . ?
O8 Mg2 O10 91.43(4) . . ?
O9 Mg2 O10 89.06(4) 2_655 . ?
O9 Mg2 O10 89.06(4) . . ?
O11 Mg2 O10 180.0 . . ?
Mg2 O8 H8A 130.1(15) . . ?
Mg2 O8 H8B 118.9(15) . . ?
H8A O8 H8B 108.6(19) . . ?
Mg2 O9 H9C 127.4(15) . . ?
Mg2 O9 H9D 124.5(16) . . ?
H9C O9 H9D 107.9(19) . . ?
Mg2 O10 H10 125.0(13) . . ?
Mg2 O11 H11 127.0(13) . . ?
H12A O12 H12B 111(2) . . ?
H13A O13 H13B 106.0(19) . . ?
H14A O14 H14B 108(2) . . ?
C13 O15 C14 109.28(15) . . ?
O15 C13 C14 110.19(17) . 5_666 ?
O15 C13 H13C 109.6 . . ?
C14 C13 H13C 109.6 5_666 . ?
O15 C13 H13D 109.6 . . ?
C14 C13 H13D 109.6 5_666 . ?
H13C C13 H13D 108.1 . . ?
O15 C14 C13 109.93(17) . 5_666 ?
O15 C14 H14C 109.7 . . ?
C13 C14 H14C 109.7 5_666 . ?
O15 C14 H14D 109.7 . . ?
C13 C14 H14D 109.7 5_666 . ?
H14C C14 H14D 108.2 . . ?

_refine_diff_density_max         0.643
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.059

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

data_16dab01b
_database_code_depnum_ccdc_archive 'CCDC 1474451'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H22 Ca2 Cl N O13'
_chemical_formula_weight         503.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.4079(5)
_cell_length_b                   11.2214(7)
_cell_length_c                   12.0301(8)
_cell_angle_alpha                108.3734(10)
_cell_angle_beta                 104.9899(10)
_cell_angle_gamma                96.6152(11)
_cell_volume                     1016.26(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3202
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      27.23

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.758
_shelx_estimated_absorpt_T_min   0.822
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15949
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.878
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5031
_reflns_number_gt                3777
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0517P)²+0.0676P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5031
_refine_ls_number_parameters     298
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1057
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.80812(6) 0.42184(5) 0.33459(4) 0.01549(12) Uani 1 1 d . . . . .
Ca2 Ca 0.75923(6) 0.25930(5) 0.62621(4) 0.01576(12) Uani 1 1 d . . . . .
O1 O 0.9668(2) 0.57423(16) 0.29081(15) 0.0171(4) Uani 1 1 d . . . . .
O2 O 1.0532(2) 0.64444(17) 0.15880(15) 0.0196(4) Uani 1 1 d . . . . .
O3 O 0.6968(2) 0.41483(17) 0.12178(15) 0.0202(4) Uani 1 1 d . . . . .
O4 O 0.7369(2) 0.27661(17) 0.42770(15) 0.0183(4) Uani 1 1 d . . . . .
O5 O 0.6159(2) 0.08133(17) 0.40610(16) 0.0205(4) Uani 1 1 d . . . . .
O6 O 0.5773(2) 0.52981(17) 0.33583(17) 0.0211(4) Uani 1 1 d . . . . .
O7 O 0.3094(2) 0.52451(17) 0.33392(17) 0.0228(4) Uani 1 1 d . . . . .
N1 N 0.5162(3) 0.2699(2) 0.21427(18) 0.0168(4) Uani 1 1 d . . . . .
C1 C 0.9490(3) 0.5755(2) 0.1837(2) 0.0174(5) Uani 1 1 d . . . . .
C2 C 0.7969(3) 0.4894(2) 0.0771(2) 0.0182(5) Uani 1 1 d . . . . .
H2A H 0.7293 0.5424 0.0408 0.022 Uiso 1 1 calc R U . . .
H2B H 0.8341 0.4318 0.0123 0.022 Uiso 1 1 calc R U . . .
C3 C 0.5553(3) 0.3259(2) 0.0381(2) 0.0188(5) Uani 1 1 d . . . . .
C4 C 0.4611(3) 0.2525(2) 0.0841(2) 0.0179(5) Uani 1 1 d . . . . .
C5 C 0.3157(3) 0.1644(3) 0.0037(2) 0.0227(6) Uani 1 1 d . . . . .
H5 H 0.2503 0.1158 0.0347 0.027 Uiso 1 1 calc R U . . .
C6 C 0.2632(3) 0.1452(3) -0.1209(2) 0.0249(6) Uani 1 1 d . . . . .
H6 H 0.1628 0.0846 -0.1747 0.030 Uiso 1 1 calc R U . . .
C7 C 0.3589(3) 0.2156(3) -0.1657(2) 0.0242(6) Uani 1 1 d . . . . .
H7 H 0.3248 0.2018 -0.2512 0.029 Uiso 1 1 calc R U . . .
C8 C 0.5043(3) 0.3060(3) -0.0875(2) 0.0220(6) Uani 1 1 d . . . . .
H8 H 0.5687 0.3541 -0.1193 0.026 Uiso 1 1 calc R U . . .
C9 C 0.6363(3) 0.1680(2) 0.3636(2) 0.0167(5) Uani 1 1 d . . . . .
C10 C 0.5347(3) 0.1453(2) 0.2308(2) 0.0185(5) Uani 1 1 d . . . . .
H10A H 0.5923 0.0986 0.1740 0.022 Uiso 1 1 calc R U . . .
H10B H 0.4217 0.0914 0.2100 0.022 Uiso 1 1 calc R U . . .
C11 C 0.4306(3) 0.4717(3) 0.3177(2) 0.0187(5) Uani 1 1 d . . . . .
C12 C 0.3969(3) 0.3260(2) 0.2765(2) 0.0192(5) Uani 1 1 d . . . . .
H12A H 0.4050 0.3010 0.3493 0.023 Uiso 1 1 calc R U . . .
H12B H 0.2805 0.2899 0.2192 0.023 Uiso 1 1 calc R U . . .
O8 O 0.8908(2) 0.57287(17) 0.55214(16) 0.0170(4) Uani 1 1 d D . . . .
H8A H 0.832(3) 0.544(3) 0.587(2) 0.026 Uiso 1 1 d D U . . .
H8B H 0.874(4) 0.6459(14) 0.561(3) 0.026 Uiso 1 1 d D U . . .
O9 O 0.8832(2) 0.24308(19) 0.19954(17) 0.0242(4) Uani 1 1 d D . . . .
H9A H 0.941(3) 0.199(3) 0.230(3) 0.036 Uiso 1 1 d D U . . .
H9B H 0.884(4) 0.219(3) 0.1265(13) 0.036 Uiso 1 1 d D U . . .
O10 O 0.9796(2) 0.14482(18) 0.60252(17) 0.0213(4) Uani 1 1 d D . . . .
H10C H 0.965(4) 0.0676(13) 0.596(3) 0.032 Uiso 1 1 d D U . . .
H10D H 1.017(4) 0.146(3) 0.5441(19) 0.032 Uiso 1 1 d D U . . .
O11 O 0.4637(2) 0.22918(18) 0.58936(18) 0.0243(4) Uani 1 1 d D . . . .
H11A H 0.434(4) 0.3001(17) 0.606(3) 0.036 Uiso 1 1 d D U . . .
H11B H 0.384(3) 0.172(2) 0.535(2) 0.036 Uiso 1 1 d D U . . .
O12 O 0.6887(2) 0.09062(18) 0.70223(17) 0.0205(4) Uani 1 1 d D . . . .
H12C H 0.745(3) 0.034(2) 0.688(3) 0.031 Uiso 1 1 d D U . . .
H12D H 0.5888(17) 0.050(3) 0.675(3) 0.031 Uiso 1 1 d D U . . .
Cl1 Cl 0.88945(8) 0.87270(6) 0.62726(6) 0.02187(15) Uani 1 1 d . . . . .
O13 O 0.8870(3) 0.1834(2) 0.96209(18) 0.0323(5) Uani 1 1 d D . . . .
H13A H 0.949(3) 0.239(3) 0.949(3) 0.048 Uiso 1 1 d D U . . .
H13B H 0.800(3) 0.145(3) 0.902(2) 0.048 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.3212(17) . ?
Ca1 O4 2.3541(17) . ?
Ca1 O6 2.4044(18) . ?
Ca1 O9 2.4146(19) . ?
Ca1 O3 2.4602(17) . ?
Ca1 O8 2.4892(18) . ?
Ca1 O8 2.5297(18) 2_766 ?
Ca1 N1 2.582(2) . ?
Ca1 Ca1 4.1206(10) 2_766 ?
Ca2 O11 2.3721(19) . ?
Ca2 O10 2.3991(19) . ?
Ca2 O4 2.4177(17) . ?
Ca2 O12 2.4257(19) . ?
Ca2 O2 2.4656(17) 2_766 ?
Ca2 O7 2.4862(18) 2_666 ?
Ca2 O1 2.5367(17) 2_766 ?
Ca2 O5 2.6293(18) . ?
O1 C1 1.263(3) . ?
O1 Ca2 2.5366(17) 2_766 ?
O2 C1 1.258(3) . ?
O2 Ca2 2.4656(17) 2_766 ?
O3 C3 1.378(3) . ?
O3 C2 1.433(3) . ?
O4 C9 1.276(3) . ?
O5 C9 1.248(3) . ?
O6 C11 1.256(3) . ?
O7 C11 1.264(3) . ?
O7 Ca2 2.4862(18) 2_666 ?
N1 C4 1.455(3) . ?
N1 C12 1.483(3) . ?
N1 C10 1.493(3) . ?
C1 C2 1.517(3) . ?
C1 Ca2 2.839(3) 2_766 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C8 1.395(3) . ?
C3 C4 1.405(3) . ?
C4 C5 1.384(3) . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.381(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.528(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.519(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O8 Ca1 2.5297(18) 2_766 ?
O8 H8A 0.833(10) . ?
O8 H8B 0.826(10) . ?
O9 H9A 0.828(10) . ?
O9 H9B 0.837(10) . ?
O10 H10C 0.837(10) . ?
O10 H10D 0.844(10) . ?
O11 H11A 0.843(10) . ?
O11 H11B 0.835(10) . ?
O12 H12C 0.836(10) . ?
O12 H12D 0.833(10) . ?
O13 H13A 0.844(10) . ?
O13 H13B 0.836(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O4 160.46(6) . . ?
O1 Ca1 O6 94.18(6) . . ?
O4 Ca1 O6 99.47(6) . . ?
O1 Ca1 O9 93.67(7) . . ?
O4 Ca1 O9 85.05(6) . . ?
O6 Ca1 O9 139.36(6) . . ?
O1 Ca1 O3 66.42(6) . . ?
O4 Ca1 O3 130.65(6) . . ?
O6 Ca1 O3 75.39(6) . . ?
O9 Ca1 O3 71.53(6) . . ?
O1 Ca1 O8 88.89(6) . . ?
O4 Ca1 O8 80.66(6) . . ?
O6 Ca1 O8 77.17(6) . . ?
O9 Ca1 O8 142.81(6) . . ?
O3 Ca1 O8 141.14(6) . . ?
O1 Ca1 O8 76.16(6) . 2_766 ?
O4 Ca1 O8 84.70(6) . 2_766 ?
O6 Ca1 O8 145.42(6) . 2_766 ?
O9 Ca1 O8 75.01(6) . 2_766 ?
O3 Ca1 O8 126.99(6) . 2_766 ?
O8 Ca1 O8 69.63(7) . 2_766 ?
O1 Ca1 N1 132.12(6) . . ?
O4 Ca1 N1 66.82(6) . . ?
O6 Ca1 N1 66.44(6) . . ?
O9 Ca1 N1 78.95(7) . . ?
O3 Ca1 N1 66.40(6) . . ?
O8 Ca1 N1 124.78(6) . . ?
O8 Ca1 N1 142.77(6) 2_766 . ?
O1 Ca1 Ca1 80.88(4) . 2_766 ?
O4 Ca1 Ca1 81.10(4) . 2_766 ?
O6 Ca1 Ca1 111.80(5) . 2_766 ?
O9 Ca1 Ca1 108.81(5) . 2_766 ?
O3 Ca1 Ca1 147.12(5) . 2_766 ?
O8 Ca1 Ca1 35.14(4) . 2_766 ?
O8 Ca1 Ca1 34.49(4) 2_766 2_766 ?
N1 Ca1 Ca1 146.45(5) . 2_766 ?
O11 Ca2 O10 142.58(7) . . ?
O11 Ca2 O4 92.76(6) . . ?
O10 Ca2 O4 88.07(6) . . ?
O11 Ca2 O12 74.93(6) . . ?
O10 Ca2 O12 79.04(6) . . ?
O4 Ca2 O12 136.74(6) . . ?
O11 Ca2 O2 118.49(7) . 2_766 ?
O10 Ca2 O2 82.02(6) . 2_766 ?
O4 Ca2 O2 139.31(6) . 2_766 ?
O12 Ca2 O2 79.81(6) . 2_766 ?
O11 Ca2 O7 73.18(6) . 2_666 ?
O10 Ca2 O7 143.37(6) . 2_666 ?
O4 Ca2 O7 80.78(6) . 2_666 ?
O12 Ca2 O7 131.22(6) . 2_666 ?
O2 Ca2 O7 84.09(6) 2_766 2_666 ?
O11 Ca2 O1 144.51(6) . 2_766 ?
O10 Ca2 O1 72.90(6) . 2_766 ?
O4 Ca2 O1 86.71(6) . 2_766 ?
O12 Ca2 O1 126.90(6) . 2_766 ?
O2 Ca2 O1 52.64(5) 2_766 2_766 ?
O7 Ca2 O1 71.71(6) 2_666 2_766 ?
O11 Ca2 O5 73.00(6) . . ?
O10 Ca2 O5 78.44(6) . . ?
O4 Ca2 O5 51.79(6) . . ?
O12 Ca2 O5 85.06(6) . . ?
O2 Ca2 O5 157.23(6) 2_766 . ?
O7 Ca2 O5 118.65(6) 2_666 . ?
O1 Ca2 O5 129.96(6) 2_766 . ?
C1 O1 Ca1 124.29(15) . . ?
C1 O1 Ca2 90.28(14) . 2_766 ?
Ca1 O1 Ca2 143.66(7) . 2_766 ?
C1 O2 Ca2 93.69(14) . 2_766 ?
C3 O3 C2 118.23(18) . . ?
C3 O3 Ca1 121.85(14) . . ?
C2 O3 Ca1 119.02(13) . . ?
C9 O4 Ca1 120.97(15) . . ?
C9 O4 Ca2 96.06(14) . . ?
Ca1 O4 Ca2 142.44(8) . . ?
C9 O5 Ca2 86.98(14) . . ?
C11 O6 Ca1 122.13(16) . . ?
C11 O7 Ca2 138.72(16) . 2_666 ?
C4 N1 C12 111.15(19) . . ?
C4 N1 C10 110.83(19) . . ?
C12 N1 C10 109.76(19) . . ?
C4 N1 Ca1 113.42(14) . . ?
C12 N1 Ca1 106.32(14) . . ?
C10 N1 Ca1 105.09(14) . . ?
O2 C1 O1 123.4(2) . . ?
O2 C1 C2 116.8(2) . . ?
O1 C1 C2 119.9(2) . . ?
O2 C1 Ca2 60.07(13) . 2_766 ?
O1 C1 Ca2 63.31(12) . 2_766 ?
C2 C1 Ca2 176.81(17) . 2_766 ?
O3 C2 C1 108.85(19) . . ?
O3 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
O3 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
O3 C3 C8 123.2(2) . . ?
O3 C3 C4 117.0(2) . . ?
C8 C3 C4 119.8(2) . . ?
C5 C4 C3 118.9(2) . . ?
C5 C4 N1 120.9(2) . . ?
C3 C4 N1 120.1(2) . . ?
C4 C5 C6 121.5(2) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 119.1(2) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C6 C7 C8 120.9(2) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C3 119.7(2) . . ?
C7 C8 H8 120.1 . . ?
C3 C8 H8 120.1 . . ?
O5 C9 O4 122.5(2) . . ?
O5 C9 C10 119.2(2) . . ?
O4 C9 C10 118.3(2) . . ?
N1 C10 C9 110.7(2) . . ?
N1 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
O6 C11 O7 125.4(2) . . ?
O6 C11 C12 117.6(2) . . ?
O7 C11 C12 117.0(2) . . ?
N1 C12 C11 112.8(2) . . ?
N1 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
N1 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
Ca1 O8 Ca1 110.37(7) . 2_766 ?
Ca1 O8 H8A 108(2) . . ?
Ca1 O8 H8A 106(2) 2_766 . ?
Ca1 O8 H8B 115(2) . . ?
Ca1 O8 H8B 112(2) 2_766 . ?
H8A O8 H8B 105(3) . . ?
Ca1 O9 H9A 119(2) . . ?
Ca1 O9 H9B 136(2) . . ?
H9A O9 H9B 104(3) . . ?
Ca2 O10 H10C 120(2) . . ?
Ca2 O10 H10D 116(2) . . ?
H10C O10 H10D 104(3) . . ?
Ca2 O11 H11A 111(2) . . ?
Ca2 O11 H11B 131(2) . . ?
H11A O11 H11B 109(3) . . ?
Ca2 O12 H12C 112(2) . . ?
Ca2 O12 H12D 117(2) . . ?
H12C O12 H12D 105(3) . . ?
H13A O13 H13B 113(2) . . ?

_refine_diff_density_max         0.593
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.084

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

data_15dab2h_P21n
_database_code_depnum_ccdc_archive 'CCDC 1474452'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H52 N2 O28 Zn3'
_chemical_formula_weight         1060.82

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

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.2960(3)
_cell_length_b                   18.4231(7)
_cell_length_c                   24.4820(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.0021(6)
_cell_angle_gamma                90
_cell_volume                     4192.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.29

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_F_000             2192
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.802
_shelx_estimated_absorpt_T_min   0.571
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6456
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59215
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.383
_diffrn_reflns_theta_max         28.305
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10445
_reflns_number_gt                8800
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'pseudo-symmetry in orthorhombic'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0654P)²+7.1282P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10445
_refine_ls_number_parameters     612
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1241
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.85841(9) 0.20081(4) 0.48608(2) 0.01636(14) Uani 1 1 d . . . . .
Zn2 Zn 0.35822(9) 0.29882(4) 0.51766(2) 0.01581(14) Uani 1 1 d . . . . .
O1 O 0.9848(5) 0.1057(2) 0.46086(16) 0.0204(9) Uani 1 1 d . . . . .
O2 O 1.0715(5) 0.2260(2) 0.49685(16) 0.0210(9) Uani 1 1 d . . . . .
O3 O 1.3057(6) 0.1974(3) 0.48925(17) 0.0237(10) Uani 1 1 d . U . . .
O4 O 0.8020(5) 0.1561(2) 0.55942(14) 0.0212(9) Uani 1 1 d . . . . .
O5 O 0.6387(6) 0.0900(2) 0.60376(15) 0.0215(9) Uani 1 1 d . . . . .
O6 O 0.8302(5) 0.2280(2) 0.40476(15) 0.0207(9) Uani 1 1 d . . . . .
O7 O 0.6525(6) 0.2385(2) 0.34197(15) 0.0255(10) Uani 1 1 d . . . . .
O8 O 0.4813(5) 0.3951(2) 0.54092(16) 0.0189(9) Uani 1 1 d . U . . .
O9 O 0.5728(5) 0.2729(2) 0.50584(17) 0.0216(9) Uani 1 1 d . . . . .
O10 O 0.8028(5) 0.3021(2) 0.51264(16) 0.0183(9) Uani 1 1 d . . . . .
O11 O 0.3257(6) 0.2724(2) 0.59828(15) 0.0220(9) Uani 1 1 d . . . . .
O12 O 0.1570(6) 0.2618(2) 0.66056(15) 0.0234(9) Uani 1 1 d . . . . .
O13 O 0.3009(5) 0.3428(2) 0.44334(14) 0.0186(8) Uani 1 1 d . . . . .
O14 O 0.1366(7) 0.4095(2) 0.39948(16) 0.0244(9) Uani 1 1 d D . . . .
N1 N 0.6946(6) 0.1184(3) 0.45933(18) 0.0167(11) Uani 1 1 d . . . . .
N2 N 0.1928(6) 0.3818(3) 0.54444(17) 0.0147(10) Uani 1 1 d . . . . .
C1 C 0.9127(7) 0.0475(3) 0.4397(2) 0.0169(11) Uani 1 1 d . . . . .
C2 C 0.7632(7) 0.0523(3) 0.4380(2) 0.0164(12) Uani 1 1 d . . . . .
C3 C 0.6821(8) -0.0068(4) 0.4187(2) 0.0243(15) Uani 1 1 d . U . . .
H3 H 0.5800 -0.0041 0.4183 0.029 Uiso 1 1 calc R U . . .
C4 C 0.7502(9) -0.0683(4) 0.4004(3) 0.0263(15) Uani 1 1 d . . . . .
H4 H 0.6950 -0.1083 0.3878 0.032 Uiso 1 1 calc R U . . .
C5 C 0.8971(9) -0.0720(3) 0.4001(3) 0.0260(15) Uani 1 1 d . . . . .
H5 H 0.9435 -0.1142 0.3864 0.031 Uiso 1 1 calc R U . . .
C6 C 0.9813(8) -0.0132(3) 0.4204(2) 0.0183(12) Uani 1 1 d . . . . .
H6 H 1.0834 -0.0160 0.4204 0.022 Uiso 1 1 calc R U . . .
C7 C 1.1384(8) 0.1095(3) 0.4608(2) 0.0180(8) Uani 1 1 d . U . . .
H7A H 1.1770 0.1047 0.4233 0.022 Uiso 1 1 calc R U . . .
H7B H 1.1805 0.0710 0.4840 0.022 Uiso 1 1 calc R U . . .
C8 C 1.1698(7) 0.1845(3) 0.4841(2) 0.0180(8) Uani 1 1 d . . . . .
C9 C 0.6909(7) 0.1167(3) 0.5615(2) 0.0187(12) Uani 1 1 d . . . . .
C10 C 0.6096(7) 0.1031(3) 0.5087(2) 0.0209(13) Uani 1 1 d . . . . .
H10A H 0.5784 0.0517 0.5079 0.025 Uiso 1 1 calc R U . . .
H10B H 0.5222 0.1338 0.5083 0.025 Uiso 1 1 calc R U . . .
C11 C 0.7034(7) 0.2106(3) 0.3850(2) 0.0191(12) Uani 1 1 d . . . . .
C12 C 0.6120(7) 0.1567(3) 0.4151(2) 0.0177(12) Uani 1 1 d . . . . .
H12A H 0.5745 0.1203 0.3889 0.021 Uiso 1 1 calc R U . . .
H12B H 0.5287 0.1821 0.4315 0.021 Uiso 1 1 calc R U . . .
C13 C 0.4138(7) 0.4545(3) 0.5617(2) 0.0154(11) Uani 1 1 d . . . . .
C14 C 0.4820(8) 0.5190(3) 0.5787(2) 0.0209(13) Uani 1 1 d . . . . .
H14 H 0.5838 0.5230 0.5772 0.025 Uiso 1 1 calc R U . . .
C15 C 0.4020(7) 0.5752(4) 0.5972(3) 0.0220(13) Uani 1 1 d . U . . .
H15 H 0.4483 0.6185 0.6087 0.026 Uiso 1 1 calc R U . . .
C16 C 0.2508(8) 0.5703(3) 0.5995(2) 0.0186(12) Uani 1 1 d . . . . .
H16 H 0.1951 0.6099 0.6125 0.022 Uiso 1 1 calc R U . . .
C17 C 0.1839(7) 0.5063(3) 0.5822(2) 0.0133(11) Uani 1 1 d . . . . .
H17 H 0.0821 0.5028 0.5840 0.016 Uiso 1 1 calc R U . . .
C18 C 0.2623(7) 0.4477(3) 0.5627(2) 0.0152(12) Uani 1 1 d . . . . .
C19 C 0.6345(8) 0.3900(3) 0.5410(2) 0.0177(10) Uani 1 1 d . . . . .
H19A H 0.6720 0.3948 0.5787 0.021 Uiso 1 1 calc R U . . .
H19B H 0.6769 0.4290 0.5184 0.021 Uiso 1 1 calc R U . . .
C20 C 0.6733(8) 0.3158(3) 0.5176(2) 0.0162(10) Uani 1 1 d . . . . .
C21 C 0.1151(8) 0.3445(3) 0.5886(2) 0.0203(13) Uani 1 1 d . . . . .
H21A H 0.0298 0.3199 0.5730 0.024 Uiso 1 1 calc R U . . .
H21B H 0.0806 0.3811 0.6152 0.024 Uiso 1 1 calc R U . . .
C22 C 0.2082(7) 0.2879(3) 0.6188(2) 0.0188(12) Uani 1 1 d . . . . .
C23 C 0.1056(7) 0.3967(3) 0.49470(19) 0.0169(11) Uani 1 1 d . . . . .
H23A H 0.0738 0.4480 0.4954 0.020 Uiso 1 1 calc R U . . .
H23B H 0.0186 0.3658 0.4954 0.020 Uiso 1 1 calc R U . . .
C24 C 0.1870(7) 0.3828(3) 0.4420(2) 0.0184(12) Uani 1 1 d . . . . .
Zn3 Zn 0.01019(4) 0.30413(2) 0.25178(4) 0.02442(10) Uani 1 1 d . . . . .
O15 O 0.2319(3) 0.31974(14) 0.2515(3) 0.0308(5) Uani 1 1 d D . . . .
H15A H 0.287(5) 0.316(3) 0.2785(15) 0.046 Uiso 1 1 d D U . . .
H15B H 0.254(5) 0.2858(14) 0.2297(13) 0.046 Uiso 1 1 d D U . . .
O16 O 0.0313(3) 0.19103(12) 0.25018(19) 0.0281(5) Uani 1 1 d D . . . .
H16A H -0.046(3) 0.168(2) 0.2439(19) 0.042 Uiso 1 1 d D U . . .
H16B H 0.051(5) 0.182(3) 0.2831(8) 0.042 Uiso 1 1 d D U . . .
O17 O -0.2134(2) 0.29671(12) 0.2510(2) 0.0193(4) Uani 1 1 d D . . . .
H17A H -0.244(6) 0.267(2) 0.2736(13) 0.029 Uiso 1 1 d D U . . .
H17B H -0.261(5) 0.294(2) 0.2224(13) 0.029 Uiso 1 1 d D U . . .
O18 O -0.0144(3) 0.41523(15) 0.2521(2) 0.0474(8) Uani 1 1 d . . . . .
H18A H -0.0971 0.4327 0.2493 0.071 Uiso 1 1 d R U . . .
H18B H 0.0335 0.4441 0.2728 0.071 Uiso 1 1 d DR U . . .
O19 O 0.0143(7) 0.3017(3) 0.16705(16) 0.0294(11) Uani 1 1 d D . . . .
H19C H 0.057(6) 0.335(2) 0.1507(19) 0.044 Uiso 1 1 d D U . . .
H19D H -0.037(7) 0.280(3) 0.1439(18) 0.044 Uiso 1 1 d D U . . .
O20 O 0.0180(6) 0.2998(3) 0.33623(16) 0.0285(11) Uani 1 1 d D . . . .
H20A H 0.012(6) 0.3439(8) 0.343(2) 0.043 Uiso 1 1 d D U . . .
H20B H -0.043(6) 0.276(3) 0.354(2) 0.043 Uiso 1 1 d D U . . .
O21 O 0.3658(7) 0.2678(3) 0.34406(19) 0.0340(12) Uani 1 1 d D . . . .
H21C H 0.452(3) 0.254(4) 0.345(3) 0.051 Uiso 1 1 d D U . . .
H21D H 0.355(7) 0.294(3) 0.3721(16) 0.051 Uiso 1 1 d D U . . .
O22 O 0.3665(6) 0.2699(3) 0.15885(16) 0.0270(10) Uani 1 1 d D . . . .
H22A H 0.4563(13) 0.268(4) 0.157(2) 0.040 Uiso 1 1 d D U . . .
H22B H 0.335(5) 0.2817(16) 0.1281(11) 0.040 Uiso 1 1 d D U . . .
O23 O 0.2051(9) 0.1391(3) 0.3315(2) 0.056(2) Uani 1 1 d D . . . .
H23C H 0.266(5) 0.169(3) 0.343(3) 0.083 Uiso 1 1 d D U . . .
H23D H 0.251(6) 0.1043(15) 0.318(3) 0.083 Uiso 1 1 d D U . . .
O24 O 0.2160(9) 0.1402(3) 0.17061(19) 0.055(2) Uani 1 1 d . . . . .
H24A H 0.2730 0.1704 0.1564 0.083 Uiso 1 1 d DR U . . .
H24B H 0.1717 0.1629 0.1950 0.083 Uiso 1 1 d DR U . . .
O25 O 0.2086(13) 0.4998(3) 0.3107(2) 0.091(3) Uani 1 1 d D U . . .
H25A H 0.1820 0.4752 0.3381 0.137 Uiso 1 1 d DR U . . .
H25B H 0.2079 0.5437 0.3200 0.137 Uiso 1 1 d DR U . . .
O26 O 0.2039(12) 0.5012(3) 0.1924(2) 0.085(3) Uani 1 1 d . U . . .
H26A H 0.1676 0.4642 0.1755 0.128 Uiso 1 1 d DR U . . .
H26B H 0.2179 0.4923 0.2261 0.128 Uiso 1 1 d DR U . . .
O27 O 0.6837(11) 0.6096(4) 0.2851(3) 0.030(2) Uani 0.564(9) 1 d . . P A 1
O28 O 0.7560(12) 0.4854(4) 0.2206(3) 0.038(3) Uani 0.564(9) 1 d . . P A 1
C25 C 0.6186(13) 0.5388(5) 0.2935(4) 0.0254(13) Uani 0.564(9) 1 d . U P A 1
H25C H 0.5209 0.5452 0.3088 0.030 Uiso 0.564(9) 1 calc R U P A 1
H25D H 0.6764 0.5112 0.3203 0.030 Uiso 0.564(9) 1 calc R U P A 1
C26 C 0.6093(14) 0.4974(5) 0.2422(4) 0.0254(13) Uani 0.564(9) 1 d . . P A 1
H26C H 0.5513 0.5246 0.2152 0.030 Uiso 0.564(9) 1 calc R U P A 1
H26D H 0.5618 0.4501 0.2490 0.030 Uiso 0.564(9) 1 calc R U P A 1
C27 C 0.8120(13) 0.5542(5) 0.2089(4) 0.0254(13) Uani 0.564(9) 1 d . . P A 1
H27A H 0.7480 0.5795 0.1828 0.030 Uiso 0.564(9) 1 calc R U P A 1
H27B H 0.9078 0.5490 0.1917 0.030 Uiso 0.564(9) 1 calc R U P A 1
C28 C 0.8259(16) 0.6002(6) 0.2621(4) 0.0254(13) Uani 0.564(9) 1 d . . P A 1
H28A H 0.8890 0.5750 0.2886 0.030 Uiso 0.564(9) 1 calc R U P A 1
H28B H 0.8687 0.6481 0.2536 0.030 Uiso 0.564(9) 1 calc R U P A 1
O27' O 0.6890(16) 0.6073(7) 0.2153(5) 0.050(4) Uani 0.436(9) 1 d . . P A 2
O28' O 0.7476(14) 0.4880(7) 0.2787(5) 0.045(3) Uani 0.436(9) 1 d . . P A 2
C25' C 0.825(3) 0.5984(13) 0.2412(10) 0.056(3) Uani 0.436(9) 1 d . U P A 2
H25E H 0.8904 0.5734 0.2156 0.067 Uiso 0.436(9) 1 calc R U P A 2
H25F H 0.8655 0.6470 0.2487 0.067 Uiso 0.436(9) 1 calc R U P A 2
C26' C 0.820(2) 0.5601(11) 0.2892(7) 0.056(3) Uani 0.436(9) 1 d . . P A 2
H26E H 0.7665 0.5877 0.3172 0.067 Uiso 0.436(9) 1 calc R U P A 2
H26F H 0.9194 0.5520 0.3029 0.067 Uiso 0.436(9) 1 calc R U P A 2
C27' C 0.613(3) 0.4909(12) 0.2572(9) 0.056(3) Uani 0.436(9) 1 d . . P A 2
H27C H 0.5441 0.5106 0.2843 0.067 Uiso 0.436(9) 1 calc R U P A 2
H27D H 0.5803 0.4418 0.2463 0.067 Uiso 0.436(9) 1 calc R U P A 2
C28' C 0.622(3) 0.5455(11) 0.2025(7) 0.056(3) Uani 0.436(9) 1 d . . P A 2
H28C H 0.6747 0.5206 0.1727 0.067 Uiso 0.436(9) 1 calc R U P A 2
H28D H 0.5236 0.5564 0.1893 0.067 Uiso 0.436(9) 1 calc R U P A 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
Zn1 O10 2.042(4) . ?
Zn1 O4 2.044(4) . ?
Zn1 O2 2.052(5) . ?
Zn1 O6 2.069(4) . ?
Zn1 O1 2.198(4) . ?
Zn1 N1 2.248(5) . ?
Zn2 O3 2.053(5) 1_455 ?
Zn2 O11 2.056(4) . ?
Zn2 O13 2.061(4) . ?
Zn2 O9 2.071(5) . ?
Zn2 O8 2.187(4) . ?
Zn2 N2 2.265(5) . ?
O1 C1 1.367(7) . ?
O1 C7 1.430(9) . ?
O2 C8 1.232(8) . ?
O3 C8 1.291(8) . ?
O3 Zn2 2.053(5) 1_655 ?
O4 C9 1.263(8) . ?
O5 C9 1.245(7) . ?
O6 C11 1.314(7) . ?
O7 C11 1.264(7) . ?
O8 C13 1.359(7) . ?
O8 C19 1.427(9) . ?
O9 C20 1.257(8) . ?
O10 C20 1.236(8) . ?
O11 C22 1.236(8) . ?
O12 C22 1.225(7) . ?
O13 C24 1.291(7) . ?
O14 C24 1.243(7) . ?
N1 C2 1.470(7) . ?
N1 C10 1.472(8) . ?
N1 C12 1.504(7) . ?
N2 C18 1.446(7) . ?
N2 C21 1.469(7) . ?
N2 C23 1.489(7) . ?
C1 C6 1.372(9) . ?
C1 C2 1.393(9) . ?
C2 C3 1.406(9) . ?
C3 C4 1.373(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.425(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.523(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 C10 1.517(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.501(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.410(8) . ?
C13 C18 1.415(9) . ?
C14 C15 1.353(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.410(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.398(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(8) . ?
C17 H17 0.9500 . ?
C19 C20 1.526(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C21 C22 1.544(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C23 C24 1.517(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
Zn3 O18 2.059(3) . ?
Zn3 O20 2.070(4) . ?
Zn3 O19 2.075(4) . ?
Zn3 O15 2.081(2) . ?
Zn3 O17 2.083(2) . ?
Zn3 O16 2.093(2) . ?
O15 H15A 0.841(10) . ?
O15 H15B 0.845(10) . ?
O16 H16A 0.849(10) . ?
O16 H16B 0.841(10) . ?
O17 H17A 0.829(10) . ?
O17 H17B 0.831(10) . ?
O18 H18A 0.8366 . ?
O18 H18B 0.8590 . ?
O19 H19C 0.835(10) . ?
O19 H19D 0.840(10) . ?
O20 H20A 0.833(10) . ?
O20 H20B 0.835(10) . ?
O21 H21C 0.841(10) . ?
O21 H21D 0.843(10) . ?
O22 H22A 0.837(10) . ?
O22 H22B 0.835(10) . ?
O23 H23C 0.840(10) . ?
O23 H23D 0.840(10) . ?
O24 H24A 0.8437 . ?
O24 H24B 0.8376 . ?
O25 H25A 0.8461 . ?
O25 H25B 0.8399 . ?
O26 H26A 0.8661 . ?
O26 H26B 0.8501 . ?
O27 C28 1.447(17) . ?
O27 C25 1.451(11) . ?
O28 C27 1.400(12) . ?
O28 C26 1.479(17) . ?
C25 C26 1.472(13) . ?
C25 H25C 0.9900 . ?
C25 H25D 0.9900 . ?
C26 H26C 0.9900 . ?
C26 H26D 0.9900 . ?
C27 C28 1.558(14) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
O27' C28' 1.34(2) . ?
O27' C25' 1.42(3) . ?
O28' C27' 1.36(3) . ?
O28' C26' 1.51(2) . ?
C25' C26' 1.37(3) . ?
C25' H25E 0.9900 . ?
C25' H25F 0.9900 . ?
C26' H26E 0.9900 . ?
C26' H26F 0.9900 . ?
C27' C28' 1.68(3) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C28' H28C 0.9900 . ?
C28' H28D 0.9900 . ?

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
O10 Zn1 O4 91.34(16) . . ?
O10 Zn1 O2 89.83(18) . . ?
O4 Zn1 O2 103.05(18) . . ?
O10 Zn1 O6 93.07(17) . . ?
O4 Zn1 O6 155.52(19) . . ?
O2 Zn1 O6 101.02(18) . . ?
O10 Zn1 O1 162.36(19) . . ?
O4 Zn1 O1 93.59(16) . . ?
O2 Zn1 O1 72.56(17) . . ?
O6 Zn1 O1 89.43(16) . . ?
O10 Zn1 N1 122.58(19) . . ?
O4 Zn1 N1 79.04(17) . . ?
O2 Zn1 N1 147.58(18) . . ?
O6 Zn1 N1 78.31(16) . . ?
O1 Zn1 N1 75.02(18) . . ?
O3 Zn2 O11 94.28(16) 1_455 . ?
O3 Zn2 O13 89.83(17) 1_455 . ?
O11 Zn2 O13 154.49(19) . . ?
O3 Zn2 O9 88.37(19) 1_455 . ?
O11 Zn2 O9 102.78(19) . . ?
O13 Zn2 O9 102.49(16) . . ?
O3 Zn2 O8 162.0(2) 1_455 . ?
O11 Zn2 O8 91.10(16) . . ?
O13 Zn2 O8 92.66(16) . . ?
O9 Zn2 O8 73.73(17) . . ?
O3 Zn2 N2 123.4(2) 1_455 . ?
O11 Zn2 N2 77.39(18) . . ?
O13 Zn2 N2 79.35(15) . . ?
O9 Zn2 N2 148.20(18) . . ?
O8 Zn2 N2 74.47(18) . . ?
C1 O1 C7 121.8(5) . . ?
C1 O1 Zn1 118.0(4) . . ?
C7 O1 Zn1 119.7(4) . . ?
C8 O2 Zn1 122.9(4) . . ?
C8 O3 Zn2 115.7(4) . 1_655 ?
C9 O4 Zn1 118.5(4) . . ?
C11 O6 Zn1 114.2(4) . . ?
C13 O8 C19 120.9(5) . . ?
C13 O8 Zn2 120.5(4) . . ?
C19 O8 Zn2 118.0(4) . . ?
C20 O9 Zn2 122.6(4) . . ?
C20 O10 Zn1 117.7(4) . . ?
C22 O11 Zn2 117.8(4) . . ?
C24 O13 Zn2 117.3(3) . . ?
C2 N1 C10 111.4(4) . . ?
C2 N1 C12 110.8(4) . . ?
C10 N1 C12 114.0(5) . . ?
C2 N1 Zn1 111.7(4) . . ?
C10 N1 Zn1 104.7(3) . . ?
C12 N1 Zn1 103.8(3) . . ?
C18 N2 C21 112.6(4) . . ?
C18 N2 C23 109.9(4) . . ?
C21 N2 C23 114.8(5) . . ?
C18 N2 Zn2 110.7(4) . . ?
C21 N2 Zn2 103.4(3) . . ?
C23 N2 Zn2 104.9(3) . . ?
O1 C1 C6 122.8(6) . . ?
O1 C1 C2 116.8(6) . . ?
C6 C1 C2 120.4(6) . . ?
C1 C2 C3 119.7(6) . . ?
C1 C2 N1 118.4(6) . . ?
C3 C2 N1 121.9(6) . . ?
C4 C3 C2 120.1(7) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.2(7) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.6(7) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 118.9(6) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
O1 C7 C8 103.6(5) . . ?
O1 C7 H7A 111.0 . . ?
C8 C7 H7A 111.0 . . ?
O1 C7 H7B 111.0 . . ?
C8 C7 H7B 111.0 . . ?
H7A C7 H7B 109.0 . . ?
O2 C8 O3 125.9(6) . . ?
O2 C8 C7 121.1(6) . . ?
O3 C8 C7 113.1(6) . . ?
O5 C9 O4 125.4(5) . . ?
O5 C9 C10 116.6(6) . . ?
O4 C9 C10 117.9(5) . . ?
N1 C10 C9 113.6(5) . . ?
N1 C10 H10A 108.8 . . ?
C9 C10 H10A 108.8 . . ?
N1 C10 H10B 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
O7 C11 O6 123.0(6) . . ?
O7 C11 C12 117.8(6) . . ?
O6 C11 C12 119.2(5) . . ?
C11 C12 N1 112.0(5) . . ?
C11 C12 H12A 109.2 . . ?
N1 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
N1 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
O8 C13 C14 125.5(6) . . ?
O8 C13 C18 113.3(6) . . ?
C14 C13 C18 121.1(6) . . ?
C15 C14 C13 119.8(6) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 120.8(6) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 119.0(6) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C18 C17 C16 121.8(6) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C13 117.5(6) . . ?
C17 C18 N2 121.7(5) . . ?
C13 C18 N2 120.9(6) . . ?
O8 C19 C20 107.1(5) . . ?
O8 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O8 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.5 . . ?
O10 C20 O9 124.9(5) . . ?
O10 C20 C19 116.7(6) . . ?
O9 C20 C19 118.3(6) . . ?
N2 C21 C22 113.1(5) . . ?
N2 C21 H21A 109.0 . . ?
C22 C21 H21A 109.0 . . ?
N2 C21 H21B 109.0 . . ?
C22 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
O12 C22 O11 126.2(6) . . ?
O12 C22 C21 116.6(6) . . ?
O11 C22 C21 117.1(5) . . ?
N2 C23 C24 113.1(5) . . ?
N2 C23 H23A 109.0 . . ?
C24 C23 H23A 109.0 . . ?
N2 C23 H23B 109.0 . . ?
C24 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
O14 C24 O13 123.7(6) . . ?
O14 C24 C23 117.2(6) . . ?
O13 C24 C23 119.0(4) . . ?
O18 Zn3 O20 92.2(2) . . ?
O18 Zn3 O19 91.5(2) . . ?
O20 Zn3 O19 175.41(11) . . ?
O18 Zn3 O15 88.43(10) . . ?
O20 Zn3 O15 88.5(3) . . ?
O19 Zn3 O15 88.9(3) . . ?
O18 Zn3 O17 87.39(10) . . ?
O20 Zn3 O17 92.4(2) . . ?
O19 Zn3 O17 90.4(2) . . ?
O15 Zn3 O17 175.76(10) . . ?
O18 Zn3 O16 178.66(16) . . ?
O20 Zn3 O16 88.70(19) . . ?
O19 Zn3 O16 87.60(19) . . ?
O15 Zn3 O16 92.56(10) . . ?
O17 Zn3 O16 91.60(9) . . ?
Zn3 O15 H15A 126(4) . . ?
Zn3 O15 H15B 98(3) . . ?
H15A O15 H15B 106(2) . . ?
Zn3 O16 H16A 114(3) . . ?
Zn3 O16 H16B 101(4) . . ?
H16A O16 H16B 105(2) . . ?
Zn3 O17 H17A 112(4) . . ?
Zn3 O17 H17B 123(4) . . ?
H17A O17 H17B 110(2) . . ?
Zn3 O18 H18A 119.0 . . ?
Zn3 O18 H18B 124.0 . . ?
H18A O18 H18B 106.6 . . ?
Zn3 O19 H19C 118(4) . . ?
Zn3 O19 H19D 132(4) . . ?
H19C O19 H19D 107(2) . . ?
Zn3 O20 H20A 100(4) . . ?
Zn3 O20 H20B 121(5) . . ?
H20A O20 H20B 110(3) . . ?
H21C O21 H21D 106(2) . . ?
H22A O22 H22B 107(2) . . ?
H23C O23 H23D 108(3) . . ?
H24A O24 H24B 105.9 . . ?
H25A O25 H25B 107.3 . . ?
H26A O26 H26B 111.9 . . ?
C28 O27 C25 109.2(8) . . ?
C27 O28 C26 106.3(8) . . ?
O27 C25 C26 111.7(8) . . ?
O27 C25 H25C 109.3 . . ?
C26 C25 H25C 109.3 . . ?
O27 C25 H25D 109.3 . . ?
C26 C25 H25D 109.3 . . ?
H25C C25 H25D 107.9 . . ?
C25 C26 O28 109.1(9) . . ?
C25 C26 H26C 109.9 . . ?
O28 C26 H26C 109.9 . . ?
C25 C26 H26D 109.9 . . ?
O28 C26 H26D 109.9 . . ?
H26C C26 H26D 108.3 . . ?
O28 C27 C28 110.6(8) . . ?
O28 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
O28 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
O27 C28 C27 108.4(10) . . ?
O27 C28 H28A 110.0 . . ?
C27 C28 H28A 110.0 . . ?
O27 C28 H28B 110.0 . . ?
C27 C28 H28B 110.0 . . ?
H28A C28 H28B 108.4 . . ?
C28' O27' C25' 114.9(16) . . ?
C27' O28' C26' 116.4(15) . . ?
C26' C25' O27' 115(2) . . ?
C26' C25' H25E 108.6 . . ?
O27' C25' H25E 108.6 . . ?
C26' C25' H25F 108.6 . . ?
O27' C25' H25F 108.6 . . ?
H25E C25' H25F 107.6 . . ?
C25' C26' O28' 108.6(17) . . ?
C25' C26' H26E 110.0 . . ?
O28' C26' H26E 110.0 . . ?
C25' C26' H26F 110.0 . . ?
O28' C26' H26F 110.0 . . ?
H26E C26' H26F 108.3 . . ?
O28' C27' C28' 106.6(18) . . ?
O28' C27' H27C 110.4 . . ?
C28' C27' H27C 110.4 . . ?
O28' C27' H27D 110.4 . . ?
C28' C27' H27D 110.4 . . ?
H27C C27' H27D 108.6 . . ?
O27' C28' C27' 110.3(15) . . ?
O27' C28' H28C 109.6 . . ?
C27' C28' H28C 109.6 . . ?
O27' C28' H28D 109.6 . . ?
C27' C28' H28D 109.6 . . ?
H28C C28' H28D 108.1 . . ?

_refine_diff_density_max         1.919
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.109

# start Validation Reply Form
_vrf_PLAT112_15dab2h_P21n        
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        b        100 %Fit  
RESPONSE: There are 318 observed reflections, which are against the
existence of b glide, i.e. an a glide in the space group Pnma. The b glide 
(the a glide after unit cell transformation) is a pseudo symmetry.
;

_vrf_PLAT113_15dab2h_P21n        
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Pnma Check 
RESPONSE: There are 318 observed reflections, which are against the
existence of b glide, i.e. an a glide in the space group Pnma. The b glide 
(the a glide after unit cell transformation) is a pseudo symmetry.
;
# end Validation Reply Form

