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

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1443836'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H38 N6 O10, 7H2O'
_chemical_formula_sum            'C30 H52 N6 O17'
_chemical_formula_weight         754.66

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'

_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                   13.691(4)
_cell_length_b                   22.544(6)
_cell_length_c                   11.572(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.98(5)
_cell_angle_gamma                90
_cell_volume                     3545.2
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    324
_cell_measurement_theta_min      1
_cell_measurement_theta_max      10

_exptl_crystal_description       prisme
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.118
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5668
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23208
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.358
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3632
_reflns_number_gt                2885
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Brurker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), 

C5(H5A,H5B), C14(H14A,H14B)
2.b Primary CH refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12) 
2.c Primary CH refined with riding coordinates:
 N6(H6), N3(H3),  

The Following ALERTS were generated by PLATON checkcif<<<

Alert level A
PLAT430_ALERT_2_A Short Inter D...A Contact  O2W    ..  O3W     ..       2.53 Ang.  
Alert level B
DIFMN02_ALERT_2_B  The minimum difference density is < -0.1*ZMAX*1.00
            _refine_diff_density_min given =     -1.040
            Test value =     -0.800
DIFMX01_ALERT_2_B  The maximum difference density is > 0.1*ZMAX*1.00
            _refine_diff_density_max given =      1.212
            Test value =      0.800
PLAT097_ALERT_2_B Large Reported Max.  (Positive) Residual Density       1.21 eA-3  
PLAT098_ALERT_2_B Large Reported Min.  (Negative) Residual Density      -1.04 eA-3  
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
And 3 other PLAT306 Alerts
Less ...
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O2W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O4W Check 

PLAT430_ALERT_2_B Short Inter D...A Contact  O1W    ..  O5      ..       2.81 Ang.  
And 5 other PLAT430 Alerts
Less ...
PLAT430_ALERT_2_B Short Inter D...A Contact  O1W    ..  O5      ..       2.81 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W    ..  O3W     ..       2.77 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W    ..  O4W     ..       2.79 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3W    ..  O4W     ..       2.71 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O4W    ..  O5      ..       2.72 Ang. 

These alerts arise because of missing water molecules in the model resulting in apparent large structural voids and missing H-bonds 

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1238P)²+24.6691P] 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         3632
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.1019
_refine_ls_wR_factor_ref         0.2711
_refine_ls_wR_factor_gt          0.2549
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0261(3) 0.37052(18) 0.9384(4) 0.0244(9) Uani 1 1 d . . . . .
H1A H -0.0153 0.4050 0.8914 0.029 Uiso 1 1 calc R U . . .
H1B H -0.0132 0.3821 1.0196 0.029 Uiso 1 1 calc R U . . .
C2 C 0.1437(3) 0.34967(18) 0.9163(4) 0.0238(9) Uani 1 1 d . . . . .
H2A H 0.1930 0.3194 0.9374 0.029 Uiso 1 1 calc R U . . .
H2B H 0.1527 0.3809 0.9743 0.029 Uiso 1 1 calc R U . . .
C3 C 0.1571(3) 0.37472(17) 0.7989(4) 0.0233(9) Uani 1 1 d . . . . .
H3A H 0.2191 0.3959 0.8041 0.028 Uiso 1 1 calc R U . . .
H3B H 0.1047 0.4028 0.7754 0.028 Uiso 1 1 calc R U . . .
C4 C 0.1323(3) 0.35156(18) 0.5873(4) 0.0229(9) Uani 1 1 d . . . . .
H4A H 0.1463 0.3219 0.5309 0.028 Uiso 1 1 calc R U . . .
H4B H 0.1744 0.3855 0.5786 0.028 Uiso 1 1 calc R U . . .
C5 C 0.0441(3) 0.27668(18) 1.0014(4) 0.0254(9) Uani 1 1 d . . . . .
H5A H -0.0229 0.2695 1.0170 0.031 Uiso 1 1 calc R U . . .
H5B H 0.0818 0.2895 1.0734 0.031 Uiso 1 1 calc R U . . .
C6 C 0.0875(3) 0.21944(18) 0.9615(4) 0.0240(9) Uani 1 1 d . . . . .
C7 C 0.0980(3) 0.11349(18) 1.0253(4) 0.0250(9) Uani 1 1 d . . . . .
C8 C 0.0845(3) 0.07706(18) 1.1209(4) 0.0267(9) Uani 1 1 d . . . . .
H8 H 0.0654 0.0937 1.1882 0.032 Uiso 1 1 calc R U . . .
C9 C 0.0995(3) 0.01693(19) 1.1150(4) 0.0281(9) Uani 1 1 d . . . . .
H9 H 0.0883 -0.0071 1.1775 0.034 Uiso 1 1 calc R U . . .
C10 C 0.1315(3) -0.00852(19) 1.0157(4) 0.0291(10) Uani 1 1 d . . . . .
C11 C 0.1485(3) 0.0278(2) 0.9244(4) 0.0303(10) Uani 1 1 d . . . . .
H11 H 0.1715 0.0111 0.8593 0.036 Uiso 1 1 calc R U . . .
C12 C 0.1321(3) 0.08829(19) 0.9269(4) 0.0292(10) Uani 1 1 d . . . . .
H12 H 0.1436 0.1120 0.8641 0.035 Uiso 1 1 calc R U . . .
C13 C 0.1420(3) -0.0742(2) 1.0047(4) 0.0325(10) Uani 1 1 d . . . . .
C14 C 0.2539(3) 0.29510(16) 0.7199(4) 0.0209(8) Uani 1 1 d . . . . .
H14A H 0.2770 0.2905 0.8020 0.025 Uiso 1 1 calc R U . . .
H14B H 0.3010 0.3199 0.6862 0.025 Uiso 1 1 calc R U . . .
C15 C 0.2519(3) 0.23454(17) 0.6624(4) 0.0214(8) Uani 1 1 d . . . . .
N1 N 0.0441(2) 0.32355(14) 0.9152(3) 0.0202(7) Uani 1 1 d . . . . .
N2 N 0.1562(2) 0.32650(14) 0.7081(3) 0.0188(7) Uani 1 1 d . . . . .
N3 N 0.0745(2) 0.17372(15) 1.0349(3) 0.0252(8) Uani 1 1 d . . . . .
H6N H 0.0480 0.1831 1.0960 0.030 Uiso 1 1 calc R U . . .
O1 O 0.1296(2) 0.21573(13) 0.8742(3) 0.0350(8) Uani 1 1 d . . . . .
O2 O 0.1410(3) -0.10299(14) 1.1038(3) 0.0408(9) Uani 1 1 d . . . . .
O3 O 0.1509(2) -0.09815(15) 0.9125(3) 0.0391(8) Uani 1 1 d . . . . .
O5 O 0.3338(2) 0.20841(12) 0.6761(3) 0.0259(7) Uani 1 1 d . . . . .
O4 O 0.1730(2) 0.21633(12) 0.6092(3) 0.0274(7) Uani 1 1 d . . . . .
O1W O 0.0000 0.22180(17) 0.2500 0.0229(9) Uani 1 2 d S T P . .
O2W O 0.0929(5) 0.5014(2) 0.8931(8) 0.121(3) Uani 1 1 d . . . . .
O3W O 0.1097(4) 0.5043(2) 0.6126(8) 0.116(3) Uani 1 1 d . . . . .
O4W O 0.3309(7) 0.0917(2) 0.7341(7) 0.141(3) Uani 1 1 d . . . . .
H3N H 0.115(3) 0.302(2) 0.724(4) 0.017(11) Uiso 1 1 d . . . . .
H13A H 0.1559 -0.1429 1.1026 0.020 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.477(5) . ?
C1 C4 1.510(5) 2_556 ?
C2 N1 1.484(5) . ?
C2 C3 1.503(6) . ?
C3 N2 1.511(5) . ?
C4 N2 1.506(5) . ?
C4 C1 1.510(5) 2_556 ?
C5 N1 1.453(5) . ?
C5 C6 1.516(6) . ?
C6 O1 1.225(5) . ?
C6 N3 1.361(5) . ?
C7 C12 1.402(6) . ?
C7 N3 1.403(5) . ?
C7 C8 1.409(6) . ?
C8 C9 1.374(6) . ?
C9 C10 1.402(6) . ?
C10 C11 1.378(7) . ?
C10 C13 1.494(6) . ?
C11 C12 1.384(6) . ?
C13 O3 1.215(6) . ?
C13 O2 1.320(6) . ?
C14 N2 1.506(4) . ?
C14 C15 1.518(5) . ?
C15 O4 1.245(5) . ?
C15 O5 1.260(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
N1 C1 C4 113.2(3) . 2_556 ?
N1 C2 C3 110.8(3) . . ?
C2 C3 N2 111.5(3) . . ?
N2 C4 C1 112.6(3) . 2_556 ?
N1 C5 C6 112.2(3) . . ?
O1 C6 N3 125.0(4) . . ?
O1 C6 C5 123.4(4) . . ?
N3 C6 C5 111.6(4) . . ?
C12 C7 N3 124.0(4) . . ?
C12 C7 C8 119.4(4) . . ?
N3 C7 C8 116.7(4) . . ?
C9 C8 C7 120.1(4) . . ?
C8 C9 C10 120.5(4) . . ?
C11 C10 C9 119.0(4) . . ?
C11 C10 C13 119.7(4) . . ?
C9 C10 C13 121.2(4) . . ?
C10 C11 C12 121.7(4) . . ?
C11 C12 C7 119.2(4) . . ?
O3 C13 O2 123.9(4) . . ?
O3 C13 C10 122.4(4) . . ?
O2 C13 C10 113.7(4) . . ?
N2 C14 C15 114.5(3) . . ?
O4 C15 O5 127.8(4) . . ?
O4 C15 C14 118.8(3) . . ?
O5 C15 C14 113.4(3) . . ?
C5 N1 C1 110.0(3) . . ?
C5 N1 C2 111.0(3) . . ?
C1 N1 C2 109.4(3) . . ?
C14 N2 C4 110.5(3) . . ?
C14 N2 C3 110.1(3) . . ?
C4 N2 C3 111.0(3) . . ?
C6 N3 C7 129.4(4) . . ?

_refine_diff_density_max         1.212
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.108

_shelxl_version_number           2014-3

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

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1443837'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        3
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H35 Mn N6 O10, 0.5(Na2 O12), 5H2O)'
_chemical_formula_sum            'C30 H45 Mn N6 Na O21'
_chemical_formula_weight         893.57
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'
Mn Mn 0.3368 0.7283 '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'
Na Na 0.0362 0.0249 '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'
Cl Cl 0.1484 0.1585 '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                   11.730(3)
_cell_length_b                   19.810(5)
_cell_length_c                   17.130(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.77(3)
_cell_angle_gamma                90
_cell_volume                     3830.7(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10636
_cell_measurement_theta_min      1.6
_cell_measurement_theta_max      26.7

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_F_000             1968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.410
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_source                   Synchrotron
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            17623
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.607
_diffrn_reflns_theta_max         26.570
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             8623
_reflns_number_gt                7786
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_structure_solution    "'SHELXL-2013 (Sheldrick, 2013)"
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), 

C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
C9(H9A, H9B), C18(H18A,H18B), C20(H20A,H20B), 
C29(H29A,H29B),  
2.b Primary CH refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C23(H23), 
C24(H24), C26(H26), C27(H27), 
2.c Primary CH refined with riding coordinates:
 N5(H5), N6(H6),  
2.d Primary CH refined with riding coordinates:
 O3(H3)


The Following ALERTS were generated by PLATON checkcif<<<


Alert level A
PLAT215_ALERT_3_A Disordered Na1       has ADP max/min Ratio ..... 5.3 Note  
PLAT241_ALERT_2_A High   'MainMol' Ueq as Compared to Neighbors of O12C Check 
PLAT241_ALERT_2_A High   'MainMol' Ueq as Compared to Neighbors of O18C Check 
PLAT430_ALERT_2_A Short Inter D...A Contact  O2C    ..  O5W     .. 2.28 Ang.  
PLAT430_ALERT_2_A Short Inter D...A Contact  O9WB    ..  O3W     .. 2.18 Ang. 

PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......  6 Report
PLAT241_ALERT_2_B High   'MainMol' Ueq as Compared to Neighbors of  O1C Check  

The structure of 3 contains disordered Na(H2O)6+.
Two sites were identified corresponding to disordered partial-occupancy 
sodium atoms (one in special position) and were refined with occupancy 
factors of 0.75/0.25.
Due to this disorder, the oxygen atoms coordinated 
to these sodium ions were located and refined with 
different occupancy factors to correlate the different 
occupancies to the presence of this Na(H2O)6+.





PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check 
And 4 other PLAT306 Alerts
More ...PLAT430_ALERT_2_B Short Inter D...A Contact  O1C    ..  O8.. 2.74 Ang.  
And 9 other PLAT430 Alerts
Less ...
PLAT430_ALERT_2_B Short Inter D...A Contact  O1C    ..  O2     ..  2.81 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O1W    ..  O3W     .. 2.63 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O1W    ..  O2W     .. 2.65 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O1W    ..  O5W     .. 2.84 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact O9WA .. O2 .. 2.56 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O9WA .. O12C .. 2.60 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O9WA .. O10 .. 2.80 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O9WA .. O3W .. 2.81 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O2C    ..  O3      .. 2.67 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W    ..  O9      .. 2.67 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3     ..  O3W     .. 2.75 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact O9WB .. O10 .. 2.78 Ang. 

PLAT939_ALERT_3_B Large Value of Not (SHELXL) Weight Optimized S .   172.28   

The hydrogen of the different hydratation water molecules present in all 
six structures were not located on Fourier map, but were added in the 
empirical formula to allow accurate determination of density and absorption
 coefficient


;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1823P)²+8.0941P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8623
_refine_ls_number_parameters     523
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.1048
_refine_ls_wR_factor_ref         0.3013
_refine_ls_wR_factor_gt          0.2944
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8294(5) 0.3379(3) 0.9462(3) 0.0484(10) Uani 1 1 d . . . . .
H1A H 0.8246 0.3859 0.9341 0.058 Uiso 1 1 calc R U . . .
H1B H 0.7941 0.3137 0.8963 0.058 Uiso 1 1 calc R U . . .
C2 C 0.9570(5) 0.3178(3) 0.9779(3) 0.0594(13) Uani 1 1 d . . . . .
H2A H 0.9625 0.2691 0.9839 0.071 Uiso 1 1 calc R U . . .
H2B H 1.0000 0.3310 0.9393 0.071 Uiso 1 1 calc R U . . .
C3 C 1.1242(5) 0.3125(5) 1.0999(4) 0.086(3) Uani 1 1 d . . . . .
H3A H 1.1658 0.2996 1.0604 0.103 Uiso 1 1 calc R U . . .
H3B H 1.1754 0.3427 1.1386 0.103 Uiso 1 1 calc R U . . .
C4 C 1.1015(6) 0.2516(4) 1.1430(4) 0.081(2) Uani 1 1 d . . . . .
H4A H 1.0545 0.2199 1.1041 0.097 Uiso 1 1 calc R U . . .
H4B H 1.1762 0.2300 1.1696 0.097 Uiso 1 1 calc R U . . .
C5 C 0.9869(6) 0.2058(3) 1.2280(4) 0.0705(17) Uani 1 1 d . . . . .
H5A H 0.9725 0.2132 1.2804 0.085 Uiso 1 1 calc R U . . .
H5B H 1.0429 0.1689 1.2335 0.085 Uiso 1 1 calc R U . . .
C6 C 0.8723(6) 0.1866(3) 1.1674(4) 0.0712(18) Uani 1 1 d . . . . .
H6A H 0.8880 0.1742 1.1165 0.085 Uiso 1 1 calc R U . . .
H6B H 0.8386 0.1476 1.1872 0.085 Uiso 1 1 calc R U . . .
C7 C 0.6909(5) 0.2309(2) 1.0765(3) 0.0527(11) Uani 1 1 d . . . . .
H7A H 0.6695 0.1835 1.0724 0.063 Uiso 1 1 calc R U . . .
H7B H 0.6214 0.2566 1.0783 0.063 Uiso 1 1 calc R U . . .
C8 C 0.7286(4) 0.2511(2) 1.0032(3) 0.0463(10) Uani 1 1 d . . . . .
H8A H 0.7955 0.2237 0.9997 0.056 Uiso 1 1 calc R U . . .
H8B H 0.6642 0.2430 0.9550 0.056 Uiso 1 1 calc R U . . .
C9 C 0.6552(4) 0.3664(2) 0.9875(3) 0.0406(9) Uani 1 1 d . . . . .
H9A H 0.6016 0.3514 1.0183 0.049 Uiso 1 1 calc R U . . .
H9B H 0.6142 0.3633 0.9302 0.049 Uiso 1 1 calc R U . . .
C10 C 0.6928(4) 0.4390(2) 1.0095(3) 0.0394(9) Uani 1 1 d . . . . .
C11 C 0.6310(3) 0.55647(19) 0.9700(3) 0.0355(8) Uani 1 1 d . . . . .
C12 C 0.6750(3) 0.5883(2) 1.0451(3) 0.0371(8) Uani 1 1 d . . . . .
H12 H 0.7059 0.5630 1.0918 0.045 Uiso 1 1 calc R U . . .
C13 C 0.6717(3) 0.65877(19) 1.0487(3) 0.0357(8) Uani 1 1 d . . . . .
H13 H 0.7005 0.6801 1.0985 0.043 Uiso 1 1 calc R U . . .
C14 C 0.6264(3) 0.69774(19) 0.9795(3) 0.0348(8) Uani 1 1 d . . . . .
C15 C 0.5847(3) 0.6651(2) 0.9051(3) 0.0376(8) Uani 1 1 d . . . . .
H15 H 0.5560 0.6904 0.8581 0.045 Uiso 1 1 calc R U . . .
C16 C 0.5855(3) 0.5951(2) 0.9005(2) 0.0377(8) Uani 1 1 d . . . . .
H16 H 0.5556 0.5739 0.8507 0.045 Uiso 1 1 calc R U . . .
C17 C 0.6224(3) 0.7737(2) 0.9846(3) 0.0436(10) Uani 1 1 d . . . . .
C18 C 1.0372(6) 0.4216(4) 1.0468(3) 0.0678(17) Uani 1 1 d . . . . .
H18A H 0.9717 0.4420 1.0065 0.081 Uiso 1 1 calc R U . . .
H18B H 1.1075 0.4253 1.0277 0.081 Uiso 1 1 calc R U . . .
C19 C 1.0567(5) 0.4593(3) 1.1268(3) 0.0623(14) Uani 1 1 d . . . . .
C20 C 1.1183(4) 0.3015(3) 1.2744(3) 0.0560(13) Uani 1 1 d . . . . .
H20A H 1.1650 0.3361 1.2574 0.067 Uiso 1 1 calc R U . . .
H20B H 1.1720 0.2687 1.3070 0.067 Uiso 1 1 calc R U . . .
C21 C 1.0427(4) 0.3328(2) 1.3237(3) 0.0408(9) Uani 1 1 d . . . . .
C22 C 1.0557(4) 0.37466(19) 1.4620(2) 0.0376(8) Uani 1 1 d . . . . .
C23 C 1.1399(4) 0.3890(2) 1.5353(3) 0.0464(10) Uani 1 1 d . . . . .
H23 H 1.2182 0.3758 1.5432 0.056 Uiso 1 1 calc R U . . .
C24 C 1.1066(4) 0.4229(2) 1.5959(3) 0.0423(9) Uani 1 1 d . . . . .
H24 H 1.1626 0.4320 1.6448 0.051 Uiso 1 1 calc R U . . .
C25 C 0.9900(4) 0.44372(18) 1.5847(2) 0.0367(8) Uani 1 1 d . . . . .
C26 C 0.9066(4) 0.4286(2) 1.5119(3) 0.0383(8) Uani 1 1 d . . . . .
H26 H 0.8284 0.4420 1.5043 0.046 Uiso 1 1 calc R U . . .
C27 C 0.9377(4) 0.3938(2) 1.4503(2) 0.0373(8) Uani 1 1 d . . . . .
H27 H 0.8810 0.3835 1.4023 0.045 Uiso 1 1 calc R U . . .
C28 C 0.9520(4) 0.4815(2) 1.6489(3) 0.0388(8) Uani 1 1 d . . . . .
C29 C 0.7326(6) 0.2509(3) 1.2221(4) 0.0675(16) Uani 1 1 d . . . . .
H29A H 0.6675 0.2192 1.2153 0.081 Uiso 1 1 calc R U . . .
H29B H 0.7911 0.2399 1.2725 0.081 Uiso 1 1 calc R U . . .
C30 C 0.6877(5) 0.3203(4) 1.2281(3) 0.0617(14) Uani 1 1 d . . . . .
Mn Mn 0.87774(5) 0.35045(3) 1.14333(3) 0.0338(3) Uani 1 1 d . . . . .
N1 N 0.7623(3) 0.32301(16) 1.0063(2) 0.0371(7) Uani 1 1 d . . . . .
N2 N 1.0109(4) 0.3500(2) 1.0567(3) 0.0547(11) Uani 1 1 d . . . . .
N3 N 1.0395(4) 0.2683(2) 1.2027(2) 0.0563(11) Uani 1 1 d . . . . .
N4 N 0.7871(4) 0.2425(2) 1.1535(3) 0.0512(9) Uani 1 1 d . . . . .
N5 N 0.6248(3) 0.48554(17) 0.9614(2) 0.0396(8) Uani 1 1 d . . . . .
H5 H 0.5712 0.4703 0.9205 0.048 Uiso 1 1 calc R U . . .
N6 N 1.0973(3) 0.34025(18) 1.4030(2) 0.0409(8) Uani 1 1 d . . . . .
H6 H 1.1660 0.3218 1.4199 0.049 Uiso 1 1 calc R U . . .
O1 O 0.7789(3) 0.45110(15) 1.0682(2) 0.0480(8) Uani 1 1 d . . . . .
O2 O 0.6566(3) 0.80160(16) 1.0533(2) 0.0524(8) Uani 1 1 d . . . . .
O1W O 0.4816(3) 0.4363(3) 0.8048(3) 0.0719(12) Uani 1 1 d . . . . .
O3 O 0.5848(3) 0.80608(18) 0.9184(3) 0.0641(11) Uani 1 1 d . . . . .
O2W O 0.7132(5) 0.0104(4) 0.7451(5) 0.150(4) Uani 1 1 d . . . . .
O4 O 1.0070(3) 0.43402(16) 1.17872(18) 0.0444(7) Uani 1 1 d . . . . .
O3W O 0.3963(10) 0.3215(5) 0.7365(5) 0.169(4) Uani 1 1 d . . . . .
O5 O 1.1148(5) 0.5119(3) 1.1371(3) 0.0959(19) Uani 1 1 d . . . . .
O6 O 0.9395(3) 0.34948(16) 1.29099(19) 0.0429(7) Uani 1 1 d . . . . .
O7 O 1.0356(3) 0.48788(17) 1.7172(2) 0.0512(8) Uani 1 1 d . . . . .
H7 H 1.0099 0.5092 1.7498 0.077 Uiso 1 1 calc R U . . .
O8 O 0.8525(3) 0.50440(19) 1.6391(2) 0.0498(8) Uani 1 1 d . . . . .
O9 O 0.7142(3) 0.36504(19) 1.1846(2) 0.0496(8) Uani 1 1 d . . . . .
O10 O 0.6282(5) 0.3318(4) 1.2774(3) 0.104(2) Uani 1 1 d . . . . .
Na1 Na 0.5000 0.0000 1.0000 0.0232(8) Uani 0.5 2 d DS . P . .
Na2 Na 0.51952(19) 0.00580(11) 0.9475(2) 0.0549(8) Uani 0.75 1 d D . P . .
O1C O 0.3487(6) 0.0573(3) 0.9635(4) 0.1035(18) Uiso 1 1 d . . . . .
O3C O 0.6261(9) 0.0537(5) 0.8806(6) 0.154(3) Uiso 1 1 d . . . . .
O4C O 0.5606(9) 0.0788(5) 1.0747(6) 0.151(3) Uiso 1 1 d . . . . .
O2C O 0.5061(14) 0.0772(8) 1.1463(10) 0.237(6) Uiso 1 1 d . . . . .
O9WA O 0.4238(14) 0.1760(19) 0.8179(10) 0.241(16) Uani 0.5 1 d . . P . .
O5W O 0.3170(7) -0.0663(6) 0.7558(8) 0.180(5) Uani 1 1 d D . . . .
O18C O 0.6380(17) 0.0426(10) 1.0274(11) 0.267(7) Uiso 1 1 d . . . . .
O12C O 0.392(2) 0.0769(9) 0.8831(13) 0.181(10) Uani 0.5 1 d . . P . .
O9WB O 0.4793(11) 0.2504(9) 0.8340(7) 0.120(5) Uani 0.5 1 d . . 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
C1 N1 1.486(6) . ?
C1 C2 1.500(8) . ?
C2 N2 1.472(6) . ?
C3 C4 1.475(12) . ?
C3 N2 1.527(9) . ?
C4 N3 1.446(7) . ?
C5 N3 1.499(9) . ?
C5 C6 1.506(8) . ?
C6 N4 1.467(7) . ?
C7 C8 1.494(7) . ?
C7 N4 1.501(6) . ?
C8 N1 1.474(5) . ?
C9 N1 1.483(5) . ?
C9 C10 1.522(6) . ?
C10 O1 1.240(5) . ?
C10 N5 1.344(5) . ?
C11 C16 1.395(6) . ?
C11 C12 1.399(6) . ?
C11 N5 1.413(5) . ?
C12 C13 1.398(5) . ?
C13 C14 1.393(6) . ?
C14 C15 1.394(6) . ?
C14 C17 1.509(5) . ?
C15 C16 1.388(6) . ?
C17 O2 1.262(6) . ?
C17 O3 1.273(6) . ?
C18 N2 1.471(8) . ?
C18 C19 1.522(8) . ?
C19 O5 1.232(7) . ?
C19 O4 1.290(6) . ?
C20 N3 1.476(6) . ?
C20 C21 1.514(6) . ?
C21 O6 1.232(5) . ?
C21 N6 1.344(5) . ?
C22 C27 1.396(6) . ?
C22 C23 1.400(6) . ?
C22 N6 1.411(6) . ?
C23 C24 1.379(6) . ?
C24 C25 1.390(6) . ?
C25 C26 1.393(6) . ?
C25 C28 1.494(6) . ?
C26 C27 1.389(6) . ?
C28 O8 1.221(5) . ?
C28 O7 1.314(5) . ?
C29 C30 1.486(10) . ?
C29 N4 1.492(7) . ?
C30 O9 1.250(7) . ?
C30 O10 1.255(7) . ?
Mn O4 2.215(3) . ?
Mn O9 2.236(3) . ?
Mn N4 2.416(4) . ?
Mn N2 2.430(4) . ?
Mn N1 2.431(3) . ?
Mn O6 2.435(3) . ?
Mn O1 2.483(3) . ?
Mn N3 2.496(4) . ?
Na1 Na2 0.994(4) 3_657 ?
Na1 Na2 0.994(4) . ?
Na1 O18C 1.771(19) 3_657 ?
Na1 O18C 1.77(2) . ?
Na1 O4C 2.022(10) 3_657 ?
Na1 O4C 2.022(10) . ?
Na1 O1C 2.055(7) 3_657 ?
Na1 O1C 2.055(7) . ?
Na1 O12C 2.562(18) 3_657 ?
Na1 O12C 2.562(19) . ?
Na1 O2C 2.920(16) . ?
Na1 O2C 2.920(16) 3_657 ?
Na2 O18C 1.817(19) . ?
Na2 O4C 1.909(10) 3_657 ?
Na2 Na2 1.988(8) 3_657 ?
Na2 O12C 2.133(16) . ?
Na2 O3C 2.134(10) . ?
Na2 O18C 2.22(2) 3_657 ?
Na2 O1C 2.235(7) 3_657 ?
Na2 O2C 2.261(16) 3_657 ?
Na2 O1C 2.330(7) . ?
Na2 O4C 2.551(11) . ?
O1C O12C 1.64(3) . ?
O1C Na2 2.235(7) 3_657 ?
O4C O2C 1.529(17) . ?
O4C O18C 1.548(19) . ?
O4C Na2 1.909(10) 3_657 ?
O2C Na2 2.261(16) 3_657 ?
O9WA O9WB 1.61(3) . ?
O18C Na2 2.22(2) 3_657 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.2(4) . . ?
N2 C2 C1 110.7(4) . . ?
C4 C3 N2 112.9(5) . . ?
N3 C4 C3 111.1(6) . . ?
N3 C5 C6 111.7(5) . . ?
N4 C6 C5 111.2(4) . . ?
C8 C7 N4 111.9(4) . . ?
N1 C8 C7 111.5(4) . . ?
N1 C9 C10 108.8(3) . . ?
O1 C10 N5 125.5(4) . . ?
O1 C10 C9 120.0(4) . . ?
N5 C10 C9 114.4(3) . . ?
C16 C11 C12 119.8(4) . . ?
C16 C11 N5 117.4(4) . . ?
C12 C11 N5 122.7(4) . . ?
C13 C12 C11 118.9(4) . . ?
C14 C13 C12 121.6(4) . . ?
C13 C14 C15 118.6(4) . . ?
C13 C14 C17 120.9(4) . . ?
C15 C14 C17 120.5(4) . . ?
C16 C15 C14 120.6(4) . . ?
C15 C16 C11 120.4(4) . . ?
O2 C17 O3 123.8(4) . . ?
O2 C17 C14 118.9(4) . . ?
O3 C17 C14 117.3(4) . . ?
N2 C18 C19 110.8(4) . . ?
O5 C19 O4 124.5(5) . . ?
O5 C19 C18 119.0(5) . . ?
O4 C19 C18 116.4(4) . . ?
N3 C20 C21 108.5(4) . . ?
O6 C21 N6 124.7(4) . . ?
O6 C21 C20 120.6(4) . . ?
N6 C21 C20 114.7(4) . . ?
C27 C22 C23 120.2(4) . . ?
C27 C22 N6 123.4(4) . . ?
C23 C22 N6 116.4(4) . . ?
C24 C23 C22 120.0(4) . . ?
C23 C24 C25 120.6(4) . . ?
C24 C25 C26 119.0(4) . . ?
C24 C25 C28 121.7(4) . . ?
C26 C25 C28 119.3(4) . . ?
C27 C26 C25 121.4(4) . . ?
C26 C27 C22 118.8(4) . . ?
O8 C28 O7 122.7(4) . . ?
O8 C28 C25 123.4(4) . . ?
O7 C28 C25 113.9(4) . . ?
C30 C29 N4 113.2(5) . . ?
O9 C30 O10 123.1(7) . . ?
O9 C30 C29 117.7(5) . . ?
O10 C30 C29 119.1(7) . . ?
O4 Mn O9 113.50(13) . . ?
O4 Mn N4 157.50(13) . . ?
O9 Mn N4 70.10(15) . . ?
O4 Mn N2 70.36(13) . . ?
O9 Mn N2 160.54(15) . . ?
N4 Mn N2 114.18(16) . . ?
O4 Mn N1 126.27(12) . . ?
O9 Mn N1 91.92(12) . . ?
N4 Mn N1 74.39(13) . . ?
N2 Mn N1 72.04(13) . . ?
O4 Mn O6 74.52(11) . . ?
O9 Mn O6 73.21(11) . . ?
N4 Mn O6 86.04(13) . . ?
N2 Mn O6 125.12(13) . . ?
N1 Mn O6 158.70(12) . . ?
O4 Mn O1 74.34(11) . . ?
O9 Mn O1 74.94(13) . . ?
N4 Mn O1 126.55(13) . . ?
N2 Mn O1 88.48(15) . . ?
N1 Mn O1 67.67(10) . . ?
O6 Mn O1 120.66(10) . . ?
O4 Mn N3 89.30(15) . . ?
O9 Mn N3 125.27(16) . . ?
N4 Mn N3 72.19(16) . . ?
N2 Mn N3 72.74(17) . . ?
N1 Mn N3 114.21(12) . . ?
O6 Mn N3 65.96(12) . . ?
O1 Mn N3 158.55(16) . . ?
C8 N1 C9 110.4(3) . . ?
C8 N1 C1 110.8(3) . . ?
C9 N1 C1 108.1(4) . . ?
C8 N1 Mn 108.9(3) . . ?
C9 N1 Mn 107.3(2) . . ?
C1 N1 Mn 111.3(3) . . ?
C18 N2 C2 111.4(5) . . ?
C18 N2 C3 110.1(5) . . ?
C2 N2 C3 109.5(5) . . ?
C18 N2 Mn 104.8(3) . . ?
C2 N2 Mn 112.0(3) . . ?
C3 N2 Mn 108.9(4) . . ?
C4 N3 C20 111.6(5) . . ?
C4 N3 C5 109.9(5) . . ?
C20 N3 C5 110.0(4) . . ?
C4 N3 Mn 109.5(3) . . ?
C20 N3 Mn 106.5(3) . . ?
C5 N3 Mn 109.2(3) . . ?
C6 N4 C29 112.1(5) . . ?
C6 N4 C7 110.1(4) . . ?
C29 N4 C7 109.2(4) . . ?
C6 N4 Mn 112.7(4) . . ?
C29 N4 Mn 104.4(3) . . ?
C7 N4 Mn 108.2(3) . . ?
C10 N5 C11 127.9(3) . . ?
C21 N6 C22 127.9(4) . . ?
C10 O1 Mn 115.3(3) . . ?
C19 O4 Mn 120.4(3) . . ?
C21 O6 Mn 116.9(3) . . ?
C30 O9 Mn 118.0(3) . . ?
Na2 Na1 Na2 180.00(12) 3_657 . ?
Na2 Na1 O18C 76.5(6) 3_657 3_657 ?
Na2 Na1 O18C 103.5(6) . 3_657 ?
Na2 Na1 O18C 103.5(6) 3_657 . ?
Na2 Na1 O18C 76.5(6) . . ?
O18C Na1 O18C 180.0 3_657 . ?
Na2 Na1 O4C 110.9(3) 3_657 3_657 ?
Na2 Na1 O4C 69.1(3) . 3_657 ?
O18C Na1 O4C 47.6(6) 3_657 3_657 ?
O18C Na1 O4C 132.4(6) . 3_657 ?
Na2 Na1 O4C 69.1(3) 3_657 . ?
Na2 Na1 O4C 110.9(3) . . ?
O18C Na1 O4C 132.4(6) 3_657 . ?
O18C Na1 O4C 47.6(6) . . ?
O4C Na1 O4C 180.0 3_657 . ?
Na2 Na1 O1C 93.0(2) 3_657 3_657 ?
Na2 Na1 O1C 87.0(2) . 3_657 ?
O18C Na1 O1C 118.0(7) 3_657 3_657 ?
O18C Na1 O1C 62.0(7) . 3_657 ?
O4C Na1 O1C 83.8(3) 3_657 3_657 ?
O4C Na1 O1C 96.2(3) . 3_657 ?
Na2 Na1 O1C 87.0(2) 3_657 . ?
Na2 Na1 O1C 93.0(2) . . ?
O18C Na1 O1C 62.0(7) 3_657 . ?
O18C Na1 O1C 118.0(7) . . ?
O4C Na1 O1C 96.2(3) 3_657 . ?
O4C Na1 O1C 83.8(3) . . ?
O1C Na1 O1C 180.0(2) 3_657 . ?
Na2 Na1 O12C 53.9(6) 3_657 3_657 ?
Na2 Na1 O12C 126.1(6) . 3_657 ?
O18C Na1 O12C 98.5(8) 3_657 3_657 ?
O18C Na1 O12C 81.5(8) . 3_657 ?
O4C Na1 O12C 92.9(5) 3_657 3_657 ?
O4C Na1 O12C 87.1(5) . 3_657 ?
O1C Na1 O12C 39.6(6) 3_657 3_657 ?
O1C Na1 O12C 140.4(6) . 3_657 ?
Na2 Na1 O12C 126.1(6) 3_657 . ?
Na2 Na1 O12C 53.9(6) . . ?
O18C Na1 O12C 81.5(8) 3_657 . ?
O18C Na1 O12C 98.5(8) . . ?
O4C Na1 O12C 87.1(5) 3_657 . ?
O4C Na1 O12C 92.9(5) . . ?
O1C Na1 O12C 140.4(6) 3_657 . ?
O1C Na1 O12C 39.6(6) . . ?
O12C Na1 O12C 180.0 3_657 . ?
Na2 Na1 O2C 40.7(4) 3_657 . ?
Na2 Na1 O2C 139.3(4) . . ?
O18C Na1 O2C 106.5(7) 3_657 . ?
O18C Na1 O2C 73.5(7) . . ?
O4C Na1 O2C 150.5(4) 3_657 . ?
O4C Na1 O2C 29.5(4) . . ?
O1C Na1 O2C 102.2(4) 3_657 . ?
O1C Na1 O2C 77.8(4) . . ?
O12C Na1 O2C 75.5(5) 3_657 . ?
O12C Na1 O2C 104.5(5) . . ?
Na2 Na1 O2C 139.3(4) 3_657 3_657 ?
Na2 Na1 O2C 40.7(4) . 3_657 ?
O18C Na1 O2C 73.5(7) 3_657 3_657 ?
O18C Na1 O2C 106.5(7) . 3_657 ?
O4C Na1 O2C 29.5(4) 3_657 3_657 ?
O4C Na1 O2C 150.5(4) . 3_657 ?
O1C Na1 O2C 77.8(4) 3_657 3_657 ?
O1C Na1 O2C 102.2(4) . 3_657 ?
O12C Na1 O2C 104.5(5) 3_657 3_657 ?
O12C Na1 O2C 75.5(5) . 3_657 ?
O2C Na1 O2C 180.0 . 3_657 ?
Na1 Na2 O18C 71.4(6) . . ?
Na1 Na2 O4C 81.7(3) . 3_657 ?
O18C Na2 O4C 137.4(7) . 3_657 ?
Na1 Na2 Na2 0.001(1) . 3_657 ?
O18C Na2 Na2 71.4(6) . 3_657 ?
O4C Na2 Na2 81.7(3) 3_657 3_657 ?
Na1 Na2 O12C 104.0(7) . . ?
O18C Na2 O12C 114.3(8) . . ?
O4C Na2 O12C 103.8(7) 3_657 . ?
Na2 Na2 O12C 104.0(7) 3_657 . ?
Na1 Na2 O3C 148.2(4) . . ?
O18C Na2 O3C 77.7(7) . . ?
O4C Na2 O3C 127.8(5) 3_657 . ?
Na2 Na2 O3C 148.2(4) 3_657 . ?
O12C Na2 O3C 82.0(9) . . ?
Na1 Na2 O18C 50.7(5) . 3_657 ?
O18C Na2 O18C 122.1(6) . 3_657 ?
O4C Na2 O18C 43.1(5) 3_657 3_657 ?
Na2 Na2 O18C 50.7(5) 3_657 3_657 ?
O12C Na2 O18C 83.1(9) . 3_657 ?
O3C Na2 O18C 159.0(6) . 3_657 ?
Na1 Na2 O1C 66.7(2) . 3_657 ?
O18C Na2 O1C 57.6(7) . 3_657 ?
O4C Na2 O1C 81.8(3) 3_657 3_657 ?
Na2 Na2 O1C 66.7(2) 3_657 3_657 ?
O12C Na2 O1C 168.7(6) . 3_657 ?
O3C Na2 O1C 102.6(3) . 3_657 ?
O18C Na2 O1C 94.8(5) 3_657 3_657 ?
Na1 Na2 O2C 122.7(5) . 3_657 ?
O18C Na2 O2C 138.9(8) . 3_657 ?
O4C Na2 O2C 42.0(5) 3_657 3_657 ?
Na2 Na2 O2C 122.7(5) 3_657 3_657 ?
O12C Na2 O2C 100.1(6) . 3_657 ?
O3C Na2 O2C 85.8(5) . 3_657 ?
O18C Na2 O2C 82.4(7) 3_657 3_657 ?
O1C Na2 O2C 90.7(4) 3_657 3_657 ?
Na1 Na2 O1C 61.8(2) . . ?
O18C Na2 O1C 104.0(7) . . ?
O4C Na2 O1C 90.9(4) 3_657 . ?
Na2 Na2 O1C 61.8(2) 3_657 . ?
O12C Na2 O1C 42.7(7) . . ?
O3C Na2 O1C 121.1(3) . . ?
O18C Na2 O1C 51.7(5) 3_657 . ?
O1C Na2 O1C 128.4(2) 3_657 . ?
O2C Na2 O1C 116.7(5) 3_657 . ?
Na1 Na2 O4C 47.8(3) . . ?
O18C Na2 O4C 36.9(6) . . ?
O4C Na2 O4C 129.5(3) 3_657 . ?
Na2 Na2 O4C 47.8(3) 3_657 . ?
O12C Na2 O4C 90.6(5) . . ?
O3C Na2 O4C 101.8(4) . . ?
O18C Na2 O4C 93.0(5) 3_657 . ?
O1C Na2 O4C 78.4(3) 3_657 . ?
O2C Na2 O4C 167.8(5) 3_657 . ?
O1C Na2 O4C 67.7(3) . . ?
O12C O1C Na1 87.1(7) . . ?
O12C O1C Na2 113.2(7) . 3_657 ?
Na1 O1C Na2 26.36(12) . 3_657 ?
O12C O1C Na2 62.2(6) . . ?
Na1 O1C Na2 25.21(12) . . ?
Na2 O1C Na2 51.6(2) 3_657 . ?
O2C O4C O18C 147.4(12) . . ?
O2C O4C Na2 81.4(8) . 3_657 ?
O18C O4C Na2 79.3(9) . 3_657 ?
O2C O4C Na1 109.8(8) . . ?
O18C O4C Na1 57.7(8) . . ?
Na2 O4C Na1 29.11(19) 3_657 . ?
O2C O4C Na2 130.5(8) . . ?
O18C O4C Na2 44.8(8) . . ?
Na2 O4C Na2 50.5(3) 3_657 . ?
Na1 O4C Na2 21.35(13) . . ?
O4C O2C Na2 56.6(6) . 3_657 ?
O4C O2C Na1 40.6(6) . . ?
Na2 O2C Na1 16.65(17) 3_657 . ?
O4C O18C Na1 74.7(9) . . ?
O4C O18C Na2 98.3(11) . . ?
Na1 O18C Na2 32.1(4) . . ?
O4C O18C Na2 57.5(7) . 3_657 ?
Na1 O18C Na2 25.8(3) . 3_657 ?
Na2 O18C Na2 57.9(6) . 3_657 ?
O1C O12C Na2 75.1(8) . . ?
O1C O12C Na1 53.3(6) . . ?
Na2 O12C Na1 22.1(2) . . ?

_refine_diff_density_max         1.992
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.122

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1443838'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        4
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H36 N6 Ni O10, H2O'
_chemical_formula_sum            'C30 H38 N6 Ni O11'
_chemical_formula_weight         715.36

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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                   18.780(4)
_cell_length_b                   18.110(4)
_cell_length_c                   9.200(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.22(5)
_cell_angle_gamma                90
_cell_volume                     3004.4(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1692
_cell_measurement_theta_min      2
_cell_measurement_theta_max      26.7

_exptl_crystal_description       prisme
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_F_000             1496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    0.668
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 CrystalClear (Rigaku-2011) was used for adsorption correction.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       'profile data from ω-scans'

_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            5619
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.249
_diffrn_reflns_theta_max         25.510
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             2984
_reflns_number_gt                2077
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear-SM Expert (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert  (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert  (Rigaku, 2011)'
_computing_structure_solution    'SIR2011 (POlidori 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C16(H14A,H14B)
2.b Primary CH refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12)
2.c Primary CH refined with riding coordinates:
 N3(H3)
2.d Primary CH refined with riding coordinates:
 O3(H3)

The Following ALERTS were generated by PLATON checkcif<<<

PLAT250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor 5.2 Note  
The low qualityy of crystals meant data collection could not
be carried out using a lab source and so beamline I19 at 
the Diamond Synchotron facility was used. The data presented
corrspond to the best collection available due to the 
poor quality of the crystals. Many of the
thermal parameters are elongated in the same direction. 

PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?)     O1W Check 
The hydrogen of the different hydratation water molecules were
 not located on Fourier map, but were added in the 
empirical formula to allow accurate determination 
of density and absorption coefficient.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1699P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2984
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0841
_refine_ls_wR_factor_ref         0.2671
_refine_ls_wR_factor_gt          0.2394
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3578(3) 0.2316(3) 0.0733(7) 0.091(2) Uani 1 1 d . . . . .
H1A H 0.3205 0.1979 0.0891 0.109 Uiso 1 1 calc R U . . .
H1B H 0.3341 0.2634 -0.0112 0.109 Uiso 1 1 calc R U . . .
C2 C 0.4565(3) 0.2312(3) -0.0579(7) 0.089(2) Uani 1 1 d . . . . .
H2A H 0.4212 0.2628 -0.1277 0.107 Uiso 1 1 calc R U . . .
H2B H 0.4766 0.1970 -0.1173 0.107 Uiso 1 1 calc R U . . .
C3 C 0.5193(3) 0.2787(3) 0.0381(7) 0.0875(19) Uani 1 1 d . . . . .
H3A H 0.5480 0.2993 -0.0251 0.105 Uiso 1 1 calc R U . . .
H3B H 0.4990 0.3192 0.0828 0.105 Uiso 1 1 calc R U . . .
C4 C 0.6130(3) 0.2791(3) 0.2842(7) 0.089(2) Uani 1 1 d . . . . .
H4A H 0.5828 0.3190 0.3050 0.107 Uiso 1 1 calc R U . . .
H4B H 0.6542 0.3005 0.2549 0.107 Uiso 1 1 calc R U . . .
C5 C 0.3863(3) 0.1201(2) -0.0447(6) 0.0705(15) Uani 1 1 d . . . . .
H5A H 0.3653 0.0907 0.0214 0.085 Uiso 1 1 calc R U . . .
H5B H 0.4262 0.0918 -0.0653 0.085 Uiso 1 1 calc R U . . .
C6 C 0.3260(3) 0.1336(3) -0.1947(6) 0.0710(14) Uani 1 1 d . . . . .
C7 C 0.2409(2) 0.0607(3) -0.3991(5) 0.0629(12) Uani 1 1 d . . . . .
C8 C 0.2092(3) 0.1187(3) -0.4930(6) 0.0729(15) Uani 1 1 d . . . . .
H8 H 0.2246 0.1669 -0.4667 0.087 Uiso 1 1 calc R U . . .
C9 C 0.1544(3) 0.1047(3) -0.6267(6) 0.0733(15) Uani 1 1 d . . . . .
H9 H 0.1328 0.1437 -0.6892 0.088 Uiso 1 1 calc R U . . .
C10 C 0.1317(3) 0.0331(3) -0.6676(6) 0.0679(14) Uani 1 1 d . . . . .
C11 C 0.1649(3) -0.0246(3) -0.5758(6) 0.0743(15) Uani 1 1 d . . . . .
H11 H 0.1512 -0.0730 -0.6045 0.089 Uiso 1 1 calc R U . . .
C12 C 0.2186(3) -0.0108(3) -0.4407(6) 0.0689(14) Uani 1 1 d . . . . .
H12 H 0.2397 -0.0499 -0.3778 0.083 Uiso 1 1 calc R U . . .
C13 C 0.0746(3) 0.0188(3) -0.8128(6) 0.0728(15) Uani 1 1 d . . . . .
C14 C 0.6163(4) 0.1838(3) 0.0988(8) 0.0893(19) Uani 1 1 d . . . . .
H14A H 0.6675 0.1985 0.1421 0.107 Uiso 1 1 calc R U . . .
H14B H 0.6044 0.1907 -0.0099 0.107 Uiso 1 1 calc R U . . .
C15 C 0.6088(3) 0.1020(3) 0.1314(6) 0.0725(15) Uani 1 1 d . . . . .
N1 N 0.4169(2) 0.1886(2) 0.0343(5) 0.0712(13) Uani 1 1 d . . . . .
N2 N 0.5680(2) 0.2325(2) 0.1594(5) 0.0727(13) Uani 1 1 d . . . . .
N3 N 0.2962(2) 0.0694(2) -0.2612(4) 0.0624(11) Uani 1 1 d . . . . .
H3 H 0.3132 0.0294 -0.2134 0.075 Uiso 1 1 calc R U . . .
O1 O 0.3073(2) 0.1949(2) -0.2459(5) 0.1014(16) Uani 1 1 d . . . . .
O2 O 0.0440(2) 0.0730(2) -0.8938(4) 0.0836(12) Uani 1 1 d . . . . .
O1W O 0.5000 0.0655(4) -0.2500 0.175(5) Uani 1 2 d S T P . .
O3 O 0.0571(2) -0.0481(2) -0.8487(4) 0.0822(12) Uani 1 1 d . . . . .
H3C H 0.0252 -0.0493 -0.9304 0.123 Uiso 1 1 calc R U . . .
O4 O 0.55889(19) 0.08349(18) 0.1909(4) 0.0685(10) Uani 1 1 d . . . . .
O5 O 0.6527(2) 0.0589(2) 0.0969(5) 0.0879(12) Uani 1 1 d . . . . .
Ni1 Ni 0.5000 0.16424(4) 0.2500 0.0640(4) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.481(7) . ?
C1 C4 1.535(7) 2_655 ?
C2 N1 1.490(7) . ?
C2 C3 1.526(6) . ?
C3 N2 1.487(6) . ?
C4 N2 1.484(6) . ?
C4 C1 1.535(7) 2_655 ?
C5 N1 1.471(5) . ?
C5 C6 1.540(6) . ?
C6 O1 1.219(6) . ?
C6 N3 1.361(6) . ?
C7 C8 1.384(7) . ?
C7 C12 1.383(7) . ?
C7 N3 1.406(5) . ?
C8 C9 1.389(6) . ?
C9 C10 1.384(6) . ?
C10 C11 1.378(7) . ?
C10 C13 1.484(6) . ?
C11 C12 1.387(6) . ?
C13 O2 1.268(6) . ?
C13 O3 1.274(6) . ?
C14 N2 1.481(8) . ?
C14 C15 1.525(7) . ?
C15 O5 1.239(7) . ?
C15 O4 1.255(7) . ?
N1 Ni1 2.200(3) . ?
N2 Ni1 2.109(5) . ?
O4 Ni1 1.999(4) . ?
Ni1 O4 1.999(4) 2_655 ?
Ni1 N2 2.109(5) 2_655 ?
Ni1 N1 2.200(3) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C4 112.8(4) . 2_655 ?
N1 C2 C3 113.0(5) . . ?
N2 C3 C2 109.3(4) . . ?
N2 C4 C1 109.4(4) . 2_655 ?
N1 C5 C6 113.3(4) . . ?
O1 C6 N3 124.6(4) . . ?
O1 C6 C5 123.5(4) . . ?
N3 C6 C5 111.9(4) . . ?
C8 C7 C12 119.5(4) . . ?
C8 C7 N3 124.0(4) . . ?
C12 C7 N3 116.4(4) . . ?
C7 C8 C9 119.9(4) . . ?
C10 C9 C8 120.5(4) . . ?
C11 C10 C9 119.5(4) . . ?
C11 C10 C13 120.6(4) . . ?
C9 C10 C13 119.9(4) . . ?
C10 C11 C12 120.2(5) . . ?
C7 C12 C11 120.4(4) . . ?
O2 C13 O3 122.8(4) . . ?
O2 C13 C10 119.3(4) . . ?
O3 C13 C10 117.9(4) . . ?
N2 C14 C15 113.8(5) . . ?
O5 C15 O4 125.1(5) . . ?
O5 C15 C14 117.1(6) . . ?
O4 C15 C14 117.8(5) . . ?
C5 N1 C1 110.3(4) . . ?
C5 N1 C2 110.1(5) . . ?
C1 N1 C2 113.1(4) . . ?
C5 N1 Ni1 110.9(3) . . ?
C1 N1 Ni1 106.1(3) . . ?
C2 N1 Ni1 106.0(3) . . ?
C4 N2 C14 110.7(5) . . ?
C4 N2 C3 111.0(4) . . ?
C14 N2 C3 111.4(5) . . ?
C4 N2 Ni1 107.7(4) . . ?
C14 N2 Ni1 107.6(3) . . ?
C3 N2 Ni1 108.3(3) . . ?
C6 N3 C7 127.5(4) . . ?
C15 O4 Ni1 117.4(3) . . ?
O4 Ni1 O4 85.9(2) . 2_655 ?
O4 Ni1 N2 168.15(17) . 2_655 ?
O4 Ni1 N2 83.05(17) 2_655 2_655 ?
O4 Ni1 N2 83.05(17) . . ?
O4 Ni1 N2 168.15(17) 2_655 . ?
N2 Ni1 N2 108.2(2) 2_655 . ?
O4 Ni1 N1 94.89(14) . 2_655 ?
O4 Ni1 N1 102.01(15) 2_655 2_655 ?
N2 Ni1 N1 83.18(16) 2_655 2_655 ?
N2 Ni1 N1 83.32(16) . 2_655 ?
O4 Ni1 N1 102.01(15) . . ?
O4 Ni1 N1 94.89(14) 2_655 . ?
N2 Ni1 N1 83.32(16) 2_655 . ?
N2 Ni1 N1 83.18(16) . . ?
N1 Ni1 N1 156.87(19) 2_655 . ?

_refine_diff_density_max         0.896
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.087

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1443839'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        5
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H34 N6 O11 Zn2, 3H2O'
_chemical_formula_sum            'C30 H40 N6 O14 Zn2'
_chemical_formula_weight         839.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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                   10.830(16)
_cell_length_b                   18.480(2)
_cell_length_c                   16.550(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.90(2)
_cell_angle_gamma                90
_cell_volume                     3215.3(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2156
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      20.3

_exptl_crystal_description       prisme
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    1.446
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           'synchrotron radiation'
_diffrn_source                   'synchrotron radiation'
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       
;
'profile data from ω-scans'
;

_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            8378
_diffrn_reflns_av_unetI/netI     0.1606
_diffrn_reflns_av_R_equivalents  0.1174
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.044
_diffrn_reflns_theta_max         21.003
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.589
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.589
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.589
_reflns_number_total             3420
_reflns_number_gt                1497
_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       'M2DM bruker'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SIR2011 (POlidori 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), 

C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
C9(H9A, H9B), C18(H18A,H18B), C20(H20A,H20B), 
C29(H29A,H29B),  
2.b Primary CH refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C23(H23), 
C24(H24), C26(H26), C27(H27), 
2.c Primary CH refined with riding coordinates:
 N5(H5), N6(H6),  
2.d Primary CH refined with riding coordinates:
 O3(H3)

Alert level A
THETM01_ALERT_3_A  The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.5203
PLAT234_ALERT_4_A Large Hirshfeld Difference C1     --  C2      ..       0.42 Ang.  
And 4 other PLAT234 Alerts
Less ...
PLAT234_ALERT_4_A Large Hirshfeld Difference C3     --  C4      ..       0.39 Ang.  
PLAT234_ALERT_4_A Large Hirshfeld Difference C5     --  C6      ..       0.41 Ang.  
PLAT234_ALERT_4_A Large Hirshfeld Difference C7     --  C8      ..       0.47 Ang.  
PLAT234_ALERT_4_A Large Hirshfeld Difference C24    --  C25     ..       0.33 Ang.  

PLAT410_ALERT_2_A Short Intra H...H Contact  H7B    ..  H29B    ..       1.79 Ang.  
Alert level B
REFNR01_ALERT_3_B  Ratio of reflections to parameters is < 8 for a
            centrosymmetric structure
            sine(theta)/lambda                0.5203
            Proportion of unique data used    1.0000
            Ratio reflections to parameters   7.2921
   
PLAT088_ALERT_3_B Poor Data / Parameter Ratio ....................       7.29 Note  
PLAT213_ALERT_2_B Atom C5              has ADP max/min Ratio .....        4.7 prolat
PLAT234_ALERT_4_B Large Hirshfeld Difference N1     --  C9      ..       0.28 Ang.  
And 2 other PLAT234 Alerts
Less ...
PLAT234_ALERT_4_B Large Hirshfeld Difference C12    --  C13     ..       0.26 Ang.  
PLAT234_ALERT_4_B Large Hirshfeld Difference C14    --  C15     ..       0.26 Ang.  

PLAT241_ALERT_2_B High   'MainMol' Ueq as Compared to Neighbors of         C4 Check 
And 3 other PLAT241 Alerts
Less ...
PLAT241_ALERT_2_B High   'MainMol' Ueq as Compared to Neighbors of         C5 Check 
PLAT241_ALERT_2_B High   'MainMol' Ueq as Compared to Neighbors of         C6 Check 
PLAT241_ALERT_2_B High   'MainMol' Ueq as Compared to Neighbors of         C8 Check 

PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O2W Check 
And 2 other PLAT306 Alerts
More ...PLAT341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............    0.03636 Ang.  
PLAT360_ALERT_2_B Short  C(sp3)-C(sp3) Bond   C1     -   C2     ..       1.28 Ang.  
PLAT360_ALERT_2_B Short  C(sp3)-C(sp3) Bond   C5     -   C6     ..       1.31 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3W    ..  O7      ..       2.73 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O4W    ..  O6      ..       2.63 Ang.  
PLAT920_ALERT_1_B Theta(Max)  in CIF and FCF Differ by ...........       0.67 Degree

RESPONSE: The sample diffracted very weakly, and at high angles the
reflections were completely absent, even when subjected to synchrotron radiation. Dispite the poor quality of the data, the connectivity and gross conformation are not in doubt.
Furthermore, Structure 5 show extensive disorder within the macrocyclic entity. 

The hydrogen of the different hydratation water molecules present in all six structures were not located on Fourier map, but were added in the empirical formula to allow accurate determination of density and absorption coefficient. 


;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1397P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3420
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1989
_refine_ls_R_factor_gt           0.0951
_refine_ls_wR_factor_ref         0.2896
_refine_ls_wR_factor_gt          0.2204
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.510(3) 0.315(2) 0.376(2) 0.20(2) Uani 1 1 d . . . . .
H1A H 0.4836 0.3299 0.4257 0.236 Uiso 1 1 calc R U . . .
H1B H 0.4874 0.2641 0.3671 0.236 Uiso 1 1 calc R U . . .
C2 C 0.631(4) 0.3199(15) 0.3913(17) 0.179(16) Uani 1 1 d . . . . .
H2A H 0.6674 0.2843 0.4335 0.215 Uiso 1 1 calc R U . . .
H2B H 0.6551 0.3673 0.4152 0.215 Uiso 1 1 calc R U . . .
C3 C 0.814(3) 0.3489(12) 0.334(2) 0.174(16) Uani 1 1 d . . . . .
H3A H 0.8572 0.3478 0.3929 0.209 Uiso 1 1 calc R U . . .
H3B H 0.8652 0.3208 0.3050 0.209 Uiso 1 1 calc R U . . .
C4 C 0.814(3) 0.419(2) 0.3079(17) 0.194(14) Uani 1 1 d . . . . .
H4A H 0.7844 0.4500 0.3467 0.232 Uiso 1 1 calc R U . . .
H4B H 0.9014 0.4332 0.3098 0.232 Uiso 1 1 calc R U . . .
C5 C 0.686(4) 0.5109(12) 0.223(2) 0.22(2) Uani 1 1 d . . . . .
H5A H 0.7516 0.5421 0.2551 0.264 Uiso 1 1 calc R U . . .
H5B H 0.6731 0.5258 0.1650 0.264 Uiso 1 1 calc R U . . .
C6 C 0.580(4) 0.5251(15) 0.245(2) 0.22(2) Uani 1 1 d . . . . .
H6A H 0.5544 0.5746 0.2308 0.270 Uiso 1 1 calc R U . . .
H6B H 0.5947 0.5201 0.3053 0.270 Uiso 1 1 calc R U . . .
C7 C 0.383(3) 0.4786(16) 0.2545(17) 0.181(15) Uani 1 1 d . . . . .
H7A H 0.3802 0.5270 0.2765 0.218 Uiso 1 1 calc R U . . .
H7B H 0.3015 0.4697 0.2162 0.218 Uiso 1 1 calc R U . . .
C8 C 0.396(4) 0.4292(16) 0.321(3) 0.25(3) Uani 1 1 d . . . . .
H8A H 0.3164 0.4263 0.3381 0.304 Uiso 1 1 calc R U . . .
H8B H 0.4606 0.4471 0.3686 0.304 Uiso 1 1 calc R U . . .
C9 C 0.314(2) 0.3153(10) 0.2673(14) 0.129(9) Uani 1 1 d . . . . .
H9A H 0.2478 0.3460 0.2345 0.155 Uiso 1 1 calc R U . . .
H9B H 0.2830 0.2958 0.3132 0.155 Uiso 1 1 calc R U . . .
C10 C 0.342(3) 0.2548(12) 0.2145(12) 0.104(7) Uani 1 1 d . . . . .
C11 C 0.262(2) 0.1427(10) 0.1466(12) 0.079(5) Uani 1 1 d . . . . .
C12 C 0.374(2) 0.1055(11) 0.1464(12) 0.093(6) Uani 1 1 d . . . . .
H12 H 0.4501 0.1212 0.1809 0.111 Uiso 1 1 calc R U . . .
C13 C 0.374(2) 0.0438(12) 0.0943(15) 0.096(6) Uani 1 1 d . . . . .
H13 H 0.4485 0.0196 0.0917 0.116 Uiso 1 1 calc R U . . .
C14 C 0.258(3) 0.0236(10) 0.0495(12) 0.082(5) Uani 1 1 d . . . . .
C15 C 0.149(2) 0.0578(13) 0.0487(11) 0.100(6) Uani 1 1 d . . . . .
H15 H 0.0726 0.0419 0.0142 0.120 Uiso 1 1 calc R U . . .
C16 C 0.151(2) 0.1169(10) 0.0999(14) 0.092(6) Uani 1 1 d . . . . .
H16 H 0.0749 0.1392 0.1023 0.110 Uiso 1 1 calc R U . . .
C17 C 0.258(3) -0.0455(13) -0.0029(14) 0.111(9) Uani 1 1 d . . . . .
C18 C 0.700(2) 0.2354(9) 0.3008(11) 0.106(7) Uani 1 1 d . . . . .
H18A H 0.7800 0.2161 0.3331 0.127 Uiso 1 1 calc R U . . .
H18B H 0.6318 0.2072 0.3139 0.127 Uiso 1 1 calc R U . . .
C19 C 0.6954(17) 0.2279(10) 0.2126(11) 0.080(5) Uani 1 1 d . . . . .
C20 C 0.7945(18) 0.4203(9) 0.1558(10) 0.086(6) Uani 1 1 d . . . . .
H20A H 0.7287 0.4297 0.1057 0.103 Uiso 1 1 calc R U . . .
H20B H 0.8189 0.3698 0.1548 0.103 Uiso 1 1 calc R U . . .
C21 C 0.914(2) 0.4692(10) 0.1548(13) 0.091(7) Uani 1 1 d . . . . .
C22 C 0.966(3) 0.5729(10) 0.0738(16) 0.100(7) Uani 1 1 d . . . . .
C23 C 1.083(3) 0.5864(9) 0.1166(14) 0.092(6) Uani 1 1 d . . . . .
H23 H 1.1159 0.5625 0.1666 0.111 Uiso 1 1 calc R U . . .
C24 C 1.159(2) 0.6380(10) 0.0860(14) 0.090(6) Uani 1 1 d . . . . .
H24 H 1.2442 0.6448 0.1130 0.108 Uiso 1 1 calc R U . . .
C25 C 1.105(3) 0.6772(12) 0.016(2) 0.111(8) Uani 1 1 d . . . . .
C26 C 0.985(3) 0.6653(10) -0.0285(15) 0.112(7) Uani 1 1 d . . . . .
H26 H 0.9510 0.6916 -0.0767 0.135 Uiso 1 1 calc R U . . .
C27 C 0.911(2) 0.6122(11) -0.0004(14) 0.113(7) Uani 1 1 d . . . . .
H27 H 0.8280 0.6029 -0.0297 0.135 Uiso 1 1 calc R U . . .
C28 C 1.176(3) 0.7353(12) -0.012(2) 0.119(10) Uani 1 1 d . . . . .
C29 C 0.413(2) 0.4897(10) 0.1186(17) 0.117(7) Uani 1 1 d . . . . .
H29A H 0.4433 0.5341 0.0988 0.141 Uiso 1 1 calc R U . . .
H29B H 0.3232 0.4959 0.1163 0.141 Uiso 1 1 calc R U . . .
C30 C 0.428(2) 0.4296(13) 0.0630(15) 0.100(6) Uani 1 1 d . . . . .
O1 O 0.4384(16) 0.2565(7) 0.1873(9) 0.125(5) Uani 1 1 d . . . . .
O2 O 0.3544(18) -0.0835(7) 0.0039(9) 0.125(6) Uani 1 1 d . . . . .
O1W O 0.4922(13) 0.2129(7) 0.0299(8) 0.119(4) Uani 1 1 d . . . . .
O3 O 0.1602(18) -0.0603(9) -0.0564(11) 0.135(6) Uani 1 1 d . . . . .
O2W O 0.0296(14) 0.2230(8) 0.2446(9) 0.136(5) Uani 1 1 d . . . . .
O4 O 0.6736(12) 0.2819(6) 0.1637(7) 0.092(4) Uani 1 1 d . . . . .
O3W O 1.506(2) 0.6757(8) 0.0917(13) 0.204(9) Uani 1 1 d . . . . .
O5 O 0.7075(12) 0.1649(6) 0.1824(7) 0.096(4) Uani 1 1 d . . . . .
O4W O 1.091(4) 0.368(2) 0.322(4) 0.52(3) Uani 1 1 d . . . . .
O6 O 1.0106(16) 0.4634(8) 0.2031(10) 0.121(5) Uani 1 1 d . . . . .
O7 O 1.2879(18) 0.7493(8) 0.0229(12) 0.146(8) Uani 1 1 d . . . . .
O8 O 1.1245(15) 0.7726(8) -0.0787(12) 0.135(6) Uani 1 1 d . . . . .
O9 O 0.4887(14) 0.3741(8) 0.0904(9) 0.114(5) Uani 1 1 d . . . . .
O10 O 0.3736(14) 0.4409(8) -0.0145(11) 0.125(5) Uani 1 1 d . . . . .
Zn1 Zn 0.5634(2) 0.36335(10) 0.21144(13) 0.0901(9) Uani 1 1 d . . . . .
Zn2 Zn 0.6812(3) 0.17267(11) 0.05962(14) 0.1022(10) Uani 1 1 d . . . . .
N1 N 0.431(2) 0.3591(11) 0.3004(13) 0.133(7) Uani 1 1 d . . . . .
N2 N 0.688(2) 0.3106(9) 0.3243(10) 0.121(6) Uani 1 1 d . . . . .
N3 N 0.7415(16) 0.4326(8) 0.2291(10) 0.100(5) Uani 1 1 d . . . . .
N4 N 0.482(2) 0.4776(9) 0.2059(14) 0.112(6) Uani 1 1 d . . . . .
N5 N 0.2548(18) 0.2027(8) 0.1966(10) 0.104(5) Uani 1 1 d . . . . .
H5 H 0.1893 0.2063 0.2172 0.125 Uiso 1 1 calc R U . . .
N6 N 0.8818(15) 0.5205(8) 0.0939(10) 0.094(5) Uani 1 1 d . . . . .
H6 H 0.8042 0.5212 0.0653 0.113 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
C1 C2 1.28(4) . ?
C1 N1 1.57(4) . ?
C2 N2 1.40(3) . ?
C3 C4 1.37(3) . ?
C3 N2 1.51(3) . ?
C4 N3 1.37(3) . ?
C5 C6 1.32(4) . ?
C5 N3 1.56(3) . ?
C6 N4 1.41(3) . ?
C7 C8 1.42(4) . ?
C7 N4 1.49(3) . ?
C8 N1 1.42(3) . ?
C9 N1 1.49(2) . ?
C9 C10 1.50(2) . ?
C10 O1 1.23(2) . ?
C10 N5 1.33(2) . ?
C11 C16 1.36(2) . ?
C11 C12 1.39(2) . ?
C11 N5 1.40(2) . ?
C12 C13 1.43(2) . ?
C13 C14 1.35(2) . ?
C14 C15 1.34(2) . ?
C14 C17 1.54(3) . ?
C15 C16 1.38(2) . ?
C17 O2 1.24(3) . ?
C17 O3 1.24(3) . ?
C18 C19 1.46(2) . ?
C18 N2 1.46(2) . ?
C19 O4 1.271(17) . ?
C19 O5 1.286(17) . ?
C20 N3 1.48(2) . ?
C20 C21 1.58(3) . ?
C21 O6 1.16(2) . ?
C21 N6 1.37(2) . ?
C22 C23 1.32(3) . ?
C22 N6 1.43(2) . ?
C22 C27 1.43(3) . ?
C23 C24 1.43(3) . ?
C24 C25 1.37(3) . ?
C25 C26 1.36(3) . ?
C25 C28 1.46(3) . ?
C26 C27 1.41(3) . ?
C28 O7 1.24(3) . ?
C28 O8 1.30(3) . ?
C28 Zn2 2.55(2) 3_765 ?
C29 N4 1.48(2) . ?
C29 C30 1.48(3) . ?
C30 O9 1.24(2) . ?
C30 O10 1.29(2) . ?
O1 Zn1 2.374(14) . ?
O2 Zn2 1.943(14) 3_655 ?
O1W Zn2 2.122(14) . ?
O4 Zn1 2.183(10) . ?
O5 Zn2 1.987(11) . ?
O7 Zn2 2.068(18) 3_765 ?
O8 Zn2 2.287(15) 3_765 ?
O9 Zn1 1.982(15) . ?
Zn1 N2 2.246(18) . ?
Zn1 N3 2.274(15) . ?
Zn1 N4 2.280(15) . ?
Zn1 N1 2.289(16) . ?
Zn2 O2 1.943(14) 3_655 ?
Zn2 O7 2.068(18) 3_765 ?
Zn2 O8 2.287(15) 3_765 ?
Zn2 C28 2.55(2) 3_765 ?

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
C2 C1 N1 117(3) . . ?
C1 C2 N2 117(3) . . ?
C4 C3 N2 119(2) . . ?
N3 C4 C3 115(3) . . ?
C6 C5 N3 121(3) . . ?
C5 C6 N4 111(3) . . ?
C8 C7 N4 118(2) . . ?
C7 C8 N1 112(2) . . ?
N1 C9 C10 110.1(19) . . ?
O1 C10 N5 123.7(19) . . ?
O1 C10 C9 120(2) . . ?
N5 C10 C9 116(2) . . ?
C16 C11 C12 118.7(18) . . ?
C16 C11 N5 116(2) . . ?
C12 C11 N5 125(2) . . ?
C11 C12 C13 121.6(19) . . ?
C14 C13 C12 114.5(18) . . ?
C15 C14 C13 125(2) . . ?
C15 C14 C17 120(2) . . ?
C13 C14 C17 114(2) . . ?
C14 C15 C16 119(2) . . ?
C11 C16 C15 121(2) . . ?
O2 C17 O3 120(2) . . ?
O2 C17 C14 122(3) . . ?
O3 C17 C14 118(3) . . ?
C19 C18 N2 112.0(14) . . ?
O4 C19 O5 118.9(15) . . ?
O4 C19 C18 121.4(15) . . ?
O5 C19 C18 119.6(16) . . ?
N3 C20 C21 113.5(13) . . ?
O6 C21 N6 127(2) . . ?
O6 C21 C20 123.1(19) . . ?
N6 C21 C20 110.0(18) . . ?
C23 C22 N6 126(2) . . ?
C23 C22 C27 121(2) . . ?
N6 C22 C27 113(2) . . ?
C22 C23 C24 120(2) . . ?
C25 C24 C23 119(2) . . ?
C26 C25 C24 122(2) . . ?
C26 C25 C28 117(3) . . ?
C24 C25 C28 121(3) . . ?
C25 C26 C27 119(2) . . ?
C26 C27 C22 119(2) . . ?
O7 C28 O8 117(2) . . ?
O7 C28 C25 122(3) . . ?
O8 C28 C25 121(3) . . ?
O7 C28 Zn2 53.6(13) . 3_765 ?
O8 C28 Zn2 63.6(11) . 3_765 ?
C25 C28 Zn2 174(2) . 3_765 ?
N4 C29 C30 112.9(18) . . ?
O9 C30 O10 125(2) . . ?
O9 C30 C29 121(2) . . ?
O10 C30 C29 114(2) . . ?
C10 O1 Zn1 117.3(14) . . ?
C17 O2 Zn2 112.3(18) . 3_655 ?
C19 O4 Zn1 110.1(10) . . ?
C19 O5 Zn2 109.3(11) . . ?
C28 O7 Zn2 97.4(18) . 3_765 ?
C28 O8 Zn2 85.8(16) . 3_765 ?
C30 O9 Zn1 120.2(15) . . ?
O9 Zn1 O4 80.1(5) . . ?
O9 Zn1 N2 154.4(6) . . ?
O4 Zn1 N2 74.4(5) . . ?
O9 Zn1 N3 101.6(6) . . ?
O4 Zn1 N3 85.1(5) . . ?
N2 Zn1 N3 79.4(7) . . ?
O9 Zn1 N4 78.9(7) . . ?
O4 Zn1 N4 149.6(6) . . ?
N2 Zn1 N4 125.7(7) . . ?
N3 Zn1 N4 78.0(7) . . ?
O9 Zn1 N1 119.1(8) . . ?
O4 Zn1 N1 133.6(6) . . ?
N2 Zn1 N1 78.1(8) . . ?
N3 Zn1 N1 125.4(6) . . ?
N4 Zn1 N1 76.3(8) . . ?
O9 Zn1 O1 80.5(5) . . ?
O4 Zn1 O1 72.8(5) . . ?
N2 Zn1 O1 89.0(6) . . ?
N3 Zn1 O1 157.2(6) . . ?
N4 Zn1 O1 124.3(7) . . ?
N1 Zn1 O1 70.1(6) . . ?
O2 Zn2 O5 116.9(5) 3_655 . ?
O2 Zn2 O7 106.1(6) 3_655 3_765 ?
O5 Zn2 O7 136.0(6) . 3_765 ?
O2 Zn2 O1W 96.7(7) 3_655 . ?
O5 Zn2 O1W 98.9(5) . . ?
O7 Zn2 O1W 84.4(6) 3_765 . ?
O2 Zn2 O8 120.4(7) 3_655 3_765 ?
O5 Zn2 O8 89.4(6) . 3_765 ?
O7 Zn2 O8 59.6(6) 3_765 3_765 ?
O1W Zn2 O8 133.0(5) . 3_765 ?
O2 Zn2 C28 117.2(7) 3_655 3_765 ?
O5 Zn2 C28 114.4(8) . 3_765 ?
O7 Zn2 C28 28.9(8) 3_765 3_765 ?
O1W Zn2 C28 108.6(8) . 3_765 ?
O8 Zn2 C28 30.7(8) 3_765 3_765 ?
C8 N1 C9 109(2) . . ?
C8 N1 C1 114(3) . . ?
C9 N1 C1 105(2) . . ?
C8 N1 Zn1 111.8(15) . . ?
C9 N1 Zn1 113.1(12) . . ?
C1 N1 Zn1 103.2(15) . . ?
C2 N2 C18 114.4(18) . . ?
C2 N2 C3 114(2) . . ?
C18 N2 C3 109.8(18) . . ?
C2 N2 Zn1 108.4(17) . . ?
C18 N2 Zn1 105.5(12) . . ?
C3 N2 Zn1 103.5(13) . . ?
C4 N3 C20 120.2(19) . . ?
C4 N3 C5 111(2) . . ?
C20 N3 C5 107.7(16) . . ?
C4 N3 Zn1 107.3(15) . . ?
C20 N3 Zn1 106.9(10) . . ?
C5 N3 Zn1 102.3(15) . . ?
C6 N4 C29 120(2) . . ?
C6 N4 C7 108(3) . . ?
C29 N4 C7 105(2) . . ?
C6 N4 Zn1 108.5(15) . . ?
C29 N4 Zn1 106.3(11) . . ?
C7 N4 Zn1 108.2(14) . . ?
C10 N5 C11 124.4(18) . . ?
C21 N6 C22 125.5(19) . . ?

_refine_diff_density_max         0.372
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.090

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1443840'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        6
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H34 N6 Ni O11 Zn, 8H2O'
_chemical_formula_sum            'C30 H50 N6 Ni O19 Zn'
_chemical_formula_weight         922.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   11.360(3)
_cell_length_b                   22.080(3)
_cell_length_c                   15.560(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.20(3)
_cell_angle_gamma                90
_cell_volume                     3902.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    576
_cell_measurement_theta_min      1
_cell_measurement_theta_max      40

_exptl_crystal_description       prisme
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_absorpt_coefficient_mu    1.084
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.70109
_diffrn_radiation_type           'synchrotron radiation'
_diffrn_source                   'synchrotron radiation'
_diffrn_measurement_device_type  'PILATUS DECTRIS 6M'
_diffrn_measurement_method       'Phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            111901
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.216
_diffrn_reflns_theta_max         22.891
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measured_fraction_theta_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_point_group_measured_fraction_full 0.713
_reflns_number_total             5038
_reflns_number_gt                4415
_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       'M2DM bruker'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SIR2011 (POlidori 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), 

C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
C9(H9A, H9B), C18(H18A,H18B), C20(H20A,H20B), 
C29(H29A,H29B),  
2.b Primary CH refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C23(H23), 
C24(H24), C26(H26), C27(H27), 
2.c Primary CH refined with riding coordinates:
 N5(H5), N6(H6),  
2.d Primary CH refined with riding coordinates:
 O3(H3)

The Following ALERTS were generated by PLATON checkcif<<<


RFACR01_ALERT_3_B  The value of the weighted R factor is > 0.35
            Weighted R factor given   0.352

THETM01_ALERT_3_B  The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5548

PLAT043_ALERT_1_B Calculated and Reported Mol. Weight Differ by ..      16.00 Check 


PLAT051_ALERT_1_B Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       8.29 %     
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O2W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O4W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O5W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O6W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O7W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O8W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O9W Check 
More ...PLAT430_ALERT_2_B Short Inter D...A Contact  O1     ..  O7W     ..       2.67 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O1W    ..  O7W     ..       2.73 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O2     ..  O2W     ..       2.82 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W    ..  O6W     ..       2.75 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3     ..  O3W     ..       2.78 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3W    ..  O9      ..       2.67 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3W    ..  O6W     ..       2.83 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O5W    ..  O8W     ..       2.73 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O5W    ..  O5W     ..       2.77 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O5W    ..  O7W     ..       2.79 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O6W    ..  O7W     ..       2.82 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O8     ..  O8W     ..       2.72 Ang.  

These alerts arise because of missing water molecules in the model resulting in apparent large structural voids and missing H-bonds

PLAT911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L=  0.565        642 Report

The exxplanation of this alert is that the data collection is performed with a rotation about one single axis. For this reason some data are missing.

PLAT934_ALERT_3_B Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          3 Check 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.2000P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5038
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.1057
_refine_ls_wR_factor_ref         0.3522
_refine_ls_wR_factor_gt          0.3426
_refine_ls_goodness_of_fit_ref   1.669
_refine_ls_restrained_S_all      1.669
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6860(7) 0.2633(4) 0.9114(7) 0.063(2) Uani 1 1 d . . . . .
H1A H 0.7067 0.2701 0.9712 0.075 Uiso 1 1 calc R U . . .
H1B H 0.7348 0.2895 0.8763 0.075 Uiso 1 1 calc R U . . .
C2 C 0.7105(8) 0.1952(5) 0.8874(7) 0.068(3) Uani 1 1 d . . . . .
H2A H 0.7049 0.1900 0.8256 0.082 Uiso 1 1 calc R U . . .
H2B H 0.7895 0.1841 0.9052 0.082 Uiso 1 1 calc R U . . .
C3 C 0.6180(7) 0.0954(4) 0.8908(6) 0.056(2) Uani 1 1 d . . . . .
H3A H 0.6818 0.0703 0.9122 0.067 Uiso 1 1 calc R U . . .
H3B H 0.6264 0.0992 0.8290 0.067 Uiso 1 1 calc R U . . .
C4 C 0.4998(7) 0.0660(4) 0.9120(5) 0.0493(19) Uani 1 1 d . . . . .
H4A H 0.4915 0.0290 0.8788 0.059 Uiso 1 1 calc R U . . .
H4B H 0.4990 0.0550 0.9724 0.059 Uiso 1 1 calc R U . . .
C5 C 0.3585(8) 0.1013(4) 0.8013(5) 0.055(2) Uani 1 1 d . . . . .
H5A H 0.2754 0.1112 0.7978 0.066 Uiso 1 1 calc R U . . .
H5B H 0.3686 0.0601 0.7809 0.066 Uiso 1 1 calc R U . . .
C6 C 0.4283(9) 0.1445(4) 0.7444(5) 0.061(2) Uani 1 1 d . . . . .
H6A H 0.5095 0.1312 0.7411 0.073 Uiso 1 1 calc R U . . .
H6B H 0.3955 0.1444 0.6867 0.073 Uiso 1 1 calc R U . . .
C7 C 0.5192(10) 0.2473(5) 0.7466(6) 0.070(3) Uani 1 1 d . . . . .
H7A H 0.4983 0.2621 0.6899 0.084 Uiso 1 1 calc R U . . .
H7B H 0.5930 0.2254 0.7423 0.084 Uiso 1 1 calc R U . . .
C8 C 0.5329(10) 0.3001(4) 0.8082(6) 0.069(3) Uani 1 1 d . . . . .
H8A H 0.5967 0.3258 0.7889 0.082 Uiso 1 1 calc R U . . .
H8B H 0.4612 0.3239 0.8079 0.082 Uiso 1 1 calc R U . . .
C9 C 0.5228(7) 0.3270(4) 0.9586(6) 0.050(2) Uani 1 1 d . . . . .
H9A H 0.5496 0.3159 1.0157 0.060 Uiso 1 1 calc R U . . .
H9B H 0.4375 0.3295 0.9599 0.060 Uiso 1 1 calc R U . . .
C10 C 0.5717(7) 0.3879(4) 0.9363(6) 0.054(2) Uani 1 1 d . . . . .
C11 C 0.5151(7) 0.4921(4) 0.8907(5) 0.051(2) Uani 1 1 d . . . . .
C12 C 0.4154(8) 0.5246(4) 0.8664(6) 0.063(2) Uani 1 1 d . . . . .
H12 H 0.3417 0.5063 0.8689 0.076 Uiso 1 1 calc R U . . .
C13 C 0.4250(8) 0.5838(4) 0.8385(6) 0.059(2) Uani 1 1 d . . . . .
H13 H 0.3580 0.6053 0.8224 0.071 Uiso 1 1 calc R U . . .
C14 C 0.5316(8) 0.6104(4) 0.8347(5) 0.057(2) Uani 1 1 d . . . . .
C15 C 0.6337(8) 0.5793(5) 0.8589(6) 0.064(2) Uani 1 1 d . . . . .
H15 H 0.7065 0.5985 0.8565 0.076 Uiso 1 1 calc R U . . .
C16 C 0.6259(8) 0.5179(4) 0.8873(6) 0.055(2) Uani 1 1 d . . . . .
H16 H 0.6927 0.4962 0.9030 0.067 Uiso 1 1 calc R U . . .
C17 C 0.5396(9) 0.6772(5) 0.8052(6) 0.064(2) Uani 1 1 d . . . . .
C18 C 0.6461(7) 0.1505(4) 1.0242(5) 0.053(2) Uani 1 1 d . . . . .
H18A H 0.7174 0.1726 1.0383 0.064 Uiso 1 1 calc R U . . .
H18B H 0.6586 0.1083 1.0391 0.064 Uiso 1 1 calc R U . . .
C19 C 0.5454(7) 0.1753(4) 1.0767(5) 0.047(2) Uani 1 1 d . . . . .
C20 C 0.2966(6) 0.0918(4) 0.9514(5) 0.0468(19) Uani 1 1 d . . . . .
H20A H 0.3251 0.0881 1.0100 0.056 Uiso 1 1 calc R U . . .
H20B H 0.2425 0.1258 0.9495 0.056 Uiso 1 1 calc R U . . .
C21 C 0.2304(7) 0.0354(4) 0.9286(5) 0.049(2) Uani 1 1 d . . . . .
C22 C 0.0284(6) -0.0001(3) 0.8890(5) 0.0404(17) Uani 1 1 d . . . . .
C23 C 0.0408(7) -0.0623(4) 0.8981(5) 0.049(2) Uani 1 1 d . . . . .
H23 H 0.1109 -0.0790 0.9181 0.059 Uiso 1 1 calc R U . . .
C24 C -0.0535(7) -0.0989(4) 0.8768(5) 0.0480(19) Uani 1 1 d . . . . .
H24 H -0.0480 -0.1404 0.8866 0.058 Uiso 1 1 calc R U . . .
C25 C -0.1531(6) -0.0764(4) 0.8422(5) 0.0439(19) Uani 1 1 d . . . . .
C26 C -0.1638(7) -0.0141(4) 0.8307(5) 0.050(2) Uani 1 1 d . . . . .
H26 H -0.2321 0.0021 0.8069 0.060 Uiso 1 1 calc R U . . .
C27 C -0.0747(7) 0.0225(4) 0.8540(5) 0.050(2) Uani 1 1 d . . . . .
H27 H -0.0826 0.0641 0.8464 0.060 Uiso 1 1 calc R U . . .
C28 C -0.2567(8) -0.1163(4) 0.8151(6) 0.055(2) Uani 1 1 d . . . . .
C29 C 0.3122(9) 0.2343(5) 0.7668(6) 0.070(3) Uani 1 1 d . . . . .
H29A H 0.2581 0.2055 0.7410 0.084 Uiso 1 1 calc R U . . .
H29B H 0.3220 0.2676 0.7266 0.084 Uiso 1 1 calc R U . . .
C30 C 0.2596(8) 0.2580(4) 0.8468(7) 0.063(2) Uani 1 1 d . . . . .
O1 O 0.6805(6) 0.3961(3) 0.9340(6) 0.081(2) Uani 1 1 d . . . . .
O2 O 0.4525(7) 0.6978(3) 0.7689(6) 0.091(3) Uani 1 1 d . . . . .
O1W O 0.4511(6) 0.1978(3) 1.3323(5) 0.0661(19) Uani 1 1 d . . . . .
O3 O 0.6335(7) 0.7051(3) 0.8157(4) 0.0679(18) Uani 1 1 d . . . . .
O2W O 0.0250(5) 0.1640(3) 0.9049(4) 0.0671(17) Uani 1 1 d . . . . .
O4 O 0.4575(5) 0.1962(2) 1.0414(4) 0.0438(13) Uani 1 1 d . . . . .
O3W O 0.2063(7) 0.2993(3) 1.0491(5) 0.084(2) Uani 1 1 d . . . . .
O5 O 0.5568(5) 0.1725(3) 1.1580(4) 0.0622(16) Uani 1 1 d . . . . .
O4W O 0.2414(5) 0.4045(3) 0.9396(6) 0.081(2) Uani 1 1 d . . . . .
O6 O 0.2805(6) -0.0145(3) 0.9253(6) 0.090(3) Uani 1 1 d . . . . .
O5W O 0.0527(7) 0.4514(3) 1.0409(6) 0.090(2) Uani 1 1 d . . . . .
O7 O -0.2477(5) -0.1717(3) 0.8219(4) 0.0580(15) Uani 1 1 d . . . . .
O6W O 0.4794(7) 0.2519(3) 0.5312(5) 0.083(2) Uani 1 1 d . . . . .
O8 O -0.3498(6) -0.0915(4) 0.7893(6) 0.097(3) Uani 1 1 d . . . . .
O7W O 0.8981(7) 0.3633(4) 0.9799(6) 0.097(3) Uani 1 1 d . . . . .
O9 O 0.3017(4) 0.2391(3) 0.9180(4) 0.0530(14) Uani 1 1 d . . . . .
O8W O 0.5466(8) 0.0016(5) 0.7033(6) 0.108(3) Uani 1 1 d . . . . .
O10 O 0.1786(7) 0.2966(3) 0.8423(6) 0.087(2) Uani 1 1 d . . . . .
O9W O 0.1632(11) 0.4262(5) 0.7620(8) 0.141(5) Uani 1 1 d . . . . .
N1 N 0.5578(6) 0.2792(3) 0.8973(4) 0.0488(16) Uani 1 1 d . . . . .
N2 N 0.6236(5) 0.1552(3) 0.9306(4) 0.0488(17) Uani 1 1 d . . . . .
N3 N 0.3993(5) 0.1056(3) 0.8939(4) 0.0430(15) Uani 1 1 d . . . . .
N4 N 0.4237(7) 0.2053(3) 0.7794(5) 0.057(2) Uani 1 1 d . . . . .
N5 N 0.4947(6) 0.4310(3) 0.9177(4) 0.0492(17) Uani 1 1 d . . . . .
H5 H 0.4219 0.4209 0.9225 0.059 Uiso 1 1 calc R U . . .
N6 N 0.1166(5) 0.0427(3) 0.9121(4) 0.0411(15) Uani 1 1 d . . . . .
H6 H 0.0922 0.0795 0.9160 0.049 Uiso 1 1 calc R U . . .
Ni1 Ni 0.45780(8) 0.19701(4) 0.91204(6) 0.0402(5) Uani 1 1 d . . . . .
Zn2 Zn 0.40499(9) 0.20611(5) 1.20849(7) 0.0562(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.513(11) . ?
C1 C2 1.576(15) . ?
C2 N2 1.486(12) . ?
C3 N2 1.460(12) . ?
C3 C4 1.529(12) . ?
C4 N3 1.465(10) . ?
C5 N3 1.515(10) . ?
C5 C6 1.526(13) . ?
C6 N4 1.450(12) . ?
C7 N4 1.516(12) . ?
C7 C8 1.516(14) . ?
C8 N1 1.487(12) . ?
C9 N1 1.478(12) . ?
C9 C10 1.495(12) . ?
C10 O1 1.250(10) . ?
C10 N5 1.325(11) . ?
C11 C16 1.383(13) . ?
C11 C12 1.392(12) . ?
C11 N5 1.431(11) . ?
C12 C13 1.382(13) . ?
C13 C14 1.347(13) . ?
C14 C15 1.399(13) . ?
C14 C17 1.547(14) . ?
C15 C16 1.427(13) . ?
C17 O2 1.225(13) . ?
C17 O3 1.242(12) . ?
C18 N2 1.481(11) . ?
C18 C19 1.511(12) . ?
C19 O4 1.228(10) . ?
C19 O5 1.274(10) . ?
C20 C21 1.497(12) . ?
C20 N3 1.503(10) . ?
C21 O6 1.240(10) . ?
C21 N6 1.327(10) . ?
C22 C27 1.383(11) . ?
C22 C23 1.389(12) . ?
C22 N6 1.423(10) . ?
C23 C24 1.381(11) . ?
C24 C25 1.346(11) . ?
C25 C26 1.391(12) . ?
C25 C28 1.529(12) . ?
C26 C27 1.344(12) . ?
C28 O7 1.232(11) . ?
C28 O8 1.255(12) . ?
C29 N4 1.432(13) . ?
C29 C30 1.479(14) . ?
C30 O10 1.256(11) . ?
C30 O9 1.275(10) . ?
O1W Zn2 2.003(8) . ?
O3 Zn2 2.044(7) 3_667 ?
O4 Ni1 2.014(6) . ?
O5 Zn2 2.038(6) . ?
O7 Zn2 1.997(6) 3_557 ?
O9 Ni1 2.004(5) . ?
N1 Ni1 2.154(7) . ?
N2 Ni1 2.117(6) . ?
N3 Ni1 2.144(6) . ?
N4 Ni1 2.106(7) . ?
Zn2 O7 1.997(6) 3_557 ?
Zn2 O3 2.044(7) 3_667 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.0(7) . . ?
N2 C2 C1 110.0(8) . . ?
N2 C3 C4 109.3(6) . . ?
N3 C4 C3 112.9(7) . . ?
N3 C5 C6 110.8(7) . . ?
N4 C6 C5 110.0(8) . . ?
N4 C7 C8 109.2(7) . . ?
N1 C8 C7 111.8(8) . . ?
N1 C9 C10 113.0(7) . . ?
O1 C10 N5 122.8(8) . . ?
O1 C10 C9 120.3(7) . . ?
N5 C10 C9 116.9(7) . . ?
C16 C11 C12 121.1(8) . . ?
C16 C11 N5 123.2(7) . . ?
C12 C11 N5 115.7(7) . . ?
C13 C12 C11 120.5(8) . . ?
C14 C13 C12 119.8(8) . . ?
C13 C14 C15 121.3(8) . . ?
C13 C14 C17 118.8(8) . . ?
C15 C14 C17 119.9(9) . . ?
C14 C15 C16 119.8(8) . . ?
C11 C16 C15 117.4(8) . . ?
O2 C17 O3 124.6(10) . . ?
O2 C17 C14 116.3(9) . . ?
O3 C17 C14 119.0(9) . . ?
N2 C18 C19 112.2(6) . . ?
O4 C19 O5 122.9(8) . . ?
O4 C19 C18 120.8(7) . . ?
O5 C19 C18 116.4(7) . . ?
C21 C20 N3 114.7(6) . . ?
O6 C21 N6 123.2(7) . . ?
O6 C21 C20 121.2(7) . . ?
N6 C21 C20 115.6(7) . . ?
C27 C22 C23 118.9(7) . . ?
C27 C22 N6 117.1(7) . . ?
C23 C22 N6 124.1(7) . . ?
C24 C23 C22 118.4(7) . . ?
C25 C24 C23 122.0(8) . . ?
C24 C25 C26 119.3(7) . . ?
C24 C25 C28 122.9(8) . . ?
C26 C25 C28 117.8(7) . . ?
C27 C26 C25 119.6(7) . . ?
C26 C27 C22 121.7(8) . . ?
O7 C28 O8 122.0(8) . . ?
O7 C28 C25 119.0(8) . . ?
O8 C28 C25 119.0(8) . . ?
N4 C29 C30 113.7(7) . . ?
O10 C30 O9 123.0(10) . . ?
O10 C30 C29 119.3(8) . . ?
O9 C30 C29 117.6(8) . . ?
C17 O3 Zn2 105.6(7) . 3_667 ?
C19 O4 Ni1 116.4(5) . . ?
C19 O5 Zn2 106.3(5) . . ?
C28 O7 Zn2 106.5(6) . 3_557 ?
C30 O9 Ni1 116.2(6) . . ?
C9 N1 C8 109.3(7) . . ?
C9 N1 C1 109.5(7) . . ?
C8 N1 C1 112.7(7) . . ?
C9 N1 Ni1 112.9(5) . . ?
C8 N1 Ni1 105.1(5) . . ?
C1 N1 Ni1 107.2(5) . . ?
C3 N2 C18 111.1(7) . . ?
C3 N2 C2 111.9(7) . . ?
C18 N2 C2 112.0(7) . . ?
C3 N2 Ni1 107.4(5) . . ?
C18 N2 Ni1 108.4(5) . . ?
C2 N2 Ni1 105.8(6) . . ?
C4 N3 C20 111.8(6) . . ?
C4 N3 C5 112.4(6) . . ?
C20 N3 C5 108.5(6) . . ?
C4 N3 Ni1 107.2(5) . . ?
C20 N3 Ni1 110.7(5) . . ?
C5 N3 Ni1 106.1(5) . . ?
C29 N4 C6 113.3(8) . . ?
C29 N4 C7 108.3(8) . . ?
C6 N4 C7 114.3(8) . . ?
C29 N4 Ni1 109.5(6) . . ?
C6 N4 Ni1 106.3(5) . . ?
C7 N4 Ni1 104.7(5) . . ?
C10 N5 C11 129.4(7) . . ?
C21 N6 C22 130.8(7) . . ?
O9 Ni1 O4 87.3(2) . . ?
O9 Ni1 N4 81.1(3) . . ?
O4 Ni1 N4 168.3(3) . . ?
O9 Ni1 N2 169.4(2) . . ?
O4 Ni1 N2 82.2(2) . . ?
N4 Ni1 N2 109.4(3) . . ?
O9 Ni1 N3 99.7(2) . . ?
O4 Ni1 N3 97.0(2) . . ?
N4 Ni1 N3 84.1(3) . . ?
N2 Ni1 N3 83.3(3) . . ?
O9 Ni1 N1 94.7(2) . . ?
O4 Ni1 N1 96.7(2) . . ?
N4 Ni1 N1 85.3(3) . . ?
N2 Ni1 N1 85.0(3) . . ?
N3 Ni1 N1 160.6(3) . . ?
O7 Zn2 O1W 115.1(3) 3_557 . ?
O7 Zn2 O5 121.9(3) 3_557 . ?
O1W Zn2 O5 96.8(3) . . ?
O7 Zn2 O3 97.5(3) 3_557 3_667 ?
O1W Zn2 O3 108.7(3) . 3_667 ?
O5 Zn2 O3 117.4(3) . 3_667 ?

_refine_diff_density_max         1.881
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.163

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1443841'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        7
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H34 Mn N6 O11 Zn, 9H2O'
_chemical_formula_sum            'C30 H52 Mn N6 O20 Zn'
_chemical_formula_weight         918.94

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'
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'
Mn1 Mn1 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn1 Zn1 0.2839 1.4301 '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'

_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                   37.000(4)
_cell_length_b                   12.500(4)
_cell_length_c                   18.680(4)
_cell_angle_alpha                90
_cell_angle_beta                 111.40(3)
_cell_angle_gamma                90
_cell_volume                     8044(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    649
_cell_measurement_theta_min      1
_cell_measurement_theta_max      40

_exptl_crystal_description       prisme
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_F_000             3768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.996
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.70109
_diffrn_radiation_type           'synchrotron radiation'
_diffrn_source                   'synchrotron radiation'
_diffrn_measurement_device_type  'PILATUS DECTRIS 6M'
_diffrn_measurement_method       'Phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29802
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.205
_diffrn_reflns_theta_max         23.822
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.766
_diffrn_measured_fraction_theta_full 0.650
_diffrn_reflns_Laue_measured_fraction_max 0.766
_diffrn_reflns_Laue_measured_fraction_full 0.650
_diffrn_reflns_point_group_measured_fraction_max 0.766
_diffrn_reflns_point_group_measured_fraction_full 0.650
_reflns_number_total             4738
_reflns_number_gt                3765
_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       'M2DM bruker'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SIR2011 (POlidori 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), 

C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
C9(H9A, H9B), C18(H18A,H18B), C20(H20A,H20B), 
C29(H29A,H29B),  
2.b Primary CH refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C23(H23), 
C24(H24), C26(H26), C27(H27), 
2.c Primary CH refined with riding coordinates:
 N5(H5), N6(H6),  
2.d Primary CH refined with riding coordinates:
 O3(H3)

The Following ALERTS were generated by PLATON checkcif<<<

PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O2W Check 
And 8 other PLAT306 Alerts
Less ...
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O3W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O4W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O5W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O6W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O7W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O8W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O9W Check 
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) O10W Check 

PLAT430_ALERT_2_B Short Inter D...A Contact  O1W  O3W     ..       2.72 Ang.  
And 13 other PLAT430 Alerts
Less ...
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W  O10        2.75 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W  O9W        2.77 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W  O5W        2.77 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3   O7W        2.71 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3W  O9         2.75 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O3W  O5W        2.78 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O4W  O6W        2.78 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O5W  O7         2.74 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O6   O10W       2.74 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O6W  O8         2.55 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O8W  O10W       2.70 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O9W  O10        2.64 Ang.  
PLAT430_ALERT_2_B Short Inter D...A Contact  O9W  O10W       2.77 Ang.  

PLAT911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L=  0.568  1116 Report


These alerts arise because of missing water molecules in the model resulting in apparent large structural voids and missing H-bonds

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.2000P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4738
_refine_ls_number_parameters     523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.1041
_refine_ls_wR_factor_ref         0.3450
_refine_ls_wR_factor_gt          0.3237
_refine_ls_goodness_of_fit_ref   1.562
_refine_ls_restrained_S_all      1.562
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1918(3) 0.7692(10) 0.7782(6) 0.112(3) Uani 1 1 d . . . . .
H1A H 0.2152 0.7914 0.8200 0.135 Uiso 1 1 calc R U . . .
H1B H 0.1974 0.7691 0.7314 0.135 Uiso 1 1 calc R U . . .
C2 C 0.1816(3) 0.6565(9) 0.7939(6) 0.107(3) Uani 1 1 d . . . . .
H2A H 0.1605 0.6300 0.7490 0.128 Uiso 1 1 calc R U . . .
H2B H 0.2038 0.6102 0.8027 0.128 Uiso 1 1 calc R U . . .
C3 C 0.1470(2) 0.5548(7) 0.8594(6) 0.091(2) Uani 1 1 d . . . . .
H3A H 0.1497 0.5373 0.9117 0.110 Uiso 1 1 calc R U . . .
H3B H 0.1575 0.4957 0.8395 0.110 Uiso 1 1 calc R U . . .
C4 C 0.1051(2) 0.5669(7) 0.8120(6) 0.092(2) Uani 1 1 d . . . . .
H4A H 0.0916 0.5011 0.8138 0.110 Uiso 1 1 calc R U . . .
H4B H 0.1021 0.5798 0.7589 0.110 Uiso 1 1 calc R U . . .
C5 C 0.0519(2) 0.6964(7) 0.7800(5) 0.088(2) Uani 1 1 d . . . . .
H5A H 0.0372 0.7372 0.8043 0.105 Uiso 1 1 calc R U . . .
H5B H 0.0362 0.6354 0.7548 0.105 Uiso 1 1 calc R U . . .
C6 C 0.0585(3) 0.7646(7) 0.7205(5) 0.095(2) Uani 1 1 d . . . . .
H6A H 0.0711 0.7222 0.6929 0.114 Uiso 1 1 calc R U . . .
H6B H 0.0336 0.7876 0.6838 0.114 Uiso 1 1 calc R U . . .
C7 C 0.0954(3) 0.9035(8) 0.6920(6) 0.099(3) Uani 1 1 d . . . . .
H7A H 0.1006 0.9793 0.7012 0.119 Uiso 1 1 calc R U . . .
H7B H 0.0753 0.8950 0.6416 0.119 Uiso 1 1 calc R U . . .
C8 C 0.1317(3) 0.8465(10) 0.6945(6) 0.106(3) Uani 1 1 d . . . . .
H8A H 0.1252 0.7734 0.6773 0.127 Uiso 1 1 calc R U . . .
H8B H 0.1417 0.8811 0.6590 0.127 Uiso 1 1 calc R U . . .
C9 C 0.1783(3) 0.9572(10) 0.7913(7) 0.117(4) Uani 1 1 d . . . . .
H9A H 0.1992 0.9686 0.7725 0.141 Uiso 1 1 calc R U . . .
H9B H 0.1582 1.0098 0.7674 0.141 Uiso 1 1 calc R U . . .
C10 C 0.1925(3) 0.9697(8) 0.8728(6) 0.090(2) Uani 1 1 d . . . . .
C11 C 0.2369(3) 1.0783(7) 0.9814(6) 0.096(3) Uani 1 1 d . . . . .
C12 C 0.2187(3) 1.0631(7) 1.0328(5) 0.088(2) Uani 1 1 d . . . . .
H12 H 0.1948 1.0289 1.0180 0.105 Uiso 1 1 calc R U . . .
C13 C 0.2370(3) 1.1003(7) 1.1075(6) 0.093(3) Uani 1 1 d . . . . .
H13 H 0.2249 1.0891 1.1427 0.112 Uiso 1 1 calc R U . . .
C14 C 0.2716(2) 1.1521(7) 1.1315(5) 0.082(2) Uani 1 1 d . . . . .
C15 C 0.2891(3) 1.1684(7) 1.0767(6) 0.091(2) Uani 1 1 d . . . . .
H15 H 0.3122 1.2067 1.0907 0.109 Uiso 1 1 calc R U . . .
C16 C 0.2723(2) 1.1279(7) 1.0012(5) 0.089(2) Uani 1 1 d . . . . .
H16 H 0.2847 1.1346 0.9663 0.106 Uiso 1 1 calc R U . . .
C17 C 0.2891(3) 1.1934(7) 1.2102(7) 0.093(3) Uani 1 1 d . . . . .
C18 C 0.2043(2) 0.6548(8) 0.9341(5) 0.090(2) Uani 1 1 d . . . . .
H18A H 0.2231 0.7056 0.9295 0.108 Uiso 1 1 calc R U . . .
H18B H 0.2164 0.5848 0.9439 0.108 Uiso 1 1 calc R U . . .
C19 C 0.1926(2) 0.6862(7) 1.0000(6) 0.088(3) Uani 1 1 d . . . . .
C20 C 0.0795(2) 0.6309(7) 0.9083(5) 0.081(2) Uani 1 1 d . . . . .
H20A H 0.0752 0.6970 0.9313 0.098 Uiso 1 1 calc R U . . .
H20B H 0.1024 0.5972 0.9450 0.098 Uiso 1 1 calc R U . . .
C21 C 0.0449(2) 0.5578(8) 0.8957(6) 0.087(2) Uani 1 1 d . . . . .
C22 C -0.0186(2) 0.5558(7) 0.9105(5) 0.085(2) Uani 1 1 d . . . . .
C23 C -0.0328(2) 0.4591(7) 0.8700(6) 0.092(2) Uani 1 1 d . . . . .
H23 H -0.0183 0.4224 0.8463 0.111 Uiso 1 1 calc R U . . .
C24 C -0.0693(3) 0.4194(8) 0.8663(6) 0.100(3) Uani 1 1 d . . . . .
H24 H -0.0789 0.3561 0.8401 0.120 Uiso 1 1 calc R U . . .
C25 C -0.0903(2) 0.4726(8) 0.9003(5) 0.085(2) Uani 1 1 d . . . . .
C26 C -0.0765(3) 0.5686(9) 0.9391(6) 0.102(3) Uani 1 1 d . . . . .
H26 H -0.0913 0.6059 0.9616 0.122 Uiso 1 1 calc R U . . .
C27 C -0.0415(2) 0.6070(7) 0.9439(5) 0.082(2) Uani 1 1 d . . . . .
H27 H -0.0326 0.6703 0.9707 0.098 Uiso 1 1 calc R U . . .
C28 C -0.1300(3) 0.4240(10) 0.8948(6) 0.098(3) Uani 1 1 d . . . . .
C29 C 0.0595(3) 0.9423(9) 0.7762(7) 0.112(3) Uani 1 1 d . . . . .
H29A H 0.0324 0.9400 0.7426 0.134 Uiso 1 1 calc R U . . .
H29B H 0.0696 1.0125 0.7719 0.134 Uiso 1 1 calc R U . . .
C30 C 0.0631(3) 0.9225(8) 0.8596(7) 0.105(3) Uani 1 1 d . . . . .
N1 N 0.16191(19) 0.8451(7) 0.7705(4) 0.091(2) Uani 1 1 d . . . . .
N2 N 0.16985(18) 0.6520(6) 0.8604(4) 0.0881(19) Uani 1 1 d . . . . .
N3 N 0.08743(16) 0.6572(5) 0.8399(4) 0.0776(16) Uani 1 1 d . . . . .
N4 N 0.0819(2) 0.8577(6) 0.7524(5) 0.095(2) Uani 1 1 d . . . . .
N5 N 0.2211(2) 1.0409(6) 0.9040(5) 0.098(2) Uani 1 1 d . . . . .
H5 H 0.2312 1.0676 0.8731 0.117 Uiso 1 1 calc R U . . .
N6 N 0.01657(17) 0.6013(5) 0.9164(4) 0.0851(19) Uani 1 1 d . . . . .
H6 H 0.0209 0.6647 0.9356 0.102 Uiso 1 1 calc R U . . .
O1 O 0.17707(18) 0.9231(5) 0.9136(4) 0.1013(19) Uani 1 1 d . . . . .
O2 O 0.27895(19) 1.1536(6) 1.2620(4) 0.1010(18) Uani 1 1 d . . . . .
O1W O 0.1981(3) 0.8652(6) 1.1424(4) 0.139(3) Uani 1 1 d . . . . .
O3 O 0.3145(2) 1.2638(7) 1.2243(4) 0.116(2) Uani 1 1 d . . . . .
O2W O 0.0257(2) 0.8143(6) 0.9871(6) 0.134(3) Uani 1 1 d . . . . .
O4 O 0.16071(14) 0.7340(5) 0.9847(3) 0.0830(15) Uani 1 1 d . . . . .
O3W O 0.1326(3) 0.9684(6) 1.0518(5) 0.131(3) Uani 1 1 d . . . . .
O5 O 0.21539(16) 0.6636(6) 1.0648(4) 0.0933(16) Uani 1 1 d . . . . .
O4W O 0.2610(3) 0.9322(7) 1.2948(6) 0.146(3) Uani 1 1 d . . . . .
O6 O 0.04282(19) 0.4730(6) 0.8630(5) 0.112(2) Uani 1 1 d . . . . .
O5W O -0.0911(4) 0.1558(9) 0.8814(8) 0.184(5) Uani 1 1 d . . . . .
O7 O -0.13599(19) 0.3329(7) 0.8750(4) 0.109(2) Uani 1 1 d . . . . .
O6W O -0.1749(4) 0.6779(9) 0.8927(8) 0.179(4) Uani 1 1 d . . . . .
O8 O -0.15093(19) 0.4848(7) 0.9152(5) 0.129(3) Uani 1 1 d . . . . .
O7W O 0.3760(6) 1.3319(15) 1.1909(15) 0.304(12) Uani 1 1 d . . . . .
O9 O 0.09413(18) 0.8823(5) 0.9083(4) 0.0988(18) Uani 1 1 d . . . . .
O8W O 0.1255(5) 1.1809(10) 0.9922(12) 0.257(9) Uani 1 1 d . . . . .
O10 O 0.0347(2) 0.9522(7) 0.8799(6) 0.134(3) Uani 1 1 d . . . . .
O9W O 0.0218(14) 1.1392(14) 0.932(3) 0.74(5) Uani 1 1 d . . . . .
O10W O 0.0661(15) 1.264(2) 0.873(2) 0.48(3) Uani 1 1 d . . . . .
Mn1 Mn1 0.13315(3) 0.80114(9) 0.86531(7) 0.0776(6) Uani 1 1 d . . . . .
Zn1 Zn1 0.18877(3) 0.70578(9) 1.13519(7) 0.0991(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.425(14) . ?
C1 C2 1.516(16) . ?
C2 N2 1.458(11) . ?
C3 N2 1.476(11) . ?
C3 C4 1.486(13) . ?
C4 N3 1.491(11) . ?
C5 N3 1.464(10) . ?
C5 C6 1.489(13) . ?
C6 N4 1.444(12) . ?
C7 N4 1.504(11) . ?
C7 C8 1.506(14) . ?
C8 N1 1.451(12) . ?
C9 C10 1.427(15) . ?
C9 N1 1.520(14) . ?
C10 O1 1.250(10) . ?
C10 N5 1.341(12) . ?
C11 C16 1.371(13) . ?
C11 C12 1.372(12) . ?
C11 N5 1.426(13) . ?
C12 C13 1.390(14) . ?
C13 C14 1.357(12) . ?
C14 C15 1.411(12) . ?
C14 C17 1.468(14) . ?
C15 C16 1.412(13) . ?
C17 O3 1.246(11) . ?
C17 O2 1.259(12) . ?
C18 N2 1.496(11) . ?
C18 C19 1.497(13) . ?
C19 O5 1.230(11) . ?
C19 O4 1.260(10) . ?
C19 Zn1 2.593(10) . ?
C20 N3 1.449(10) . ?
C20 C21 1.519(11) . ?
C21 O6 1.211(10) . ?
C21 N6 1.358(11) . ?
C22 C27 1.379(12) . ?
C22 N6 1.388(10) . ?
C22 C23 1.421(13) . ?
C23 C24 1.418(12) . ?
C24 C25 1.343(13) . ?
C25 C26 1.399(14) . ?
C25 C28 1.559(13) . ?
C26 C27 1.353(12) . ?
C28 O7 1.194(12) . ?
C28 O8 1.240(12) . ?
C29 N4 1.508(13) . ?
C29 C30 1.534(16) . ?
C30 O9 1.280(13) . ?
C30 O10 1.292(12) . ?
N1 Mn1 2.439(6) . ?
N2 Mn1 2.328(7) . ?
N3 Mn1 2.395(6) . ?
N4 Mn1 2.371(8) . ?
O1 Mn1 2.170(6) . ?
O2 Zn1 1.967(7) 4_557 ?
O1W Zn1 2.019(8) . ?
O4 Mn1 2.249(6) . ?
O5 Zn1 1.980(6) . ?
O7 Zn1 1.953(6) 5_567 ?
O9 Mn1 2.145(6) . ?
Zn1 O7 1.953(6) 5_567 ?
Zn1 O2 1.967(7) 4_547 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 113.5(7) . . ?
N2 C2 C1 111.9(9) . . ?
N2 C3 C4 113.0(8) . . ?
C3 C4 N3 111.4(7) . . ?
N3 C5 C6 114.7(6) . . ?
N4 C6 C5 112.9(8) . . ?
N4 C7 C8 109.4(8) . . ?
N1 C8 C7 113.3(9) . . ?
C10 C9 N1 109.3(8) . . ?
O1 C10 N5 120.5(9) . . ?
O1 C10 C9 121.8(8) . . ?
N5 C10 C9 117.4(8) . . ?
C16 C11 C12 122.4(10) . . ?
C16 C11 N5 114.9(8) . . ?
C12 C11 N5 122.6(9) . . ?
C11 C12 C13 118.3(9) . . ?
C14 C13 C12 123.0(7) . . ?
C13 C14 C15 117.3(9) . . ?
C13 C14 C17 121.1(8) . . ?
C15 C14 C17 121.6(8) . . ?
C14 C15 C16 121.3(8) . . ?
C11 C16 C15 117.5(8) . . ?
O3 C17 O2 122.0(10) . . ?
O3 C17 C14 118.9(8) . . ?
O2 C17 C14 119.0(9) . . ?
N2 C18 C19 111.0(6) . . ?
O5 C19 O4 125.5(8) . . ?
O5 C19 C18 116.8(8) . . ?
O4 C19 C18 117.7(9) . . ?
O5 C19 Zn1 47.4(4) . . ?
O4 C19 Zn1 78.2(5) . . ?
C18 C19 Zn1 163.8(7) . . ?
N3 C20 C21 115.4(7) . . ?
O6 C21 N6 125.4(8) . . ?
O6 C21 C20 120.1(7) . . ?
N6 C21 C20 114.2(8) . . ?
C27 C22 N6 119.1(8) . . ?
C27 C22 C23 117.9(7) . . ?
N6 C22 C23 122.9(8) . . ?
C24 C23 C22 118.9(8) . . ?
C25 C24 C23 120.5(9) . . ?
C24 C25 C26 120.4(8) . . ?
C24 C25 C28 118.0(9) . . ?
C26 C25 C28 121.6(9) . . ?
C27 C26 C25 119.8(9) . . ?
C26 C27 C22 122.4(9) . . ?
O7 C28 O8 128.0(10) . . ?
O7 C28 C25 117.1(9) . . ?
O8 C28 C25 114.9(11) . . ?
N4 C29 C30 109.5(8) . . ?
O9 C30 O10 121.3(11) . . ?
O9 C30 C29 120.4(8) . . ?
O10 C30 C29 118.2(10) . . ?
C1 N1 C8 113.5(8) . . ?
C1 N1 C9 111.4(7) . . ?
C8 N1 C9 109.4(8) . . ?
C1 N1 Mn1 107.8(6) . . ?
C8 N1 Mn1 109.2(5) . . ?
C9 N1 Mn1 105.2(5) . . ?
C2 N2 C3 111.6(8) . . ?
C2 N2 C18 111.4(6) . . ?
C3 N2 C18 108.7(7) . . ?
C2 N2 Mn1 111.2(6) . . ?
C3 N2 Mn1 108.7(4) . . ?
C18 N2 Mn1 104.9(5) . . ?
C20 N3 C5 109.6(6) . . ?
C20 N3 C4 113.2(7) . . ?
C5 N3 C4 111.8(7) . . ?
C20 N3 Mn1 110.5(5) . . ?
C5 N3 Mn1 105.8(5) . . ?
C4 N3 Mn1 105.6(4) . . ?
C6 N4 C7 108.1(8) . . ?
C6 N4 C29 112.0(7) . . ?
C7 N4 C29 108.9(8) . . ?
C6 N4 Mn1 107.0(6) . . ?
C7 N4 Mn1 113.9(5) . . ?
C29 N4 Mn1 107.1(6) . . ?
C10 N5 C11 128.6(7) . . ?
C21 N6 C22 127.8(8) . . ?
C10 O1 Mn1 120.9(6) . . ?
C17 O2 Zn1 112.0(7) . 4_557 ?
C19 O4 Mn1 116.7(5) . . ?
C19 O5 Zn1 105.4(5) . . ?
C28 O7 Zn1 109.4(7) . 5_567 ?
C30 O9 Mn1 118.3(6) . . ?
O9 Mn1 O1 90.9(2) . . ?
O9 Mn1 O4 85.9(2) . . ?
O1 Mn1 O4 81.4(2) . . ?
O9 Mn1 N2 151.1(2) . . ?
O1 Mn1 N2 102.7(2) . . ?
O4 Mn1 N2 71.4(2) . . ?
O9 Mn1 N4 76.3(3) . . ?
O1 Mn1 N4 113.2(3) . . ?
O4 Mn1 N4 156.8(2) . . ?
N2 Mn1 N4 119.5(3) . . ?
O9 Mn1 N3 84.6(2) . . ?
O1 Mn1 N3 167.9(2) . . ?
O4 Mn1 N3 87.0(2) . . ?
N2 Mn1 N3 76.7(2) . . ?
N4 Mn1 N3 76.7(2) . . ?
O9 Mn1 N1 134.2(3) . . ?
O1 Mn1 N1 71.6(2) . . ?
O4 Mn1 N1 130.1(2) . . ?
N2 Mn1 N1 74.7(3) . . ?
N4 Mn1 N1 72.9(2) . . ?
N3 Mn1 N1 119.3(2) . . ?
O7 Zn1 O2 104.0(3) 5_567 4_547 ?
O7 Zn1 O5 126.3(3) 5_567 . ?
O2 Zn1 O5 106.8(3) 4_547 . ?
O7 Zn1 O1W 113.0(4) 5_567 . ?
O2 Zn1 O1W 103.5(3) 4_547 . ?
O5 Zn1 O1W 101.1(3) . . ?
O7 Zn1 C19 106.9(3) 5_567 . ?
O2 Zn1 C19 133.7(3) 4_547 . ?
O5 Zn1 C19 27.2(2) . . ?
O1W Zn1 C19 95.1(3) . . ?

_refine_diff_density_max         1.176
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.115

_shelxl_version_number           2013-2

