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

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

data_cobmox3
_database_code_depnum_ccdc_archive 'CCDC 1039718'
_audit_update_record             
;
2014-12-16 deposited with the CCDC.
2015-04-27 downloaded from the CCDC.
;

_vrf_PLAT058_cobmox3             
;
PROBLEM: Maximum Transmission Factor Missing ............          ?      
RESPONSE: Data not available. The ratio of minimum to maximum apparent 
          transmission, as reported in the .abs file, is 0.746324. 
          That comes from the applied 'SADABS-2004/1 - Bruker Nonius area 
          detector scaling and absorption correction'
;
_vrf_PLAT059_cobmox3             
;
PROBLEM: Minimum Transmission Factor Missing ............          ?      
RESPONSE: See above.
;
_vrf_PLAT430_cobmox3             
;
PROBLEM: Short Inter D...A Contact  O1W    ..  O3W     ..       1.50 Ang.  
RESPONSE: As described in the main text, the water molecules of crystallization
          present in the structure are interconnected through H-bonds into
          pentameric motifs (rings) residing in the supramolecular channels
          generated by the superimposition of the [Co2(bpm)(ox)4]n layers along
          the crystallographic c-axis. By applying the symmetry operations of
          the space group C2/m to the water oxygen atoms in the asymmetric unit,
          a 10-member ring with a series of short Ow...Ow contact is generated.
          As already established for published structures (see ref.s 37and 40
          in the main text), this false image is the result of the superimposition
          of two staggered rings along the c-axis (truly it should be said groups
          of rings). Each one of the three water oxygen atoms in the asymmetric
          unit participates to the construction of both rings. To account for
          this disorder, and in line with TGA data, the total occupancy of these
          water oxygen atoms is imposed as 2.5 (there are 5 water molecules every
          two metal ions). 
 
;
_vrf_PLAT043_cobmox3             
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      10.08 Check
RESPONSE: The hydrogen atoms on the water molecules of crystallization have
          not be found neither placed because of the disorder discussed above.
          Nonetheless, these hydrogen atoms have been included for the calculation
          of the molecular weight (hence the discrepancy between reported and 
          calculated values).
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Co2 N4 O8, (O5)'
_chemical_formula_sum            'C12 H16 Co2 N4 O13'
_chemical_formula_weight         542.15

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   9.4514(2)
_cell_length_b                   16.7427(4)
_cell_length_c                   6.1969(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.4550(10)
_cell_angle_gamma                90
_cell_volume                     961.08(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3299
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_F_000             548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.804
_shelx_estimated_absorpt_T_min   0.840
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_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            7834
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.433
_diffrn_reflns_theta_max         31.291
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1603
_reflns_number_gt                1361
_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    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
'the water molecules of crystallization are disordered'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0569P)²+0.7362P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Direct
_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         1603
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.1004
_refine_ls_wR_factor_gt          0.0935
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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
Co1 Co 0.5000 0.67009(2) 0.5000 0.02892(13) Uani 1 2 d S T P . .
C1 C 0.4531(3) 0.5000 0.3892(4) 0.0247(5) Uani 1 2 d S T P . .
N1 N 0.41576(17) 0.57079(10) 0.2989(3) 0.0285(3) Uani 1 1 d . . . . .
C2 C 0.3353(2) 0.57085(14) 0.0938(3) 0.0370(4) Uani 1 1 d . . . . .
H2 H 0.3064 0.6192 0.0249 0.044 Uiso 1 1 calc R U . . .
C3 C 0.2950(4) 0.5000 -0.0158(5) 0.0413(7) Uani 1 2 d S T P . .
H3 H 0.2423 0.5000 -0.1595 0.050 Uiso 1 2 calc R U P . .
C4 C 0.2416(2) 0.72762(11) 0.6064(3) 0.0296(4) Uani 1 1 d . . . . .
O1 O 0.33683(17) 0.67763(9) 0.6800(3) 0.0391(4) Uani 1 1 d . . . . .
O2 O 0.36585(16) 0.75479(10) 0.3141(3) 0.0376(3) Uani 1 1 d . . . . .
O1W O 1.0000 0.3417(4) 1.0000 0.0662(16) Uiso 0.5 2 d S . P . .
O2W O 1.0790(8) 0.4576(5) 1.3521(13) 0.129(3) Uiso 0.5 1 d . . P . .
O3W O 1.0406(7) 0.6172(4) 1.2191(10) 0.0972(17) Uiso 0.5 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0279(2) 0.02237(19) 0.0364(2) 0.000 0.00606(14) 0.000
C1 0.0233(10) 0.0243(11) 0.0264(11) 0.000 0.0042(9) 0.000
N1 0.0284(7) 0.0258(7) 0.0300(7) 0.0030(6) 0.0024(6) 0.0000(6)
C2 0.0374(10) 0.0391(11) 0.0327(9) 0.0086(8) 0.0024(8) 0.0020(8)
C3 0.0396(15) 0.0528(19) 0.0276(13) 0.000 -0.0025(11) 0.000
C4 0.0319(9) 0.0257(8) 0.0316(9) 0.0054(7) 0.0071(7) 0.0000(7)
O1 0.0380(8) 0.0388(8) 0.0430(8) 0.0174(6) 0.0146(6) 0.0128(6)
O2 0.0358(8) 0.0381(8) 0.0420(8) 0.0126(6) 0.0155(6) 0.0085(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.0788(16) . ?
Co1 O1 2.0788(16) 2_656 ?
Co1 O2 2.0893(15) . ?
Co1 O2 2.0894(15) 2_656 ?
Co1 N1 2.1348(16) . ?
Co1 N1 2.1348(16) 2_656 ?
Co1 Co1 5.4306(4) 8_565 ?
Co1 Co1 5.4306(4) 7_566 ?
Co1 Co1 5.6956(7) 6_565 ?
Co1 Co1 9.4514(2) 1_655 ?
Co1 Co1 9.61310(19) 3_545 ?
Co1 Co1 11.0349(4) 6_665 ?
C1 N1 1.3281(19) 6_565 ?
C1 N1 1.3281(19) . ?
C1 C1 1.479(5) 2_656 ?
N1 C2 1.345(2) . ?
C2 C3 1.382(3) . ?
C2 H2 0.9300 . ?
C3 C2 1.382(3) 6_565 ?
C3 H3 0.9300 . ?
C4 O1 1.247(2) . ?
C4 O2 1.249(2) 7_566 ?
C4 C4 1.552(4) 7_566 ?
O2 C4 1.249(2) 7_566 ?
O1W O3W 1.502(7) 6_565 ?
O1W O3W 1.502(7) 5_767 ?
O1W O2W 2.904(10) . ?
O1W O2 2.915(4) 4_646 ?
O2W O2W 1.420(17) 6_565 ?
O2W O3W 1.504(10) 6_565 ?
O2W O3W 2.799(11) . ?
O2W O2W 2.949(17) 5_768 ?
O3W O1W 1.502(7) 5_767 ?
O3W O2W 1.504(10) 6_565 ?
O3W O3W 2.671(12) 2_757 ?
O3W O2 2.838(7) 8_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 173.04(9) . 2_656 ?
O1 Co1 O2 79.69(5) . . ?
O1 Co1 O2 95.55(6) 2_656 . ?
O1 Co1 O2 95.55(6) . 2_656 ?
O1 Co1 O2 79.69(6) 2_656 2_656 ?
O2 Co1 O2 94.51(10) . 2_656 ?
O1 Co1 N1 97.48(7) . . ?
O1 Co1 N1 87.96(6) 2_656 . ?
O2 Co1 N1 95.26(6) . . ?
O2 Co1 N1 164.93(6) 2_656 . ?
O1 Co1 N1 87.96(6) . 2_656 ?
O1 Co1 N1 97.47(7) 2_656 2_656 ?
O2 Co1 N1 164.93(6) . 2_656 ?
O2 Co1 N1 95.26(6) 2_656 2_656 ?
N1 Co1 N1 77.69(8) . 2_656 ?
O1 Co1 Co1 135.10(5) . 8_565 ?
O1 Co1 Co1 39.81(4) 2_656 8_565 ?
O2 Co1 Co1 95.65(4) . 8_565 ?
O2 Co1 Co1 39.90(4) 2_656 8_565 ?
N1 Co1 Co1 127.40(4) . 8_565 ?
N1 Co1 Co1 99.21(4) 2_656 8_565 ?
O1 Co1 Co1 39.81(4) . 7_566 ?
O1 Co1 Co1 135.10(5) 2_656 7_566 ?
O2 Co1 Co1 39.90(4) . 7_566 ?
O2 Co1 Co1 95.65(4) 2_656 7_566 ?
N1 Co1 Co1 99.21(4) . 7_566 ?
N1 Co1 Co1 127.40(4) 2_656 7_566 ?
Co1 Co1 Co1 120.963(13) 8_565 7_566 ?
O1 Co1 Co1 93.48(4) . 6_565 ?
O1 Co1 Co1 93.48(4) 2_656 6_565 ?
O2 Co1 Co1 132.74(5) . 6_565 ?
O2 Co1 Co1 132.74(5) 2_656 6_565 ?
N1 Co1 Co1 38.85(4) . 6_565 ?
N1 Co1 Co1 38.85(4) 2_656 6_565 ?
Co1 Co1 Co1 119.519(7) 8_565 6_565 ?
Co1 Co1 Co1 119.519(7) 7_566 6_565 ?
O1 Co1 Co1 148.04(5) . 1_655 ?
O1 Co1 Co1 31.96(5) 2_656 1_655 ?
O2 Co1 Co1 119.83(4) . 1_655 ?
O2 Co1 Co1 60.17(4) 2_656 1_655 ?
N1 Co1 Co1 104.89(4) . 1_655 ?
N1 Co1 Co1 75.11(4) 2_656 1_655 ?
Co1 Co1 Co1 29.519(7) 8_565 1_655 ?
Co1 Co1 Co1 150.481(7) 7_566 1_655 ?
Co1 Co1 Co1 90.0 6_565 1_655 ?
O1 Co1 Co1 118.03(4) . 3_545 ?
O1 Co1 Co1 68.64(5) 2_656 3_545 ?
O2 Co1 Co1 146.67(4) . 3_545 ?
O2 Co1 Co1 110.28(5) 2_656 3_545 ?
N1 Co1 Co1 56.50(4) . 3_545 ?
N1 Co1 Co1 36.43(4) 2_656 3_545 ?
Co1 Co1 Co1 90.074(7) 8_565 3_545 ?
Co1 Co1 Co1 148.964(7) 7_566 3_545 ?
Co1 Co1 Co1 29.445(2) 6_565 3_545 ?
Co1 Co1 Co1 60.555(1) 1_655 3_545 ?
O1 Co1 Co1 139.29(4) . 6_665 ?
O1 Co1 Co1 45.95(5) 2_656 6_665 ?
O2 Co1 Co1 140.92(4) . 6_665 ?
O2 Co1 Co1 85.66(4) 2_656 6_665 ?
N1 Co1 Co1 79.52(4) . 6_665 ?
N1 Co1 Co1 51.53(4) 2_656 6_665 ?
Co1 Co1 Co1 60.593(4) 8_565 6_665 ?
Co1 Co1 Co1 178.444(10) 7_566 6_665 ?
Co1 Co1 Co1 58.926(3) 6_565 6_665 ?
Co1 Co1 Co1 31.074(3) 1_655 6_665 ?
Co1 Co1 Co1 29.481(3) 3_545 6_665 ?
N1 C1 N1 126.3(2) 6_565 . ?
N1 C1 C1 116.83(11) 6_565 2_656 ?
N1 C1 C1 116.83(11) . 2_656 ?
C1 N1 C2 116.86(18) . . ?
C1 N1 Co1 114.32(13) . . ?
C2 N1 Co1 128.78(14) . . ?
N1 C2 C3 120.8(2) . . ?
N1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C2 C3 C2 118.2(3) . 6_565 ?
C2 C3 H3 120.9 . . ?
C2 C3 H3 120.9 6_565 . ?
O1 C4 O2 126.75(17) . 7_566 ?
O1 C4 C4 116.6(2) . 7_566 ?
O2 C4 C4 116.7(2) 7_566 7_566 ?
C4 O1 Co1 113.76(12) . . ?
C4 O2 Co1 113.25(12) 7_566 . ?
O3W O1W O3W 125.5(7) 6_565 5_767 ?
O3W O1W O2W 14.9(3) 6_565 . ?
O3W O1W O2W 110.8(4) 5_767 . ?
O3W O1W O2 139.9(3) 6_565 4_646 ?
O3W O1W O2 72.0(3) 5_767 4_646 ?
O2W O1W O2 138.95(17) . 4_646 ?
O2W O2W O3W 146.4(4) 6_565 6_565 ?
O2W O2W O3W 17.29(19) 6_565 . ?
O3W O2W O3W 129.1(5) 6_565 . ?
O2W O2W O1W 131.91(18) 6_565 . ?
O3W O2W O1W 14.9(3) 6_565 . ?
O3W O2W O1W 114.7(3) . . ?
O2W O2W O2W 61.2(3) 6_565 5_768 ?
O3W O2W O2W 130.1(6) 6_565 5_768 ?
O3W O2W O2W 70.8(3) . 5_768 ?
O1W O2W O2W 134.6(4) . 5_768 ?
O1W O3W O2W 150.1(6) 5_767 6_565 ?
O1W O3W O3W 27.2(3) 5_767 2_757 ?
O2W O3W O3W 123.1(4) 6_565 2_757 ?
O1W O3W O2W 134.3(5) 5_767 . ?
O2W O3W O2W 16.3(3) 6_565 . ?
O3W O3W O2W 107.07(19) 2_757 . ?
O1W O3W O2 77.7(3) 5_767 8_566 ?
O2W O3W O2 127.1(4) 6_565 8_566 ?
O3W O3W O2 98.6(2) 2_757 8_566 ?
O2W O3W O2 135.0(3) . 8_566 ?

_refine_diff_density_max         1.014
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.082

_shelxl_version_number           2013-4

_shelx_res_file                  
;
TITL cobmox3 in C2/m
CELL 0.71073   9.4514  16.7427   6.1969  90.000 101.455  90.000
ZERR    2.00   0.0002   0.0004   0.0002   0.000   0.001   0.000
LATT  7
SYMM -X, Y, -Z
SFAC C H N O CO
UNIT 24 32 8 26 4
TEMP 23
SIZE 0.10 0.10 0.04
L.S. 20

FMAP 2

ACTA

PLAN 10

EQIV $1 x, y, -1+z
EQIV $2 x, 1-y, z
EQIV $3 0.5+x, 1.5-y, z
EQIV $4 0.5-x, 1.5-y, 1-z
EQIV $5 2-x, y, 2-z
EQIV $6 1+x, y, z
EQIV $7 1+x, 1-y, z
EQIV $8 0.5+x, -0.5+y, z
EQIV $9 1.5-x, -0.5+y, 1-z
EQIV $10 2-x, 1-y, 3-z
EQIV $11 0.5+x, 1.5-y, 1+z
EQIV $12 1-X, Y, 1-Z
EQIV $13 1-X, 1-Y, 1-Z

BOND $H

BIND Co1 Co1_$2
BIND Co1 Co1_$3
BIND CO1 CO1_$4
BIND Co1 Co1_$6
BIND Co1 Co1_$7
BIND Co1 Co1_$8
BIND O1W O2w
BIND O2w O3W
BIND O3w O3w_$5
BIND O1W O2_$9
BIND O2W O2W_$10
BIND O3W O2_$11

MPLA 12 C1 N1 C2 C3 C2_$2 N1_$2 C1_$12 N1_$12 C2_$12 C3_$12 C2_$13 N1_$13 CO1
MPLA 6 O1 O2 C4 O1_$4 O2_$4 C4_$4 Co1
MPLA 5 O1W O2W O3W O2W_$5 O3W_$5
MPLA CO1 CO1_$2 CO1_$3 CO1_$6 CO1_$7 CO1_$8

WGHT    0.056900    0.736200
FVAR       0.55015
CO1   5    0.500000    0.670093    0.500000    10.50000    0.02786    0.02237 =
         0.03638    0.00000    0.00606    0.00000
C1    1    0.453079    0.500000    0.389218    10.50000    0.02326    0.02426 =
         0.02635    0.00000    0.00418    0.00000
N1    3    0.415762    0.570786    0.298887    11.00000    0.02839    0.02578 =
         0.02995    0.00302    0.00243    0.00004
C2    1    0.335290    0.570846    0.093803    11.00000    0.03736    0.03910 =
         0.03275    0.00862    0.00237    0.00198
AFIX  43
H2    2    0.306378    0.619161    0.024924    11.00000   -1.20000
AFIX   0
C3    1    0.295034    0.500000   -0.015837    10.50000    0.03965    0.05281 =
         0.02761    0.00000   -0.00253    0.00000
AFIX  43
H3    2    0.242285    0.500000   -0.159507    10.50000   -1.20000
AFIX   0
C4    1    0.241650    0.727624    0.606419    11.00000    0.03190    0.02567 =
         0.03161    0.00540    0.00710    0.00004
O1    4    0.336831    0.677631    0.679982    11.00000    0.03802    0.03879 =
         0.04305    0.01743    0.01459    0.01282
O2    4    0.365848    0.754790    0.314111    11.00000    0.03581    0.03809 =
         0.04197    0.01261    0.01552    0.00849
O1W   4    1.000000    0.341730    1.000000    10.25000    0.06625
O2W   4    1.079035    0.457594    1.352073    10.50000    0.12948
O3W   4    1.040558    0.617210    1.219106    10.50000    0.09723

HKLF 4

REM  cobmox3 in C2/m
REM R1 =  0.0355 for    1361 Fo > 4sig(Fo)  and  0.0456 for all    1603 data
REM     73 parameters refined using      0 restraints

END

WGHT      0.0569      0.7362

REM Highest difference peak  1.014,  deepest hole -0.377,  1-sigma level  0.082
Q1    1   1.0474  0.3391  1.0674  11.00000  0.05    1.01
Q2    1   0.2500  0.7500  0.5000  10.50000  0.05    0.47
Q3    1   0.5000  0.5000  0.5000  10.25000  0.05    0.40
Q4    1   1.0657  0.6017  1.3206  11.00000  0.05    0.38
Q5    1   1.0443  0.3077  0.8997  11.00000  0.05    0.37
Q6    1   1.0205  0.5000  1.2383  10.50000  0.05    0.35
Q7    1   1.1027  0.5000  1.4658  10.50000  0.05    0.31
Q8    1   0.4938  0.6309  0.5572  11.00000  0.05    0.31
Q9    1   0.4351  0.6073  0.3647  11.00000  0.05    0.29
Q10   1   0.3812  0.7664  0.2547  11.00000  0.05    0.27
;
_shelx_res_checksum              61243

_exptl_crystal_recrystallization_method 'slow diffusion'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_zn2dc2m
_database_code_depnum_ccdc_archive 'CCDC 1039719'
_audit_update_record             
;
2014-12-16 deposited with the CCDC.
2015-04-27 downloaded from the CCDC.
;

_vrf_PLAT058_zn2dc2m             
;
PROBLEM: Maximum Transmission Factor Missing ............          ?      
RESPONSE: Data not available. The ratio of minimum to maximum apparent 
          transmission, as reported in the .abs file, is 0.795483. 
          That comes from the applied 'SADABS-2004/1 - Bruker Nonius area 
          detector scaling and absorption correction'
;
_vrf_PLAT059_zn2dc2m             
;
PROBLEM: Minimum Transmission Factor Missing ............          ?      
RESPONSE: See above.
;
_vrf_PLAT430_zn2dc2m             
;
PROBLEM: Short Inter D...A Contact  O1W    ..  O3W     ..       1.50 Ang.  
RESPONSE: As described in the main text, the water molecules of crystallization
          present in the structure are interconnected through H-bonds into
          pentameric motifs (rings) residing in the supramolecular channels
          generated by the superimposition of the [Zn2(bpm)(ox)4]n layers along
          the crystallographic c-axis. By applying the symmetry operations of
          the space group C2/m to the water oxygen atoms in the asymmetric unit,
          a 10-member ring with a series of short Ow...Ow contact is generated.
          As already established for published structures (see ref.s 37and 40
          in the main text), this false image is the result of the superimposition
          of two staggered rings along the c-axis (truly it should be said groups
          of rings). Each one of the three water oxygen atoms in the asymmetric
          unit participates to the construction of both rings. To account for
          this disorder, and in line with TGA data, the total occupancy of these
          water oxygen atoms is imposed as 2.5 (there are 5 water molecules every
          two metal ions). 
;
_vrf_PLAT043_zn2dc2m             
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      10.04 Check 
RESPONSE: The hydrogen atoms on the water molecules of crystallization have
          not be found neither placed because of the disorder discussed above.
          Nonetheless, these hydrogen atoms have been included for the calculation
          of the molecular weight (hence the discrepancy between reported and 
          calculated values).
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 N4 O8 Zn2, (O5)'
_chemical_formula_sum            'C12 H16 N4 O13 Zn2'
_chemical_formula_weight         555.03

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   9.5335(10)
_cell_length_b                   16.614(2)
_cell_length_c                   6.1915(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.659(3)
_cell_angle_gamma                90
_cell_volume                     960.42(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4932
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      31.42

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_F_000             560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    2.576
_shelx_estimated_absorpt_T_min   0.861
_shelx_estimated_absorpt_T_max   0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_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            10829
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.452
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1520
_reflns_number_gt                1359
_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    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0475P)²+0.9680P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Direct
_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         1520
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.67327(2) 0.5000 0.02821(12) Uani 1 2 d S T P . .
C1 C 0.4533(2) 0.5000 0.3882(4) 0.0227(4) Uani 1 2 d S T P . .
N1 N 0.41625(16) 0.57100(9) 0.2979(2) 0.0268(3) Uani 1 1 d . . . . .
C2 C 0.3357(2) 0.57075(13) 0.0931(3) 0.0339(4) Uani 1 1 d . . . . .
H2 H 0.3068 0.6194 0.0239 0.041 Uiso 1 1 calc R U . . .
C3 C 0.2952(3) 0.5000 -0.0156(5) 0.0383(6) Uani 1 2 d S T P . .
H3 H 0.2418 0.5000 -0.1591 0.046 Uiso 1 2 calc R U P . .
C4 C 0.2440(2) 0.72824(11) 0.6085(3) 0.0281(4) Uani 1 1 d . . . . .
O1 O 0.34123(18) 0.68067(9) 0.6859(3) 0.0368(3) Uani 1 1 d . . . . .
O2 O 0.36311(16) 0.75521(9) 0.3118(2) 0.0352(3) Uani 1 1 d . . . . .
O1W O 1.0000 0.3434(4) 1.0000 0.0619(15) Uiso 0.5 2 d S . P . .
O2W O 1.0824(9) 0.4581(5) 1.3573(13) 0.124(3) Uiso 0.5 1 d . . P . .
O3W O 1.0389(8) 0.6162(4) 1.2205(11) 0.1017(19) Uiso 0.5 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.02560(17) 0.02310(17) 0.03567(19) 0.000 0.00557(12) 0.000
C1 0.0210(10) 0.0236(10) 0.0232(10) 0.000 0.0035(8) 0.000
N1 0.0256(7) 0.0255(7) 0.0280(7) 0.0035(6) 0.0024(6) 0.0004(6)
C2 0.0334(9) 0.0365(10) 0.0294(9) 0.0084(8) 0.0007(7) 0.0018(8)
C3 0.0361(14) 0.0509(18) 0.0237(12) 0.000 -0.0040(10) 0.000
C4 0.0292(8) 0.0254(8) 0.0294(8) 0.0041(7) 0.0050(7) 0.0008(7)
O1 0.0345(7) 0.0394(8) 0.0383(8) 0.0153(6) 0.0120(6) 0.0123(6)
O2 0.0328(7) 0.0368(7) 0.0388(8) 0.0114(6) 0.0140(6) 0.0077(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O2 2.0736(14) . ?
Zn1 O2 2.0736(15) 2_656 ?
Zn1 O1 2.0820(16) 2_656 ?
Zn1 O1 2.0820(16) . ?
Zn1 N1 2.1649(16) . ?
Zn1 N1 2.1649(16) 2_656 ?
Zn1 Zn1 5.4058(5) 8_565 ?
Zn1 Zn1 5.4058(5) 7_566 ?
Zn1 Zn1 5.7572(9) 6_565 ?
Zn1 Zn1 9.5335(10) 1_655 ?
Zn1 Zn1 9.5774(9) 3_545 ?
Zn1 Zn1 11.1370(10) 6_665 ?
C1 N1 1.3225(18) 6_565 ?
C1 N1 1.3225(18) . ?
C1 C1 1.487(5) 2_656 ?
N1 C2 1.343(2) . ?
C2 C3 1.371(3) . ?
C2 H2 0.9300 . ?
C3 C2 1.371(3) 6_565 ?
C3 H3 0.9300 . ?
C4 O1 1.239(2) . ?
C4 O2 1.251(2) 7_566 ?
C4 C4 1.550(4) 7_566 ?
O2 C4 1.251(2) 7_566 ?
O1W O3W 1.499(7) 6_565 ?
O1W O3W 1.499(7) 5_767 ?
O1W O2W 2.906(9) . ?
O1W O2 2.931(4) 4_646 ?
O2W O2W 1.392(16) 6_565 ?
O2W O3W 1.507(9) 6_565 ?
O2W O3W 2.765(11) . ?
O2W O2W 2.941(16) 5_768 ?
O3W O1W 1.499(7) 5_767 ?
O3W O2W 1.507(9) 6_565 ?
O3W O3W 2.680(14) 2_757 ?
O3W O2 2.842(7) 8_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O2 97.93(9) . 2_656 ?
O2 Zn1 O1 95.50(6) . 2_656 ?
O2 Zn1 O1 80.01(5) 2_656 2_656 ?
O2 Zn1 O1 80.01(5) . . ?
O2 Zn1 O1 95.50(6) 2_656 . ?
O1 Zn1 O1 173.23(8) 2_656 . ?
O2 Zn1 N1 94.22(6) . . ?
O2 Zn1 N1 163.11(6) 2_656 . ?
O1 Zn1 N1 87.20(6) 2_656 . ?
O1 Zn1 N1 98.14(6) . . ?
O2 Zn1 N1 163.11(6) . 2_656 ?
O2 Zn1 N1 94.23(6) 2_656 2_656 ?
O1 Zn1 N1 98.13(6) 2_656 2_656 ?
O1 Zn1 N1 87.20(6) . 2_656 ?
N1 Zn1 N1 76.59(8) . 2_656 ?
O2 Zn1 Zn1 98.35(4) . 8_565 ?
O2 Zn1 Zn1 40.14(4) 2_656 8_565 ?
O1 Zn1 Zn1 39.88(4) 2_656 8_565 ?
O1 Zn1 Zn1 135.38(5) . 8_565 ?
N1 Zn1 Zn1 126.32(4) . 8_565 ?
N1 Zn1 Zn1 98.51(4) 2_656 8_565 ?
O2 Zn1 Zn1 40.14(4) . 7_566 ?
O2 Zn1 Zn1 98.34(4) 2_656 7_566 ?
O1 Zn1 Zn1 135.38(5) 2_656 7_566 ?
O1 Zn1 Zn1 39.88(4) . 7_566 ?
N1 Zn1 Zn1 98.51(4) . 7_566 ?
N1 Zn1 Zn1 126.32(4) 2_656 7_566 ?
Zn1 Zn1 Zn1 123.716(13) 8_565 7_566 ?
O2 Zn1 Zn1 131.04(5) . 6_565 ?
O2 Zn1 Zn1 131.04(5) 2_656 6_565 ?
O1 Zn1 Zn1 93.38(4) 2_656 6_565 ?
O1 Zn1 Zn1 93.39(4) . 6_565 ?
N1 Zn1 Zn1 38.30(4) . 6_565 ?
N1 Zn1 Zn1 38.30(4) 2_656 6_565 ?
Zn1 Zn1 Zn1 118.142(6) 8_565 6_565 ?
Zn1 Zn1 Zn1 118.142(7) 7_566 6_565 ?
O2 Zn1 Zn1 121.05(4) . 1_655 ?
O2 Zn1 Zn1 58.95(4) 2_656 1_655 ?
O1 Zn1 Zn1 32.99(5) 2_656 1_655 ?
O1 Zn1 Zn1 147.01(5) . 1_655 ?
N1 Zn1 Zn1 104.59(4) . 1_655 ?
N1 Zn1 Zn1 75.41(4) 2_656 1_655 ?
Zn1 Zn1 Zn1 28.142(6) 8_565 1_655 ?
Zn1 Zn1 Zn1 151.858(7) 7_566 1_655 ?
Zn1 Zn1 Zn1 90.0 6_565 1_655 ?
O2 Zn1 Zn1 145.70(4) . 3_545 ?
O2 Zn1 Zn1 108.22(5) 2_656 3_545 ?
O1 Zn1 Zn1 68.52(4) 2_656 3_545 ?
O1 Zn1 Zn1 117.95(4) . 3_545 ?
N1 Zn1 Zn1 56.27(4) . 3_545 ?
N1 Zn1 Zn1 36.28(4) 2_656 3_545 ?
Zn1 Zn1 Zn1 88.294(10) 8_565 3_545 ?
Zn1 Zn1 Zn1 147.991(5) 7_566 3_545 ?
Zn1 Zn1 Zn1 29.849(4) 6_565 3_545 ?
Zn1 Zn1 Zn1 60.151(4) 1_655 3_545 ?
O2 Zn1 Zn1 141.34(4) . 6_665 ?
O2 Zn1 Zn1 84.14(4) 2_656 6_665 ?
O1 Zn1 Zn1 46.57(5) 2_656 6_665 ?
O1 Zn1 Zn1 138.46(4) . 6_665 ?
N1 Zn1 Zn1 79.05(4) . 6_665 ?
N1 Zn1 Zn1 51.58(4) 2_656 6_665 ?
Zn1 Zn1 Zn1 59.269(9) 8_565 6_665 ?
Zn1 Zn1 Zn1 177.015(8) 7_566 6_665 ?
Zn1 Zn1 Zn1 58.873(5) 6_565 6_665 ?
Zn1 Zn1 Zn1 31.127(5) 1_655 6_665 ?
Zn1 Zn1 Zn1 29.024(3) 3_545 6_665 ?
N1 C1 N1 126.2(2) 6_565 . ?
N1 C1 C1 116.88(11) 6_565 2_656 ?
N1 C1 C1 116.88(11) . 2_656 ?
C1 N1 C2 116.70(17) . . ?
C1 N1 Zn1 114.82(12) . . ?
C2 N1 Zn1 128.46(13) . . ?
N1 C2 C3 121.12(19) . . ?
N1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C2 C3 C2 118.1(3) . 6_565 ?
C2 C3 H3 121.0 . . ?
C2 C3 H3 121.0 6_565 . ?
O1 C4 O2 126.46(17) . 7_566 ?
O1 C4 C4 116.9(2) . 7_566 ?
O2 C4 C4 116.7(2) 7_566 7_566 ?
C4 O1 Zn1 113.26(12) . . ?
C4 O2 Zn1 113.17(12) 7_566 . ?
O3W O1W O3W 126.7(7) 6_565 5_767 ?
O3W O1W O2W 14.9(3) 6_565 . ?
O3W O1W O2W 112.2(5) 5_767 . ?
O3W O1W O2 139.7(3) 6_565 4_646 ?
O3W O1W O2 71.7(3) 5_767 4_646 ?
O2W O1W O2 137.85(17) . 4_646 ?
O2W O2W O3W 145.0(4) 6_565 6_565 ?
O2W O2W O3W 18.2(2) 6_565 . ?
O3W O2W O3W 126.7(5) 6_565 . ?
O2W O2W O1W 131.00(18) 6_565 . ?
O3W O2W O1W 14.8(3) 6_565 . ?
O3W O2W O1W 112.9(3) . . ?
O2W O2W O2W 61.8(3) 6_565 5_768 ?
O3W O2W O2W 127.3(6) 6_565 5_768 ?
O3W O2W O2W 70.7(3) . 5_768 ?
O1W O2W O2W 132.3(4) . 5_768 ?
O1W O3W O2W 150.3(6) 5_767 6_565 ?
O1W O3W O3W 26.6(3) 5_767 2_757 ?
O2W O3W O3W 124.1(4) 6_565 2_757 ?
O1W O3W O2W 134.3(5) 5_767 . ?
O2W O3W O2W 16.8(3) 6_565 . ?
O3W O3W O2W 107.8(2) 2_757 . ?
O1W O3W O2 78.3(3) 5_767 8_566 ?
O2W O3W O2 127.6(4) 6_565 8_566 ?
O3W O3W O2 98.6(3) 2_757 8_566 ?
O2W O3W O2 135.3(3) . 8_566 ?

_refine_diff_density_max         1.087
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.084

_shelxl_version_number           2013-4

_shelx_res_file                  
;
TITL zn2dc2m in C2/m
CELL 0.71073   9.5335  16.6138   6.1915  90.000 101.659  90.000
ZERR    2.00   0.0010   0.0021   0.0006   0.000   0.003   0.000
LATT 7
SYMM -X, Y, -Z
SFAC C  H  N  O  Zn
UNIT 24  32  8  26  4
TEMP 23
SIZE 0.060 0.060 0.060

L.S. 20

ACTA

FMAP 2

PLAN 10

EQIV $1 x, y, -1+z
EQIV $2 x, 1-y, z
EQIV $3 0.5+x, 1.5-y, z
EQIV $4 0.5-x, 1.5-y, 1-z
EQIV $5 2-x, y, 2-z
EQIV $6 1+x, y, z
EQIV $7 1+x, 1-y, z
EQIV $8 0.5+x, -0.5+y, z
EQIV $9 1.5-x, -0.5+y, 1-z
EQIV $10 2-x, 1-y, 3-z
EQIV $11 0.5+x, 1.5-y, 1+z
EQIV $12 1-X, Y, 1-Z
EQIV $13 1-X, 1-Y, 1-Z

BOND $H

BIND Zn1 Zn1_$2
BIND Zn1 Zn1_$3
BIND Zn1 Zn1_$4
BIND Zn1 Zn1_$6
BIND Zn1 Zn1_$7
BIND Zn1 Zn1_$8
BIND O1W O2w
BIND O2w O3W
BIND O3W O3W_$5
BIND O1W O2_$9
BIND O2W O2W_$10
BIND O3W O2_$11

MPLA 12 C1 N1 C2 C3 C2_$2 N1_$2 C1_$12 N1_$12 C2_$12 C3_$12 C2_$13 N1_$13 Zn1
MPLA 6 O1 O2 C4 O1_$4 O2_$4 C4_$4 Zn1
MPLA 5 O1W O2W O3W O2W_$5 O3W_$5
MPLA Zn1 Zn1_$2 Zn1_$3 Zn1_$6 Zn1_$7 Zn1_$8

WGHT    0.047500    0.968000
FVAR       0.50102
ZN1   5    0.500000    0.673266    0.500000    10.50000    0.02560    0.02310 =
         0.03567    0.00000    0.00557    0.00000
C1    1    0.453306    0.500000    0.388179    10.50000    0.02099    0.02362 =
         0.02318    0.00000    0.00352    0.00000
N1    3    0.416255    0.570998    0.297859    11.00000    0.02558    0.02551 =
         0.02798    0.00349    0.00237    0.00044
C2    1    0.335658    0.570746    0.093107    11.00000    0.03345    0.03647 =
         0.02942    0.00845    0.00069    0.00175
AFIX  43
H2    2    0.306808    0.619402    0.023939    11.00000   -1.20000
AFIX   0
C3    1    0.295202    0.500000   -0.015647    10.50000    0.03607    0.05094 =
         0.02375    0.00000   -0.00404    0.00000
AFIX  43
H3    2    0.241842    0.500000   -0.159085    10.50000   -1.20000
AFIX   0
C4    1    0.243952    0.728241    0.608476    11.00000    0.02918    0.02537 =
         0.02936    0.00413    0.00498    0.00081
O1    4    0.341226    0.680667    0.685862    11.00000    0.03452    0.03938 =
         0.03832    0.01532    0.01195    0.01229
O2    4    0.363113    0.755208    0.311777    11.00000    0.03276    0.03680 =
         0.03883    0.01143    0.01402    0.00769
O1W   4    1.000000    0.343383    1.000000    10.25000    0.06191
O2W   4    1.082407    0.458115    1.357327    10.50000    0.12437
O3W   4    1.038893    0.616174    1.220454    10.50000    0.10167

HKLF 4

REM  zn2dc2m in C2/m
REM R1 =  0.0307 for    1359 Fo > 4sig(Fo)  and  0.0357 for all    1520 data
REM     73 parameters refined using      0 restraints

END

WGHT      0.0475      0.9680

REM Highest difference peak  1.087,  deepest hole -0.368,  1-sigma level  0.084
Q1    1   1.0449  0.3405  1.0680  11.00000  0.05    1.09
Q2    1   0.5000  0.5000  0.5000  10.25000  0.05    0.46
Q3    1   1.0436  0.5000  1.2708  10.50000  0.05    0.46
Q4    1   1.0835  0.5988  1.3337  11.00000  0.05    0.46
Q5    1   0.2500  0.7500  0.5000  10.50000  0.05    0.41
Q6    1   0.3728  0.5688  0.2093  11.00000  0.05    0.37
Q7    1   0.4415  0.5358  0.3233  11.00000  0.05    0.34
Q8    1   1.0431  0.3067  0.8932  11.00000  0.05    0.28
Q9    1   0.3321  0.4728  0.0580  11.00000  0.05    0.27
Q10   1   0.3973  0.5906  0.3593  11.00000  0.05    0.24
;
_shelx_res_checksum              47849

_exptl_crystal_recrystallization_method 'slow diffusion'
####################################################################### 
# 
# 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_nibpox
_database_code_depnum_ccdc_archive 'CCDC 1039720'
_audit_update_record             
;
2014-12-16 deposited with the CCDC.
2015-04-27 downloaded from the CCDC.
;

_vrf_PLAT058_nibpox              
;
PROBLEM: Maximum Transmission Factor Missing ............          ?      
RESPONSE: Data not available. The ratio of minimum to maximum apparent 
          transmission, as reported in the .abs file, is 0.875871. 
          That comes from the applied 'SADABS-2004/1 - Bruker Nonius area 
          detector scaling and absorption correction'
;
_vrf_PLAT059_nibpox              
;
PROBLEM: Minimum Transmission Factor Missing ............          ?      
RESPONSE: See above.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 N8 Ni O4, 2(H2 O)'
_chemical_formula_sum            'C18 H16 N8 Ni O6'
_chemical_formula_weight         499.10

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

_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                   19.038(2)
_cell_length_b                   8.8357(8)
_cell_length_c                   15.2941(14)
_cell_angle_alpha                90
_cell_angle_beta                 128.246(6)
_cell_angle_gamma                90
_cell_volume                     2020.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5189
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      31.27

_exptl_crystal_description       prismatic
_exptl_crystal_colour            pale-violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_F_000             1024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.017
_shelx_estimated_absorpt_T_min   0.862
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   Sadabs


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_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            18070
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.678
_diffrn_reflns_theta_max         32.018
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3204
_reflns_number_gt                2860
_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    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0395P)²+0.9090P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Direct
_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         3204
_refine_ls_number_parameters     156
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0724
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.75524(2) 0.2500 0.02464(7) Uani 1 2 d S T P . .
C5 C 0.12170(7) 0.93045(13) 0.23388(9) 0.0284(2) Uani 1 1 d . . . . .
C4 C 0.06200(7) 0.85019(13) 0.12500(9) 0.0284(2) Uani 1 1 d . . . . .
C6 C 0.15740(8) 0.97287(14) 0.40428(10) 0.0340(2) Uani 1 1 d . . . . .
H6 H 0.1469 0.9582 0.4555 0.041 Uiso 1 1 calc R U . . .
C1 C -0.06129(9) 0.69933(16) 0.01335(10) 0.0366(3) Uani 1 1 d . . . . .
H1 H -0.1085 0.6443 0.0005 0.044 Uiso 1 1 calc R U . . .
C2 C -0.05120(10) 0.70688(18) -0.06852(11) 0.0430(3) Uani 1 1 d . . . . .
H2 H -0.0909 0.6584 -0.1366 0.052 Uiso 1 1 calc R U . . .
C7 C 0.22894(9) 1.06042(15) 0.43369(11) 0.0396(3) Uani 1 1 d . . . . .
H7 H 0.2681 1.1028 0.5043 0.048 Uiso 1 1 calc R U . . .
C3 C 0.01991(11) 0.78886(18) -0.04526(12) 0.0420(3) Uani 1 1 d . . . . .
H3 H 0.0286 0.7936 -0.0987 0.050 Uiso 1 1 calc R U . . .
C8 C 0.23968(9) 1.08201(17) 0.35384(12) 0.0449(3) Uani 1 1 d . . . . .
H8 H 0.2856 1.1449 0.3701 0.054 Uiso 1 1 calc R U . . .
N2 N 0.07743(8) 0.86254(14) 0.05152(9) 0.0379(2) Uani 1 1 d . . . . .
N1 N -0.00398(7) 0.77014(11) 0.11099(8) 0.0292(2) Uani 1 1 d . . . . .
N3 N 0.10257(6) 0.90831(11) 0.30375(8) 0.02713(18) Uani 1 1 d . . . . .
N4 N 0.18680(7) 1.01639(14) 0.25315(10) 0.0399(2) Uani 1 1 d . . . . .
O1 O 0.08808(5) 0.58028(10) 0.31283(8) 0.03409(18) Uani 1 1 d . . . . .
O2 O 0.09187(7) 0.32891(11) 0.31034(8) 0.0454(2) Uani 1 1 d . . . . .
C9 C 0.05217(7) 0.44940(13) 0.28561(9) 0.0289(2) Uani 1 1 d . . . . .
O1W O 0.24694(8) 0.66572(14) 0.35148(11) 0.0548(3) Uani 1 1 d D . . . .
H1W H 0.2665(13) 0.591(2) 0.3270(18) 0.082 Uiso 1 1 d D U . . .
H2W H 0.1942(10) 0.621(2) 0.3340(18) 0.082 Uiso 1 1 d D U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.02238(10) 0.02892(11) 0.02495(10) 0.000 0.01581(8) 0.000
C5 0.0258(4) 0.0298(5) 0.0306(5) 0.0026(4) 0.0179(4) 0.0008(4)
C4 0.0283(5) 0.0313(5) 0.0293(5) 0.0022(4) 0.0198(4) 0.0029(4)
C6 0.0338(5) 0.0346(6) 0.0290(5) -0.0018(4) 0.0171(4) -0.0008(4)
C1 0.0350(6) 0.0436(7) 0.0298(5) -0.0061(5) 0.0193(5) -0.0053(5)
C2 0.0481(7) 0.0506(7) 0.0304(6) -0.0065(5) 0.0243(6) -0.0004(6)
C7 0.0326(6) 0.0353(6) 0.0340(6) -0.0026(5) 0.0122(5) -0.0036(5)
C3 0.0529(8) 0.0492(7) 0.0366(6) 0.0020(6) 0.0340(6) 0.0060(6)
C8 0.0328(6) 0.0449(7) 0.0481(7) -0.0016(6) 0.0205(6) -0.0121(5)
N2 0.0431(5) 0.0451(6) 0.0386(5) 0.0019(5) 0.0318(5) 0.0007(5)
N1 0.0279(4) 0.0348(5) 0.0270(5) -0.0015(3) 0.0180(4) -0.0007(3)
N3 0.0255(4) 0.0290(4) 0.0265(4) 0.0001(3) 0.0160(3) -0.0003(3)
N4 0.0343(5) 0.0451(6) 0.0418(6) 0.0010(5) 0.0243(5) -0.0084(4)
O1 0.0255(4) 0.0337(4) 0.0412(4) 0.0005(3) 0.0198(3) 0.0019(3)
O2 0.0436(5) 0.0358(5) 0.0453(5) 0.0023(4) 0.0217(4) 0.0107(4)
C9 0.0309(5) 0.0335(5) 0.0238(5) 0.0013(4) 0.0176(4) 0.0033(4)
O1W 0.0510(6) 0.0566(7) 0.0753(8) -0.0013(6) 0.0483(6) 0.0033(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0323(9) 2 ?
Ni1 O1 2.0323(9) . ?
Ni1 N3 2.0810(10) . ?
Ni1 N3 2.0810(10) 2 ?
Ni1 N1 2.0842(10) 2 ?
Ni1 N1 2.0842(10) . ?
Ni1 Ni1 7.6794(10) 7_465 ?
Ni1 Ni1 8.7855(7) 5_575 ?
Ni1 Ni1 10.4941(9) 4_545 ?
Ni1 Ni1 15.2212(11) 5_585 ?
C5 N4 1.3219(15) . ?
C5 N3 1.3396(14) . ?
C5 C4 1.4915(16) . ?
C4 N2 1.3304(14) . ?
C4 N1 1.3381(15) . ?
C6 N3 1.3386(15) . ?
C6 C7 1.3775(18) . ?
C6 H6 0.9300 . ?
C1 N1 1.3397(16) . ?
C1 C2 1.3808(19) . ?
C1 H1 0.9300 . ?
C2 C3 1.374(2) . ?
C2 H2 0.9300 . ?
C7 C8 1.371(2) . ?
C7 H7 0.9300 . ?
C3 N2 1.3442(19) . ?
C3 H3 0.9300 . ?
C8 N4 1.3423(19) . ?
C8 H8 0.9300 . ?
O1 C9 1.2751(15) . ?
O2 C9 1.2222(15) . ?
C9 C9 1.566(2) 2 ?
O1W H1W 0.942(9) . ?
O1W H2W 0.950(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 80.95(5) 2 . ?
O1 Ni1 N3 168.23(4) 2 . ?
O1 Ni1 N3 90.56(4) . . ?
O1 Ni1 N3 90.56(4) 2 2 ?
O1 Ni1 N3 168.23(4) . 2 ?
N3 Ni1 N3 98.93(5) . 2 ?
O1 Ni1 N1 91.64(4) 2 2 ?
O1 Ni1 N1 93.86(4) . 2 ?
N3 Ni1 N1 97.09(4) . 2 ?
N3 Ni1 N1 78.15(4) 2 2 ?
O1 Ni1 N1 93.86(4) 2 . ?
O1 Ni1 N1 91.64(4) . . ?
N3 Ni1 N1 78.15(4) . . ?
N3 Ni1 N1 97.09(4) 2 . ?
N1 Ni1 N1 172.76(6) 2 . ?
O1 Ni1 Ni1 50.85(3) 2 7_465 ?
O1 Ni1 Ni1 127.81(3) . 7_465 ?
N3 Ni1 Ni1 133.06(3) . 7_465 ?
N3 Ni1 Ni1 48.16(3) 2 7_465 ?
N1 Ni1 Ni1 104.86(3) 2 7_465 ?
N1 Ni1 Ni1 75.23(3) . 7_465 ?
O1 Ni1 Ni1 114.05(3) 2 5_575 ?
O1 Ni1 Ni1 109.97(3) . 5_575 ?
N3 Ni1 Ni1 61.20(3) . 5_575 ?
N3 Ni1 Ni1 80.90(3) 2 5_575 ?
N1 Ni1 Ni1 146.85(3) 2 5_575 ?
N1 Ni1 Ni1 25.92(3) . 5_575 ?
Ni1 Ni1 Ni1 78.877(8) 7_465 5_575 ?
O1 Ni1 Ni1 99.36(3) 2 4_545 ?
O1 Ni1 Ni1 36.57(3) . 4_545 ?
N3 Ni1 Ni1 69.16(3) . 4_545 ?
N3 Ni1 Ni1 154.55(3) 2 4_545 ?
N1 Ni1 Ni1 124.50(3) 2 4_545 ?
N1 Ni1 Ni1 59.12(3) . 4_545 ?
Ni1 Ni1 Ni1 124.064(7) 7_465 4_545 ?
Ni1 Ni1 Ni1 73.651(5) 5_575 4_545 ?
O1 Ni1 Ni1 132.59(3) 2 5_585 ?
O1 Ni1 Ni1 129.69(3) . 5_585 ?
N3 Ni1 Ni1 49.06(3) . 5_585 ?
N3 Ni1 Ni1 62.06(3) 2 5_585 ?
N1 Ni1 Ni1 116.53(3) 2 5_585 ?
N1 Ni1 Ni1 56.24(3) . 5_585 ?
Ni1 Ni1 Ni1 84.010(6) 7_465 5_585 ?
Ni1 Ni1 Ni1 30.349(1) 5_575 5_585 ?
Ni1 Ni1 Ni1 94.698(5) 4_545 5_585 ?
N4 C5 N3 125.90(11) . . ?
N4 C5 C4 118.90(10) . . ?
N3 C5 C4 115.19(9) . . ?
N2 C4 N1 125.76(11) . . ?
N2 C4 C5 119.34(10) . . ?
N1 C4 C5 114.90(9) . . ?
N3 C6 C7 121.65(12) . . ?
N3 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
N1 C1 C2 120.92(12) . . ?
N1 C1 H1 119.5 . . ?
C2 C1 H1 119.5 . . ?
C3 C2 C1 117.29(13) . . ?
C3 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C8 C7 C6 116.74(12) . . ?
C8 C7 H7 121.6 . . ?
C6 C7 H7 121.6 . . ?
N2 C3 C2 122.74(12) . . ?
N2 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
N4 C8 C7 122.86(12) . . ?
N4 C8 H8 118.6 . . ?
C7 C8 H8 118.6 . . ?
C4 N2 C3 115.79(11) . . ?
C4 N1 C1 117.47(10) . . ?
C4 N1 Ni1 115.61(8) . . ?
C1 N1 Ni1 126.72(9) . . ?
C6 N3 C5 116.76(10) . . ?
C6 N3 Ni1 127.19(8) . . ?
C5 N3 Ni1 115.58(7) . . ?
C5 N4 C8 115.95(11) . . ?
C9 O1 Ni1 114.64(7) . . ?
O2 C9 O1 125.81(11) . . ?
O2 C9 C9 119.36(7) . 2 ?
O1 C9 C9 114.83(6) . 2 ?
H1W O1W H2W 102.0(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H2W O1 0.950(9) 1.873(9) 2.8022(14) 165.5(18) .
O1W H1W N4 0.942(9) 2.019(12) 2.8969(16) 154.3(19) 4_545

_refine_diff_density_max         0.373
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.047

_shelxl_version_number           2013-4

_shelx_res_file                  
;
TITL nibpox in C2/c
CELL 0.71073  19.0378   8.8357  15.2941  90.000 128.246  90.000
ZERR    4.00   0.0020   0.0008   0.0014   0.000   0.006   0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C  H  N  O  Ni
UNIT 72  64  32  24  4
TEMP 23
SIZE 0.15 0.15 0.10
L.S. 20

ACTA

FMAP 2

PLAN 5

DFIX 0.96 0.01 O1W H1W O1W H2W
DFIX 1.48 0.01 H1W H2W

EQIV_$1 -X, Y, -Z+1/2
EQIV_$2 -X+1/2, Y-1/2, -Z+1/2
EQIV_$3 -X, -Y+2, -Z
EQIV_$4 -X, -Y+3, -Z
EQIV_$5 -X-1/2, -Y+3/2, -Z

BOND $H

BIND NI1 NI1_$2
BIND NI1 NI1_$3
BIND NI1 NI1_$4
BIND NI1 NI1_$5

MPLA 12 C1 C2 C3 C4 C5 C6 C7 C8 N1 N2 N3 N4 NI1
MPLA 12 C1_$1 C2_$1 C3_$1 C4_$1 C5_$1 C6_$1 C7_$1 C8_$1 N1_$1 N2_$1 N3_$1 N4_$1
MPLA 6 C9 O1 O2 C9_$1 O1_$1 O2_$1 NI1
MPLA 12 C1 C2 C3 C4 C5 C6 C7 C8 N1 N2 N3 N4 NI1
HTAB O1W O1
HTAB O1W N4_$2

WGHT    0.039500    0.909000
FVAR       0.34996
NI1   5    0.000000    0.755243    0.250000    10.50000    0.02238    0.02892 =
         0.02495    0.00000    0.01581    0.00000
C5    1    0.121699    0.930445    0.233882    11.00000    0.02579    0.02980 =
         0.03055    0.00259    0.01792    0.00082
C4    1    0.061995    0.850188    0.124996    11.00000    0.02833    0.03132 =
         0.02932    0.00218    0.01976    0.00286
C6    1    0.157398    0.972866    0.404277    11.00000    0.03376    0.03458 =
         0.02905   -0.00177    0.01712   -0.00079
AFIX  43
H6    2    0.146922    0.958241    0.455546    11.00000   -1.20000
AFIX   0
C1    1   -0.061287    0.699334    0.013345    11.00000    0.03496    0.04365 =
         0.02976   -0.00614    0.01927   -0.00533
AFIX  43
H1    2   -0.108520    0.644333    0.000522    11.00000   -1.20000
AFIX   0
C2    1   -0.051204    0.706883   -0.068522    11.00000    0.04809    0.05061 =
         0.03041   -0.00650    0.02433   -0.00040
AFIX  43
H2    2   -0.090931    0.658449   -0.136636    11.00000   -1.20000
AFIX   0
C7    1    0.228943    1.060416    0.433690    11.00000    0.03263    0.03534 =
         0.03397   -0.00263    0.01224   -0.00361
AFIX  43
H7    2    0.268052    1.102798    0.504277    11.00000   -1.20000
AFIX   0
C3    1    0.019913    0.788865   -0.045260    11.00000    0.05295    0.04919 =
         0.03656    0.00195    0.03402    0.00596
AFIX  43
H3    2    0.028620    0.793576   -0.098698    11.00000   -1.20000
AFIX   0
C8    1    0.239675    1.082015    0.353835    11.00000    0.03275    0.04487 =
         0.04812   -0.00158    0.02051   -0.01210
AFIX  43
H8    2    0.285587    1.144871    0.370123    11.00000   -1.20000
AFIX   0
N2    3    0.077426    0.862543    0.051516    11.00000    0.04314    0.04506 =
         0.03862    0.00195    0.03182    0.00069
N1    3   -0.003975    0.770138    0.110988    11.00000    0.02790    0.03475 =
         0.02701   -0.00155    0.01801   -0.00073
N3    3    0.102571    0.908309    0.303751    11.00000    0.02553    0.02905 =
         0.02653    0.00006    0.01597   -0.00026
N4    3    0.186800    1.016387    0.253145    11.00000    0.03430    0.04514 =
         0.04180    0.00102    0.02432   -0.00835
O1    4    0.088081    0.580284    0.312833    11.00000    0.02552    0.03368 =
         0.04125    0.00049    0.01975    0.00188
O2    4    0.091873    0.328906    0.310339    11.00000    0.04358    0.03578 =
         0.04529    0.00232    0.02170    0.01074
C9    1    0.052173    0.449396    0.285613    11.00000    0.03087    0.03347 =
         0.02376    0.00132    0.01760    0.00329
O1W   4    0.246938    0.665717    0.351483    11.00000    0.05098    0.05662 =
         0.07527   -0.00128    0.04828    0.00333
H1W   2    0.266483    0.590990    0.326965    11.00000   -1.50000
H2W   2    0.194169    0.621273    0.333975    11.00000   -1.50000
HKLF 4

REM  nibpox in C2/c
REM R1 =  0.0259 for    2860 Fo > 4sig(Fo)  and  0.0298 for all    3204 data
REM    156 parameters refined using      3 restraints

END

WGHT      0.0395      0.9090

REM Highest difference peak  0.373,  deepest hole -0.210,  1-sigma level  0.047
Q1    1   0.0000  0.4490  0.2500  10.50000  0.05    0.37
Q2    1   0.0892  0.8926  0.1799  11.00000  0.05    0.33
Q3    1  -0.0647  0.7195 -0.0397  11.00000  0.05    0.30
Q4    1   0.1126  0.9229  0.2716  11.00000  0.05    0.29
Q5    1  -0.0258  0.7414  0.0690  11.00000  0.05    0.27
;
_shelx_res_checksum              77768

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
