# Electronic Supplementary Material (ESI) for RSC Advances.
# 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. 
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data_JTM371_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1056388'
_audit_update_record             
;
2015-03-26 deposited with the CCDC.
2015-08-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H6 Cr N2 O10, C7 H11 N2, 4(H2 O)'
_chemical_formula_sum            'C21 H25 Cr N4 O14'
_chemical_formula_weight         609.45

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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   15.097(3)
_cell_length_b                   8.9400(17)
_cell_length_c                   19.597(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.171(3)
_cell_angle_gamma                90
_cell_volume                     2552.8(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9955
_cell_measurement_theta_min      2.5199
_cell_measurement_theta_max      29.0715
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_F_000             1260
_exptl_transmission_factor_min   0.812
_exptl_transmission_factor_max   0.971
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.528
_shelx_estimated_absorpt_T_min   0.888
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.95

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, collected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 20 sec/frame.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3660
_diffrn_reflns_number            47440
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.975
_diffrn_reflns_theta_max         29.096
_diffrn_reflns_theta_full        28.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             13194
_reflns_number_gt                12180
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_max     0.944
_reflns_Friedel_fraction_full    0.988

_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2014)'

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms attached to carbon 
were placed in calculated positions (C---H = 0.95 - 0.98 Å) while those 
attached to nitrogen and oxygen were placed in locations derived from a 
difference map (except for tose on the disordered lattice water molecules) 
and their coordinates adjusted to give N---H = 0.91 %A and O---H = 0.84 Å. 
For the disordered water molecules, the H-atoms were placed based on formation 
of reasonable H-bonding interactions. All were included as riding 
contributions with isotropic displacement parameters 1.2 - 1.5 times those of 
the attached atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0344P)²+0.8596P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5109 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons et al., 2013.
;
_refine_ls_abs_structure_Flack   -0.007(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         13194
_refine_ls_number_parameters     733
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
Cr1 Cr 0.26923(3) 0.56940(5) 0.23900(2) 0.01166(9) Uani 1 1 d . . . . .
O1 O 0.36222(14) 0.4145(2) 0.28430(11) 0.0156(4) Uani 1 1 d . . . . .
O2 O 0.48262(14) 0.2810(2) 0.27251(11) 0.0199(4) Uani 1 1 d . . . . .
O3 O 0.20354(13) 0.7103(2) 0.16467(10) 0.0139(4) Uani 1 1 d . . . . .
O4 O 0.19599(14) 0.7995(2) 0.05650(11) 0.0201(4) Uani 1 1 d . . . . .
O5 O 0.47974(15) 0.4861(3) 0.01954(12) 0.0261(5) Uani 1 1 d . . . . .
H5A H 0.4540 0.5268 -0.0192 0.031 Uiso 1 1 d R U . . .
O6 O 0.34230(13) 0.7394(2) 0.29202(10) 0.0142(4) Uani 1 1 d . . . . .
O7 O 0.36214(14) 0.8838(2) 0.38859(11) 0.0173(4) Uani 1 1 d . . . . .
O8 O 0.16770(13) 0.4170(2) 0.21486(10) 0.0147(4) Uani 1 1 d . . . . .
O9 O 0.04831(14) 0.3214(2) 0.24861(11) 0.0198(4) Uani 1 1 d . . . . .
O10 O 0.07326(14) 0.6740(2) 0.46644(10) 0.0175(4) Uani 1 1 d . . . . .
H10A H 0.1012 0.7354 0.4970 0.021 Uiso 1 1 d R U . . .
N1 N 0.33650(16) 0.5402(3) 0.16657(12) 0.0132(5) Uani 1 1 d . . . . .
N2 N 0.20671(15) 0.6024(3) 0.31418(12) 0.0126(4) Uani 1 1 d . . . . .
C1 C 0.42109(19) 0.3739(3) 0.25088(15) 0.0149(5) Uani 1 1 d . . . . .
C2 C 0.40881(19) 0.4479(3) 0.17960(15) 0.0144(5) Uani 1 1 d . . . . .
C3 C 0.4590(2) 0.4289(3) 0.13091(16) 0.0187(6) Uani 1 1 d . . . . .
H3 H 0.5106 0.3639 0.1404 0.022 Uiso 1 1 calc R U . . .
C4 C 0.4320(2) 0.5081(3) 0.06651(16) 0.0183(6) Uani 1 1 d . . . . .
C5 C 0.35584(19) 0.6057(3) 0.05428(14) 0.0156(5) Uani 1 1 d . . . . .
H5 H 0.3368 0.6611 0.0116 0.019 Uiso 1 1 calc R U . . .
C6 C 0.31014(18) 0.6180(3) 0.10633(14) 0.0134(5) Uani 1 1 d . . . . .
C7 C 0.22984(19) 0.7183(3) 0.10668(15) 0.0148(5) Uani 1 1 d . . . . .
C8 C 0.32189(18) 0.7853(3) 0.34842(14) 0.0135(5) Uani 1 1 d . . . . .
C9 C 0.23916(18) 0.7084(3) 0.36253(14) 0.0123(5) Uani 1 1 d . . . . .
C10 C 0.19741(18) 0.7370(3) 0.41599(14) 0.0133(5) Uani 1 1 d . . . . .
H10 H 0.2207 0.8114 0.4506 0.016 Uiso 1 1 calc R U . . .
C11 C 0.11948(19) 0.6527(3) 0.41762(14) 0.0128(5) Uani 1 1 d . . . . .
C12 C 0.08618(19) 0.5416(3) 0.36630(14) 0.0133(5) Uani 1 1 d . . . . .
H12 H 0.0336 0.4834 0.3667 0.016 Uiso 1 1 calc R U . . .
C13 C 0.13338(19) 0.5209(3) 0.31537(14) 0.0126(5) Uani 1 1 d . . . . .
C14 C 0.11248(19) 0.4096(3) 0.25492(15) 0.0144(5) Uani 1 1 d . . . . .
Cr2 Cr 0.20757(3) 0.09174(5) 0.73646(2) 0.01432(10) Uani 1 1 d . . . . .
O11 O 0.29254(14) 0.2439(2) 0.79183(11) 0.0190(4) Uani 1 1 d . . . . .
O12 O 0.42191(16) 0.3720(3) 0.79835(14) 0.0303(6) Uani 1 1 d . . . . .
O13 O 0.15511(13) -0.0522(2) 0.65642(10) 0.0173(4) Uani 1 1 d . . . . .
O14 O 0.18019(15) -0.1505(3) 0.55775(11) 0.0240(5) Uani 1 1 d . . . . .
O15 O 0.50656(13) 0.0969(2) 0.58532(10) 0.0177(4) Uani 1 1 d . . . . .
H15A H 0.5018 0.0231 0.5581 0.021 Uiso 1 1 d R U . . .
O16 O 0.26972(14) -0.0751(2) 0.79953(11) 0.0184(4) Uani 1 1 d . . . . .
O17 O 0.26452(15) -0.2144(3) 0.89326(12) 0.0244(5) Uani 1 1 d . . . . .
O18 O 0.11240(14) 0.2434(2) 0.69615(11) 0.0174(4) Uani 1 1 d . . . . .
O19 O -0.01085(14) 0.3632(2) 0.71287(11) 0.0187(4) Uani 1 1 d . . . . .
O20 O -0.02405(14) 0.0714(3) 0.94254(10) 0.0213(4) Uani 1 1 d . . . . .
H20A H -0.0025 0.0232 0.9800 0.026 Uiso 1 1 d R U . . .
N3 N 0.29843(16) 0.1074(3) 0.68069(12) 0.0150(5) Uani 1 1 d . . . . .
N4 N 0.12922(15) 0.0743(3) 0.80121(11) 0.0133(4) Uani 1 1 d . . . . .
C15 C 0.3641(2) 0.2797(3) 0.77006(16) 0.0194(6) Uani 1 1 d . . . . .
C16 C 0.37190(19) 0.1944(3) 0.70504(15) 0.0160(5) Uani 1 1 d . . . . .
C17 C 0.44305(19) 0.1951(3) 0.67313(15) 0.0166(5) Uani 1 1 d . . . . .
H17 H 0.4946 0.2586 0.6896 0.020 Uiso 1 1 calc R U . . .
C18 C 0.43686(18) 0.0983(3) 0.61513(14) 0.0141(5) Uani 1 1 d . . . . .
C19 C 0.35861(19) 0.0084(3) 0.59079(15) 0.0152(5) Uani 1 1 d . . . . .
H19 H 0.3530 -0.0564 0.5515 0.018 Uiso 1 1 calc R U . . .
C20 C 0.29046(19) 0.0166(3) 0.62535(14) 0.0142(5) Uani 1 1 d . . . . .
C21 C 0.2019(2) -0.0705(3) 0.61104(15) 0.0162(5) Uani 1 1 d . . . . .
C22 C 0.2352(2) -0.1130(3) 0.85109(15) 0.0166(6) Uani 1 1 d . . . . .
C23 C 0.15192(19) -0.0226(3) 0.85508(14) 0.0140(5) Uani 1 1 d . . . . .
C24 C 0.10339(19) -0.0296(3) 0.90533(15) 0.0153(5) Uani 1 1 d . . . . .
H24 H 0.1199 -0.0978 0.9437 0.018 Uiso 1 1 calc R U . . .
C25 C 0.02793(18) 0.0685(3) 0.89781(13) 0.0148(5) Uani 1 1 d . . . . .
C26 C 0.00567(18) 0.1686(3) 0.84020(14) 0.0143(5) Uani 1 1 d . . . . .
H26 H -0.0452 0.2345 0.8341 0.017 Uiso 1 1 calc R U . . .
C27 C 0.05861(18) 0.1690(3) 0.79357(14) 0.0126(5) Uani 1 1 d . . . . .
C28 C 0.0501(2) 0.2691(3) 0.72991(15) 0.0158(5) Uani 1 1 d . . . . .
N5 N 0.7429(2) 1.0054(4) 0.3982(2) 0.0412(9) Uani 1 1 d . . . . .
H5N H 0.7195 1.0735 0.3636 0.049 Uiso 1 1 d R U . . .
N6 N 0.8385(2) 0.6992(4) 0.55834(17) 0.0333(7) Uani 1 1 d . . . . .
C29 C 0.8068(2) 0.7970(4) 0.5059(2) 0.0296(8) Uani 1 1 d . . . . .
C30 C 0.8574(2) 0.8354(4) 0.45713(19) 0.0273(7) Uani 1 1 d . . . . .
H30 H 0.9148 0.7885 0.4602 0.033 Uiso 1 1 calc R U . . .
C31 C 0.8247(3) 0.9386(4) 0.4059(2) 0.0345(8) Uani 1 1 d . . . . .
H31 H 0.8608 0.9644 0.3745 0.041 Uiso 1 1 calc R U . . .
C32 C 0.6918(3) 0.9701(5) 0.4413(3) 0.0485(13) Uani 1 1 d . . . . .
H32 H 0.6337 1.0168 0.4347 0.058 Uiso 1 1 calc R U . . .
C33 C 0.7194(2) 0.8689(5) 0.4951(3) 0.0431(11) Uani 1 1 d . . . . .
H33 H 0.6809 0.8465 0.5251 0.052 Uiso 1 1 calc R U . . .
C34 C 0.9288(3) 0.6294(4) 0.5685(2) 0.0342(8) Uani 1 1 d . . . . .
H34A H 0.9318 0.5787 0.5248 0.051 Uiso 1 1 calc R U . . .
H34B H 0.9384 0.5564 0.6070 0.051 Uiso 1 1 calc R U . . .
H34C H 0.9765 0.7065 0.5804 0.051 Uiso 1 1 calc R U . . .
C35 C 0.7845(3) 0.6587(5) 0.6078(3) 0.0507(12) Uani 1 1 d . . . . .
H35A H 0.7663 0.7497 0.6285 0.076 Uiso 1 1 calc R U . . .
H35B H 0.8216 0.5956 0.6454 0.076 Uiso 1 1 calc R U . . .
H35C H 0.7295 0.6037 0.5825 0.076 Uiso 1 1 calc R U . . .
N7 N 0.7684(2) 0.8087(4) 1.04725(16) 0.0344(7) Uani 1 1 d . . . . .
H7N H 0.7852 0.8650 1.0873 0.041 Uiso 1 1 d R U . . .
N8 N 0.68951(16) 0.5858(3) 0.85717(14) 0.0228(5) Uani 1 1 d . . . . .
C36 C 0.7166(2) 0.6556(4) 0.91911(18) 0.0230(6) Uani 1 1 d . . . . .
C37 C 0.6659(2) 0.6449(4) 0.97083(19) 0.0289(7) Uani 1 1 d . . . . .
H37 H 0.6126 0.5839 0.9619 0.035 Uiso 1 1 calc R U . . .
C38 C 0.6930(2) 0.7212(5) 1.03285(19) 0.0344(8) Uani 1 1 d . . . . .
H38 H 0.6582 0.7127 1.0666 0.041 Uiso 1 1 calc R U . . .
C39 C 0.8190(2) 0.8201(4) 1.0002(2) 0.0333(8) Uani 1 1 d . . . . .
H39 H 0.8725 0.8810 1.0116 0.040 Uiso 1 1 calc R U . . .
C40 C 0.7966(2) 0.7480(4) 0.93752(18) 0.0266(7) Uani 1 1 d . . . . .
H40 H 0.8339 0.7587 0.9056 0.032 Uiso 1 1 calc R U . . .
C41 C 0.7428(2) 0.5870(4) 0.80445(17) 0.0251(6) Uani 1 1 d . . . . .
H41A H 0.7683 0.6872 0.8022 0.038 Uiso 1 1 calc R U . . .
H41B H 0.7029 0.5604 0.7580 0.038 Uiso 1 1 calc R U . . .
H41C H 0.7930 0.5143 0.8179 0.038 Uiso 1 1 calc R U . . .
C42 C 0.6057(2) 0.4954(4) 0.8397(2) 0.0298(7) Uani 1 1 d . . . . .
H42A H 0.6094 0.4191 0.8763 0.045 Uiso 1 1 calc R U . . .
H42B H 0.5992 0.4466 0.7939 0.045 Uiso 1 1 calc R U . . .
H42C H 0.5525 0.5599 0.8373 0.045 Uiso 1 1 calc R U . . .
O21 O 0.02747(17) 0.0562(3) 0.18081(12) 0.0299(5) Uani 1 1 d . . . . .
H21A H 0.0263 -0.0052 0.2130 0.036 Uiso 1 1 d R U . . .
H21B H 0.0398 0.1403 0.2000 0.036 Uiso 1 1 d R U . . .
O22 O 0.03666(15) 0.9372(2) 0.05777(11) 0.0209(4) Uani 1 1 d . . . . .
H22A H 0.0829 0.8820 0.0625 0.025 Uiso 1 1 d R U . . .
H22B H 0.0405 0.9773 0.0972 0.025 Uiso 1 1 d R U . . .
O23 O 0.8399(3) 0.0119(6) 0.1459(3) 0.0355(9) Uani 0.569(5) 1 d . . P A 1
H23A H 0.8973 0.0217 0.1586 0.043 Uiso 0.569(5) 1 d R U P A 1
H23B H 0.8216 0.0852 0.1191 0.043 Uiso 0.569(5) 1 d R U P A 1
O23A O 0.8063(5) -0.0249(8) 0.1718(3) 0.0355(9) Uani 0.431(5) 1 d . . P A 2
H23C H 0.7566 -0.0182 0.1833 0.043 Uiso 0.431(5) 1 d R U P A 2
H23D H 0.8395 0.0426 0.1951 0.043 Uiso 0.431(5) 1 d R U P A 2
O24 O 0.8897(4) 0.1815(6) 0.2788(3) 0.0562(12) Uani 0.648(6) 1 d . . P B 1
H24A H 0.9433 0.1991 0.2760 0.067 Uiso 0.648(6) 1 d R U P B 1
H24B H 0.8769 0.2542 0.3016 0.067 Uiso 0.648(6) 1 d R U P B 1
O24A O 0.8342(7) 0.1277(11) 0.2839(6) 0.0562(12) Uani 0.352(6) 1 d . . P B 2
H24C H 0.8238 0.1739 0.3184 0.067 Uiso 0.352(6) 1 d R U P B 2
H24D H 0.7832 0.1251 0.2537 0.067 Uiso 0.352(6) 1 d R U P B 2
O25 O 0.66913(17) 0.2048(3) 0.29022(17) 0.0442(7) Uani 1 1 d . . . . .
H25A H 0.6916 0.2624 0.2653 0.053 Uiso 1 1 d R U . . .
H25B H 0.6124 0.2212 0.2810 0.053 Uiso 1 1 d R U . . .
O26 O 0.51078(15) 0.8563(2) 0.51567(11) 0.0221(5) Uani 1 1 d . . . . .
H26A H 0.4736 0.8386 0.4764 0.027 Uiso 1 1 d R U . . .
H26B H 0.5096 0.7859 0.5438 0.027 Uiso 1 1 d R U . . .
O27 O 0.51510(15) 0.6242(2) 0.60517(12) 0.0238(5) Uani 1 1 d . . . . .
H27A H 0.5194 0.6719 0.6428 0.029 Uiso 1 1 d R U . . .
H27B H 0.5522 0.5523 0.6135 0.029 Uiso 1 1 d R U . . .
O28 O 0.41099(14) 0.5958(3) 0.89554(10) 0.0217(4) Uani 1 1 d . . . . .
H28A H 0.3641 0.6504 0.8861 0.026 Uiso 1 1 d R U . . .
H28B H 0.3984 0.5290 0.8643 0.026 Uiso 1 1 d 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
Cr1 N1 1.967(2) . ?
Cr1 N2 1.969(2) . ?
Cr1 O3 1.9841(19) . ?
Cr1 O6 2.001(2) . ?
Cr1 O1 2.006(2) . ?
Cr1 O8 2.013(2) . ?
O1 C1 1.286(3) . ?
O2 C1 1.236(3) . ?
O3 C7 1.300(3) . ?
O4 C7 1.222(3) . ?
O5 C4 1.324(3) . ?
O5 H5A 0.8402 . ?
O6 C8 1.290(3) . ?
O7 C8 1.230(3) . ?
O8 C14 1.288(3) . ?
O9 C14 1.230(3) . ?
O10 C11 1.337(3) . ?
O10 H10A 0.8400 . ?
N1 C6 1.337(3) . ?
N1 C2 1.339(3) . ?
N2 C13 1.331(3) . ?
N2 C9 1.339(3) . ?
C1 C2 1.512(4) . ?
C2 C3 1.375(4) . ?
C3 C4 1.411(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.413(4) . ?
C5 C6 1.377(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.509(4) . ?
C8 C9 1.513(4) . ?
C9 C10 1.381(4) . ?
C10 C11 1.404(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.410(4) . ?
C12 C13 1.382(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.516(4) . ?
Cr2 N4 1.954(2) . ?
Cr2 N3 1.970(2) . ?
Cr2 O18 1.983(2) . ?
Cr2 O11 1.986(2) . ?
Cr2 O16 2.007(2) . ?
Cr2 O13 2.023(2) . ?
O11 C15 1.301(4) . ?
O12 C15 1.223(4) . ?
O13 C21 1.283(3) . ?
O14 C21 1.237(4) . ?
O15 C18 1.331(3) . ?
O15 H15A 0.8400 . ?
O16 C22 1.298(4) . ?
O17 C22 1.228(4) . ?
O18 C28 1.304(3) . ?
O19 C28 1.227(3) . ?
O20 C25 1.321(3) . ?
O20 H20A 0.8400 . ?
N3 C20 1.335(4) . ?
N3 C16 1.336(4) . ?
N4 C27 1.339(3) . ?
N4 C23 1.339(4) . ?
C15 C16 1.516(4) . ?
C16 C17 1.377(4) . ?
C17 C18 1.412(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.405(4) . ?
C19 C20 1.374(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.508(4) . ?
C22 C23 1.513(4) . ?
C23 C24 1.374(4) . ?
C24 C25 1.414(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.411(4) . ?
C26 C27 1.362(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.514(4) . ?
N5 C32 1.323(6) . ?
N5 C31 1.345(5) . ?
N5 H5N 0.9104 . ?
N6 C29 1.339(5) . ?
N6 C34 1.465(5) . ?
N6 C35 1.465(5) . ?
C29 C30 1.413(5) . ?
C29 C33 1.432(5) . ?
C30 C31 1.358(5) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.369(7) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
N7 C39 1.346(5) . ?
N7 C38 1.349(5) . ?
N7 H7N 0.9101 . ?
N8 C36 1.331(4) . ?
N8 C42 1.465(4) . ?
N8 C41 1.467(4) . ?
C36 C37 1.425(5) . ?
C36 C40 1.429(5) . ?
C37 C38 1.360(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.350(5) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O21 H21A 0.8400 . ?
O21 H21B 0.8400 . ?
O22 H22A 0.8400 . ?
O22 H22B 0.8399 . ?
O23 H23A 0.8400 . ?
O23 H23B 0.8399 . ?
O23A H23C 0.8399 . ?
O23A H23D 0.8400 . ?
O24 H24A 0.8402 . ?
O24 H24B 0.8402 . ?
O24A H24C 0.8401 . ?
O24A H24D 0.8401 . ?
O25 H25A 0.8399 . ?
O25 H25B 0.8400 . ?
O26 H26A 0.8400 . ?
O26 H26B 0.8401 . ?
O27 H27A 0.8400 . ?
O27 H27B 0.8399 . ?
O28 H28A 0.8399 . ?
O28 H28B 0.8399 . ?

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 Cr1 N2 177.53(10) . . ?
N1 Cr1 O3 78.91(9) . . ?
N2 Cr1 O3 102.04(9) . . ?
N1 Cr1 O6 99.02(9) . . ?
N2 Cr1 O6 78.74(9) . . ?
O3 Cr1 O6 90.04(8) . . ?
N1 Cr1 O1 78.12(9) . . ?
N2 Cr1 O1 100.92(9) . . ?
O3 Cr1 O1 157.03(8) . . ?
O6 Cr1 O1 93.88(8) . . ?
N1 Cr1 O8 104.24(9) . . ?
N2 Cr1 O8 78.04(9) . . ?
O3 Cr1 O8 93.08(8) . . ?
O6 Cr1 O8 156.71(8) . . ?
O1 Cr1 O8 92.20(8) . . ?
C1 O1 Cr1 117.77(18) . . ?
C7 O3 Cr1 117.90(17) . . ?
C4 O5 H5A 110.9 . . ?
C8 O6 Cr1 117.64(17) . . ?
C14 O8 Cr1 117.78(17) . . ?
C11 O10 H10A 110.1 . . ?
C6 N1 C2 121.9(2) . . ?
C6 N1 Cr1 118.52(18) . . ?
C2 N1 Cr1 119.56(19) . . ?
C13 N2 C9 121.8(2) . . ?
C13 N2 Cr1 119.67(18) . . ?
C9 N2 Cr1 118.52(18) . . ?
O2 C1 O1 124.9(3) . . ?
O2 C1 C2 120.7(3) . . ?
O1 C1 C2 114.4(2) . . ?
N1 C2 C3 120.9(3) . . ?
N1 C2 C1 110.0(2) . . ?
C3 C2 C1 129.1(3) . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
O5 C4 C3 117.7(3) . . ?
O5 C4 C5 122.7(3) . . ?
C3 C4 C5 119.6(3) . . ?
C6 C5 C4 117.8(2) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
N1 C6 C5 121.4(2) . . ?
N1 C6 C7 111.0(2) . . ?
C5 C6 C7 127.5(2) . . ?
O4 C7 O3 125.2(3) . . ?
O4 C7 C6 121.1(3) . . ?
O3 C7 C6 113.6(2) . . ?
O7 C8 O6 126.0(3) . . ?
O7 C8 C9 120.1(2) . . ?
O6 C8 C9 113.9(2) . . ?
N2 C9 C10 120.9(2) . . ?
N2 C9 C8 111.0(2) . . ?
C10 C9 C8 128.1(2) . . ?
C9 C10 C11 118.0(2) . . ?
C9 C10 H10 121.0 . . ?
C11 C10 H10 121.0 . . ?
O10 C11 C10 122.5(2) . . ?
O10 C11 C12 117.1(2) . . ?
C10 C11 C12 120.4(2) . . ?
C13 C12 C11 117.0(2) . . ?
C13 C12 H12 121.5 . . ?
C11 C12 H12 121.5 . . ?
N2 C13 C12 121.9(2) . . ?
N2 C13 C14 110.5(2) . . ?
C12 C13 C14 127.6(2) . . ?
O9 C14 O8 126.2(3) . . ?
O9 C14 C13 119.8(3) . . ?
O8 C14 C13 114.0(2) . . ?
N4 Cr2 N3 173.52(10) . . ?
N4 Cr2 O18 79.33(9) . . ?
N3 Cr2 O18 105.50(9) . . ?
N4 Cr2 O11 96.56(9) . . ?
N3 Cr2 O11 79.07(9) . . ?
O18 Cr2 O11 92.65(9) . . ?
N4 Cr2 O16 78.79(9) . . ?
N3 Cr2 O16 96.52(9) . . ?
O18 Cr2 O16 157.96(8) . . ?
O11 Cr2 O16 92.39(9) . . ?
N4 Cr2 O13 105.77(9) . . ?
N3 Cr2 O13 78.66(9) . . ?
O18 Cr2 O13 91.74(9) . . ?
O11 Cr2 O13 157.67(8) . . ?
O16 Cr2 O13 91.70(9) . . ?
C15 O11 Cr2 117.53(19) . . ?
C21 O13 Cr2 116.32(18) . . ?
C18 O15 H15A 109.9 . . ?
C22 O16 Cr2 117.09(18) . . ?
C28 O18 Cr2 117.51(18) . . ?
C25 O20 H20A 114.1 . . ?
C20 N3 C16 122.3(2) . . ?
C20 N3 Cr2 118.67(19) . . ?
C16 N3 Cr2 118.48(19) . . ?
C27 N4 C23 122.0(2) . . ?
C27 N4 Cr2 118.45(18) . . ?
C23 N4 Cr2 119.34(18) . . ?
O12 C15 O11 124.9(3) . . ?
O12 C15 C16 121.2(3) . . ?
O11 C15 C16 113.9(3) . . ?
N3 C16 C17 120.9(3) . . ?
N3 C16 C15 110.7(2) . . ?
C17 C16 C15 128.4(3) . . ?
C16 C17 C18 117.9(3) . . ?
C16 C17 H17 121.1 . . ?
C18 C17 H17 121.1 . . ?
O15 C18 C19 122.4(2) . . ?
O15 C18 C17 117.8(2) . . ?
C19 C18 C17 119.8(2) . . ?
C20 C19 C18 118.3(3) . . ?
C20 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
N3 C20 C19 120.9(3) . . ?
N3 C20 C21 110.6(2) . . ?
C19 C20 C21 128.5(3) . . ?
O14 C21 O13 125.9(3) . . ?
O14 C21 C20 118.8(3) . . ?
O13 C21 C20 115.3(2) . . ?
O17 C22 O16 124.7(3) . . ?
O17 C22 C23 121.2(3) . . ?
O16 C22 C23 114.2(2) . . ?
N4 C23 C24 121.3(3) . . ?
N4 C23 C22 110.5(2) . . ?
C24 C23 C22 128.2(3) . . ?
C23 C24 C25 117.6(2) . . ?
C23 C24 H24 121.2 . . ?
C25 C24 H24 121.2 . . ?
O20 C25 C26 117.4(2) . . ?
O20 C25 C24 123.1(3) . . ?
C26 C25 C24 119.6(2) . . ?
C27 C26 C25 118.6(2) . . ?
C27 C26 H26 120.7 . . ?
C25 C26 H26 120.7 . . ?
N4 C27 C26 120.9(2) . . ?
N4 C27 C28 111.1(2) . . ?
C26 C27 C28 128.0(2) . . ?
O19 C28 O18 124.9(3) . . ?
O19 C28 C27 121.7(3) . . ?
O18 C28 C27 113.4(2) . . ?
C32 N5 C31 119.6(4) . . ?
C32 N5 H5N 117.3 . . ?
C31 N5 H5N 123.1 . . ?
C29 N6 C34 121.0(3) . . ?
C29 N6 C35 121.3(3) . . ?
C34 N6 C35 117.6(4) . . ?
N6 C29 C30 122.0(3) . . ?
N6 C29 C33 122.5(4) . . ?
C30 C29 C33 115.6(4) . . ?
C31 C30 C29 120.6(3) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
N5 C31 C30 122.0(4) . . ?
N5 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
N5 C32 C33 122.7(4) . . ?
N5 C32 H32 118.7 . . ?
C33 C32 H32 118.7 . . ?
C32 C33 C29 119.5(4) . . ?
C32 C33 H33 120.2 . . ?
C29 C33 H33 120.2 . . ?
N6 C34 H34A 109.5 . . ?
N6 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N6 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N6 C35 H35A 109.5 . . ?
N6 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N6 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C39 N7 C38 120.0(3) . . ?
C39 N7 H7N 118.0 . . ?
C38 N7 H7N 122.0 . . ?
C36 N8 C42 120.9(3) . . ?
C36 N8 C41 123.0(3) . . ?
C42 N8 C41 116.1(3) . . ?
N8 C36 C37 121.5(3) . . ?
N8 C36 C40 122.7(3) . . ?
C37 C36 C40 115.8(3) . . ?
C38 C37 C36 120.7(3) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
N7 C38 C37 121.2(3) . . ?
N7 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
N7 C39 C40 122.3(3) . . ?
N7 C39 H39 118.8 . . ?
C40 C39 H39 118.8 . . ?
C39 C40 C36 120.0(3) . . ?
C39 C40 H40 120.0 . . ?
C36 C40 H40 120.0 . . ?
N8 C41 H41A 109.5 . . ?
N8 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N8 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N8 C42 H42A 109.5 . . ?
N8 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N8 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H21A O21 H21B 107.1 . . ?
H22A O22 H22B 107.0 . . ?
H23A O23 H23B 104.4 . . ?
H23C O23A H23D 104.4 . . ?
H24A O24 H24B 104.4 . . ?
H24C O24A H24D 104.5 . . ?
H25A O25 H25B 108.2 . . ?
H26A O26 H26B 109.7 . . ?
H27A O27 H27B 108.9 . . ?
H28A O28 H28B 103.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C1 O2 179.3(2) . . . . ?
Cr1 O1 C1 C2 -1.9(3) . . . . ?
C6 N1 C2 C3 -0.3(4) . . . . ?
Cr1 N1 C2 C3 -177.9(2) . . . . ?
C6 N1 C2 C1 -179.1(2) . . . . ?
Cr1 N1 C2 C1 3.3(3) . . . . ?
O2 C1 C2 N1 178.0(3) . . . . ?
O1 C1 C2 N1 -0.8(3) . . . . ?
O2 C1 C2 C3 -0.6(5) . . . . ?
O1 C1 C2 C3 -179.5(3) . . . . ?
N1 C2 C3 C4 -0.5(4) . . . . ?
C1 C2 C3 C4 178.0(3) . . . . ?
C2 C3 C4 O5 -178.6(3) . . . . ?
C2 C3 C4 C5 1.0(4) . . . . ?
O5 C4 C5 C6 178.9(3) . . . . ?
C3 C4 C5 C6 -0.7(4) . . . . ?
C2 N1 C6 C5 0.6(4) . . . . ?
Cr1 N1 C6 C5 178.2(2) . . . . ?
C2 N1 C6 C7 -177.4(2) . . . . ?
Cr1 N1 C6 C7 0.3(3) . . . . ?
C4 C5 C6 N1 -0.1(4) . . . . ?
C4 C5 C6 C7 177.5(3) . . . . ?
Cr1 O3 C7 O4 180.0(2) . . . . ?
Cr1 O3 C7 C6 -1.4(3) . . . . ?
N1 C6 C7 O4 179.4(3) . . . . ?
C5 C6 C7 O4 1.6(4) . . . . ?
N1 C6 C7 O3 0.7(3) . . . . ?
C5 C6 C7 O3 -177.1(3) . . . . ?
Cr1 O6 C8 O7 176.8(2) . . . . ?
Cr1 O6 C8 C9 -4.4(3) . . . . ?
C13 N2 C9 C10 0.1(4) . . . . ?
Cr1 N2 C9 C10 179.4(2) . . . . ?
C13 N2 C9 C8 -179.2(2) . . . . ?
Cr1 N2 C9 C8 0.1(3) . . . . ?
O7 C8 C9 N2 -178.4(2) . . . . ?
O6 C8 C9 N2 2.8(3) . . . . ?
O7 C8 C9 C10 2.3(4) . . . . ?
O6 C8 C9 C10 -176.5(3) . . . . ?
N2 C9 C10 C11 -0.6(4) . . . . ?
C8 C9 C10 C11 178.6(2) . . . . ?
C9 C10 C11 O10 -178.7(2) . . . . ?
C9 C10 C11 C12 0.6(4) . . . . ?
O10 C11 C12 C13 179.2(2) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C9 N2 C13 C12 0.4(4) . . . . ?
Cr1 N2 C13 C12 -178.9(2) . . . . ?
C9 N2 C13 C14 -179.7(2) . . . . ?
Cr1 N2 C13 C14 1.0(3) . . . . ?
C11 C12 C13 N2 -0.4(4) . . . . ?
C11 C12 C13 C14 179.7(2) . . . . ?
Cr1 O8 C14 O9 -178.4(2) . . . . ?
Cr1 O8 C14 C13 0.3(3) . . . . ?
N2 C13 C14 O9 178.0(2) . . . . ?
C12 C13 C14 O9 -2.1(4) . . . . ?
N2 C13 C14 O8 -0.8(3) . . . . ?
C12 C13 C14 O8 179.1(3) . . . . ?
Cr2 O11 C15 O12 179.5(3) . . . . ?
Cr2 O11 C15 C16 -1.2(3) . . . . ?
C20 N3 C16 C17 0.7(4) . . . . ?
Cr2 N3 C16 C17 171.8(2) . . . . ?
C20 N3 C16 C15 -177.4(2) . . . . ?
Cr2 N3 C16 C15 -6.3(3) . . . . ?
O12 C15 C16 N3 -175.9(3) . . . . ?
O11 C15 C16 N3 4.7(4) . . . . ?
O12 C15 C16 C17 6.2(5) . . . . ?
O11 C15 C16 C17 -173.2(3) . . . . ?
N3 C16 C17 C18 -1.6(4) . . . . ?
C15 C16 C17 C18 176.1(3) . . . . ?
C16 C17 C18 O15 -178.6(2) . . . . ?
C16 C17 C18 C19 1.6(4) . . . . ?
O15 C18 C19 C20 179.5(3) . . . . ?
C17 C18 C19 C20 -0.8(4) . . . . ?
C16 N3 C20 C19 0.2(4) . . . . ?
Cr2 N3 C20 C19 -170.9(2) . . . . ?
C16 N3 C20 C21 178.5(3) . . . . ?
Cr2 N3 C20 C21 7.4(3) . . . . ?
C18 C19 C20 N3 -0.2(4) . . . . ?
C18 C19 C20 C21 -178.1(3) . . . . ?
Cr2 O13 C21 O14 -178.1(2) . . . . ?
Cr2 O13 C21 C20 1.2(3) . . . . ?
N3 C20 C21 O14 173.9(3) . . . . ?
C19 C20 C21 O14 -7.9(5) . . . . ?
N3 C20 C21 O13 -5.4(4) . . . . ?
C19 C20 C21 O13 172.7(3) . . . . ?
Cr2 O16 C22 O17 178.7(2) . . . . ?
Cr2 O16 C22 C23 -0.1(3) . . . . ?
C27 N4 C23 C24 0.1(4) . . . . ?
Cr2 N4 C23 C24 174.4(2) . . . . ?
C27 N4 C23 C22 -178.9(2) . . . . ?
Cr2 N4 C23 C22 -4.6(3) . . . . ?
O17 C22 C23 N4 -175.9(3) . . . . ?
O16 C22 C23 N4 2.9(3) . . . . ?
O17 C22 C23 C24 5.2(5) . . . . ?
O16 C22 C23 C24 -176.0(3) . . . . ?
N4 C23 C24 C25 0.6(4) . . . . ?
C22 C23 C24 C25 179.4(3) . . . . ?
C23 C24 C25 O20 179.6(3) . . . . ?
C23 C24 C25 C26 -0.2(4) . . . . ?
O20 C25 C26 C27 179.4(3) . . . . ?
C24 C25 C26 C27 -0.7(4) . . . . ?
C23 N4 C27 C26 -1.1(4) . . . . ?
Cr2 N4 C27 C26 -175.4(2) . . . . ?
C23 N4 C27 C28 178.1(2) . . . . ?
Cr2 N4 C27 C28 3.8(3) . . . . ?
C25 C26 C27 N4 1.4(4) . . . . ?
C25 C26 C27 C28 -177.7(3) . . . . ?
Cr2 O18 C28 O19 177.2(2) . . . . ?
Cr2 O18 C28 C27 -3.5(3) . . . . ?
N4 C27 C28 O19 179.2(3) . . . . ?
C26 C27 C28 O19 -1.7(4) . . . . ?
N4 C27 C28 O18 -0.2(3) . . . . ?
C26 C27 C28 O18 179.0(3) . . . . ?
C34 N6 C29 C30 1.3(5) . . . . ?
C35 N6 C29 C30 -179.0(3) . . . . ?
C34 N6 C29 C33 -179.1(3) . . . . ?
C35 N6 C29 C33 0.7(5) . . . . ?
N6 C29 C30 C31 -177.8(3) . . . . ?
C33 C29 C30 C31 2.5(5) . . . . ?
C32 N5 C31 C30 -0.3(5) . . . . ?
C29 C30 C31 N5 -1.6(5) . . . . ?
C31 N5 C32 C33 1.1(5) . . . . ?
N5 C32 C33 C29 -0.1(6) . . . . ?
N6 C29 C33 C32 178.7(3) . . . . ?
C30 C29 C33 C32 -1.6(5) . . . . ?
C42 N8 C36 C37 0.3(5) . . . . ?
C41 N8 C36 C37 -176.3(3) . . . . ?
C42 N8 C36 C40 -178.3(3) . . . . ?
C41 N8 C36 C40 5.1(5) . . . . ?
N8 C36 C37 C38 -177.7(3) . . . . ?
C40 C36 C37 C38 1.0(5) . . . . ?
C39 N7 C38 C37 -0.9(5) . . . . ?
C36 C37 C38 N7 -0.1(5) . . . . ?
C38 N7 C39 C40 1.0(5) . . . . ?
N7 C39 C40 C36 0.0(5) . . . . ?
N8 C36 C40 C39 177.8(3) . . . . ?
C37 C36 C40 C39 -0.9(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O28 0.84 1.74 2.574(3) 172 1_554
O10 H10A O14 0.84 1.77 2.599(3) 168 1_565
O15 H15A O26 0.84 1.73 2.557(3) 168 1_545
O20 H20A O22 0.84 1.67 2.509(3) 176 1_546
N5 H5N O25 0.91 1.86 2.768(5) 177 1_565
N7 H7N O23 0.91 1.80 2.666(6) 159 1_566
N7 H7N O23A 0.91 1.88 2.786(7) 173 1_566
O21 H21A O19 0.84 1.93 2.766(3) 174 2_546
O21 H21B O9 0.84 1.87 2.696(3) 170 .
O22 H22A O4 0.84 1.89 2.708(3) 164 .
O22 H22B O21 0.84 1.84 2.672(3) 170 1_565
O23 H23A O21 0.84 1.92 2.761(5) 175 1_655
O23 H23B O17 0.84 2.19 2.903(6) 143 2_656
O24 H24A O9 0.84 2.11 2.897(6) 156 1_655
O24 H24B O13 0.84 2.03 2.861(6) 172 2_656
O25 H25A O16 0.84 2.11 2.944(4) 172 2_656
O25 H25B O2 0.84 2.00 2.829(3) 171 .
O26 H26A O7 0.84 2.11 2.894(3) 156 .
O26 H26B O27 0.84 1.87 2.706(3) 176 .
O27 H27A O2 0.84 1.93 2.769(3) 175 2_656
O27 H27B O7 0.84 1.99 2.820(3) 168 2_646
O28 H28A O17 0.84 1.96 2.778(3) 164 1_565
O28 H28B O12 0.84 2.00 2.797(3) 158 .

_refine_diff_density_max         0.408
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.059

_vrf_PLAT_417                    
;
PROBLEM: ALERT_2_B Short Inter D-H..H-D       H7N ..  H23B  ..     2.09 Ang.
ALERT_2_B Short Inter D-H..H-D       H21A   ..  H23A    ..       1.97 Ang.
ALERT_2_B Short Inter D-H..H-D       H25A   ..  H24D    ..       1.91 Ang.
RESPONSE: This is likely the result of the disorder associated with lattice 
waters involving O23 and O24.
;


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1056389'
_audit_update_record             
;
2015-03-26 deposited with the CCDC.
2015-08-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C14 H6 Cr N2 O10, C6 H10 N3, C6 H9 N3, 3(H2 O)'
_chemical_formula_sum            'C26 H31 Cr N8 O13'
_chemical_formula_weight         715.59

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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   18.7610(18)
_cell_length_b                   8.3037(8)
_cell_length_c                   18.9883(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2958.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9943
_cell_measurement_theta_min      2.677
_cell_measurement_theta_max      28.278

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_F_000             1484
_exptl_transmission_factor_min   0.756
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.470
_shelx_estimated_absorpt_T_min   0.884
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.98

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, colllected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was sec/frame.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            24049
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.145
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_full        27.850
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             6807
_reflns_number_gt                6134
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_max     0.887
_reflns_Friedel_fraction_full    0.923

_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2014)'

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms attached to carbon 
were placed in calculated positions (C---H = 0.95 - 0.98 Å) while those 
attached to nitrogen and oxygen were placed in locations derived from a  
difference map and their coordinate4s adjusted to give N---H = 0.91 Å 
and O---H = 0.84 Å. All were included as riding contributions with isotropic 
displacement parameters 1.2 - 1.5 times those of the attached atoms
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0677P)²+0.9115P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2582 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons et al., 2013.
;
_refine_ls_abs_structure_Flack   0.017(12)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         6807
_refine_ls_number_parameters     437
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1146
_refine_ls_wR_factor_gt          0.1088
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
Cr1 Cr 0.88927(3) 0.54820(6) 0.89514(4) 0.01440(14) Uani 1 1 d . . . . .
O1 O 0.91823(14) 0.7154(3) 0.82517(16) 0.0198(6) Uani 1 1 d . . . . .
O2 O 0.88889(15) 0.8383(4) 0.72471(16) 0.0218(7) Uani 1 1 d . . . . .
O3 O 0.82873(14) 0.3789(3) 0.93880(14) 0.0172(5) Uani 1 1 d . . . . .
O4 O 0.72336(15) 0.2550(3) 0.93376(16) 0.0203(6) Uani 1 1 d . . . . .
O5 O 0.63322(16) 0.5766(3) 0.70503(16) 0.0228(6) Uani 1 1 d . . . . .
H5O H 0.5970 0.5313 0.7219 0.027 Uiso 1 1 d R U . . .
O6 O 0.95083(14) 0.3847(3) 0.85002(14) 0.0177(6) Uani 1 1 d . . . . .
O7 O 1.05644(15) 0.2600(3) 0.85570(15) 0.0206(6) Uani 1 1 d . . . . .
O8 O 0.85786(14) 0.7096(3) 0.96578(15) 0.0186(6) Uani 1 1 d . . . . .
O9 O 0.88019(15) 0.8110(4) 1.07263(17) 0.0220(6) Uani 1 1 d . . . . .
O10 O 1.13803(16) 0.5554(4) 1.09446(16) 0.0231(7) Uani 1 1 d . . . . .
H10O H 1.1726 0.5240 1.0699 0.028 Uiso 1 1 d R U . . .
N1 N 0.80729(17) 0.5476(4) 0.83080(18) 0.0154(6) Uani 1 1 d . . . . .
N2 N 0.96944(17) 0.5443(4) 0.96084(18) 0.0147(6) Uani 1 1 d . . . . .
C1 C 0.8771(2) 0.7413(5) 0.7720(2) 0.0180(8) Uani 1 1 d . . . . .
C2 C 0.8082(2) 0.6438(4) 0.7747(2) 0.0148(7) Uani 1 1 d . . . . .
C3 C 0.7505(2) 0.6518(4) 0.7296(2) 0.0167(8) Uani 1 1 d . . . . .
H3 H 0.7518 0.7161 0.6882 0.020 Uiso 1 1 calc R U . . .
C4 C 0.6893(2) 0.5606(4) 0.7474(2) 0.0165(8) Uani 1 1 d . . . . .
C5 C 0.6898(2) 0.4598(4) 0.8067(2) 0.0160(8) Uani 1 1 d . . . . .
H5 H 0.6495 0.3961 0.8186 0.019 Uiso 1 1 calc R U . . .
C6 C 0.7510(2) 0.4565(4) 0.8471(2) 0.0148(7) Uani 1 1 d . . . . .
C7 C 0.76620(19) 0.3543(4) 0.91156(19) 0.0150(8) Uani 1 1 d . . . . .
C8 C 1.0125(2) 0.3562(4) 0.8792(2) 0.0178(8) Uani 1 1 d . . . . .
C9 C 1.0259(2) 0.4518(4) 0.9457(2) 0.0158(8) Uani 1 1 d . . . . .
C10 C 1.0849(2) 0.4499(4) 0.9890(2) 0.0166(8) Uani 1 1 d . . . . .
H10 H 1.1251 0.3852 0.9780 0.020 Uiso 1 1 calc R U . . .
C11 C 1.0838(2) 0.5467(5) 1.0499(2) 0.0175(8) Uani 1 1 d . . . . .
C12 C 1.0227(2) 0.6388(4) 1.0660(2) 0.0175(7) Uani 1 1 d . . . . .
H12 H 1.0203 0.7011 1.1079 0.021 Uiso 1 1 calc R U . . .
C13 C 0.9664(2) 0.6359(4) 1.0189(2) 0.0161(7) Uani 1 1 d . . . . .
C14 C 0.8965(2) 0.7297(5) 1.0217(2) 0.0166(8) Uani 1 1 d . . . . .
N3 N 0.51099(18) 0.5053(4) -0.03154(18) 0.0190(7) Uani 1 1 d . . . . .
N4 N 0.63028(17) 0.6111(4) -0.03318(18) 0.0182(7) Uani 1 1 d . . . . .
N5 N 0.55198(18) 0.6604(4) -0.12374(17) 0.0201(7) Uani 1 1 d . . . . .
H5A H 0.5060 0.6655 -0.1388 0.024 Uiso 1 1 d R U . . .
H5B H 0.5864 0.7296 -0.1388 0.024 Uiso 1 1 d R U . . .
C15 C 0.5645(2) 0.5905(4) -0.0611(2) 0.0166(7) Uani 1 1 d . . . . .
C16 C 0.5256(2) 0.4327(4) 0.0304(2) 0.0197(8) Uani 1 1 d . . . . .
C17 C 0.5922(2) 0.4440(5) 0.0616(2) 0.0212(8) Uani 1 1 d . . . . .
H17 H 0.6024 0.3902 0.1045 0.025 Uiso 1 1 calc R U . . .
C18 C 0.6435(2) 0.5365(5) 0.0279(2) 0.0193(8) Uani 1 1 d . . . . .
C19 C 0.4666(2) 0.3400(5) 0.0647(3) 0.0267(9) Uani 1 1 d . . . . .
H19A H 0.4300 0.4150 0.0816 0.040 Uiso 1 1 calc R U . . .
H19B H 0.4856 0.2785 0.1045 0.040 Uiso 1 1 calc R U . . .
H19C H 0.4454 0.2659 0.0304 0.040 Uiso 1 1 calc R U . . .
C20 C 0.7158(2) 0.5612(5) 0.0601(2) 0.0250(9) Uani 1 1 d . . . . .
H20A H 0.7526 0.5431 0.0243 0.038 Uiso 1 1 calc R U . . .
H20B H 0.7225 0.4850 0.0989 0.038 Uiso 1 1 calc R U . . .
H20C H 0.7196 0.6716 0.0780 0.038 Uiso 1 1 calc R U . . .
N6 N 0.77030(18) 0.0174(4) 0.82079(18) 0.0196(7) Uani 1 1 d . . . . .
H6N H 0.8100 0.0182 0.8483 0.024 Uiso 1 1 d R U . . .
N7 N 0.65302(18) -0.0853(4) 0.81802(18) 0.0185(7) Uani 1 1 d . . . . .
N8 N 0.72917(18) -0.1499(4) 0.90857(18) 0.0207(7) Uani 1 1 d . . . . .
H8A H 0.7714 -0.1479 0.9321 0.025 Uiso 1 1 d R U . . .
H8B H 0.6949 -0.2181 0.9248 0.025 Uiso 1 1 d R U . . .
C21 C 0.7170(2) -0.0726(4) 0.8494(2) 0.0167(8) Uani 1 1 d . . . . .
C22 C 0.7607(2) 0.1026(5) 0.7606(2) 0.0191(8) Uani 1 1 d . . . . .
C23 C 0.6958(2) 0.0934(5) 0.7278(2) 0.0223(8) Uani 1 1 d . . . . .
H23 H 0.6869 0.1511 0.6855 0.027 Uiso 1 1 calc R U . . .
C24 C 0.6428(2) -0.0035(5) 0.7584(2) 0.0186(8) Uani 1 1 d . . . . .
C25 C 0.8238(2) 0.1962(5) 0.7346(2) 0.0239(9) Uani 1 1 d . . . . .
H25A H 0.8535 0.1268 0.7049 0.036 Uiso 1 1 calc R U . . .
H25B H 0.8518 0.2343 0.7749 0.036 Uiso 1 1 calc R U . . .
H25C H 0.8073 0.2888 0.7071 0.036 Uiso 1 1 calc R U . . .
C26 C 0.5722(2) -0.0209(5) 0.7223(2) 0.0249(9) Uani 1 1 d . . . . .
H26A H 0.5415 -0.0929 0.7498 0.037 Uiso 1 1 calc R U . . .
H26B H 0.5793 -0.0662 0.6752 0.037 Uiso 1 1 calc R U . . .
H26C H 0.5494 0.0850 0.7183 0.037 Uiso 1 1 calc R U . . .
O11 O 0.26097(16) 0.4361(4) 0.05633(17) 0.0270(7) Uani 1 1 d . . . . .
H1A H 0.2580 0.4128 0.0993 0.032 Uiso 0.5 1 d R U P A 1
H1B H 0.2874 0.5094 0.0406 0.032 Uiso 0.5 1 d R U P A 1
H1AA H 0.2585 0.4082 0.0139 0.032 Uiso 0.5 1 d R U P B 2
H1BA H 0.3016 0.4763 0.0626 0.032 Uiso 0.5 1 d R U P B 2
O12 O 0.51358(16) 0.4285(4) 0.73587(17) 0.0247(6) Uani 1 1 d . . . . .
H12A H 0.5160 0.3853 0.7758 0.030 Uiso 1 1 d R U . . .
H12B H 0.4802 0.4923 0.7455 0.030 Uiso 1 1 d R U . . .
O13 O 0.87716(18) 0.0600(3) 0.9140(2) 0.0361(9) Uani 1 1 d . . . . .
H13A H 0.8962 0.0720 0.8744 0.043 Uiso 1 1 d R U . . .
H13B H 0.9133 0.0131 0.9303 0.043 Uiso 1 1 d 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
Cr1 N2 1.955(3) . ?
Cr1 N1 1.964(3) . ?
Cr1 O6 1.977(3) . ?
Cr1 O8 1.986(3) . ?
Cr1 O3 1.988(3) . ?
Cr1 O1 1.997(3) . ?
O1 C1 1.289(5) . ?
O2 C1 1.225(5) . ?
O3 C7 1.298(4) . ?
O4 C7 1.226(5) . ?
O5 C4 1.332(5) . ?
O5 H5O 0.8400 . ?
O6 C8 1.304(5) . ?
O7 C8 1.232(5) . ?
O8 C14 1.297(5) . ?
O9 C14 1.218(5) . ?
O10 C11 1.324(5) . ?
O10 H10O 0.8400 . ?
N1 C2 1.332(5) . ?
N1 C6 1.336(5) . ?
N2 C9 1.339(5) . ?
N2 C13 1.341(5) . ?
C1 C2 1.526(5) . ?
C2 C3 1.382(5) . ?
C3 C4 1.416(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(6) . ?
C5 C6 1.381(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.516(5) . ?
C8 C9 1.514(5) . ?
C9 C10 1.378(6) . ?
C10 C11 1.409(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.411(6) . ?
C12 C13 1.383(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.527(5) . ?
N3 C16 1.350(5) . ?
N3 C15 1.350(5) . ?
N4 C18 1.338(5) . ?
N4 C15 1.353(5) . ?
N5 C15 1.345(5) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9099 . ?
C16 C17 1.386(6) . ?
C16 C19 1.497(6) . ?
C17 C18 1.387(6) . ?
C17 H17 0.9500 . ?
C18 C20 1.502(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N6 C22 1.356(5) . ?
N6 C21 1.362(5) . ?
N6 H6N 0.9100 . ?
N7 C24 1.334(5) . ?
N7 C21 1.344(5) . ?
N8 C21 1.314(5) . ?
N8 H8A 0.9099 . ?
N8 H8B 0.9100 . ?
C22 C23 1.370(6) . ?
C22 C25 1.498(6) . ?
C23 C24 1.406(6) . ?
C23 H23 0.9500 . ?
C24 C26 1.498(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O11 H1A 0.8400 . ?
O11 H1B 0.8401 . ?
O11 H1AA 0.8400 . ?
O11 H1BA 0.8400 . ?
O12 H12A 0.8400 . ?
O12 H12B 0.8401 . ?
O13 H13A 0.8402 . ?
O13 H13B 0.8402 . ?

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
N2 Cr1 N1 178.37(14) . . ?
N2 Cr1 O6 79.37(12) . . ?
N1 Cr1 O6 100.74(12) . . ?
N2 Cr1 O8 78.96(13) . . ?
N1 Cr1 O8 100.92(12) . . ?
O6 Cr1 O8 158.32(12) . . ?
N2 Cr1 O3 99.30(12) . . ?
N1 Cr1 O3 79.07(12) . . ?
O6 Cr1 O3 91.67(10) . . ?
O8 Cr1 O3 91.50(12) . . ?
N2 Cr1 O1 103.11(12) . . ?
N1 Cr1 O1 78.52(12) . . ?
O6 Cr1 O1 91.72(12) . . ?
O8 Cr1 O1 93.48(11) . . ?
O3 Cr1 O1 157.57(12) . . ?
C1 O1 Cr1 118.3(2) . . ?
C7 O3 Cr1 117.5(2) . . ?
C4 O5 H5O 111.4 . . ?
C8 O6 Cr1 117.3(2) . . ?
C14 O8 Cr1 118.3(2) . . ?
C11 O10 H10O 102.7 . . ?
C2 N1 C6 122.4(3) . . ?
C2 N1 Cr1 119.1(3) . . ?
C6 N1 Cr1 118.5(3) . . ?
C9 N2 C13 122.3(3) . . ?
C9 N2 Cr1 118.8(3) . . ?
C13 N2 Cr1 118.9(3) . . ?
O2 C1 O1 125.2(4) . . ?
O2 C1 C2 121.7(4) . . ?
O1 C1 C2 113.1(3) . . ?
N1 C2 C3 120.9(3) . . ?
N1 C2 C1 110.9(3) . . ?
C3 C2 C1 128.1(3) . . ?
C2 C3 C4 117.5(3) . . ?
C2 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
O5 C4 C5 123.3(4) . . ?
O5 C4 C3 116.3(3) . . ?
C5 C4 C3 120.4(4) . . ?
C6 C5 C4 117.6(4) . . ?
C6 C5 H5 121.2 . . ?
C4 C5 H5 121.2 . . ?
N1 C6 C5 121.2(3) . . ?
N1 C6 C7 110.8(3) . . ?
C5 C6 C7 128.0(3) . . ?
O4 C7 O3 124.1(3) . . ?
O4 C7 C6 122.0(3) . . ?
O3 C7 C6 113.8(3) . . ?
O7 C8 O6 124.0(4) . . ?
O7 C8 C9 122.1(4) . . ?
O6 C8 C9 114.0(3) . . ?
N2 C9 C10 120.9(4) . . ?
N2 C9 C8 110.4(3) . . ?
C10 C9 C8 128.7(4) . . ?
C9 C10 C11 118.2(4) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
O10 C11 C10 123.0(4) . . ?
O10 C11 C12 117.2(4) . . ?
C10 C11 C12 119.8(4) . . ?
C13 C12 C11 118.1(4) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
N2 C13 C12 120.6(4) . . ?
N2 C13 C14 110.7(3) . . ?
C12 C13 C14 128.7(4) . . ?
O9 C14 O8 125.6(4) . . ?
O9 C14 C13 121.7(4) . . ?
O8 C14 C13 112.7(3) . . ?
C16 N3 C15 116.4(3) . . ?
C18 N4 C15 116.7(3) . . ?
C15 N5 H5A 117.6 . . ?
C15 N5 H5B 115.2 . . ?
H5A N5 H5B 123.0 . . ?
N5 C15 N3 117.6(4) . . ?
N5 C15 N4 116.8(3) . . ?
N3 C15 N4 125.6(4) . . ?
N3 C16 C17 121.6(4) . . ?
N3 C16 C19 117.3(4) . . ?
C17 C16 C19 121.1(4) . . ?
C16 C17 C18 117.8(4) . . ?
C16 C17 H17 121.1 . . ?
C18 C17 H17 121.1 . . ?
N4 C18 C17 121.8(4) . . ?
N4 C18 C20 117.2(4) . . ?
C17 C18 C20 121.0(4) . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 N6 C21 121.7(3) . . ?
C22 N6 H6N 126.1 . . ?
C21 N6 H6N 112.1 . . ?
C24 N7 C21 117.7(4) . . ?
C21 N8 H8A 124.2 . . ?
C21 N8 H8B 118.1 . . ?
H8A N8 H8B 117.4 . . ?
N8 C21 N7 119.7(4) . . ?
N8 C21 N6 118.8(4) . . ?
N7 C21 N6 121.5(4) . . ?
N6 C22 C23 118.2(4) . . ?
N6 C22 C25 116.4(4) . . ?
C23 C22 C25 125.5(4) . . ?
C22 C23 C24 118.2(4) . . ?
C22 C23 H23 120.9 . . ?
C24 C23 H23 120.9 . . ?
N7 C24 C23 122.7(4) . . ?
N7 C24 C26 117.8(4) . . ?
C23 C24 C26 119.5(4) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
H1A O11 H1B 123.4 . . ?
H1AA O11 H1BA 107.3 . . ?
H12A O12 H12B 96.6 . . ?
H13A O13 H13B 92.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C1 O2 -178.9(3) . . . . ?
Cr1 O1 C1 C2 4.2(4) . . . . ?
C6 N1 C2 C3 -1.0(6) . . . . ?
Cr1 N1 C2 C3 -177.5(3) . . . . ?
C6 N1 C2 C1 176.2(3) . . . . ?
Cr1 N1 C2 C1 -0.2(4) . . . . ?
O2 C1 C2 N1 -179.6(4) . . . . ?
O1 C1 C2 N1 -2.6(5) . . . . ?
O2 C1 C2 C3 -2.6(6) . . . . ?
O1 C1 C2 C3 174.4(4) . . . . ?
N1 C2 C3 C4 3.2(5) . . . . ?
C1 C2 C3 C4 -173.5(4) . . . . ?
C2 C3 C4 O5 176.7(3) . . . . ?
C2 C3 C4 C5 -3.4(5) . . . . ?
O5 C4 C5 C6 -178.7(3) . . . . ?
C3 C4 C5 C6 1.4(6) . . . . ?
C2 N1 C6 C5 -1.2(6) . . . . ?
Cr1 N1 C6 C5 175.3(3) . . . . ?
C2 N1 C6 C7 177.5(3) . . . . ?
Cr1 N1 C6 C7 -6.0(4) . . . . ?
C4 C5 C6 N1 0.9(6) . . . . ?
C4 C5 C6 C7 -177.5(3) . . . . ?
Cr1 O3 C7 O4 -179.2(3) . . . . ?
Cr1 O3 C7 C6 2.8(4) . . . . ?
N1 C6 C7 O4 -176.0(3) . . . . ?
C5 C6 C7 O4 2.5(6) . . . . ?
N1 C6 C7 O3 2.0(4) . . . . ?
C5 C6 C7 O3 -179.5(4) . . . . ?
Cr1 O6 C8 O7 -178.5(3) . . . . ?
Cr1 O6 C8 C9 1.8(4) . . . . ?
C13 N2 C9 C10 -1.6(5) . . . . ?
Cr1 N2 C9 C10 177.4(3) . . . . ?
C13 N2 C9 C8 177.1(3) . . . . ?
Cr1 N2 C9 C8 -3.9(4) . . . . ?
O7 C8 C9 N2 -178.5(3) . . . . ?
O6 C8 C9 N2 1.2(4) . . . . ?
O7 C8 C9 C10 0.1(6) . . . . ?
O6 C8 C9 C10 179.8(4) . . . . ?
N2 C9 C10 C11 0.6(6) . . . . ?
C8 C9 C10 C11 -177.8(4) . . . . ?
C9 C10 C11 O10 -179.0(4) . . . . ?
C9 C10 C11 C12 1.5(6) . . . . ?
O10 C11 C12 C13 177.8(3) . . . . ?
C10 C11 C12 C13 -2.8(6) . . . . ?
C9 N2 C13 C12 0.4(5) . . . . ?
Cr1 N2 C13 C12 -178.7(3) . . . . ?
C9 N2 C13 C14 179.2(3) . . . . ?
Cr1 N2 C13 C14 0.1(4) . . . . ?
C11 C12 C13 N2 1.8(6) . . . . ?
C11 C12 C13 C14 -176.8(4) . . . . ?
Cr1 O8 C14 O9 -171.8(3) . . . . ?
Cr1 O8 C14 C13 7.0(4) . . . . ?
N2 C13 C14 O9 174.3(4) . . . . ?
C12 C13 C14 O9 -7.0(6) . . . . ?
N2 C13 C14 O8 -4.5(4) . . . . ?
C12 C13 C14 O8 174.2(4) . . . . ?
C16 N3 C15 N5 178.2(3) . . . . ?
C16 N3 C15 N4 -1.4(6) . . . . ?
C18 N4 C15 N5 -177.6(3) . . . . ?
C18 N4 C15 N3 2.0(6) . . . . ?
C15 N3 C16 C17 -0.5(5) . . . . ?
C15 N3 C16 C19 179.0(3) . . . . ?
N3 C16 C17 C18 1.6(6) . . . . ?
C19 C16 C17 C18 -177.8(4) . . . . ?
C15 N4 C18 C17 -0.7(5) . . . . ?
C15 N4 C18 C20 -178.8(3) . . . . ?
C16 C17 C18 N4 -1.0(6) . . . . ?
C16 C17 C18 C20 177.0(4) . . . . ?
C24 N7 C21 N8 179.4(3) . . . . ?
C24 N7 C21 N6 -1.4(5) . . . . ?
C22 N6 C21 N8 -178.6(3) . . . . ?
C22 N6 C21 N7 2.2(6) . . . . ?
C21 N6 C22 C23 -1.5(6) . . . . ?
C21 N6 C22 C25 -179.8(3) . . . . ?
N6 C22 C23 C24 0.1(6) . . . . ?
C25 C22 C23 C24 178.3(4) . . . . ?
C21 N7 C24 C23 0.1(6) . . . . ?
C21 N7 C24 C26 178.4(3) . . . . ?
C22 C23 C24 N7 0.5(6) . . . . ?
C22 C23 C24 C26 -177.7(4) . . . . ?

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
O5 H5O O12 0.84 1.80 2.625(4) 166 .
O10 H10O O11 0.84 1.83 2.613(4) 154 1_656
N5 H5A O1 0.91 2.04 2.881(4) 153 3_464
N5 H5B N7 0.91 2.14 3.046(5) 170 1_564
N6 H6N O13 0.91 1.81 2.698(5) 166 .
N8 H8A O8 0.91 2.11 2.893(4) 144 1_545
N8 H8B N4 0.91 2.03 2.933(5) 172 1_546
O11 H1BA O9 0.84 2.31 3.084(4) 153 3_464
O11 H1AA O4 0.84 2.14 2.904(4) 151 3_454
O11 H1BA O9 0.84 2.31 3.084(4) 153 3_464
O12 H12A O7 0.84 2.08 2.876(4) 1578 3_455
O12 H12B O2 0.84 2.25 3.045(4) 157 3_465
O13 H13B N3 0.84 1.98 2.769(5) 157 3_556

_refine_diff_density_max         1.286
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.091


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1056390'
_audit_update_record             
;
2015-03-26 deposited with the CCDC.
2015-08-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C7 H9 Co N O8, H2 O'
_chemical_formula_sum            'C7 H11 Co N O9'
_chemical_formula_iupac          ?
_chemical_formula_weight         312.10

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.7083(5)
_cell_length_b                   6.8757(3)
_cell_length_c                   22.4140(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.387(1)
_cell_angle_gamma                90
_cell_volume                     2266.67(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1477
_cell_measurement_theta_min      2.7726
_cell_measurement_theta_max      28.8911
_cell_measurement_temperature    150.(2)

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272

_exptl_absorpt_coefficient_mu    1.556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2013b)'
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.87

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5 deg. in omega, colllected at phi = 0.00,
90.00 and 180.00 deg. and 2 sets of 800 frames, each of
width 0.45 deg in phi, collected at omega = -30.00 and 210.00
deg. The scan time was 10 sec/frame.
;

_diffrn_ambient_temperature      150.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              ?

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            19842
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_full        29.13
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29

_refine_special_details          SQUEEZE

_reflns_number_total             3005
_reflns_number_gt                2780
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1079
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.071
_refine_ls_number_reflns         3005
_refine_ls_number_parameters     173
_refine_ls_number_restraints     4
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0599P)²+5.7649P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.399
_refine_diff_density_min         -0.594
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX2 (Bruker AXS, 2013)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2013a)'
_computing_data_reduction        'SAINT (Bruker AXS, 2013a)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker AXS, 2008)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.481388(18) 0.24666(4) 0.63839(12) 0.01454(11) Uani d D 1.0 . .
O O1 0.52452(9) 0.2093(2) 0.54538(6) 0.0148(3) Uani d . 1.0 A .
O O2 0.48172(10) 0.2644(2) 0.45091(7) 0.0157(3) Uani d . 1.0 A .
O O3 0.3858(3) 0.3470(12) 0.70431(10) 0.0193(12) Uani d PD 0.814(5) A 1
O O4 0.27065(15) 0.5568(4) 0.71425(8) 0.0251(5) Uani d PD 0.814(5) A 1
C C7 0.32203(18) 0.4509(4) 0.68429(9) 0.0154(6) Uani d PD 0.814(5) A 1
O O3A 0.3792(15) 0.323(7) 0.7031(4) 0.0193(12) Uani d PD 0.186(5) A 2
O O4A 0.2400(7) 0.4562(17) 0.7117(4) 0.0251(5) Uani d PD 0.186(5) A 2
C C7A 0.3076(8) 0.400(2) 0.68302(19) 0.0154(6) Uani d PD 0.186(5) A 2
O O5 0.16837(9) 0.5768(2) 0.48938(6) 0.0152(3) Uani d . 1.0 . .
H H5O 0.1267 0.6259 0.5099 0.018 Uiso d R 1.0 . .
O O6 0.42619(10) -0.0396(2) 0.63500(6) 0.0187(3) Uani d . 1.0 A .
H H6A 0.4414 -0.0866 0.6019 0.022 Uiso d R 1.0 . .
H H6B 0.3691 -0.043 0.6343 0.022 Uiso d R 1.0 . .
O O7 0.57408(10) 0.1362(2) 0.69569(7) 0.0216(3) Uani d . 1.0 A .
H H7A 0.5972 0.2013 0.7237 0.026 Uiso d R 1.0 . .
H H7B 0.5725 0.0218 0.7089 0.026 Uiso d R 1.0 . .
O O8 0.55734(11) 0.5092(2) 0.64473(8) 0.0253(3) Uani d . 1.0 A .
H H8A 0.554 0.5717 0.6126 0.03 Uiso d R 1.0 . .
H H8B 0.6131 0.4843 0.6478 0.03 Uiso d R 1.0 . .
N N1 0.38130(10) 0.3714(2) 0.58895(7) 0.0125(3) Uani d . 1.0 A .
C C1 0.46970(13) 0.2733(3) 0.50546(9) 0.0113(3) Uani d . 1.0 . .
C C2 0.38404(11) 0.3669(3) 0.52934(8) 0.0101(3) Uani d . 1.0 A .
C C3 0.31363(12) 0.4390(3) 0.49459(8) 0.0109(3) Uani d . 1.0 . .
H H3A 0.3169 0.4367 0.4523 0.013 Uiso calc R 1.0 A .
C C4 0.23734(12) 0.5156(3) 0.52350(8) 0.0113(3) Uani d . 1.0 A .
C C5 0.23568(13) 0.5223(3) 0.58602(9) 0.0147(3) Uani d . 1.0 . .
H H5A 0.1853 0.5758 0.6066 0.018 Uiso calc R 1.0 A .
C C6 0.30992(13) 0.4485(3) 0.61670(8) 0.0147(4) Uani d D 1.0 A .
O O9 0.25957(12) 0.4434(3) 0.83080(8) 0.0313(4) Uani d . 1.0 . .
H H9A 0.2479 0.5562 0.8432 0.038 Uiso d R 1.0 . .
H H9B 0.2487 0.4517 0.794 0.038 Uiso d R 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O7 . 2.0154(14) ?
Co1 N1 . 2.0271(16) ?
Co1 O8 . 2.1270(17) ?
Co1 O6 . 2.1304(16) ?
Co1 O3A . 2.1592(18) ?
Co1 O3 . 2.1592(16) ?
Co1 O1 . 2.1982(15) ?
O1 C1 . 1.278(2) ?
O2 C1 . 1.238(2) ?
O3 C7 . 1.260(3) ?
O4 C7 . 1.248(3) ?
C7 C6 . 1.524(3) ?
O3A C7A . 1.260(3) ?
O4A C7A . 1.248(3) ?
C7A C6 . 1.524(3) ?
O5 C4 . 1.334(2) ?
O5 H5O . 0.8397 ?
O6 H6A . 0.8405 ?
O6 H6B . 0.8402 ?
O7 H7A . 0.8405 ?
O7 H7B . 0.8404 ?
O8 H8A . 0.8401 ?
O8 H8B . 0.8408 ?
N1 C6 . 1.334(2) ?
N1 C2 . 1.337(2) ?
C1 C2 . 1.516(2) ?
C2 C3 . 1.384(2) ?
C3 C4 . 1.402(2) ?
C3 H3A . 0.95 ?
C4 C5 . 1.402(3) ?
C5 C6 . 1.383(3) ?
C5 H5A . 0.95 ?
O9 H9A . 0.8416 ?
O9 H9B . 0.8414 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O7 Co1 N1 . . 173.50(6) ?
O7 Co1 O8 . . 85.68(7) ?
N1 Co1 O8 . . 93.24(6) ?
O7 Co1 O6 . . 86.01(6) ?
N1 Co1 O6 . . 95.53(6) ?
O8 Co1 O6 . . 170.51(6) ?
O7 Co1 O3A . . 97.7(2) ?
N1 Co1 O3A . . 76.0(2) ?
O8 Co1 O3A . . 96.7(13) ?
O6 Co1 O3A . . 88.9(13) ?
O7 Co1 O3 . . 97.19(7) ?
N1 Co1 O3 . . 76.42(8) ?
O8 Co1 O3 . . 91.6(2) ?
O6 Co1 O3 . . 94.0(2) ?
O7 Co1 O1 . . 111.23(6) ?
N1 Co1 O1 . . 75.17(6) ?
O8 Co1 O1 . . 90.43(6) ?
O6 Co1 O1 . . 88.32(6) ?
O3A Co1 O1 . . 150.6(3) ?
O3 Co1 O1 . . 151.59(7) ?
C1 O1 Co1 . . 116.04(12) ?
C7 O3 Co1 . . 115.11(16) ?
O4 C7 O3 . . 126.2(2) ?
O4 C7 C6 . . 118.3(2) ?
O3 C7 C6 . . 115.4(2) ?
C7A O3A Co1 . . 116.6(6) ?
O4A C7A O3A . . 127.9(5) ?
O4A C7A C6 . . 117.2(7) ?
O3A C7A C6 . . 114.6(7) ?
C4 O5 H5O . . 111.6 ?
Co1 O6 H6A . . 106.4 ?
Co1 O6 H6B . . 114.0 ?
H6A O6 H6B . . 104.1 ?
Co1 O7 H7A . . 122.9 ?
Co1 O7 H7B . . 123.8 ?
H7A O7 H7B . . 104.4 ?
Co1 O8 H8A . . 110.4 ?
Co1 O8 H8B . . 110.2 ?
H8A O8 H8B . . 103.0 ?
C6 N1 C2 . . 120.29(16) ?
C6 N1 Co1 . . 118.96(12) ?
C2 N1 Co1 . . 120.64(12) ?
O2 C1 O1 . . 125.49(18) ?
O2 C1 C2 . . 119.62(17) ?
O1 C1 C2 . . 114.89(17) ?
N1 C2 C3 . . 121.78(16) ?
N1 C2 C1 . . 113.16(15) ?
C3 C2 C1 . . 125.05(16) ?
C2 C3 C4 . . 118.21(16) ?
C2 C3 H3A . . 120.9 ?
C4 C3 H3A . . 120.9 ?
O5 C4 C3 . . 117.46(16) ?
O5 C4 C5 . . 122.96(16) ?
C3 C4 C5 . . 119.57(16) ?
C6 C5 C4 . . 117.76(17) ?
C6 C5 H5A . . 121.1 ?
C4 C5 H5A . . 121.1 ?
N1 C6 C5 . . 122.36(17) ?
N1 C6 C7A . . 113.0(4) ?
C5 C6 C7A . . 122.8(4) ?
N1 C6 C7 . . 112.40(17) ?
C5 C6 C7 . . 125.21(18) ?
H9A O9 H9B . . 102.9 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O9 H9B O4A . 0.84 1.85 2.685(9) 172 ?
O9 H9B O4 . 0.84 1.96 2.732(3) 153 ?
O8 H8B O9 2_656 0.84 1.95 2.782(2) 170 ?
O8 H8A O2 5_666 0.84 1.89 2.708(2) 165 ?
O7 H7A O3A 2_656 0.84 1.87 2.692(14) 164 ?
O7 H7A O3 2_656 0.84 1.91 2.731(4) 163 ?
O6 H6B O9 4_546 0.84 2.06 2.845(2) 156 ?
O6 H6A O2 5_656 0.84 2.05 2.822(2) 153 ?
O5 H5O O1 3_455 0.84 1.80 2.6304(19) 170 ?


# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.210 0.750 16 9 ' '
2 0.500 0.290 0.250 16 9 ' '
3 0.500 0.710 0.750 16 9 ' '
4 0.000 0.790 0.250 16 9 ' '
_platon_squeeze_details          
;
A region of density centered on the 2-fold axis and possibly 
attributable to lattice methanol was removed with the SQUEEZE 
option of PLATON (Spek, 2013) following several unsuccessful 
attempts to refine models for it.
;

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1056391'
_audit_update_record             
;
2015-03-26 deposited with the CCDC.
2015-08-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C7 H9 N Ni O8, H2 O'
_chemical_formula_sum            'C7 H11 N Ni O9'
_chemical_formula_iupac          ?
_chemical_formula_weight         311.86

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.7013(6)
_cell_length_b                   6.8433(3)
_cell_length_c                   22.2874(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.163(1)
_cell_angle_gamma                90
_cell_volume                     2242.22(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9870
_cell_measurement_theta_min      2.7417
_cell_measurement_theta_max      29.1132
_cell_measurement_temperature    150(2)

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280

_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012b)'
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.83

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5 deg. in omega, colllected at phi = 0.00,
90.00 and 180.00 deg. and 2 sets of 800 frames, each of
width 0.45 deg in phi, collected at omega = -30.00 and 210.00
deg. The scan time was 10 sec/frame.
;

_diffrn_ambient_temperature      150.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              MoK\a

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            19570
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_full        29.11
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30

_refine_special_details          SQUEEZE

_reflns_number_total             2961
_reflns_number_gt                2776
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1189
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.164
_refine_ls_number_reflns         2961
_refine_ls_number_parameters     173
_refine_ls_number_restraints     40
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0460P)²+13.1004P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.323
_refine_diff_density_min         -0.653
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX2 (Bruker AXS, 2012)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2012a)'
_computing_data_reduction        'SAINT (Bruker AXS, 2012a)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker AXS, 2008)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.97863(2) 0.24998(5) 0.638043(15) 0.01434(12) Uani d D 1.0 . .
O O1 1.02688(12) 0.2084(3) 0.54608(8) 0.0131(4) Uani d . 1.0 A .
O O2 0.98446(13) 0.2613(3) 0.45082(9) 0.0149(4) Uani d . 1.0 A .
O O3 0.8881(2) 0.3495(6) 0.70541(11) 0.0155(9) Uani d PDU 0.863(8) A 1
O O4 0.7722(2) 0.5600(5) 0.71518(11) 0.0228(8) Uani d PDU 0.863(8) A 1
C C7 0.8236(2) 0.4527(6) 0.68528(12) 0.0134(8) Uani d PDU 0.863(8) A 1
O O3A 0.8803(15) 0.315(6) 0.7046(6) 0.0155(9) Uani d PDU 0.137(8) A 2
O O4A 0.7456(13) 0.470(4) 0.7130(7) 0.0228(8) Uani d PDU 0.137(8) A 2
C C7A 0.8111(14) 0.402(4) 0.6842(3) 0.0134(8) Uani d PDU 0.137(8) A 2
O O5 0.67008(12) 0.5757(3) 0.48965(8) 0.0135(4) Uani d . 1.0 . .
H H5O 0.6287 0.6273 0.5102 0.016 Uiso d R 1.0 . .
O O6 0.92304(14) -0.0291(3) 0.63493(9) 0.0167(4) Uani d . 1.0 A .
H H6A 0.9392 -0.0894 0.6039 0.02 Uiso d R 1.0 . .
H H6B 0.8662 -0.0375 0.6381 0.02 Uiso d R 1.0 . .
O O7 1.07385(14) 0.1354(3) 0.69255(9) 0.0196(4) Uani d . 1.0 A .
H H7A 1.0581 0.0298 0.7087 0.023 Uiso d R 1.0 . .
H H7B 1.0966 0.1934 0.7222 0.023 Uiso d R 1.0 . .
O O8 1.05307(14) 0.5080(3) 0.64438(10) 0.0216(4) Uani d . 1.0 A .
H H8A 1.1092 0.4857 0.6449 0.026 Uiso d R 1.0 . .
H H8B 1.0483 0.5717 0.6123 0.026 Uiso d R 1.0 . .
N N1 0.88265(14) 0.3711(3) 0.58911(9) 0.0107(4) Uani d . 1.0 A .
C C1 0.97187(17) 0.2714(4) 0.50571(12) 0.0107(4) Uani d . 1.0 . .
C C2 0.88559(16) 0.3652(4) 0.52943(11) 0.0088(4) Uani d . 1.0 A .
C C3 0.81540(16) 0.4370(4) 0.49444(11) 0.0098(4) Uani d . 1.0 . .
H H3 0.8187 0.4341 0.4519 0.012 Uiso calc R 1.0 A .
C C4 0.73910(16) 0.5144(4) 0.52369(11) 0.0105(4) Uani d . 1.0 A .
C C5 0.73717(17) 0.5229(4) 0.58661(11) 0.0127(5) Uani d . 1.0 . .
H H5 0.6867 0.5772 0.6073 0.015 Uiso calc R 1.0 A .
C C6 0.81143(17) 0.4496(4) 0.61742(11) 0.0126(5) Uani d D 1.0 A .
O O9 0.76190(16) 0.4475(4) 0.83197(10) 0.0282(5) Uani d . 1.0 . .
H H9A 0.7617 0.5081 0.7992 0.034 Uiso d R 1.0 . .
H H9B 0.7629 0.3353 0.8167 0.034 Uiso d R 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 . 1.965(2) ?
Ni1 O7 . 2.010(2) ?
Ni1 O6 . 2.079(2) ?
Ni1 O8 . 2.082(2) ?
Ni1 O3A . 2.122(2) ?
Ni1 O3 . 2.122(2) ?
Ni1 O1 . 2.1893(19) ?
O1 C1 . 1.283(3) ?
O2 C1 . 1.240(3) ?
O3 C7 . 1.263(3) ?
O4 C7 . 1.248(4) ?
C7 C6 . 1.523(4) ?
O3A C7A . 1.263(4) ?
O4A C7A . 1.248(4) ?
C7A C6 . 1.523(4) ?
O5 C4 . 1.333(3) ?
O5 H5O . 0.84 ?
O6 H6A . 0.8401 ?
O6 H6B . 0.84 ?
O7 H7A . 0.84 ?
O7 H7B . 0.8399 ?
O8 H8A . 0.84 ?
O8 H8B . 0.8399 ?
N1 C2 . 1.331(3) ?
N1 C6 . 1.337(3) ?
C1 C2 . 1.518(3) ?
C2 C3 . 1.382(3) ?
C3 C4 . 1.403(3) ?
C3 H3 . 0.95 ?
C4 C5 . 1.404(3) ?
C5 C6 . 1.382(4) ?
C5 H5 . 0.95 ?
O9 H9A . 0.8401 ?
O9 H9B . 0.84 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 O7 . . 176.41(8) ?
N1 Ni1 O6 . . 95.02(9) ?
O7 Ni1 O6 . . 86.26(9) ?
N1 Ni1 O8 . . 93.23(9) ?
O7 Ni1 O8 . . 85.70(9) ?
O6 Ni1 O8 . . 171.17(8) ?
N1 Ni1 O3A . . 79.0(4) ?
O7 Ni1 O3A . . 97.7(4) ?
O6 Ni1 O3A . . 87.0(12) ?
O8 Ni1 O3A . . 97.7(12) ?
N1 Ni1 O3 . . 78.83(10) ?
O7 Ni1 O3 . . 97.75(10) ?
O6 Ni1 O3 . . 94.07(13) ?
O8 Ni1 O3 . . 90.61(14) ?
N1 Ni1 O1 . . 76.66(8) ?
O7 Ni1 O1 . . 106.75(8) ?
O6 Ni1 O1 . . 88.72(7) ?
O8 Ni1 O1 . . 90.13(8) ?
O3A Ni1 O1 . . 154.8(5) ?
O3 Ni1 O1 . . 155.48(9) ?
C1 O1 Ni1 . . 114.06(16) ?
C7 O3 Ni1 . . 113.6(2) ?
O4 C7 O3 . . 126.5(3) ?
O4 C7 C6 . . 117.9(3) ?
O3 C7 C6 . . 115.5(3) ?
C7A O3A Ni1 . . 113.4(10) ?
O4A C7A O3A . . 127.7(9) ?
O4A C7A C6 . . 115.4(12) ?
O3A C7A C6 . . 116.6(12) ?
C4 O5 H5O . . 111.9 ?
Ni1 O6 H6A . . 111.5 ?
Ni1 O6 H6B . . 116.8 ?
H6A O6 H6B . . 108.6 ?
Ni1 O7 H7A . . 113.7 ?
Ni1 O7 H7B . . 124.5 ?
H7A O7 H7B . . 100.4 ?
Ni1 O8 H8A . . 111.3 ?
Ni1 O8 H8B . . 109.8 ?
H8A O8 H8B . . 100.7 ?
C2 N1 C6 . . 120.8(2) ?
C2 N1 Ni1 . . 121.08(17) ?
C6 N1 Ni1 . . 118.02(17) ?
O2 C1 O1 . . 125.3(2) ?
O2 C1 C2 . . 119.6(2) ?
O1 C1 C2 . . 115.1(2) ?
N1 C2 C3 . . 121.8(2) ?
N1 C2 C1 . . 113.0(2) ?
C3 C2 C1 . . 125.3(2) ?
C2 C3 C4 . . 118.0(2) ?
C2 C3 H3 . . 121.0 ?
C4 C3 H3 . . 121.0 ?
O5 C4 C3 . . 117.6(2) ?
O5 C4 C5 . . 122.5(2) ?
C3 C4 C5 . . 119.9(2) ?
C6 C5 C4 . . 117.6(2) ?
C6 C5 H5 . . 121.2 ?
C4 C5 H5 . . 121.2 ?
N1 C6 C5 . . 122.0(2) ?
N1 C6 C7A . . 112.4(6) ?
C5 C6 C7A . . 123.9(7) ?
N1 C6 C7 . . 112.6(2) ?
C5 C6 C7 . . 125.4(2) ?
H9A O9 H9B . . 95.7 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O9 H9B O4 4_646 0.84 2.08 2.896(4) 164 ?
O9 H9A O4A . 0.84 1.95 2.666(17) 142 ?
O9 H9A O4 . 0.84 1.91 2.719(3) 161 ?
O8 H8B O2 5_766 0.84 1.87 2.701(3) 167 ?
O8 H8A O9 2_756 0.84 1.98 2.800(3) 166 ?
O7 H7B O3A 2_756 0.84 1.86 2.686(16) 166 ?
O7 H7B O3 2_756 0.84 1.95 2.761(3) 163 ?
O6 H6B O9 4_646 0.84 2.00 2.824(3) 165 ?
O6 H6A O2 5_756 0.84 2.03 2.835(3) 159 ?
O5 H5O O1 3_455 0.84 1.79 2.618(3) 169 ?


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.212 0.750 14 9 ' '
2 0.000 0.287 0.250 14 9 ' '
3 0.000 0.713 0.750 14 9 ' '
4 0.500 0.787 0.250 14 9 ' '
_platon_squeeze_details          
;
A region of density well-removed from the primary molecule and attributed to 
lattice solvent which could not be identified with certainty was removed 
with the SQUEEZE option of PLATON (Spek, 2013).
;

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_jtm370_0m
_database_code_depnum_ccdc_archive 'CCDC 1402098'
_audit_update_record             
;
2015-05-20 deposited with the CCDC.
2015-08-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'Bis(2-amino-4-methylpydidinium) trichlorido(pyridine-2,6-dicarboxylato)ferrate(III) hydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H3 Cl3 Fe N O4, 2(C6 H9 N2), H2 O'
_chemical_formula_sum            'C19 H23 Cl3 Fe N5 O5'
_chemical_formula_weight         563.62

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'
Fe Fe 0.3463 0.8444 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.0736(9)
_cell_length_b                   11.177(1)
_cell_length_c                   11.6302(11)
_cell_angle_alpha                87.916(1)
_cell_angle_beta                 79.547(1)
_cell_angle_gamma                64.073(1)
_cell_volume                     1156.77(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.2871
_cell_measurement_theta_max      29.1647
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_F_000             578
_exptl_transmission_factor_min   0.805
_exptl_transmission_factor_max   0.970
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.040
_shelx_estimated_absorpt_T_min   0.796
_shelx_estimated_absorpt_T_max   0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  0.86

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, colllected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 20 sec/frame.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            20506
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.028
_diffrn_reflns_theta_max         29.157
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5818
_reflns_number_gt                4974
_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2014)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. H-atoms attached to carbon
 were placed in calculated positions (C---H = 0.95 - 0.98 Å) while those
 attached to nitrogen and oxygen were placed in locations derived from a
 difference map and their coordinates adjusted to give N---H  and O---H
 distances, respectively, of 0.91 and 0.86 Å. All were included as
 riding contributions with isotropic displacement  parameters 1.2 - 1.5
 times those of the attached atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0348P)²+0.6109P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5818
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0750
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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
Fe1 Fe 0.77917(3) 0.74760(2) 0.21243(2) 0.01293(7) Uani 1 1 d . . . . .
Cl1 Cl 0.52113(5) 0.88677(4) 0.30599(3) 0.01648(9) Uani 1 1 d . . . . .
Cl2 Cl 1.01991(4) 0.60268(4) 0.11485(4) 0.01708(9) Uani 1 1 d . . . . .
Cl3 Cl 0.85846(5) 0.76782(4) 0.37782(4) 0.01946(10) Uani 1 1 d . . . . .
O1 O 0.72095(13) 0.59062(11) 0.23102(10) 0.0146(2) Uani 1 1 d . . . . .
O2 O 0.61578(14) 0.47940(11) 0.15470(11) 0.0172(2) Uani 1 1 d . . . . .
O3 O 0.78639(13) 0.90838(11) 0.12351(10) 0.0152(2) Uani 1 1 d . . . . .
O4 O 0.74412(14) 1.02429(11) -0.03853(10) 0.0166(2) Uani 1 1 d . . . . .
N1 N 0.69011(15) 0.74863(13) 0.06437(11) 0.0119(3) Uani 1 1 d . . . . .
C1 C 0.65903(18) 0.56678(15) 0.15186(14) 0.0132(3) Uani 1 1 d . . . . .
C2 C 0.64047(18) 0.65860(15) 0.05130(14) 0.0126(3) Uani 1 1 d . . . . .
C3 C 0.57693(18) 0.65803(16) -0.04497(14) 0.0151(3) Uani 1 1 d . . . . .
H3 H 0.5413 0.5939 -0.0549 0.018 Uiso 1 1 calc R U . . .
C4 C 0.56723(19) 0.75452(17) -0.12640(15) 0.0168(3) Uani 1 1 d . . . . .
H4 H 0.5249 0.7562 -0.1934 0.020 Uiso 1 1 calc R U . . .
C5 C 0.61889(18) 0.84868(16) -0.11060(14) 0.0147(3) Uani 1 1 d . . . . .
H5 H 0.6121 0.9152 -0.1656 0.018 Uiso 1 1 calc R U . . .
C6 C 0.68058(17) 0.84210(15) -0.01188(14) 0.0121(3) Uani 1 1 d . . . . .
C7 C 0.74095(18) 0.93434(15) 0.02382(14) 0.0128(3) Uani 1 1 d . . . . .
N2 N 0.29282(16) 0.52474(14) 0.55171(12) 0.0151(3) Uani 1 1 d . . . . .
H2N H 0.2971 0.4772 0.6173 0.018 Uiso 1 1 d R U . . .
N3 N 0.37604(16) 0.66016(14) 0.63088(12) 0.0165(3) Uani 1 1 d . . . . .
H3A H 0.3838 0.6148 0.6978 0.020 Uiso 1 1 d R U . . .
H3B H 0.4104 0.7234 0.6191 0.020 Uiso 1 1 d R U . . .
C8 C 0.24787(19) 0.48303(16) 0.46308(15) 0.0165(3) Uani 1 1 d . . . . .
H8 H 0.2221 0.4106 0.4738 0.020 Uiso 1 1 calc R U . . .
C9 C 0.23981(19) 0.54421(17) 0.36031(15) 0.0176(3) Uani 1 1 d . . . . .
H9 H 0.2086 0.5150 0.2990 0.021 Uiso 1 1 calc R U . . .
C10 C 0.27845(18) 0.65266(16) 0.34461(15) 0.0150(3) Uani 1 1 d . . . . .
C11 C 0.32477(19) 0.69138(16) 0.43404(14) 0.0153(3) Uani 1 1 d . . . . .
H11 H 0.3522 0.7629 0.4242 0.018 Uiso 1 1 calc R U . . .
C12 C 0.33237(18) 0.62628(16) 0.54100(14) 0.0144(3) Uani 1 1 d . . . . .
C13 C 0.2650(2) 0.72268(17) 0.23216(15) 0.0181(3) Uani 1 1 d . . . . .
H13A H 0.3003 0.7915 0.2335 0.027 Uiso 1 1 calc R U . . .
H13B H 0.1598 0.7641 0.2227 0.027 Uiso 1 1 calc R U . . .
H13C H 0.3263 0.6583 0.1666 0.027 Uiso 1 1 calc R U . . .
C14 C 0.9534(2) 0.04511(18) 0.30787(16) 0.0216(4) Uani 1 1 d . . . . .
H14 H 0.9458 -0.0256 0.3520 0.026 Uiso 1 1 calc R U . . .
N4 N 0.90402(17) 0.07128(14) 0.20388(13) 0.0172(3) Uani 1 1 d . . . . .
H4N H 0.8666 0.0198 0.1758 0.021 Uiso 1 1 d R U . . .
N5 N 0.86503(17) 0.18858(14) 0.03555(13) 0.0184(3) Uani 1 1 d . . . . .
H5A H 0.8262 0.1370 0.0096 0.022 Uiso 1 1 d R U . . .
H5B H 0.8685 0.2580 -0.0061 0.022 Uiso 1 1 d R U . . .
C15 C 1.0128(2) 0.11847(18) 0.34883(16) 0.0208(4) Uani 1 1 d . . . . .
H15 H 1.0489 0.0984 0.4205 0.025 Uiso 1 1 calc R U . . .
C16 C 1.02109(19) 0.22587(16) 0.28407(15) 0.0168(3) Uani 1 1 d . . . . .
C17 C 0.96983(19) 0.25159(16) 0.18015(15) 0.0160(3) Uani 1 1 d . . . . .
H17 H 0.9734 0.3240 0.1365 0.019 Uiso 1 1 calc R U . . .
C18 C 0.91167(18) 0.17087(16) 0.13757(15) 0.0151(3) Uani 1 1 d . . . . .
C19 C 1.0840(2) 0.30985(18) 0.33000(16) 0.0208(4) Uani 1 1 d . . . . .
H19A H 1.0280 0.3468 0.4086 0.031 Uiso 1 1 calc R U . . .
H19B H 1.0752 0.3827 0.2778 0.031 Uiso 1 1 calc R U . . .
H19C H 1.1900 0.2549 0.3337 0.031 Uiso 1 1 calc R U . . .
O5 O 0.50099(18) 0.84516(14) 0.58879(12) 0.0316(3) Uani 1 1 d . . . . .
H5OA H 0.4752 0.9225 0.6201 0.038 Uiso 1 1 d R U . . .
H5OB H 0.5114 0.8586 0.5151 0.038 Uiso 1 1 d 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
Fe1 O3 2.0630(11) . ?
Fe1 O1 2.0726(11) . ?
Fe1 N1 2.0786(13) . ?
Fe1 Cl3 2.2662(5) . ?
Fe1 Cl2 2.3437(5) . ?
Fe1 Cl1 2.4334(5) . ?
O1 C1 1.2958(19) . ?
O2 C1 1.2286(19) . ?
O3 C7 1.3000(19) . ?
O4 C7 1.2264(19) . ?
N1 C6 1.328(2) . ?
N1 C2 1.328(2) . ?
C1 C2 1.510(2) . ?
C2 C3 1.388(2) . ?
C3 C4 1.392(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.509(2) . ?
N2 C12 1.353(2) . ?
N2 C8 1.369(2) . ?
N2 H2N 0.9100 . ?
N3 C12 1.331(2) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9099 . ?
C8 C9 1.353(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.423(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.368(2) . ?
C10 C13 1.496(2) . ?
C11 C12 1.415(2) . ?
C11 H11 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.349(3) . ?
C14 N4 1.364(2) . ?
C14 H14 0.9500 . ?
N4 C18 1.353(2) . ?
N4 H4N 0.9101 . ?
N5 C18 1.331(2) . ?
N5 H5A 0.9099 . ?
N5 H5B 0.9101 . ?
C15 C16 1.419(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.372(2) . ?
C16 C19 1.499(2) . ?
C17 C18 1.415(2) . ?
C17 H17 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O5 H5OA 0.8600 . ?
O5 H5OB 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Fe1 O1 151.09(5) . . ?
O3 Fe1 N1 75.63(5) . . ?
O1 Fe1 N1 75.52(5) . . ?
O3 Fe1 Cl3 101.07(3) . . ?
O1 Fe1 Cl3 107.52(3) . . ?
N1 Fe1 Cl3 174.26(4) . . ?
O3 Fe1 Cl2 92.25(4) . . ?
O1 Fe1 Cl2 89.94(4) . . ?
N1 Fe1 Cl2 90.76(4) . . ?
Cl3 Fe1 Cl2 94.089(18) . . ?
O3 Fe1 Cl1 89.97(4) . . ?
O1 Fe1 Cl1 86.01(4) . . ?
N1 Fe1 Cl1 85.57(4) . . ?
Cl3 Fe1 Cl1 89.762(17) . . ?
Cl2 Fe1 Cl1 175.104(16) . . ?
C1 O1 Fe1 119.23(10) . . ?
C7 O3 Fe1 119.50(10) . . ?
C6 N1 C2 122.40(14) . . ?
C6 N1 Fe1 118.65(11) . . ?
C2 N1 Fe1 118.91(10) . . ?
O2 C1 O1 125.31(15) . . ?
O2 C1 C2 120.48(14) . . ?
O1 C1 C2 114.21(13) . . ?
N1 C2 C3 120.64(14) . . ?
N1 C2 C1 112.12(13) . . ?
C3 C2 C1 127.22(14) . . ?
C2 C3 C4 117.78(15) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
C3 C4 C5 120.67(15) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 117.74(15) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
N1 C6 C5 120.76(14) . . ?
N1 C6 C7 112.38(14) . . ?
C5 C6 C7 126.86(14) . . ?
O4 C7 O3 125.42(15) . . ?
O4 C7 C6 120.78(14) . . ?
O3 C7 C6 113.79(13) . . ?
C12 N2 C8 122.39(14) . . ?
C12 N2 H2N 122.7 . . ?
C8 N2 H2N 114.9 . . ?
C12 N3 H3A 121.9 . . ?
C12 N3 H3B 117.0 . . ?
H3A N3 H3B 120.6 . . ?
C9 C8 N2 120.47(15) . . ?
C9 C8 H8 119.8 . . ?
N2 C8 H8 119.8 . . ?
C8 C9 C10 119.57(15) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 118.81(15) . . ?
C11 C10 C13 121.76(15) . . ?
C9 C10 C13 119.42(15) . . ?
C10 C11 C12 120.84(15) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
N3 C12 N2 118.76(15) . . ?
N3 C12 C11 123.32(15) . . ?
N2 C12 C11 117.91(15) . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N4 120.76(16) . . ?
C15 C14 H14 119.6 . . ?
N4 C14 H14 119.6 . . ?
C18 N4 C14 122.20(15) . . ?
C18 N4 H4N 117.6 . . ?
C14 N4 H4N 120.2 . . ?
C18 N5 H5A 122.2 . . ?
C18 N5 H5B 117.1 . . ?
H5A N5 H5B 120.6 . . ?
C14 C15 C16 119.53(17) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 118.98(15) . . ?
C17 C16 C19 121.03(15) . . ?
C15 C16 C19 119.98(16) . . ?
C16 C17 C18 120.36(15) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
N5 C18 N4 118.99(15) . . ?
N5 C18 C17 122.88(15) . . ?
N4 C18 C17 118.13(15) . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
H5OA O5 H5OB 102.8 . . ?

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
O5 H5OB Cl1 0.86 2.43 3.2870(14) 174 .
O5 H5OA Cl1 0.86 2.34 3.1793(14) 164 2_676
N5 H5B Cl2 0.91 2.48 3.3435(15) 158 2_765
N5 H5A O4 0.91 1.93 2.8371(18) 177 1_545
N4 H4N O3 0.91 1.92 2.8294(18) 176 1_545
N3 H3B O5 0.91 1.93 2.842(2) 175 .
N3 H3A O2 0.91 1.98 2.8875(18) 176 2_666
N2 H2N O1 0.91 1.90 2.8034(18) 169 2_666

_refine_diff_density_max         0.416
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.081


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
