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

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

data_Cpx1
_database_code_depnum_ccdc_archive 'CCDC 1058283'

# publcif _publ_body_element loop end

_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_publcif_datablock.id            {ca4ab78e-a65b-4f65-a499-6ab46f929d01}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H16 Cu3 N2 O16, H2 O'
_chemical_formula_sum            'C18 H18 Cu3 N2 O17'
_chemical_formula_weight         724.96

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5827(3)
_cell_length_b                   10.6301(4)
_cell_length_c                   13.4395(5)
_cell_angle_alpha                95.3540(10)
_cell_angle_beta                 95.6380(10)
_cell_angle_gamma                112.3110(10)
_cell_volume                     1117.45(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9072
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      29.73

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             726
_exptl_absorpt_coefficient_mu    2.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3873
_exptl_absorpt_correction_T_max  0.8440
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'

_exptl_special_details           ?

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21401
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         29.13
_reflns_number_total             6027
_reflns_number_gt                5167
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'ApexII (Bruker, 2011)'
_computing_cell_refinement       'ApexII (Bruker, 2011)'
_computing_data_reduction        'ApexII (Bruker, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 3.2f (Crystal Impact GbR, 1997-2010)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0409P)²+0.8588P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6027
_refine_ls_number_parameters     387
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.051
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.48041(3) 0.45401(3) 0.35623(2) 0.02242(8) Uani 1 1 d . . .
Cu2 Cu 0.57705(3) 0.26796(3) 0.53110(2) 0.02116(8) Uani 1 1 d . . .
Cu3 Cu 0.64920(3) 0.10599(3) 0.72765(2) 0.02171(8) Uani 1 1 d . . .
O1W O 0.3744(3) 0.4723(2) 0.2264(2) 0.0623(8) Uani 1 1 d D . .
H1W1 H 0.286(3) 0.411(3) 0.202(3) 0.075 Uiso 1 1 d D . .
H2W1 H 0.406(5) 0.544(2) 0.204(3) 0.075 Uiso 1 1 d D . .
O1 O 0.34956(19) 0.15352(17) 0.45297(13) 0.0256(3) Uani 1 1 d . . .
O2W O 0.7809(2) 0.0861(2) 0.84692(14) 0.0339(4) Uani 1 1 d D . .
H1W2 H 0.794(4) 0.151(2) 0.889(2) 0.041 Uiso 1 1 d D . .
H2W2 H 0.738(4) 0.021(2) 0.877(2) 0.041 Uiso 1 1 d D . .
O2 O 0.2952(2) 0.27669(18) 0.33727(14) 0.0327(4) Uani 1 1 d . . .
O3 O -0.3008(3) -0.1275(2) -0.05312(15) 0.0465(5) Uani 1 1 d . . .
O3W O 0.0822(2) 0.3118(2) 0.11038(15) 0.0362(4) Uani 1 1 d D . .
H1W3 H 0.009(3) 0.331(3) 0.083(2) 0.043 Uiso 1 1 d D . .
H2W3 H 0.118(4) 0.280(3) 0.0662(19) 0.043 Uiso 1 1 d D . .
O4 O -0.1952(3) -0.2286(2) 0.05667(15) 0.0416(5) Uani 1 1 d . . .
O5 O -0.3643(2) -0.36396(18) 0.34759(14) 0.0337(4) Uani 1 1 d . . .
O6 O -0.1318(2) -0.31874(19) 0.45929(14) 0.0299(4) Uani 1 1 d . . .
O7 O 0.7963(2) 0.3901(2) 0.61070(16) 0.0433(5) Uani 1 1 d . . .
O8 O 0.8523(2) 0.26832(17) 0.72571(14) 0.0292(4) Uani 1 1 d . . .
O9 O 1.3995(2) 0.6945(2) 1.12977(14) 0.0404(5) Uani 1 1 d . . .
O10 O 1.1887(3) 0.6987(3) 1.02126(16) 0.0579(7) Uani 1 1 d . . .
O11 O 1.4753(2) 0.93331(18) 0.74513(13) 0.0329(4) Uani 1 1 d . . .
O12 O 1.2960(2) 0.8538(2) 0.59941(14) 0.0380(5) Uani 1 1 d . . .
O13 O 0.6062(2) 0.4210(2) 0.46411(17) 0.0402(5) Uani 1 1 d D . .
H13O H 0.696(2) 0.482(2) 0.483(2) 0.044(9) Uiso 1 1 d D . .
O14 O 0.5372(2) 0.12541(19) 0.60908(15) 0.0352(4) Uani 1 1 d D . .
H14O H 0.462(3) 0.054(2) 0.586(2) 0.045(10) Uiso 1 1 d D . .
N1 N -0.1464(2) -0.03103(19) 0.21406(14) 0.0204(4) Uani 1 1 d . . .
N2 N 1.2743(2) 0.5837(2) 0.86222(15) 0.0225(4) Uani 1 1 d . . .
C1 C 0.2610(3) 0.1726(2) 0.38152(16) 0.0195(4) Uani 1 1 d . . .
C2 C 0.0931(3) 0.0573(2) 0.34181(16) 0.0186(4) Uani 1 1 d . . .
C3 C 0.0267(3) -0.0599(2) 0.38756(16) 0.0186(4) Uani 1 1 d . . .
H3 H 0.0875 -0.0712 0.4448 0.022 Uiso 1 1 calc R . .
C4 C -0.1322(3) -0.1601(2) 0.34660(17) 0.0187(4) Uani 1 1 d . . .
C5 C -0.2170(3) -0.1427(2) 0.25975(17) 0.0213(4) Uani 1 1 d . . .
H5 H -0.3239 -0.2086 0.2325 0.026 Uiso 1 1 calc R . .
C6 C 0.0044(3) 0.0686(2) 0.25372(17) 0.0213(4) Uani 1 1 d . . .
H6 H 0.0497 0.1457 0.2218 0.026 Uiso 1 1 calc R . .
C7 C -0.2123(3) -0.2915(2) 0.39104(17) 0.0205(4) Uani 1 1 d . . .
C8 C -0.2330(3) -0.0245(2) 0.11555(18) 0.0262(5) Uani 1 1 d . . .
H8A H -0.1731 0.0644 0.0950 0.031 Uiso 1 1 calc R . .
H8B H -0.3478 -0.0330 0.1226 0.031 Uiso 1 1 calc R . .
C9 C -0.2412(3) -0.1372(3) 0.03334(19) 0.0291(5) Uani 1 1 d . . .
C10 C 0.8822(3) 0.3723(2) 0.68309(17) 0.0218(4) Uani 1 1 d . . .
C11 C 1.0463(3) 0.4915(2) 0.72755(17) 0.0208(4) Uani 1 1 d . . .
C12 C 1.1129(3) 0.6090(2) 0.68215(18) 0.0229(4) Uani 1 1 d . . .
H12 H 1.0574 0.6178 0.6218 0.027 Uiso 1 1 calc R . .
C13 C 1.2651(3) 0.7136(2) 0.72923(17) 0.0216(4) Uani 1 1 d . . .
C14 C 1.3428(3) 0.6984(2) 0.81941(18) 0.0230(4) Uani 1 1 d . . .
H14 H 1.4439 0.7682 0.8512 0.028 Uiso 1 1 calc R . .
C15 C 1.1294(3) 0.4806(2) 0.81815(18) 0.0226(4) Uani 1 1 d . . .
H15 H 1.0846 0.4017 0.8483 0.027 Uiso 1 1 calc R . .
C16 C 1.3506(3) 0.8445(2) 0.68498(18) 0.0234(4) Uani 1 1 d . . .
C17 C 1.3544(3) 0.5802(3) 0.96361(19) 0.0283(5) Uani 1 1 d . . .
H17A H 1.4770 0.6158 0.9658 0.034 Uiso 1 1 calc R . .
H17B H 1.3164 0.4859 0.9770 0.034 Uiso 1 1 calc R . .
C18 C 1.3093(3) 0.6657(3) 1.0453(2) 0.0315(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O13 1.8615(18) . ?
Cu1 O5 1.9101(17) 1_665 ?
Cu1 O2 1.9237(17) . ?
Cu1 O1W 1.949(2) . ?
Cu2 O14 1.8667(18) . ?
Cu2 O13 1.8786(18) . ?
Cu2 O7 1.9653(18) . ?
Cu2 O1 1.9874(15) . ?
Cu3 O14 1.8484(18) . ?
Cu3 O11 1.9291(17) 1_445 ?
Cu3 O8 1.9366(16) . ?
Cu3 O2W 1.9441(19) . ?
O1W H1W1 0.805(13) . ?
O1W H2W1 0.804(13) . ?
O1 C1 1.246(3) . ?
O2W H1W2 0.811(13) . ?
O2W H2W2 0.816(13) . ?
O2 C1 1.255(3) . ?
O3 C9 1.252(3) . ?
O3W H1W3 0.804(12) . ?
O3W H2W3 0.803(13) . ?
O4 C9 1.234(3) . ?
O5 C7 1.280(3) . ?
O5 Cu1 1.9101(17) 1_445 ?
O6 C7 1.216(3) . ?
O7 C10 1.235(3) . ?
O8 C10 1.244(3) . ?
O9 C18 1.251(3) . ?
O10 C18 1.237(3) . ?
O11 C16 1.269(3) . ?
O11 Cu3 1.9291(17) 1_665 ?
O12 C16 1.226(3) . ?
O13 H13O 0.794(13) . ?
O14 H14O 0.796(13) . ?
N1 C6 1.341(3) . ?
N1 C5 1.347(3) . ?
N1 C8 1.474(3) . ?
N2 C15 1.341(3) . ?
N2 C14 1.347(3) . ?
N2 C17 1.475(3) . ?
C1 C2 1.500(3) . ?
C2 C6 1.383(3) . ?
C2 C3 1.388(3) . ?
C3 C4 1.392(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(3) . ?
C4 C7 1.513(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.527(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 C11 1.511(3) . ?
C11 C15 1.387(3) . ?
C11 C12 1.389(3) . ?
C12 C13 1.395(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.378(3) . ?
C13 C16 1.514(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C17 C18 1.532(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?

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
O13 Cu1 O5 97.54(7) . 1_665 ?
O13 Cu1 O2 95.82(8) . . ?
O5 Cu1 O2 166.60(7) 1_665 . ?
O13 Cu1 O1W 168.16(13) . . ?
O5 Cu1 O1W 82.72(8) 1_665 . ?
O2 Cu1 O1W 83.98(8) . . ?
O14 Cu2 O13 173.16(10) . . ?
O14 Cu2 O7 95.82(8) . . ?
O13 Cu2 O7 83.45(8) . . ?
O14 Cu2 O1 85.90(7) . . ?
O13 Cu2 O1 94.46(7) . . ?
O7 Cu2 O1 176.34(8) . . ?
O14 Cu3 O11 95.81(8) . 1_445 ?
O14 Cu3 O8 94.12(8) . . ?
O11 Cu3 O8 169.14(8) 1_445 . ?
O14 Cu3 O2W 175.74(9) . . ?
O11 Cu3 O2W 86.42(8) 1_445 . ?
O8 Cu3 O2W 83.40(8) . . ?
Cu1 O1W H1W1 117(3) . . ?
Cu1 O1W H2W1 121(3) . . ?
H1W1 O1W H2W1 121(4) . . ?
C1 O1 Cu2 133.16(15) . . ?
Cu3 O2W H1W2 106(2) . . ?
Cu3 O2W H2W2 119(2) . . ?
H1W2 O2W H2W2 102(3) . . ?
C1 O2 Cu1 134.33(15) . . ?
H1W3 O3W H2W3 106(3) . . ?
C7 O5 Cu1 132.58(15) . 1_445 ?
C10 O7 Cu2 131.17(16) . . ?
C10 O8 Cu3 133.68(15) . . ?
C16 O11 Cu3 132.30(16) . 1_665 ?
Cu1 O13 Cu2 134.00(10) . . ?
Cu1 O13 H13O 114(3) . . ?
Cu2 O13 H13O 112(3) . . ?
Cu3 O14 Cu2 133.62(10) . . ?
Cu3 O14 H14O 110(3) . . ?
Cu2 O14 H14O 116(3) . . ?
C6 N1 C5 121.13(19) . . ?
C6 N1 C8 120.22(19) . . ?
C5 N1 C8 118.53(18) . . ?
C15 N2 C14 121.2(2) . . ?
C15 N2 C17 120.7(2) . . ?
C14 N2 C17 117.96(19) . . ?
O1 C1 O2 128.0(2) . . ?
O1 C1 C2 116.76(19) . . ?
O2 C1 C2 115.21(19) . . ?
C6 C2 C3 119.37(19) . . ?
C6 C2 C1 117.45(19) . . ?
C3 C2 C1 123.1(2) . . ?
C2 C3 C4 119.1(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 119.2(2) . . ?
C5 C4 C7 118.37(19) . . ?
C3 C4 C7 122.3(2) . . ?
N1 C5 C4 120.61(19) . . ?
N1 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
N1 C6 C2 120.5(2) . . ?
N1 C6 H6 119.8 . . ?
C2 C6 H6 119.8 . . ?
O6 C7 O5 127.5(2) . . ?
O6 C7 C4 120.17(19) . . ?
O5 C7 C4 112.31(19) . . ?
N1 C8 C9 112.63(19) . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
O4 C9 O3 126.5(3) . . ?
O4 C9 C8 119.3(2) . . ?
O3 C9 C8 114.2(2) . . ?
O7 C10 O8 128.8(2) . . ?
O7 C10 C11 116.9(2) . . ?
O8 C10 C11 114.4(2) . . ?
C15 C11 C12 120.1(2) . . ?
C15 C11 C10 117.1(2) . . ?
C12 C11 C10 122.7(2) . . ?
C11 C12 C13 118.4(2) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C14 C13 C12 119.4(2) . . ?
C14 C13 C16 118.0(2) . . ?
C12 C13 C16 122.6(2) . . ?
N2 C14 C13 120.9(2) . . ?
N2 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
N2 C15 C11 120.0(2) . . ?
N2 C15 H15 120.0 . . ?
C11 C15 H15 120.0 . . ?
O12 C16 O11 128.0(2) . . ?
O12 C16 C13 119.3(2) . . ?
O11 C16 C13 112.7(2) . . ?
N2 C17 C18 111.24(19) . . ?
N2 C17 H17A 109.4 . . ?
C18 C17 H17A 109.4 . . ?
N2 C17 H17B 109.4 . . ?
C18 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
O10 C18 O9 127.0(3) . . ?
O10 C18 C17 117.1(2) . . ?
O9 C18 C17 115.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        29.13
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.084

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?
####################################################################### 
# 
# 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_Cpx2
_database_code_depnum_ccdc_archive 'CCDC 1058284'

_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_publcif_datablock.id            {f3bd641e-01f1-4718-b2c9-9c64828c0a45}

# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H9 Cu N O8, O0.50, O0.50, H2 O'
_chemical_formula_sum            'C9 H11 Cu N O10'
_chemical_formula_weight         356.73

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.2384(18)
_cell_length_b                   7.4454(15)
_cell_length_c                   23.041(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.23(3)
_cell_angle_gamma                90
_cell_volume                     1456.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    7764
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      28.94

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_F_000             724
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.548
_shelx_estimated_absorpt_T_min   0.576
_shelx_estimated_absorpt_T_max   0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5764
_exptl_absorpt_correction_T_max  0.8360
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'

_exptl_special_details           ?

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14424
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.345
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3336
_reflns_number_gt                2704
_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       'ApexII (Bruker, 2011)'
_computing_cell_refinement       'ApexII (Bruker, 2011)'
_computing_data_reduction        'ApexII (Bruker, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 3.2f (Crystal Impact GbR, 1997-2010)'
_computing_publication_material  'publCIF (Westrip, 2010)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0831P)²+3.1982P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3336
_refine_ls_number_parameters     211
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1748
_refine_ls_wR_factor_gt          0.1651
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.150
_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
Cu1 Cu 0.61893(6) 0.45584(7) 0.28820(2) 0.0250(2) Uani 1 1 d . . . . .
O1 O 0.4012(4) 0.4839(5) 0.23051(16) 0.0332(8) Uani 1 1 d . . . . .
O1W O 0.8351(4) 0.4214(6) 0.34788(17) 0.0402(9) Uani 1 1 d D . . . .
H1W1 H 0.812(8) 0.530(3) 0.350(3) 0.048 Uiso 1 1 d D U . . .
H2W1 H 0.850(7) 0.371(7) 0.3830(16) 0.048 Uiso 1 1 d D U . . .
O2 O 0.4111(4) 0.2483(5) 0.17152(16) 0.0358(8) Uani 1 1 d . . . . .
O2W O 0.5408(4) 0.3248(5) 0.34429(16) 0.0351(8) Uani 1 1 d D . . . .
H1W2 H 0.612(5) 0.281(7) 0.3770(17) 0.042 Uiso 1 1 d D U . . .
H2W2 H 0.478(5) 0.246(6) 0.320(2) 0.042 Uiso 1 1 d D U . . .
O3 O -0.0594(5) 0.1991(7) -0.03793(18) 0.0585(12) Uani 1 1 d . . . . .
O4 O -0.2839(5) 0.3259(7) -0.04683(18) 0.0581(12) Uani 1 1 d . . . . .
O5 O -0.3089(4) 0.5775(4) 0.22862(15) 0.0286(7) Uani 1 1 d . . . . .
O6 O -0.1680(5) 0.3453(5) 0.21793(17) 0.0435(9) Uani 1 1 d . . . . .
O3W O 0.4981(11) 0.3666(18) 0.0688(4) 0.077(3) Uani 0.5 1 d . . P . .
O4W O 0.7530(13) 0.8853(15) 0.0377(4) 0.071(3) Uani 0.5 1 d . . P . .
O5W O 0.8966(5) 0.0528(6) 0.1567(2) 0.0616(12) Uani 1 1 d . . . . .
H1W5 H 0.9442 0.1483 0.1542 0.074 Uiso 1 1 d R U . . .
H2W5 H 0.8857 0.0551 0.1916 0.074 Uiso 1 1 d R U . . .
N1 N -0.0762(4) 0.5255(5) 0.13468(17) 0.0247(8) Uani 1 1 d . . . . .
C1 C 0.3418(5) 0.3731(6) 0.1850(2) 0.0254(9) Uani 1 1 d . . . . .
C2 C 0.1693(5) 0.4022(6) 0.1453(2) 0.0231(8) Uani 1 1 d . . . . .
C3 C 0.0803(5) 0.5044(6) 0.1689(2) 0.0257(9) Uani 1 1 d . . . . .
H3 H 0.1287 0.5600 0.2091 0.031 Uiso 1 1 calc R U . . .
C4 C -0.1477(5) 0.4564(6) 0.0759(2) 0.0302(10) Uani 1 1 d . . . . .
H4 H -0.2570 0.4761 0.0527 0.036 Uiso 1 1 calc R U . . .
C5 C -0.0627(5) 0.3574(6) 0.04955(19) 0.0278(9) Uani 1 1 d . . . . .
C6 C 0.0978(5) 0.3280(6) 0.0854(2) 0.0267(9) Uani 1 1 d . . . . .
H6 H 0.1578 0.2570 0.0688 0.032 Uiso 1 1 calc R U . . .
C7 C -0.1427(6) 0.2850(7) -0.0169(2) 0.0341(11) Uani 1 1 d . . . . .
C8 C -0.1711(5) 0.6229(6) 0.1641(2) 0.0301(10) Uani 1 1 d . . . . .
H8A H -0.2672 0.6722 0.1305 0.036 Uiso 1 1 calc R U . . .
H8B H -0.1090 0.7247 0.1894 0.036 Uiso 1 1 calc R U . . .
C9 C -0.2180(5) 0.4984(6) 0.2066(2) 0.0252(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.936(3) . ?
Cu1 O1W 1.944(4) . ?
Cu1 O5 1.968(3) 1_655 ?
Cu1 O2W 1.969(3) . ?
Cu1 O2 2.425(4) 2_655 ?
Cu1 H1W1 1.88(6) . ?
O1 C1 1.276(6) . ?
O1W H1W1 0.843(19) . ?
O1W H2W1 0.851(19) . ?
O2 C1 1.235(5) . ?
O2 Cu1 2.425(4) 2_645 ?
O2W H1W2 0.845(19) . ?
O2W H2W2 0.858(19) . ?
O3 C7 1.237(6) . ?
O4 C7 1.249(6) . ?
O5 C9 1.284(5) . ?
O5 Cu1 1.968(3) 1_455 ?
O6 C9 1.219(6) . ?
O5W H1W5 0.8499 . ?
O5W H2W5 0.8500 . ?
N1 C4 1.352(6) . ?
N1 C3 1.356(6) . ?
N1 C8 1.491(5) . ?
C1 C2 1.508(6) . ?
C2 C3 1.380(6) . ?
C2 C6 1.387(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(6) . ?
C5 C7 1.513(6) . ?
C6 H6 0.9500 . ?
C8 C9 1.529(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1W 177.90(15) . . ?
O1 Cu1 O5 91.00(14) . 1_655 ?
O1W Cu1 O5 91.03(14) . 1_655 ?
O1 Cu1 O2W 87.33(15) . . ?
O1W Cu1 O2W 90.62(15) . . ?
O5 Cu1 O2W 176.96(14) 1_655 . ?
O1 Cu1 O2 85.47(13) . 2_655 ?
O1W Cu1 O2 95.08(15) . 2_655 ?
O5 Cu1 O2 88.57(12) 1_655 2_655 ?
O2W Cu1 O2 93.82(14) . 2_655 ?
O1 Cu1 H1W1 155.5(7) . . ?
O1W Cu1 H1W1 25.4(6) . . ?
O5 Cu1 H1W1 84.9(17) 1_655 . ?
O2W Cu1 H1W1 97.6(17) . . ?
O2 Cu1 H1W1 70.3(8) 2_655 . ?
C1 O1 Cu1 119.2(3) . . ?
Cu1 O1W H1W1 73(4) . . ?
Cu1 O1W H2W1 118(4) . . ?
H1W1 O1W H2W1 108(4) . . ?
C1 O2 Cu1 115.5(3) . 2_645 ?
Cu1 O2W H1W2 115(4) . . ?
Cu1 O2W H2W2 103(4) . . ?
H1W2 O2W H2W2 114(4) . . ?
C9 O5 Cu1 121.3(3) . 1_455 ?
H1W5 O5W H2W5 107.7 . . ?
C4 N1 C3 121.7(4) . . ?
C4 N1 C8 119.9(4) . . ?
C3 N1 C8 118.4(4) . . ?
O2 C1 O1 126.6(4) . . ?
O2 C1 C2 119.0(4) . . ?
O1 C1 C2 114.5(4) . . ?
C3 C2 C6 119.2(4) . . ?
C3 C2 C1 119.5(4) . . ?
C6 C2 C1 121.4(4) . . ?
N1 C3 C2 120.0(4) . . ?
N1 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
N1 C4 C5 120.4(4) . . ?
N1 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 118.5(4) . . ?
C4 C5 C7 120.0(4) . . ?
C6 C5 C7 121.5(4) . . ?
C2 C6 C5 120.2(4) . . ?
C2 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
O3 C7 O4 125.8(5) . . ?
O3 C7 C5 116.7(4) . . ?
O4 C7 C5 117.3(4) . . ?
N1 C8 C9 111.2(4) . . ?
N1 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
O6 C9 O5 126.5(4) . . ?
O6 C9 C8 121.7(4) . . ?
O5 C9 C8 111.7(4) . . ?

_refine_diff_density_max         1.207
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.130

_shelxl_version_number           2013-2


loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?
####################################################################### 
# 
# 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_Cpx3
_database_code_depnum_ccdc_archive 'CCDC 1058285'

# publcif _publ_body_element loop end

_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_publcif_datablock.id            {ebd7af0b-d308-48e7-a90d-7a6ecc6c02e0}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 Cu N3 O6, 3(H2 O)'
_chemical_formula_sum            'C19 H19 Cu N3 O9'
_chemical_formula_weight         496.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   9.1905(5)
_cell_length_b                   7.7875(4)
_cell_length_c                   27.5073(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0020(8)
_cell_angle_gamma                90.00
_cell_volume                     1963.93(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6674
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      30.10

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_T_max  0.7197
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'

_exptl_special_details           ?

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17069
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         28.70
_reflns_number_total             5066
_reflns_number_gt                4415
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'ApexII (Bruker, 2011)'
_computing_cell_refinement       'ApexII (Bruker, 2011)'
_computing_data_reduction        'ApexII (Bruker, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 3.2f (Crystal Impact GbR, 1997-2010)'
_computing_publication_material  'publCIF (Westrip, 2010)'


_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0364P)²+1.2000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5066
_refine_ls_number_parameters     307
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.52842(2) 0.47511(3) 0.868051(7) 0.02131(7) Uani 1 1 d . . .
O1 O 0.24603(15) 0.36821(17) 0.81063(5) 0.0300(3) Uani 1 1 d . . .
O1W O 0.3521(2) 0.4367(3) 0.60218(9) 0.0702(6) Uani 1 1 d D . .
H1W1 H 0.382(4) 0.508(4) 0.6242(11) 0.084 Uiso 1 1 d D . .
H2W1 H 0.2601(19) 0.442(4) 0.6018(12) 0.084 Uiso 1 1 d D . .
O2 O 0.38463(13) 0.59961(16) 0.82647(4) 0.0235(3) Uani 1 1 d . . .
O2W O 0.0224(2) 0.1471(3) 0.82704(8) 0.0608(5) Uani 1 1 d D . .
H1W2 H 0.094(3) 0.215(3) 0.8196(11) 0.073 Uiso 1 1 d D . .
H2W2 H 0.022(3) 0.074(3) 0.8034(9) 0.073 Uiso 1 1 d D . .
O3 O -0.45104(15) 0.4174(2) 0.74941(5) 0.0384(4) Uani 1 1 d . . .
O3W O 0.56891(19) 0.1804(3) 0.61367(7) 0.0507(4) Uani 1 1 d D . .
H1W3 H 0.513(3) 0.266(3) 0.6078(11) 0.061 Uiso 1 1 d D . .
H2W3 H 0.652(2) 0.219(4) 0.6121(10) 0.061 Uiso 1 1 d D . .
O4 O -0.32472(14) 0.4646(2) 0.82053(5) 0.0329(3) Uani 1 1 d . . .
O5 O 0.05133(16) 0.4474(2) 0.60335(5) 0.0376(3) Uani 1 1 d . . .
O6 O -0.12829(14) 0.25742(18) 0.61113(4) 0.0303(3) Uani 1 1 d . . .
N1 N 0.39195(16) 0.4434(2) 0.92141(5) 0.0238(3) Uani 1 1 d . . .
N2 N 0.65367(16) 0.3255(2) 0.91306(5) 0.0240(3) Uani 1 1 d . . .
N3 N 0.04699(15) 0.55893(18) 0.75145(5) 0.0198(3) Uani 1 1 d . . .
C1 C 0.2578(2) 0.5083(3) 0.92270(7) 0.0326(4) Uani 1 1 d . . .
H1 H 0.2237 0.5824 0.8979 0.039 Uiso 1 1 calc R . .
C2 C 0.1677(2) 0.4700(3) 0.95929(8) 0.0396(5) Uani 1 1 d . . .
H2 H 0.0736 0.5143 0.9586 0.048 Uiso 1 1 calc R . .
C3 C 0.2197(2) 0.3647(3) 0.99693(8) 0.0391(5) Uani 1 1 d . . .
H3 H 0.1616 0.3385 1.0223 0.047 Uiso 1 1 calc R . .
C4 C 0.3592(2) 0.2988(3) 0.99653(7) 0.0313(4) Uani 1 1 d . . .
H4 H 0.3968 0.2288 1.0218 0.038 Uiso 1 1 calc R . .
C5 C 0.44204(19) 0.3388(2) 0.95792(6) 0.0233(3) Uani 1 1 d . . .
C6 C 0.59134(19) 0.2732(2) 0.95353(6) 0.0236(3) Uani 1 1 d . . .
C7 C 0.6636(2) 0.1688(3) 0.98797(7) 0.0337(4) Uani 1 1 d . . .
H7 H 0.6188 0.1351 1.0157 0.040 Uiso 1 1 calc R . .
C8 C 0.8035(2) 0.1156(3) 0.98037(8) 0.0420(5) Uani 1 1 d . . .
H8 H 0.8544 0.0458 1.0031 0.050 Uiso 1 1 calc R . .
C9 C 0.8671(2) 0.1670(3) 0.93867(8) 0.0413(5) Uani 1 1 d . . .
H9 H 0.9609 0.1312 0.9328 0.050 Uiso 1 1 calc R . .
C10 C 0.7896(2) 0.2722(3) 0.90589(7) 0.0342(4) Uani 1 1 d . . .
H10 H 0.8326 0.3072 0.8779 0.041 Uiso 1 1 calc R . .
C11 C 0.27493(18) 0.5216(2) 0.80697(6) 0.0195(3) Uani 1 1 d . . .
C12 C 0.17224(19) 0.6441(2) 0.77814(6) 0.0232(3) Uani 1 1 d . . .
H12A H 0.1355 0.7275 0.8004 0.028 Uiso 1 1 calc R . .
H12B H 0.2273 0.7061 0.7550 0.028 Uiso 1 1 calc R . .
C13 C 0.05602(18) 0.5141(2) 0.70425(6) 0.0222(3) Uani 1 1 d . . .
H13 H 0.1415 0.5357 0.6891 0.027 Uiso 1 1 calc R . .
C14 C -0.06010(18) 0.4367(2) 0.67834(6) 0.0196(3) Uani 1 1 d . . .
C15 C -0.18847(18) 0.4132(2) 0.70129(6) 0.0217(3) Uani 1 1 d . . .
H15 H -0.2689 0.3639 0.6843 0.026 Uiso 1 1 calc R . .
C16 C -0.19740(18) 0.4632(2) 0.74960(6) 0.0197(3) Uani 1 1 d . . .
C17 C -0.07545(18) 0.5331(2) 0.77441(6) 0.0215(3) Uani 1 1 d . . .
H17 H -0.0782 0.5622 0.8071 0.026 Uiso 1 1 calc R . .
C18 C -0.33884(19) 0.4464(2) 0.77474(6) 0.0220(3) Uani 1 1 d . . .
C19 C -0.04410(18) 0.3761(2) 0.62596(6) 0.0232(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O4 1.9452(13) 1_655 ?
Cu1 O2 1.9451(12) . ?
Cu1 N2 2.0042(14) . ?
Cu1 N1 2.0112(15) . ?
Cu1 O6 2.4353(15) 2_556 ?
O1 C11 1.229(2) . ?
O1W H1W1 0.854(18) . ?
O1W H2W1 0.846(18) . ?
O2 C11 1.264(2) . ?
O2W H1W2 0.878(17) . ?
O2W H2W2 0.865(17) . ?
O3 C18 1.225(2) . ?
O3W H1W3 0.848(17) . ?
O3W H2W3 0.828(17) . ?
O4 C18 1.265(2) . ?
O4 Cu1 1.9452(13) 1_455 ?
O5 C19 1.241(2) . ?
O6 C19 1.255(2) . ?
O6 Cu1 2.4353(15) 2_546 ?
N1 C1 1.335(2) . ?
N1 C5 1.349(2) . ?
N2 C10 1.344(2) . ?
N2 C6 1.350(2) . ?
N3 C17 1.343(2) . ?
N3 C13 1.353(2) . ?
N3 C12 1.479(2) . ?
C1 C2 1.380(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.380(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.477(2) . ?
C6 C7 1.383(2) . ?
C7 C8 1.380(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.383(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.379(3) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.525(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.380(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.388(2) . ?
C14 C19 1.533(2) . ?
C15 C16 1.393(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(2) . ?
C16 C18 1.520(2) . ?
C17 H17 0.9300 . ?

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
O4 Cu1 O2 95.77(5) 1_655 . ?
O4 Cu1 N2 89.72(6) 1_655 . ?
O2 Cu1 N2 172.05(6) . . ?
O4 Cu1 N1 169.29(6) 1_655 . ?
O2 Cu1 N1 93.30(6) . . ?
N2 Cu1 N1 80.70(6) . . ?
O4 Cu1 O6 85.88(6) 1_655 2_556 ?
O2 Cu1 O6 85.28(5) . 2_556 ?
N2 Cu1 O6 100.88(5) . 2_556 ?
N1 Cu1 O6 100.56(5) . 2_556 ?
H1W1 O1W H2W1 104(3) . . ?
C11 O2 Cu1 119.93(11) . . ?
H1W2 O2W H2W2 101(2) . . ?
H1W3 O3W H2W3 105(3) . . ?
C18 O4 Cu1 130.24(12) . 1_455 ?
C19 O6 Cu1 111.99(11) . 2_546 ?
C1 N1 C5 118.45(16) . . ?
C1 N1 Cu1 126.65(13) . . ?
C5 N1 Cu1 114.82(12) . . ?
C10 N2 C6 118.70(16) . . ?
C10 N2 Cu1 126.05(13) . . ?
C6 N2 Cu1 115.23(12) . . ?
C17 N3 C13 121.46(14) . . ?
C17 N3 C12 118.85(14) . . ?
C13 N3 C12 119.65(14) . . ?
N1 C1 C2 122.67(18) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C1 C2 C3 118.80(19) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C2 C3 C4 119.20(18) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 118.87(18) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.97(17) . . ?
N1 C5 C6 114.75(15) . . ?
C4 C5 C6 123.28(16) . . ?
N2 C6 C7 122.08(17) . . ?
N2 C6 C5 114.41(15) . . ?
C7 C6 C5 123.50(16) . . ?
C8 C7 C6 118.74(19) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 C9 119.42(19) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 118.99(19) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
N2 C10 C9 122.06(19) . . ?
N2 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
O1 C11 O2 127.08(16) . . ?
O1 C11 C12 121.41(15) . . ?
O2 C11 C12 111.48(14) . . ?
N3 C12 C11 114.18(14) . . ?
N3 C12 H12A 108.7 . . ?
C11 C12 H12A 108.7 . . ?
N3 C12 H12B 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
N3 C13 C14 120.77(15) . . ?
N3 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C15 118.28(15) . . ?
C13 C14 C19 119.91(15) . . ?
C15 C14 C19 121.80(15) . . ?
C14 C15 C16 120.37(15) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 118.77(15) . . ?
C17 C16 C18 119.92(15) . . ?
C15 C16 C18 121.29(15) . . ?
N3 C17 C16 120.25(15) . . ?
N3 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
O3 C18 O4 127.66(16) . . ?
O3 C18 C16 118.02(15) . . ?
O4 C18 C16 114.32(15) . . ?
O5 C19 O6 127.43(16) . . ?
O5 C19 C14 116.78(16) . . ?
O6 C19 C14 115.78(15) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.058

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?
####################################################################### 
# 
# 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_Cpx4
_database_code_depnum_ccdc_archive 'CCDC 1058286'

# publcif _publ_body_element loop end

_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_publcif_datablock.id            {ccba218f-f590-4fe7-add3-e558618435e4}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H9 Cu N O8, H2 O'
_chemical_formula_sum            'C9 H11 Cu N O9'
_chemical_formula_weight         340.73

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1654(9)
_cell_length_b                   7.6594(9)
_cell_length_c                   11.4555(14)
_cell_angle_alpha                77.713(2)
_cell_angle_beta                 75.932(2)
_cell_angle_gamma                74.525(2)
_cell_volume                     580.34(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3580
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      28.37

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             346
_exptl_absorpt_coefficient_mu    1.931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5951
_exptl_absorpt_correction_T_max  0.7605
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'

_exptl_special_details           ?

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4395
_diffrn_reflns_av_R_equivalents  0.0137
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         26.36
_reflns_number_total             2370
_reflns_number_gt                2257
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'ApexII (Bruker, 2011)'
_computing_cell_refinement       'ApexII (Bruker, 2011)'
_computing_data_reduction        'ApexII (Bruker, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 3.2f (Crystal Impact GbR, 1997-2010)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0381P)²+1.5702P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2370
_refine_ls_number_parameters     199
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0863
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.51064(5) 0.79425(4) 0.44813(3) 0.01258(12) Uani 1 1 d . . .
O1 O -0.7076(3) 0.9259(3) 0.56619(17) 0.0144(4) Uani 1 1 d . . .
O1W O -0.3200(3) 0.6698(3) 0.32351(18) 0.0188(4) Uani 1 1 d D . .
H1W1 H -0.304(6) 0.557(3) 0.330(3) 0.023 Uiso 1 1 d D . .
H2W1 H -0.312(5) 0.716(4) 0.2490(19) 0.023 Uiso 1 1 d D . .
O2W O -0.6190(3) 0.9964(3) 0.32477(17) 0.0137(4) Uani 1 1 d D . .
H1W2 H -0.552(4) 1.017(4) 0.2538(19) 0.016 Uiso 1 1 d D . .
H2W2 H -0.650(5) 1.092(3) 0.355(3) 0.016 Uiso 1 1 d D . .
O2 O -0.7678(4) 0.6820(3) 0.7061(2) 0.0286(5) Uani 1 1 d . . .
O3 O -1.2422(3) 0.7980(3) 1.09417(18) 0.0240(5) Uani 1 1 d . . .
O3W O 0.3290(11) 0.5053(7) 0.9540(5) 0.116(2) Uani 1 1 d D . .
H1W3 H 0.197(6) 0.516(13) 1.004(6) 0.139 Uiso 1 1 d D . .
H2W3 H 0.293(11) 0.585(10) 0.887(5) 0.139 Uiso 1 1 d D . .
O4 O -1.4184(3) 1.0841(3) 1.10780(19) 0.0247(5) Uani 1 1 d . . .
O5 O -1.2904(3) 1.3955(3) 0.55241(19) 0.0205(4) Uani 1 1 d . . .
O6 O -1.3377(3) 1.6900(3) 0.56941(18) 0.0166(4) Uani 1 1 d . . .
N1 N -1.1452(3) 1.2746(3) 0.7640(2) 0.0129(5) Uani 1 1 d . . .
C1 C -0.7977(4) 0.8472(4) 0.6653(2) 0.0147(5) Uani 1 1 d . . .
C2 C -0.9568(4) 0.9756(4) 0.7402(2) 0.0120(5) Uani 1 1 d . . .
C3 C -1.0077(4) 1.1598(4) 0.6951(2) 0.0125(5) Uani 1 1 d . . .
H3 H -0.9472 1.2050 0.6172 0.015 Uiso 1 1 calc R . .
C4 C -1.2392(4) 1.2130(4) 0.8763(2) 0.0145(5) Uani 1 1 d . . .
H4 H -1.3352 1.2946 0.9212 0.017 Uiso 1 1 calc R . .
C5 C -1.1937(4) 1.0294(4) 0.9246(2) 0.0135(5) Uani 1 1 d . . .
C6 C -1.0506(4) 0.9093(4) 0.8559(2) 0.0138(5) Uani 1 1 d . . .
H6 H -1.0178 0.7851 0.8873 0.017 Uiso 1 1 calc R . .
C7 C -1.2951(4) 0.9653(4) 1.0533(2) 0.0158(6) Uani 1 1 d . . .
C8 C -1.1901(4) 1.4737(4) 0.7165(3) 0.0157(5) Uani 1 1 d . . .
H8A H -1.0692 1.5175 0.6972 0.019 Uiso 1 1 calc R . .
H8B H -1.2810 1.5382 0.7796 0.019 Uiso 1 1 calc R . .
C9 C -1.2809(4) 1.5189(4) 0.6024(2) 0.0126(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.9315(19) . ?
Cu1 O1W 1.936(2) . ?
Cu1 O6 1.9851(19) 1_645 ?
Cu1 O2W 1.9893(19) . ?
Cu1 O5 2.293(2) 2_376 ?
O1 C1 1.277(3) . ?
O1W H1W1 0.831(18) . ?
O1W H2W1 0.846(18) . ?
O2W H1W2 0.844(18) . ?
O2W H2W2 0.834(18) . ?
O2 C1 1.232(4) . ?
O3 C7 1.256(4) . ?
O3W H1W3 0.97(2) . ?
O3W H2W3 0.91(2) . ?
O4 C7 1.243(4) . ?
O5 C9 1.229(3) . ?
O5 Cu1 2.293(2) 2_376 ?
O6 C9 1.267(3) . ?
O6 Cu1 1.9851(19) 1_465 ?
N1 C4 1.349(4) . ?
N1 C3 1.350(3) . ?
N1 C8 1.481(3) . ?
C1 C2 1.512(4) . ?
C2 C3 1.377(4) . ?
C2 C6 1.390(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(4) . ?
C5 C7 1.518(4) . ?
C6 H6 0.9300 . ?
C8 C9 1.534(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1W 177.15(8) . . ?
O1 Cu1 O6 90.62(8) . 1_645 ?
O1W Cu1 O6 92.15(9) . 1_645 ?
O1 Cu1 O2W 85.14(8) . . ?
O1W Cu1 O2W 92.09(8) . . ?
O6 Cu1 O2W 151.62(9) 1_645 . ?
O1 Cu1 O5 92.39(8) . 2_376 ?
O1W Cu1 O5 87.21(9) . 2_376 ?
O6 Cu1 O5 111.98(8) 1_645 2_376 ?
O2W Cu1 O5 96.24(8) . 2_376 ?
C1 O1 Cu1 123.50(18) . . ?
Cu1 O1W H1W1 119(2) . . ?
Cu1 O1W H2W1 121(2) . . ?
H1W1 O1W H2W1 108(3) . . ?
Cu1 O2W H1W2 121(2) . . ?
Cu1 O2W H2W2 107(2) . . ?
H1W2 O2W H2W2 108(3) . . ?
H1W3 O3W H2W3 97(4) . . ?
C9 O5 Cu1 142.6(2) . 2_376 ?
C9 O6 Cu1 122.60(18) . 1_465 ?
C4 N1 C3 121.6(2) . . ?
C4 N1 C8 119.2(2) . . ?
C3 N1 C8 119.2(2) . . ?
O2 C1 O1 127.5(3) . . ?
O2 C1 C2 117.7(2) . . ?
O1 C1 C2 114.8(2) . . ?
C3 C2 C6 119.4(2) . . ?
C3 C2 C1 120.3(2) . . ?
C6 C2 C1 120.3(2) . . ?
N1 C3 C2 120.0(2) . . ?
N1 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
N1 C4 C5 120.3(2) . . ?
N1 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 119.0(2) . . ?
C4 C5 C7 119.2(2) . . ?
C6 C5 C7 121.7(2) . . ?
C5 C6 C2 119.7(3) . . ?
C5 C6 H6 120.2 . . ?
C2 C6 H6 120.2 . . ?
O4 C7 O3 126.9(3) . . ?
O4 C7 C5 116.7(3) . . ?
O3 C7 C5 116.3(2) . . ?
N1 C8 C9 112.7(2) . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
O5 C9 O6 127.0(3) . . ?
O5 C9 C8 120.5(2) . . ?
O6 C9 C8 112.5(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.097

# start Validation Reply Form
_vrf_PLAT420                     
;
PROBLEM: Test for D-H without acceptor
Response: One B alert left is due to the lack of acceptor for O3W - H1W3, this
is probably imposed by the geometry of the other O-H donor (O3W -- H2W3) which
is involved in the hydrogen bonding.
;

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?
####################################################################### 
# 
# 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_Cpx5
_database_code_depnum_ccdc_archive 'CCDC 1058287'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C21 H13 Cu N3 O7), 6(H2 O), 2(H O0.50)'
_chemical_formula_sum            'C42 H40 Cu2 N6 O21'
_chemical_formula_weight         1091.88

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.6748(17)
_cell_length_b                   11.213(2)
_cell_length_c                   12.653(3)
_cell_angle_alpha                112.47(3)
_cell_angle_beta                 93.34(3)
_cell_angle_gamma                99.01(3)
_cell_volume                     1113.8(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3216
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      24.74

_exptl_crystal_description       block
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_F_000             560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.048
_shelx_estimated_absorpt_T_min   0.755
_shelx_estimated_absorpt_T_max   0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7035
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.756
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             3763
_reflns_number_gt                3414
_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       'ApexII (Bruker, 2011)'
_computing_cell_refinement       'ApexII (Bruker, 2011)'
_computing_data_reduction        'ApexII (Bruker, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 3.2f (Crystal Impact GbR, 1997-2010)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0637P)²+8.5537P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3763
_refine_ls_number_parameters     341
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1734
_refine_ls_wR_factor_gt          0.1702
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.30737(7) 0.10495(6) 0.26886(6) 0.0131(2) Uani 1 1 d D . . . .
O1 O 0.4275(4) 0.1206(4) 0.1456(3) 0.0182(8) Uani 1 1 d . . . . .
O1WA O 0.1317(5) -0.0566(4) 0.1265(4) 0.0089(9) Uani 0.837(7) 1 d D . P A 1
O1WB O 0.0688(15) -0.0228(17) 0.2033(18) 0.0089(9) Uani 0.163(7) 1 d D . P A 2
O2 O 0.6331(5) 0.2522(4) 0.2758(4) 0.0244(9) Uani 1 1 d . . . . .
O2W O -0.2051(5) -0.0894(5) 0.0628(4) 0.0289(10) Uani 1 1 d D . . . .
H1W2 H -0.248(8) -0.102(8) 0.007(4) 0.035 Uiso 1 1 d D U . . .
H2W2 H -0.134(6) -0.059(7) 0.105(5) 0.035 Uiso 1 1 d D U . . .
O3 O 0.8271(4) 0.6670(4) 0.0816(4) 0.0206(9) Uani 1 1 d . . . . .
O3W O 0.4444(5) 0.4350(5) 0.0833(5) 0.0348(11) Uani 1 1 d D . . . .
H1W3 H 0.391(8) 0.420(8) 0.030(4) 0.042 Uiso 1 1 d D U . . .
H2W3 H 0.428(9) 0.436(9) 0.140(3) 0.042 Uiso 1 1 d D U . . .
O4 O 1.0815(5) 0.7202(4) 0.1553(4) 0.0254(10) Uani 1 1 d . . . . .
O4W O 0.8481(11) 0.4890(6) 0.4373(7) 0.093(3) Uani 1 1 d . . . . .
H1W4 H 0.8150 0.4197 0.3768 0.112 Uiso 1 1 d R U . . .
H2W4 H 0.9213 0.5367 0.4213 0.112 Uiso 1 1 d R U . . .
O5 O 1.1670(5) 0.2194(4) 0.2559(4) 0.0235(9) Uani 1 1 d . . . . .
O5W O 1.4619(15) 0.4469(13) 0.5031(11) 0.061(3) Uani 0.5 1 d . . P B -1
H1W5 H 1.4708 0.4848 0.4564 0.073 Uiso 0.5 1 d R U P B -1
H2W5 H 1.3750 0.4568 0.5299 0.073 Uiso 0.5 1 d R U P B -1
O6 O 1.3257(5) 0.4081(4) 0.2780(4) 0.0331(11) Uani 1 1 d . . . . .
N1 N 0.2381(6) 0.1207(5) 0.4227(4) 0.0224(11) Uani 1 1 d . . . . .
N2 N 0.4020(5) -0.0414(5) 0.2868(4) 0.0154(10) Uani 1 1 d . . . . .
N3 N 0.7917(5) 0.3067(4) 0.1121(4) 0.0125(9) Uani 1 1 d . . . . .
C1 C 0.1648(8) 0.2079(7) 0.4931(5) 0.0293(15) Uani 1 1 d . . . . .
H1 H 0.1455 0.2797 0.4755 0.035 Uiso 1 1 calc R U . . .
C2 C 0.1142(8) 0.1972(7) 0.5943(6) 0.0331(16) Uani 1 1 d . . . . .
H2 H 0.0631 0.2620 0.6439 0.040 Uiso 1 1 calc R U . . .
C3 C 0.1390(8) 0.0930(7) 0.6208(6) 0.0315(15) Uani 1 1 d . . . . .
H3 H 0.1044 0.0855 0.6882 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2159(7) -0.0026(6) 0.5475(5) 0.0259(14) Uani 1 1 d . . . . .
C5 C 0.2470(8) -0.1156(7) 0.5657(6) 0.0308(15) Uani 1 1 d . . . . .
H5 H 0.2144 -0.1297 0.6311 0.037 Uiso 1 1 calc R U . . .
C6 C 0.3228(8) -0.2035(7) 0.4906(6) 0.0304(15) Uani 1 1 d . . . . .
H6 H 0.3395 -0.2787 0.5038 0.036 Uiso 1 1 calc R U . . .
C7 C 0.3779(7) -0.1847(6) 0.3920(5) 0.0232(13) Uani 1 1 d . . . . .
C8 C 0.4615(7) -0.2682(6) 0.3123(6) 0.0282(14) Uani 1 1 d . . . . .
H8 H 0.4797 -0.3467 0.3187 0.034 Uiso 1 1 calc R U . . .
C9 C 0.5152(7) -0.2355(6) 0.2270(6) 0.0262(14) Uani 1 1 d . . . . .
H9 H 0.5742 -0.2897 0.1744 0.031 Uiso 1 1 calc R U . . .
C10 C 0.4840(6) -0.1220(5) 0.2164(5) 0.0174(12) Uani 1 1 d . . . . .
H10 H 0.5233 -0.1011 0.1558 0.021 Uiso 1 1 calc R U . . .
C11 C 0.3504(7) -0.0723(6) 0.3734(5) 0.0207(12) Uani 1 1 d . . . . .
C12 C 0.2660(7) 0.0163(6) 0.4502(5) 0.0211(13) Uani 1 1 d . . . . .
C13 C 0.5652(6) 0.1967(5) 0.1771(5) 0.0161(12) Uani 1 1 d . . . . .
C14 C 0.6393(6) 0.2097(5) 0.0746(5) 0.0141(11) Uani 1 1 d . . . . .
H14A H 0.6579 0.1228 0.0227 0.017 Uiso 1 1 calc R U . . .
H14B H 0.5653 0.2381 0.0307 0.017 Uiso 1 1 calc R U . . .
C15 C 0.7989(6) 0.4239(5) 0.1021(4) 0.0123(11) Uani 1 1 d . . . . .
H15 H 0.7080 0.4429 0.0710 0.015 Uiso 1 1 calc R U . . .
C16 C 0.9381(6) 0.5153(5) 0.1372(4) 0.0118(11) Uani 1 1 d . . . . .
C17 C 1.0686(6) 0.4851(5) 0.1858(5) 0.0147(11) Uani 1 1 d . . . . .
H17 H 1.1650 0.5472 0.2117 0.018 Uiso 1 1 calc R U . . .
C18 C 1.0580(6) 0.3654(5) 0.1962(5) 0.0148(11) Uani 1 1 d . . . . .
C19 C 0.9172(6) 0.2763(5) 0.1573(5) 0.0139(11) Uani 1 1 d . . . . .
H19 H 0.9087 0.1932 0.1623 0.017 Uiso 1 1 calc R U . . .
C20 C 1.1976(7) 0.3309(6) 0.2487(5) 0.0169(12) Uani 1 1 d . . . . .
C21 C 0.9493(6) 0.6453(5) 0.1233(5) 0.0140(11) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O5 1.945(4) 1_455 ?
Cu1 O1 1.973(4) . ?
Cu1 N1 2.021(5) . ?
Cu1 N2 2.025(5) . ?
Cu1 O1WB 2.233(10) . ?
Cu1 O1WA 2.274(4) . ?
O1 C13 1.296(7) . ?
O2 C13 1.224(7) . ?
O2W H1W2 0.74(2) . ?
O2W H2W2 0.74(2) . ?
O3 C21 1.255(7) . ?
O3W H1W3 0.74(2) . ?
O3W H2W3 0.74(2) . ?
O4 C21 1.253(7) . ?
O4W H1W4 0.8499 . ?
O4W H2W4 0.8499 . ?
O5 C20 1.275(7) . ?
O5 Cu1 1.945(4) 1_655 ?
O5W H1W5 0.8500 . ?
O5W H2W5 0.8499 . ?
O6 C20 1.236(7) . ?
N1 C1 1.322(8) . ?
N1 C12 1.394(8) . ?
N2 C10 1.333(7) . ?
N2 C11 1.350(7) . ?
N3 C19 1.350(7) . ?
N3 C15 1.359(7) . ?
N3 C14 1.496(7) . ?
C1 C2 1.419(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.375(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.411(9) . ?
C3 H3 0.9500 . ?
C4 C12 1.408(9) . ?
C4 C5 1.433(9) . ?
C5 C6 1.366(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.438(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.413(9) . ?
C7 C11 1.418(8) . ?
C8 C9 1.351(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.395(8) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.429(8) . ?
C13 C14 1.526(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.382(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.404(7) . ?
C16 C21 1.522(7) . ?
C17 C18 1.388(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(8) . ?
C18 C20 1.520(7) . ?
C19 H19 0.9500 . ?

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
O5 Cu1 O1 94.31(16) 1_455 . ?
O5 Cu1 N1 90.26(18) 1_455 . ?
O1 Cu1 N1 164.41(19) . . ?
O5 Cu1 N2 165.29(17) 1_455 . ?
O1 Cu1 N2 96.80(17) . . ?
N1 Cu1 N2 81.56(19) . . ?
O5 Cu1 O1WB 74.0(5) 1_455 . ?
O1 Cu1 O1WB 113.6(6) . . ?
N1 Cu1 O1WB 82.0(6) . . ?
N2 Cu1 O1WB 92.7(5) . . ?
O5 Cu1 O1WA 84.62(17) 1_455 . ?
O1 Cu1 O1WA 86.76(16) . . ?
N1 Cu1 O1WA 108.53(18) . . ?
N2 Cu1 O1WA 86.41(17) . . ?
C13 O1 Cu1 117.2(4) . . ?
H1W2 O2W H2W2 149(8) . . ?
H1W3 O3W H2W3 131(7) . . ?
H1W4 O4W H2W4 107.7 . . ?
C20 O5 Cu1 130.1(4) . 1_655 ?
H1W5 O5W H2W5 107.7 . . ?
C1 N1 C12 118.2(5) . . ?
C1 N1 Cu1 129.9(4) . . ?
C12 N1 Cu1 111.7(4) . . ?
C10 N2 C11 116.9(5) . . ?
C10 N2 Cu1 129.5(4) . . ?
C11 N2 Cu1 112.6(4) . . ?
C19 N3 C15 121.9(5) . . ?
C19 N3 C14 118.9(4) . . ?
C15 N3 C14 119.2(4) . . ?
N1 C1 C2 121.9(6) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 120.0(6) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.9(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C12 C4 C3 116.8(6) . . ?
C12 C4 C5 118.4(6) . . ?
C3 C4 C5 124.8(6) . . ?
C6 C5 C4 121.1(6) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 121.4(6) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C11 116.6(6) . . ?
C8 C7 C6 125.1(6) . . ?
C11 C7 C6 118.3(6) . . ?
C9 C8 C7 119.4(6) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.9(6) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N2 C10 C9 123.5(5) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N2 C11 C7 123.7(5) . . ?
N2 C11 C12 116.6(5) . . ?
C7 C11 C12 119.7(5) . . ?
N1 C12 C4 123.1(6) . . ?
N1 C12 C11 115.9(5) . . ?
C4 C12 C11 121.0(5) . . ?
O2 C13 O1 126.1(5) . . ?
O2 C13 C14 122.0(5) . . ?
O1 C13 C14 111.9(5) . . ?
N3 C14 C13 111.8(4) . . ?
N3 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
N3 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
N3 C15 C16 120.1(5) . . ?
N3 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 118.3(5) . . ?
C15 C16 C21 120.7(5) . . ?
C17 C16 C21 121.0(5) . . ?
C18 C17 C16 120.6(5) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C19 C18 C17 118.8(5) . . ?
C19 C18 C20 119.8(5) . . ?
C17 C18 C20 121.4(5) . . ?
N3 C19 C18 120.3(5) . . ?
N3 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
O6 C20 O5 126.7(5) . . ?
O6 C20 C18 119.6(5) . . ?
O5 C20 C18 113.7(5) . . ?
O4 C21 O3 126.6(5) . . ?
O4 C21 C16 115.8(5) . . ?
O3 C21 C16 117.6(5) . . ?

_refine_diff_density_max         1.371
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.134


# start Validation Reply Form
_vrf_PLAT420                     
;
PROBLEM: Test for D-H without acceptor
Response: One B alert left is due to the lack of acceptor for O4W - H2W4, this
is probably imposed by the geometry of the other O-H donor (O4W -- H1W4) which
is involved in the hydrogen bonding. The crystal is weakly diffracted at the
high resolution. A resolution cut-off to 0.85 \%A is thus applied.
;

_shelxl_version_number           2013-2

