# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CP-4-Cd

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-poly[diaquabis-μ-{N, N-bis(3-pyridyl)butanediamido}cadmium(II)
 perchlorate dihydrate]  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H40 Cu N8 O6, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C32 H44 Cd Cl2 N8 O16'
_chemical_formula_weight         980.05

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'
Cd Cd -0.8075 1.2024 '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'
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'
H H 0.0000 0.0000 '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                   9.0727(2)
_cell_length_b                   9.0760(2)
_cell_length_c                   15.3648(3)
_cell_angle_alpha                106.099(2)
_cell_angle_beta                 90.817(2)
_cell_angle_gamma                93.146(2)
_cell_volume                     1213.17(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    11214
_cell_measurement_theta_min      3.5011
_cell_measurement_theta_max      29.0248

_exptl_crystal_description       plate
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             502
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_min  0.97793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_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  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.1049
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            19787
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4260
_reflns_number_gt                3982
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction,2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  PLATON(Spek,2009)

_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)+(0.1115P)²+0.3356P] 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         4260
_refine_ls_number_parameters     255
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1728
_refine_ls_wR_factor_gt          0.1679
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001

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
C C1 0.6175(6) 0.8336(6) 0.9833(3) 0.0429(11) Uani d . 1 . .
H H1 0.5799 0.8609 1.0412 0.052 Uiso calc R 1 . .
C C2 0.6928(7) 0.9448(6) 0.9531(4) 0.0518(13) Uani d . 1 . .
H H2 0.7053 1.0451 0.9901 0.062 Uiso calc R 1 . .
C C3 0.7496(6) 0.9059(6) 0.8673(4) 0.0481(12) Uani d . 1 . .
H H3 0.8029 0.9786 0.8461 0.058 Uiso calc R 1 . .
C C4 0.7255(5) 0.7579(5) 0.8144(3) 0.0369(10) Uani d . 1 . .
C C5 0.6490(5) 0.6535(5) 0.8500(3) 0.0367(10) Uani d . 1 . .
H H5 0.6334 0.5529 0.8139 0.044 Uiso calc R 1 . .
C C6 0.8087(6) 0.7872(6) 0.6671(4) 0.0467(12) Uani d . 1 . .
C C7 0.8759(7) 0.6951(6) 0.5807(4) 0.0544(14) Uani d . 1 . .
H H7A 0.9708 0.6626 0.5956 0.065 Uiso calc R 1 . .
H H7B 0.8124 0.6034 0.5544 0.065 Uiso calc R 1 . .
C C8 0.8970(10) 0.7839(7) 0.5112(5) 0.081(2) Uani d . 1 . .
H H8A 0.8017 0.8151 0.4958 0.097 Uiso calc R 1 . .
H H8B 0.9591 0.8763 0.538 0.097 Uiso calc R 1 . .
C C9 0.9658(7) 0.6937(6) 0.4255(4) 0.0532(13) Uani d . 1 . .
H H9A 1.065 0.6707 0.4396 0.064 Uiso calc R 1 . .
H H9B 0.9087 0.5971 0.401 0.064 Uiso calc R 1 . .
C C10 0.9724(9) 0.7808(7) 0.3552(5) 0.077(2) Uani d . 1 . .
H H10A 0.8726 0.8008 0.3403 0.092 Uiso calc R 1 . .
H H10B 1.0256 0.8793 0.3812 0.092 Uiso calc R 1 . .
C C11 1.0449(6) 0.7001(5) 0.2691(4) 0.0452(12) Uani d . 1 . .
C C12 1.0742(5) 0.7100(5) 0.1115(3) 0.0375(10) Uani d . 1 . .
C C13 0.9950(6) 0.7261(6) 0.0376(4) 0.0499(12) Uani d . 1 . .
H H13 0.9021 0.7656 0.0444 0.06 Uiso calc R 1 . .
C C14 1.0575(6) 0.6817(7) -0.0476(4) 0.0552(14) Uani d . 1 . .
H H14 1.0067 0.6906 -0.0987 0.066 Uiso calc R 1 . .
C C15 0.1939(6) 0.6253(6) 0.9455(3) 0.0445(11) Uani d . 1 . .
H H15 0.2346 0.5948 0.8885 0.053 Uiso calc R 1 . .
C C16 0.2133(5) 0.6566(6) 1.0982(3) 0.0391(10) Uani d . 1 . .
H H16 0.2694 0.6515 1.1483 0.047 Uiso calc R 1 . .
Cd Cd1 0.5 0.5 1.0 0.0328(2) Uani d S 1 . .
Cl Cl1 0.7604(3) 0.1224(3) 0.24172(13) 0.1004(8) Uani d . 1 . .
O O4 0.6462(10) 0.1520(11) 0.1888(7) 0.149(3) Uiso d . 1 . .
O O6 0.8829(16) 0.0638(17) 0.1934(10) 0.112(4) Uiso d P 0.5 . .
O O5 0.781(3) 0.146(3) 0.3307(16) 0.160(8) Uiso d P 0.5 . .
N N1 0.5963(4) 0.6887(4) 0.9329(3) 0.0351(8) Uani d . 1 . .
N N2 0.7824(5) 0.7028(5) 0.7272(3) 0.0514(11) Uani d . 1 . .
H H2A 0.8023 0.6077 0.7103 0.062 Uiso calc R 1 . .
N N3 1.0138(5) 0.7554(5) 0.1976(3) 0.0499(11) Uani d . 1 . .
H H3A 0.9509 0.8252 0.2061 0.06 Uiso calc R 1 . .
N N4 0.2715(4) 0.6118(4) 1.0163(3) 0.0366(8) Uani d . 1 . .
O O1 0.7829(5) 0.9203(4) 0.6822(3) 0.0621(11) Uani d . 1 . .
O O2 1.1265(5) 0.5978(5) 0.2640(3) 0.0603(11) Uani d . 1 . .
O O1W 0.5793(4) 0.6557(4) 1.1442(2) 0.0494(8) Uani d . 1 . .
H H1WA 0.5577 0.6096 1.1849 0.074 Uiso d R 1 . .
H H1WB 0.5363 0.7411 1.1564 0.074 Uiso d R 1 . .
O O2W 0.4507(12) 0.9028(13) 0.2409(8) 0.179(4) Uiso d G 1 . .
O O6A 0.7711(19) -0.046(2) 0.1903(12) 0.136(5) Uiso d P 0.5 . .
O O3 0.849(2) 0.294(2) 0.2634(13) 0.305(9) Uiso d . 1 . .
O O5A 0.708(3) 0.094(3) 0.3187(17) 0.164(8) Uiso d P 0.5 . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.330(6) ?
C1 C2 . 1.375(8) ?
C1 H1 . 0.93 ?
C2 C3 . 1.381(7) ?
C2 H2 . 0.93 ?
C3 C4 . 1.368(7) ?
C3 H3 . 0.93 ?
C4 C5 . 1.380(6) ?
C4 N2 . 1.410(6) ?
C5 N1 . 1.326(6) ?
C5 H5 . 0.93 ?
C6 O1 . 1.202(6) ?
C6 N2 . 1.369(7) ?
C6 C7 . 1.515(7) ?
C7 C8 . 1.515(8) ?
C7 H7A . 0.97 ?
C7 H7B . 0.97 ?
C8 C9 . 1.509(7) ?
C8 H8A . 0.97 ?
C8 H8B . 0.97 ?
C9 C10 . 1.505(8) ?
C9 H9A . 0.97 ?
C9 H9B . 0.97 ?
C10 C11 . 1.503(7) ?
C10 H10A . 0.97 ?
C10 H10B . 0.97 ?
C11 O2 . 1.205(6) ?
C11 N3 . 1.361(7) ?
C12 C16 1_654 1.375(6) ?
C12 C13 . 1.381(7) ?
C12 N3 . 1.401(6) ?
C13 C14 . 1.396(8) ?
C13 H13 . 0.93 ?
C14 C15 1_654 1.359(8) ?
C14 H14 . 0.93 ?
C15 N4 . 1.326(6) ?
C15 C14 1_456 1.359(8) ?
C15 H15 . 0.93 ?
C16 N4 . 1.336(6) ?
C16 C12 1_456 1.375(6) ?
C16 H16 . 0.93 ?
Cd1 N4 . 2.344(4) ?
Cd1 N4 2_667 2.344(4) ?
Cd1 O1W 2_667 2.352(3) ?
Cd1 O1W . 2.352(3) ?
Cd1 N1 2_667 2.367(4) ?
Cd1 N1 . 2.367(4) ?
Cl1 O5 . 1.33(2) ?
Cl1 O5A . 1.37(2) ?
Cl1 O4 . 1.391(10) ?
Cl1 O6 . 1.393(14) ?
Cl1 O6A . 1.523(18) ?
Cl1 O3 . 1.66(2) ?
N2 H2A . 0.86 ?
N3 H3A . 0.86 ?
O1W H1WA . 0.8621 ?
O1W H1WB . 0.8618 ?

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 C1 C2 . . 122.6(4) ?
N1 C1 H1 . . 118.7 ?
C2 C1 H1 . . 118.7 ?
C1 C2 C3 . . 119.4(5) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
C4 C3 C2 . . 118.4(5) ?
C4 C3 H3 . . 120.8 ?
C2 C3 H3 . . 120.8 ?
C3 C4 C5 . . 118.5(4) ?
C3 C4 N2 . . 123.7(4) ?
C5 C4 N2 . . 117.7(4) ?
N1 C5 C4 . . 123.7(4) ?
N1 C5 H5 . . 118.1 ?
C4 C5 H5 . . 118.1 ?
O1 C6 N2 . . 123.4(5) ?
O1 C6 C7 . . 124.0(5) ?
N2 C6 C7 . . 112.6(4) ?
C8 C7 C6 . . 113.2(5) ?
C8 C7 H7A . . 108.9 ?
C6 C7 H7A . . 108.9 ?
C8 C7 H7B . . 108.9 ?
C6 C7 H7B . . 108.9 ?
H7A C7 H7B . . 107.7 ?
C9 C8 C7 . . 113.6(5) ?
C9 C8 H8A . . 108.9 ?
C7 C8 H8A . . 108.9 ?
C9 C8 H8B . . 108.9 ?
C7 C8 H8B . . 108.9 ?
H8A C8 H8B . . 107.7 ?
C10 C9 C8 . . 111.8(5) ?
C10 C9 H9A . . 109.3 ?
C8 C9 H9A . . 109.3 ?
C10 C9 H9B . . 109.3 ?
C8 C9 H9B . . 109.3 ?
H9A C9 H9B . . 107.9 ?
C11 C10 C9 . . 114.7(5) ?
C11 C10 H10A . . 108.6 ?
C9 C10 H10A . . 108.6 ?
C11 C10 H10B . . 108.6 ?
C9 C10 H10B . . 108.6 ?
H10A C10 H10B . . 107.6 ?
O2 C11 N3 . . 122.7(5) ?
O2 C11 C10 . . 123.2(5) ?
N3 C11 C10 . . 114.1(5) ?
C16 C12 C13 1_654 . 118.3(5) ?
C16 C12 N3 1_654 . 122.4(4) ?
C13 C12 N3 . . 119.3(4) ?
C12 C13 C14 . . 118.5(4) ?
C12 C13 H13 . . 120.7 ?
C14 C13 H13 . . 120.7 ?
C15 C14 C13 1_654 . 118.9(5) ?
C15 C14 H14 1_654 . 120.5 ?
C13 C14 H14 . . 120.5 ?
N4 C15 C14 . 1_456 122.9(5) ?
N4 C15 H15 . . 118.6 ?
C14 C15 H15 1_456 . 118.6 ?
N4 C16 C12 . 1_456 122.9(4) ?
N4 C16 H16 . . 118.6 ?
C12 C16 H16 1_456 . 118.6 ?
N4 Cd1 N4 . 2_667 179.9990(10) ?
N4 Cd1 O1W . 2_667 89.58(13) ?
N4 Cd1 O1W 2_667 2_667 90.41(13) ?
N4 Cd1 O1W . . 90.42(13) ?
N4 Cd1 O1W 2_667 . 89.59(13) ?
O1W Cd1 O1W 2_667 . 180.00(18) ?
N4 Cd1 N1 . 2_667 89.49(13) ?
N4 Cd1 N1 2_667 2_667 90.51(12) ?
O1W Cd1 N1 2_667 2_667 90.38(13) ?
O1W Cd1 N1 . 2_667 89.62(13) ?
N4 Cd1 N1 . . 90.51(12) ?
N4 Cd1 N1 2_667 . 89.49(13) ?
O1W Cd1 N1 2_667 . 89.62(13) ?
O1W Cd1 N1 . . 90.38(13) ?
N1 Cd1 N1 2_667 . 179.9990(10) ?
O5 Cl1 O4 . . 133.3(11) ?
O5A Cl1 O4 . . 110.8(11) ?
O5 Cl1 O6 . . 112.2(12) ?
O5A Cl1 O6 . . 128.1(12) ?
O4 Cl1 O6 . . 114.4(7) ?
O5 Cl1 O6A . . 111.6(12) ?
O5A Cl1 O6A . . 95.2(12) ?
O4 Cl1 O6A . . 96.9(8) ?
O5 Cl1 O3 . . 82.5(12) ?
O5A Cl1 O3 . . 111.7(12) ?
O4 Cl1 O3 . . 96.7(8) ?
O6 Cl1 O3 . . 87.0(9) ?
O6A Cl1 O3 . . 142.9(9) ?
C5 N1 C1 . . 117.5(4) ?
C5 N1 Cd1 . . 122.6(3) ?
C1 N1 Cd1 . . 119.4(3) ?
C6 N2 C4 . . 125.8(4) ?
C6 N2 H2A . . 117.1 ?
C4 N2 H2A . . 117.1 ?
C11 N3 C12 . . 126.4(4) ?
C11 N3 H3A . . 116.8 ?
C12 N3 H3A . . 116.8 ?
C15 N4 C16 . . 118.5(4) ?
C15 N4 Cd1 . . 121.7(3) ?
C16 N4 Cd1 . . 119.8(3) ?
Cd1 O1W H1WA . . 110.1 ?
Cd1 O1W H1WB . . 109.9 ?
H1WA O1W H1WB . . 108.8 ?


_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.969
_refine_diff_density_min         -1.010

_vrf_PLAT601_I                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 241 Ang3
RESPONSE: The solvent-accessible void (241 A3) can be due to loss of 
ethanol solvent from which crystals were grown. However, the residual 
electron density in the final refinement is very close to 1 e/A3. 
Thus, there was no unaccounted electron density left in the structure 
and no further treatment to the data (SQUEEZE for example) was done.
;
_database_code_depnum_ccdc_archive 'CCDC 963405'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CP-3-Cu

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-poly[diaquabis-μ-{N, N-bis(3-pyridyl)butanediamido}copper (II) 
perchlorate dihydrate]
 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H40 Cu N8 O6, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C32 H44 Cl2 Cu N8 O16'
_chemical_formula_weight         931.19

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21212'
_symmetry_space_group_name_Hall  '-P 2 2ab'

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

_cell_length_a                   11.3423(3)
_cell_length_b                   19.2826(7)
_cell_length_c                   9.5549(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2089.74(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6996
_cell_measurement_theta_min      3.4913
_cell_measurement_theta_max      29.1146

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             966
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_min  0.82798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_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  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.1049
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15254
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.50
_diffrn_reflns_theta_max         24.98
_reflns_number_total             3675
_reflns_number_gt                2989
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction,2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  PLATON(Spek,2009)

_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)+(0.0967P)²+2.9459P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_number_reflns         3675
_refine_ls_number_parameters     270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0679
_refine_ls_wR_factor_ref         0.1867
_refine_ls_wR_factor_gt          0.1726
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_restrained_S_all      0.972
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.004


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
C C1 0.6117(5) 0.3808(3) 0.3618(6) 0.0366(14) Uani d . 1 . .
H H1 0.6728 0.3893 0.4244 0.044 Uiso calc R 1 . .
C C2 0.6141(6) 0.3228(4) 0.2810(6) 0.0451(17) Uani d . 1 . .
H H2 0.6758 0.2914 0.2904 0.054 Uiso calc R 1 . .
C C3 0.5256(6) 0.3100(3) 0.1850(6) 0.0401(16) Uani d . 1 . .
H H3 0.5255 0.2696 0.1317 0.048 Uiso calc R 1 . .
C C4 0.4368(5) 0.3593(3) 0.1702(6) 0.0317(13) Uani d . 1 . .
C C5 0.4376(5) 0.4162(3) 0.2567(6) 0.0321(13) Uani d . 1 . .
H H5 0.3776 0.4488 0.2484 0.038 Uiso calc R 1 . .
C C6 0.2818(5) 0.3943(3) 0.0056(8) 0.0329(11) Uani d . 1 . .
C C7 0.1917(6) 0.3665(3) -0.0988(7) 0.0415(15) Uani d . 1 . .
H H7A 0.2145 0.3801 -0.1928 0.05 Uiso calc R 1 . .
H H7B 0.1905 0.3163 -0.0947 0.05 Uiso calc R 1 . .
C C8 0.0693(6) 0.3946(4) -0.0667(7) 0.0412(16) Uani d . 1 . .
H H8A 0.0711 0.4447 -0.0736 0.049 Uiso calc R 1 . .
H H8B 0.0149 0.3776 -0.137 0.049 Uiso calc R 1 . .
C C9 0.0236(5) 0.3747(3) 0.0760(7) 0.0393(16) Uani d . 1 . .
H H9A 0.0744 0.3951 0.1466 0.047 Uiso calc R 1 . .
H H9B 0.0281 0.3247 0.0858 0.047 Uiso calc R 1 . .
C C10 -0.1046(6) 0.3980(3) 0.1041(6) 0.0378(14) Uani d . 1 . .
H H10A -0.1246 0.3882 0.2008 0.045 Uiso calc R 1 . .
H H10B -0.1107 0.4477 0.0901 0.045 Uiso calc R 1 . .
C C11 -0.1901(5) 0.3620(3) 0.0102(7) 0.0321(12) Uani d . 1 . .
C C12 -0.5240(5) 0.3641(3) -0.3528(6) 0.0381(14) Uani d . 1 . .
H H12 -0.5836 0.3564 -0.4178 0.046 Uiso calc R 1 . .
C C13 -0.4903(7) 0.3109(3) -0.2647(7) 0.0450(15) Uani d . 1 . .
H H13 -0.5266 0.2678 -0.2714 0.054 Uiso calc R 1 . .
C C14 -0.4037(6) 0.3217(3) -0.1674(7) 0.0424(16) Uani d . 1 . .
H H14 -0.3787 0.2856 -0.1101 0.051 Uiso calc R 1 . .
C C15 -0.3539(5) 0.3868(3) -0.1556(6) 0.0306(12) Uani d . 1 . .
C C16 -0.3913(5) 0.4376(3) -0.2462(6) 0.0327(13) Uani d . 1 . .
H H16 -0.3588 0.4817 -0.2376 0.039 Uiso calc R 1 . .
Cu Cu1 0.5 0.5 0.50370(10) 0.0310(3) Uani d S 1 . .
N N1 0.5213(5) 0.4261(3) 0.3520(5) 0.0310(12) Uani d . 1 . .
N N2 0.3457(4) 0.3456(2) 0.0740(5) 0.0338(11) Uani d . 1 . .
H H2A 0.3294 0.3028 0.0573 0.041 Uiso calc R 1 . .
N N3 -0.4724(4) 0.4269(3) -0.3467(5) 0.0314(12) Uani d . 1 . .
N N4 -0.2665(4) 0.4045(2) -0.0572(5) 0.0330(11) Uani d . 1 . .
H H4 -0.2609 0.4478 -0.0373 0.04 Uiso calc R 1 . .
O O1 0.2955(4) 0.4560(2) 0.0224(6) 0.0503(12) Uani d . 1 . .
O O2 -0.1925(4) 0.2987(2) -0.0025(6) 0.0455(10) Uani d . 1 . .
Cl Cl1 0.3980(6) 0.1684(5) 0.4364(5) 0.224(4) Uani d . 1 . .
O O4 0.3993(9) 0.1644(5) 0.5735(10) 0.043(2) Uiso d P 0.5 . .
O O6 0.3375(14) 0.2160(15) 0.3459(18) 0.326(14) Uani d . 1 . .
O O5 0.5133(6) 0.1738(4) 0.3973(8) 0.110(3) Uani d . 1 . .
O O3 0.3508(13) 0.1048(10) 0.3950(17) 0.258(10) Uani d . 1 . .
O O1W 0.2846(4) 0.4720(3) 0.5056(8) 0.0706(15) Uani d . 1 . .
H H1WA 0.2662 0.4293 0.4598 0.106 Uiso d R 1 . .
H H1WB 0.2359 0.5057 0.4597 0.106 Uiso d R 1 . .
O O2W 0.2099(10) 0.3429(6) 0.4163(13) 0.143(4) Uani d G 1 . .
H H2WA 0.1351 0.3409 0.414 0.215 Uiso d G 1 . .
H H2WB 0.2362 0.3113 0.4701 0.215 Uiso d G 1 . .
O O4A 0.3490(17) 0.1964(10) 0.567(2) 0.113(6) Uiso d P 0.5 . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.352(8) ?
C1 C2 . 1.359(9) ?
C1 H1 . 0.93 ?
C2 C3 . 1.381(9) ?
C2 H2 . 0.93 ?
C3 C4 . 1.393(8) ?
C3 H3 . 0.93 ?
C4 C5 . 1.374(8) ?
C4 N2 . 1.408(8) ?
C5 N1 . 1.329(7) ?
C5 H5 . 0.93 ?
C6 O1 . 1.211(6) ?
C6 N2 . 1.354(7) ?
C6 C7 . 1.525(9) ?
C7 C8 . 1.521(9) ?
C7 H7A . 0.97 ?
C7 H7B . 0.97 ?
C8 C9 . 1.508(9) ?
C8 H8A . 0.97 ?
C8 H8B . 0.97 ?
C9 C10 . 1.545(9) ?
C9 H9A . 0.97 ?
C9 H9B . 0.97 ?
C10 C11 . 1.493(8) ?
C10 H10A . 0.97 ?
C10 H10B . 0.97 ?
C11 O2 . 1.227(6) ?
C11 N4 . 1.355(7) ?
C12 N3 . 1.347(8) ?
C12 C13 . 1.381(9) ?
C12 H12 . 0.93 ?
C13 C14 . 1.368(9) ?
C13 H13 . 0.93 ?
C14 C15 . 1.381(9) ?
C14 H14 . 0.93 ?
C15 C16 . 1.375(8) ?
C15 N4 . 1.408(7) ?
C16 N3 . 1.345(7) ?
C16 H16 . 0.93 ?
Cu1 N3 2_566 2.031(5) ?
Cu1 N3 1_656 2.031(5) ?
Cu1 N1 . 2.046(5) ?
Cu1 N1 2_665 2.046(5) ?
Cu1 O1W . 2.502(5) ?
N2 H2A . 0.86 ?
N3 Cu1 1_454 2.031(5) ?
N4 H4 . 0.86 ?
Cl1 O4 . 1.312(9) ?
Cl1 O5 . 1.364(9) ?
Cl1 O3 . 1.395(13) ?
Cl1 O6 . 1.436(17) ?
Cl1 O4A . 1.472(19) ?
O1W H1WA . 0.9555 ?
O1W H1WB . 0.9599 ?
O2W H2WA . 0.85 ?
O2W H2WB . 0.85 ?

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 C1 C2 . . 120.6(6) ?
N1 C1 H1 . . 119.7 ?
C2 C1 H1 . . 119.7 ?
C1 C2 C3 . . 120.6(6) ?
C1 C2 H2 . . 119.7 ?
C3 C2 H2 . . 119.7 ?
C2 C3 C4 . . 118.1(6) ?
C2 C3 H3 . . 121.0 ?
C4 C3 H3 . . 121.0 ?
C5 C4 C3 . . 118.6(5) ?
C5 C4 N2 . . 123.2(5) ?
C3 C4 N2 . . 118.0(5) ?
N1 C5 C4 . . 122.2(5) ?
N1 C5 H5 . . 118.9 ?
C4 C5 H5 . . 118.9 ?
O1 C6 N2 . . 123.3(6) ?
O1 C6 C7 . . 121.1(6) ?
N2 C6 C7 . . 115.6(5) ?
C8 C7 C6 . . 110.8(5) ?
C8 C7 H7A . . 109.5 ?
C6 C7 H7A . . 109.5 ?
C8 C7 H7B . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 108.1 ?
C9 C8 C7 . . 114.0(5) ?
C9 C8 H8A . . 108.8 ?
C7 C8 H8A . . 108.8 ?
C9 C8 H8B . . 108.8 ?
C7 C8 H8B . . 108.8 ?
H8A C8 H8B . . 107.7 ?
C8 C9 C10 . . 114.0(5) ?
C8 C9 H9A . . 108.7 ?
C10 C9 H9A . . 108.7 ?
C8 C9 H9B . . 108.7 ?
C10 C9 H9B . . 108.7 ?
H9A C9 H9B . . 107.6 ?
C11 C10 C9 . . 111.9(5) ?
C11 C10 H10A . . 109.2 ?
C9 C10 H10A . . 109.2 ?
C11 C10 H10B . . 109.2 ?
C9 C10 H10B . . 109.2 ?
H10A C10 H10B . . 107.9 ?
O2 C11 N4 . . 122.7(6) ?
O2 C11 C10 . . 122.4(5) ?
N4 C11 C10 . . 114.9(5) ?
N3 C12 C13 . . 121.4(6) ?
N3 C12 H12 . . 119.3 ?
C13 C12 H12 . . 119.3 ?
C14 C13 C12 . . 120.0(6) ?
C14 C13 H13 . . 120.0 ?
C12 C13 H13 . . 120.0 ?
C13 C14 C15 . . 119.1(6) ?
C13 C14 H14 . . 120.4 ?
C15 C14 H14 . . 120.4 ?
C16 C15 C14 . . 118.0(6) ?
C16 C15 N4 . . 117.7(5) ?
C14 C15 N4 . . 124.3(5) ?
N3 C16 C15 . . 123.5(6) ?
N3 C16 H16 . . 118.3 ?
C15 C16 H16 . . 118.3 ?
N3 Cu1 N3 2_566 1_656 90.5(3) ?
N3 Cu1 N1 2_566 . 177.9(2) ?
N3 Cu1 N1 1_656 . 89.88(17) ?
N3 Cu1 N1 2_566 2_665 89.88(17) ?
N3 Cu1 N1 1_656 2_665 177.9(2) ?
N1 Cu1 N1 . 2_665 89.8(3) ?
N3 Cu1 O1W 2_566 . 89.68(19) ?
N3 Cu1 O1W 1_656 . 89.7(2) ?
N1 Cu1 O1W . . 88.3(2) ?
N1 Cu1 O1W 2_665 . 92.3(2) ?
C5 N1 C1 . . 119.7(5) ?
C5 N1 Cu1 . . 120.1(4) ?
C1 N1 Cu1 . . 119.4(4) ?
C6 N2 C4 . . 125.3(5) ?
C6 N2 H2A . . 117.4 ?
C4 N2 H2A . . 117.4 ?
C16 N3 C12 . . 117.8(5) ?
C16 N3 Cu1 . 1_454 120.1(4) ?
C12 N3 Cu1 . 1_454 121.7(4) ?
C11 N4 C15 . . 128.4(5) ?
C11 N4 H4 . . 115.8 ?
C15 N4 H4 . . 115.8 ?
O4 Cl1 O5 . . 105.5(8) ?
O4 Cl1 O3 . . 103.6(11) ?
O5 Cl1 O3 . . 111.0(10) ?
O4 Cl1 O6 . . 130.1(14) ?
O5 Cl1 O6 . . 104.1(9) ?
O3 Cl1 O6 . . 102.0(12) ?
O5 Cl1 O4A . . 124.6(10) ?
O3 Cl1 O4A . . 114.7(11) ?
O6 Cl1 O4A . . 95.6(14) ?
Cu1 O1W H1WA . . 113.3 ?
Cu1 O1W H1WB . . 114.4 ?
H1WA O1W H1WB . . 104.4 ?
H2WA O2W H2WB . . 109.5 ?



_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.733

_database_code_depnum_ccdc_archive 'CCDC 963406'
