# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Ki-Min Park'
_publ_contact_author_email       KMPARK@GNU.AC.KR

_publ_section_title              
;
An unusual anionic copper(I) cyanide 3D framework
encapsulating cationic copper(II) complex as a guest
;
loop_
_publ_author_name
'Ki-Min Park.'
'Youngjin Kang.'
'Sanjina Lee.'
'Shim Sung Lee.'
;
Suk-Hee Moon
;

# Attachment 'cucns-R.cif'

data_cucns
_database_code_depnum_ccdc_archive 'CCDC 699391'

_audit_creation_method           SHELXTL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H16 Cu4 N9 O2'
_chemical_formula_weight         488.43

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           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   7.8845(3)
_cell_length_b                   10.4605(4)
_cell_length_c                   18.8317(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1553.16(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4501
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.94

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             964
_exptl_absorpt_coefficient_mu    5.416
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2206
_exptl_absorpt_correction_T_max  0.3446
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9263
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3364
_reflns_number_gt                3005
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0252P)^2^+1.3966P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_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   0.00(2)
_refine_ls_number_reflns         3364
_refine_ls_number_parameters     183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0656
_refine_ls_wR_factor_gt          0.0625
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_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 0.68565(7) 0.39715(5) 0.49163(2) 0.01671(12) Uani 1 1 d . . .
Cu2 Cu 0.81709(7) 0.40032(5) 0.37150(3) 0.01966(12) Uani 1 1 d . . .
Cu3 Cu 0.68337(7) 0.20718(5) 0.13458(3) 0.01910(12) Uani 1 1 d . . .
Cu4 Cu 0.25549(7) 0.40503(5) 0.13840(3) 0.01788(12) Uani 1 1 d . . .
C1 C 0.6000(6) 0.5108(4) 0.4075(2) 0.0154(9) Uani 1 1 d . . .
N1 N 0.5099(5) 0.5890(4) 0.38876(19) 0.0202(8) Uani 1 1 d . . .
C2 C 0.8854(6) 0.2826(4) 0.4658(2) 0.0169(9) Uani 1 1 d . . .
N2 N 0.9932(5) 0.2113(3) 0.47633(18) 0.0161(8) Uani 1 1 d . . .
C3 C 0.7452(6) 0.2995(4) 0.2919(2) 0.0175(8) Uani 1 1 d . . .
N3 N 0.6985(5) 0.2506(3) 0.24062(19) 0.0224(9) Uani 1 1 d . . .
X4 C 1.0080(6) 0.5165(4) 0.3714(2) 0.0227(11) Uani 0.66(4) 1 d P . .
X4' N 1.0080(6) 0.5165(4) 0.3714(2) 0.0227(11) Uani 0.34(4) 1 d P . .
X5 N 1.1204(5) 0.5866(4) 0.3746(2) 0.0265(11) Uani 0.66(4) 1 d P . .
X5' C 1.1204(5) 0.5866(4) 0.3746(2) 0.0265(11) Uani 0.34(4) 1 d P . .
X6 C 0.7896(5) 0.6308(4) 0.5856(2) 0.0159(11) Uani 0.74(4) 1 d P . .
X6' N 0.7896(5) 0.6308(4) 0.5856(2) 0.0159(11) Uani 0.26(4) 1 d P . .
X7 N 0.7580(5) 0.5351(3) 0.55845(19) 0.0178(10) Uani 0.74(4) 1 d P . .
X7' C 0.7580(5) 0.5351(3) 0.55845(19) 0.0178(10) Uani 0.26(4) 1 d P . .
N8 N 0.4284(5) 0.4771(4) 0.2087(2) 0.0278(10) Uani 1 1 d . . .
H8A H 0.4714 0.5516 0.1914 0.033 Uiso 1 1 calc R . .
H8B H 0.5140 0.4198 0.2147 0.033 Uiso 1 1 calc R . .
H8C H 0.3768 0.4919 0.2511 0.033 Uiso 1 1 calc R . .
N9 N 0.2155(6) 0.2535(4) 0.2038(2) 0.0332(11) Uani 1 1 d . . .
H9A H 0.2608 0.2703 0.2473 0.040 Uiso 1 1 calc R . .
H9B H 0.2658 0.1827 0.1852 0.040 Uiso 1 1 calc R . .
H9C H 0.1021 0.2396 0.2083 0.040 Uiso 1 1 calc R . .
N10 N 0.1308(5) 0.3068(4) 0.0600(2) 0.0266(9) Uani 1 1 d . . .
H10A H 0.1280 0.3550 0.0198 0.032 Uiso 1 1 calc R . .
H10B H 0.0230 0.2897 0.0744 0.032 Uiso 1 1 calc R . .
H10C H 0.1861 0.2322 0.0511 0.032 Uiso 1 1 calc R . .
N11 N 0.3417(5) 0.5283(4) 0.0628(2) 0.0312(10) Uani 1 1 d . . .
H11A H 0.2786 0.6011 0.0637 0.037 Uiso 1 1 calc R . .
H11B H 0.3330 0.4911 0.0193 0.037 Uiso 1 1 calc R . .
H11C H 0.4522 0.5478 0.0716 0.037 Uiso 1 1 calc R . .
O1 O 0.0351(5) 0.5198(4) 0.1790(2) 0.0425(10) Uani 1 1 d . . .
H1A H 0.0286 0.5390 0.2254 0.051 Uiso 1 1 d R . .
H1B H -0.0010 0.6132 0.1740 0.051 Uiso 1 1 d R . .
O2 O 0.3340(7) 0.2709(5) 0.3539(2) 0.086(2) Uani 1 1 d . . .
H2A H 0.3520 0.3633 0.3397 0.104 Uiso 1 1 d R . .
H2B H 0.2788 0.3018 0.3990 0.104 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0156(2) 0.0131(2) 0.0214(3) 0.0011(2) 0.0008(2) -0.0009(3)
Cu2 0.0237(3) 0.0177(2) 0.0176(2) -0.0012(2) -0.0018(2) -0.0015(3)
Cu3 0.0220(3) 0.0152(2) 0.0201(3) -0.0021(2) -0.0018(3) -0.0031(2)
Cu4 0.0206(2) 0.0137(2) 0.0193(2) 0.0010(2) -0.0002(2) 0.0015(2)
C1 0.015(2) 0.010(2) 0.021(2) -0.0039(18) -0.0043(17) -0.0019(18)
N1 0.022(2) 0.0135(18) 0.025(2) -0.0016(17) -0.0002(15) 0.0001(18)
C2 0.018(2) 0.015(2) 0.018(2) -0.0030(18) -0.0019(17) -0.0032(19)
N2 0.018(2) 0.0146(18) 0.0163(19) 0.0005(15) -0.0022(15) -0.0013(16)
C3 0.021(2) 0.0153(19) 0.016(2) 0.0023(18) 0.0003(17) 0.0027(19)
N3 0.032(2) 0.0145(18) 0.0212(19) -0.0013(15) -0.0026(19) 0.0043(17)
X4 0.025(3) 0.020(2) 0.023(2) 0.004(2) 0.0030(19) -0.0013(19)
X4' 0.025(3) 0.020(2) 0.023(2) 0.004(2) 0.0030(19) -0.0013(19)
X5 0.026(2) 0.020(2) 0.034(2) 0.005(2) 0.0039(18) -0.002(2)
X5' 0.026(2) 0.020(2) 0.034(2) 0.005(2) 0.0039(18) -0.002(2)
X6 0.014(2) 0.019(2) 0.014(2) 0.0013(16) 0.0008(16) -0.0013(16)
X6' 0.014(2) 0.019(2) 0.014(2) 0.0013(16) 0.0008(16) -0.0013(16)
X7 0.0175(19) 0.020(2) 0.0157(19) -0.0025(16) 0.0051(16) 0.0022(17)
X7' 0.0175(19) 0.020(2) 0.0157(19) -0.0025(16) 0.0051(16) 0.0022(17)
N8 0.025(2) 0.020(2) 0.038(2) -0.0065(19) -0.0073(18) 0.0077(18)
N9 0.056(3) 0.024(2) 0.020(2) 0.0022(17) -0.005(2) -0.006(2)
N10 0.031(2) 0.026(2) 0.022(2) -0.0003(18) 0.0027(17) -0.0015(18)
N11 0.021(2) 0.027(2) 0.046(3) 0.0163(19) 0.0031(19) 0.0054(18)
O1 0.042(3) 0.043(2) 0.042(2) -0.0121(19) 0.0033(18) 0.008(2)
O2 0.123(5) 0.114(4) 0.023(2) 0.001(3) -0.004(3) -0.079(4)

_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 N2 1.988(4) 4_456 ?
Cu1 X7 1.998(4) . ?
Cu1 C2 2.038(5) . ?
Cu1 C1 2.093(4) . ?
Cu1 Cu2 2.4885(7) . ?
Cu2 C3 1.918(4) . ?
Cu2 X4 1.934(4) . ?
Cu2 C1 2.173(4) . ?
Cu2 C2 2.228(4) . ?
Cu3 X6' 1.942(4) 2_664 ?
Cu3 X6 1.942(4) 2_664 ?
Cu3 X5' 2.004(4) 3_745 ?
Cu3 X5 2.004(4) 3_745 ?
Cu3 N1 2.011(4) 3_645 ?
Cu3 N3 2.051(4) . ?
Cu4 N9 2.032(4) . ?
Cu4 N11 2.038(4) . ?
Cu4 N8 2.044(4) . ?
Cu4 N10 2.049(4) . ?
Cu4 O1 2.246(4) . ?
C1 N1 1.139(6) . ?
N1 Cu3 2.011(4) 3_655 ?
C2 N2 1.148(5) . ?
N2 Cu1 1.988(4) 4_556 ?
C3 N3 1.153(5) . ?
X4 X5 1.152(6) . ?
X5 Cu3 2.004(4) 3_755 ?
X6 X7 1.150(5) . ?
X6 Cu3 1.942(4) 2_665 ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 H8C 0.9100 . ?
N9 H9A 0.9100 . ?
N9 H9B 0.9100 . ?
N9 H9C 0.9100 . ?
N10 H10A 0.9100 . ?
N10 H10B 0.9100 . ?
N10 H10C 0.9100 . ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 H11C 0.9100 . ?
O1 H1A 0.8990 . ?
O1 H1B 1.0214 . ?
O2 H2A 1.0133 . ?
O2 H2B 1.0081 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 X7 116.04(15) 4_456 . ?
N2 Cu1 C2 109.06(16) 4_456 . ?
X7 Cu1 C2 110.74(16) . . ?
N2 Cu1 C1 107.91(16) 4_456 . ?
X7 Cu1 C1 99.14(15) . . ?
C2 Cu1 C1 113.76(17) . . ?
N2 Cu1 Cu2 126.96(10) 4_456 . ?
X7 Cu1 Cu2 116.36(11) . . ?
C2 Cu1 Cu2 57.95(12) . . ?
C1 Cu1 Cu2 55.84(12) . . ?
C3 Cu2 X4 125.10(19) . . ?
C3 Cu2 C1 107.64(18) . . ?
X4 Cu2 C1 106.21(17) . . ?
C3 Cu2 C2 112.99(16) . . ?
X4 Cu2 C2 99.18(17) . . ?
C1 Cu2 C2 103.63(16) . . ?
C3 Cu2 Cu1 125.44(14) . . ?
X4 Cu2 Cu1 109.44(13) . . ?
C1 Cu2 Cu1 52.82(11) . . ?
C2 Cu2 Cu1 50.83(12) . . ?
X6' Cu3 X6 0.0(2) 2_664 2_664 ?
X6' Cu3 X5' 115.09(17) 2_664 3_745 ?
X6 Cu3 X5' 115.09(17) 2_664 3_745 ?
X6' Cu3 X5 115.09(17) 2_664 3_745 ?
X6 Cu3 X5 115.09(17) 2_664 3_745 ?
X5' Cu3 X5 0.0(3) 3_745 3_745 ?
X6' Cu3 N1 121.06(16) 2_664 3_645 ?
X6 Cu3 N1 121.06(16) 2_664 3_645 ?
X5' Cu3 N1 100.33(15) 3_745 3_645 ?
X5 Cu3 N1 100.33(15) 3_745 3_645 ?
X6' Cu3 N3 105.25(15) 2_664 . ?
X6 Cu3 N3 105.25(15) 2_664 . ?
X5' Cu3 N3 100.26(16) 3_745 . ?
X5 Cu3 N3 100.26(16) 3_745 . ?
N1 Cu3 N3 113.14(15) 3_645 . ?
N9 Cu4 N11 165.67(17) . . ?
N9 Cu4 N8 89.92(17) . . ?
N11 Cu4 N8 89.79(18) . . ?
N9 Cu4 N10 88.35(16) . . ?
N11 Cu4 N10 88.51(17) . . ?
N8 Cu4 N10 166.17(16) . . ?
N9 Cu4 O1 95.21(17) . . ?
N11 Cu4 O1 99.07(16) . . ?
N8 Cu4 O1 95.66(15) . . ?
N10 Cu4 O1 98.17(15) . . ?
N1 C1 Cu1 147.5(4) . . ?
N1 C1 Cu2 140.9(4) . . ?
Cu1 C1 Cu2 71.34(14) . . ?
C1 N1 Cu3 168.9(4) . 3_655 ?
N2 C2 Cu1 156.0(4) . . ?
N2 C2 Cu2 132.5(4) . . ?
Cu1 C2 Cu2 71.22(14) . . ?
C2 N2 Cu1 171.1(3) . 4_556 ?
N3 C3 Cu2 173.0(4) . . ?
C3 N3 Cu3 158.8(4) . . ?
X5 X4 Cu2 177.0(4) . . ?
X4 X5 Cu3 172.1(4) . 3_755 ?
X7 X6 Cu3 173.6(4) . 2_665 ?
X6 X7 Cu1 165.8(3) . . ?
Cu4 N8 H8A 109.5 . . ?
Cu4 N8 H8B 109.5 . . ?
H8A N8 H8B 109.5 . . ?
Cu4 N8 H8C 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
Cu4 N9 H9A 109.5 . . ?
Cu4 N9 H9B 109.5 . . ?
H9A N9 H9B 109.5 . . ?
Cu4 N9 H9C 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
Cu4 N10 H10A 109.5 . . ?
Cu4 N10 H10B 109.5 . . ?
H10A N10 H10B 109.5 . . ?
Cu4 N10 H10C 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
Cu4 N11 H11A 109.5 . . ?
Cu4 N11 H11B 109.5 . . ?
H11A N11 H11B 109.5 . . ?
Cu4 N11 H11C 109.5 . . ?
H11A N11 H11C 109.5 . . ?
H11B N11 H11C 109.5 . . ?
Cu4 O1 H1A 119.6 . . ?
Cu4 O1 H1B 134.1 . . ?
H1A O1 H1B 81.9 . . ?
H2A O2 H2B 88.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N9 H9A O2 0.91 2.09 2.982(5) 166.7 .
N8 H8B Cg1 0.91 2.43 3.32 163.7 .
N9 H9B Cg2 0.91 2.53 3.39 158.4 3_645
N10 H10B Cg3 0.91 2.77 3.33 121.1 3_645
N10 H10B Cg4 0.91 2.69 3.40 135.2 2_564
N10 H10C Cg4 0.91 2.53 3.39 158.4 3_645
N11 H11A Cg5 0.91 2.39 3.25 157.3 3_655
N11 H11C Cg4 0.91 2.56 3.25 133.6 2_664
O1 H1A Cg3 0.90 2.80 3.68 166.4 1_455
O2 H2A Cg2 1.01 2.75 3.50 130.7 .
O2 H2B Cg5 1.01 2.80 3.40 118.9 4_456

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.115