Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
_publ_author_address
'Pilar Amo-Ochoa'
;
Departamento de Tecnologia Industrial.
Universidad Alfonso X 'El Sabio', E-28691 Villanueva de la Canada,
Madrid, Spain
;
'Pablo J. Sanz Miguel'
;
Departamento de Quimica Inorganica.
Universidad Autonoma de Madrid, E-28049 Madrid, Spain
;
'Oscar Castillo'
;
Departamento de Quimica Inorganica.
Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain
;
'Felix Zamora'
;
Departamento de Quimica Inorganica.
Universidad Autonoma de Madrid, E-28049 Madrid, Spain
;
_publ_contact_author             
;
Felix Zamora, Departamento de Quimica Inorganica.
Universidad Autonoma de Madrid, E-28049 Madrid, Spain
;
_publ_contact_author_email       felix.zamora@uam.es
_publ_contact_author_fax         '34 91 4974833'
_publ_contact_author_phone       '34 91 4973962'
_publ_section_title              
;
An unusual triple parallel interpenetrated 2D Cu-polymer,
with a 3D triple interpenetration via H-bonding
;
_publ_contact_author_name        
'Felix Zamora, Departamento de Quimica Inorganica.'

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 630735'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
catena-(\m-cyanido-\kC,N)(\m-isonicotinato-\kN,O)
(\m-isonicotinic acid-\kN,O)dicopper(I)
;
_chemical_formula_moiety         'C13 H9 Cu2 N3 O4'
_chemical_formula_sum            'C13 H9 Cu2 N3 O4'
_chemical_formula_iupac          'C13 H9 Cu2 N3 O4'
_chemical_formula_weight         398.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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           monoclinic
_symmetry_space_group_name_H-M   Pc
_symmetry_space_group_name_Hall  'P -2yc'

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

_cell_length_a                   10.864(2)
_cell_length_b                   5.116(1)
_cell_length_c                   12.282(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.53(1)
_cell_angle_gamma                90.00
_cell_volume                     660.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3232
_cell_measurement_theta_min      3.43
_cell_measurement_theta_max      30.30

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             396
_exptl_absorpt_coefficient_mu    3.240
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_absorpt_correction_T_min  0.307
_exptl_absorpt_correction_T_max  0.623

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         30.30
_reflns_number_total             3232
_reflns_number_gt                2367
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_structure_solution    'Sir92 (Altamore et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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^)+(0.0466P)^2^] 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    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   0.40(4)
_refine_ls_number_reflns         3232
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0756
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_restrained_S_all      0.962
_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 0.49893(4) 0.4292(2) 0.62014(4) 0.0318(3) Uani 1 1 d . . .
Cu2 Cu 0.19115(4) 1.0696(2) 0.42557(4) 0.0311(3) Uani 1 1 d . . .
N1 N 0.3805(8) 0.6775(17) 0.5468(7) 0.0320(12) Uani 1 1 d U . .
C1 C 0.3076(9) 0.8281(19) 0.5018(8) 0.0257(12) Uani 1 1 d U . .
N11 N 0.5592(7) 0.1488(15) 0.7230(6) 0.0228(12) Uani 1 1 d U . .
C12 C 0.5094(8) 0.0984(16) 0.8176(7) 0.0272(13) Uani 1 1 d U . .
H12 H 0.4430 0.2031 0.8273 0.033 Uiso 1 1 calc R . .
C13 C 0.5505(8) -0.0846(16) 0.8915(8) 0.0248(13) Uani 1 1 d U . .
H13 H 0.5115 -0.1109 0.9498 0.030 Uiso 1 1 calc R . .
C14 C 0.6532(8) -0.2419(16) 0.8833(8) 0.0186(12) Uani 1 1 d U . .
C15 C 0.7061(7) -0.1905(15) 0.7890(7) 0.0230(12) Uani 1 1 d U . .
H15 H 0.7741 -0.2879 0.7778 0.028 Uiso 1 1 calc R . .
C16 C 0.6566(9) -0.006(2) 0.7207(7) 0.0254(13) Uani 1 1 d U . .
H16 H 0.6942 0.0224 0.6616 0.031 Uiso 1 1 calc R . .
C17 C 0.7092(10) -0.4454(16) 0.9714(7) 0.0195(14) Uani 1 1 d U . .
O171 O 0.6645(7) -0.4728(14) 1.0533(6) 0.0298(14) Uani 1 1 d U . .
O172 O 0.8027(7) -0.5785(11) 0.9506(6) 0.0299(16) Uani 1 1 d U . .
N21 N 0.1288(7) 1.3475(15) 0.3174(6) 0.0232(12) Uani 1 1 d U . .
C22 C 0.1785(8) 1.3892(15) 0.2384(7) 0.0291(14) Uani 1 1 d U . .
H22 H 0.2488 1.2905 0.2336 0.035 Uiso 1 1 calc R . .
C23 C 0.1308(9) 1.5859(17) 0.1533(8) 0.0285(14) Uani 1 1 d U . .
H23 H 0.1676 1.6060 0.0931 0.034 Uiso 1 1 calc R . .
C24 C 0.0319(8) 1.7413(16) 0.1620(8) 0.0199(12) Uani 1 1 d U . .
C25 C -0.0134(7) 1.7107(14) 0.2510(7) 0.0239(13) Uani 1 1 d U . .
H25 H -0.0767 1.8228 0.2617 0.029 Uiso 1 1 calc R . .
C26 C 0.0338(8) 1.5033(18) 0.3337(7) 0.0230(13) Uani 1 1 d U . .
H26 H -0.0004 1.4794 0.3953 0.028 Uiso 1 1 calc R . .
C27 C -0.0213(10) 1.9462(16) 0.0734(8) 0.0193(14) Uani 1 1 d U . .
O271 O 0.0184(6) 1.9711(13) -0.0094(6) 0.0281(13) Uani 1 1 d U . .
O272 O -0.1096(7) 2.0798(11) 0.0917(6) 0.0320(17) Uani 1 1 d U . .
H172 H 0.824(5) -0.721(12) 0.995(4) 0.059(16) Uiso 1 1 d . . .

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 0.0345(7) 0.0266(7) 0.0319(7) 0.0096(6) 0.0041(6) 0.0119(6)
Cu2 0.0343(7) 0.0262(7) 0.0312(7) 0.0099(6) 0.0050(6) 0.0141(6)
N1 0.030(2) 0.032(2) 0.036(2) 0.015(2) 0.012(2) 0.002(2)
C1 0.021(2) 0.027(2) 0.032(2) 0.012(2) 0.012(2) 0.010(2)
N11 0.026(3) 0.025(2) 0.020(2) 0.001(2) 0.011(2) 0.000(2)
C12 0.029(2) 0.035(3) 0.025(2) 0.001(2) 0.0211(19) 0.007(2)
C13 0.025(3) 0.029(3) 0.027(3) 0.005(2) 0.020(2) 0.009(2)
C14 0.022(2) 0.017(2) 0.018(2) -0.0005(19) 0.007(2) 0.001(2)
C15 0.026(2) 0.027(2) 0.023(2) 0.0023(19) 0.018(2) 0.005(2)
C16 0.028(3) 0.033(3) 0.021(2) 0.006(2) 0.016(2) -0.001(2)
C17 0.023(3) 0.019(3) 0.018(3) 0.000(2) 0.007(2) 0.001(2)
O171 0.035(3) 0.036(3) 0.023(3) 0.011(2) 0.017(2) 0.006(2)
O172 0.031(2) 0.032(2) 0.030(2) 0.0087(15) 0.0134(17) 0.0106(15)
N21 0.024(2) 0.019(2) 0.026(3) 0.011(2) 0.004(2) 0.012(2)
C22 0.032(3) 0.024(2) 0.032(3) 0.018(2) 0.010(2) 0.022(2)
C23 0.033(3) 0.030(3) 0.026(3) 0.014(2) 0.013(2) 0.013(2)
C24 0.021(2) 0.017(2) 0.022(2) 0.006(2) 0.005(2) 0.005(2)
C25 0.025(2) 0.019(2) 0.026(3) 0.0110(19) 0.004(2) 0.0130(19)
C26 0.026(2) 0.021(2) 0.022(2) 0.0082(19) 0.006(2) 0.013(2)
C27 0.020(3) 0.016(3) 0.022(3) 0.006(2) 0.005(2) 0.001(2)
O271 0.031(3) 0.028(3) 0.029(3) 0.009(2) 0.015(2) 0.010(2)
O272 0.036(2) 0.032(2) 0.035(3) 0.0248(18) 0.023(2) 0.0254(18)

_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 N1 1.871(9) . ?
Cu1 N11 1.915(7) . ?
Cu1 O171 2.168(6) 2_554 ?
Cu2 C1 1.846(9) . ?
Cu2 N21 1.948(6) . ?
Cu2 O271 2.226(6) 2_585 ?
N1 C1 1.143(13) . ?
N11 C16 1.328(11) . ?
N11 C12 1.423(9) . ?
C12 C13 1.302(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.399(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.440(10) . ?
C14 C17 1.515(11) . ?
C15 C16 1.287(11) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 O171 1.229(9) . ?
C17 O172 1.300(10) . ?
O171 Cu1 2.168(6) 2 ?
O172 H172 0.91(6) . ?
N21 C22 1.243(9) . ?
N21 C26 1.358(10) . ?
C22 C23 1.450(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.362(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.316(11) . ?
C24 C27 1.517(11) . ?
C25 C26 1.470(10) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 O271 1.207(10) . ?
C27 O272 1.243(10) . ?
O271 Cu2 2.226(6) 2_584 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N11 155.0(3) . . ?
N1 Cu1 O171 106.5(3) . 2_554 ?
N11 Cu1 O171 98.5(3) . 2_554 ?
C1 Cu2 N21 155.7(3) . . ?
C1 Cu2 O271 106.7(3) . 2_585 ?
N21 Cu2 O271 97.6(3) . 2_585 ?
C1 N1 Cu1 179.6(9) . . ?
N1 C1 Cu2 178.5(9) . . ?
C16 N11 C12 112.2(7) . . ?
C16 N11 Cu1 125.1(5) . . ?
C12 N11 Cu1 122.5(6) . . ?
C13 C12 N11 124.4(8) . . ?
C13 C12 H12 117.8 . . ?
N11 C12 H12 117.8 . . ?
C12 C13 C14 120.3(8) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 116.0(8) . . ?
C13 C14 C17 121.9(8) . . ?
C15 C14 C17 122.0(7) . . ?
C16 C15 C14 118.2(7) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
C15 C16 N11 128.9(7) . . ?
C15 C16 H16 115.5 . . ?
N11 C16 H16 115.5 . . ?
O171 C17 O172 126.1(9) . . ?
O171 C17 C14 119.5(8) . . ?
O172 C17 C14 114.4(7) . . ?
C17 O171 Cu1 146.5(7) . 2 ?
C17 O172 H172 113(4) . . ?
C22 N21 C26 120.7(7) . . ?
C22 N21 Cu2 120.9(5) . . ?
C26 N21 Cu2 118.4(5) . . ?
N21 C22 C23 122.4(8) . . ?
N21 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
C24 C23 C22 119.7(8) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C25 C24 C23 117.5(8) . . ?
C25 C24 C27 121.6(7) . . ?
C23 C24 C27 120.9(8) . . ?
C24 C25 C26 121.5(7) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
N21 C26 C25 117.9(7) . . ?
N21 C26 H26 121.1 . . ?
C25 C26 H26 121.1 . . ?
O271 C27 O272 123.3(8) . . ?
O271 C27 C24 121.7(8) . . ?
O272 C27 C24 115.0(7) . . ?
C27 O271 Cu2 143.5(7) . 2_584 ?

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
O172 H172 O272 0.91(6) 1.59(5) 2.478(9) 164(6) 1_626

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        30.30
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.150
_chemical_name_common            
;
catena-(mu-cyanido-kappaC,N)(mu-isonicotinato-kappaN,O) (mu-
isonicotinic acid-kappaN,O)dicopper(i)
;

