#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:53:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180361 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/30/7203068.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7203068
loop_
_publ_author_name
'Amo-Ochoa, Pilar'
'Miguel, Pablo J. Sanz'
'Castillo, Oscar'
'Zamora, Félix'
_publ_section_title
;
 An unusual triple parallel interpenetrated 2D Cu-polymer, with a 3D
 triple interpenetration via H-bonding
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              987
_journal_paper_doi               10.1039/b709457d
_journal_volume                  9
_journal_year                    2007
_chemical_formula_iupac          'C13 H9 Cu2 N3 O4'
_chemical_formula_moiety         'C13 H9 Cu2 N3 O4'
_chemical_formula_sum            'C13 H9 Cu2 N3 O4'
_chemical_formula_weight         398.32
_chemical_name_common
;
catena-(mu-cyanido-kappaC,N)(mu-isonicotinato-kappaN,O) (mu-
isonicotinic acid-kappaN,O)dicopper(i)
;
_chemical_name_systematic
;
catena-(μ-cyanido-\kC,N)(μ-isonicotinato-\kN,O)
(μ-isonicotinic acid-\kN,O)dicopper(I)
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.53(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.864(2)
_cell_length_b                   5.116(1)
_cell_length_c                   12.282(2)
_cell_measurement_reflns_used    3232
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.30
_cell_measurement_theta_min      3.43
_cell_volume                     660.8(2)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altamore et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6073
_diffrn_reflns_theta_full        30.30
_diffrn_reflns_theta_max         30.30
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.240
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_correction_T_min  0.307
_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_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.40(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0466P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                2367
_reflns_number_total             3232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b709457d.txt
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      Pc
_cod_database_code               7203068
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
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_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'
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_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_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
