#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/58/2205801.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2205801
loop_
_publ_author_name
'Petra Stachová'
'Dušan Valigura'
'Marian Koman'
'Glowiak Tadeus'
_publ_section_title
catena-Poly[[bis(2-nitrobenzoato-κO)copper(II)]di-μ-3-pyridylmethanol-κ²N,O;κ²O:N]
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m994
_journal_page_last               m996
_journal_paper_doi               10.1107/S1600536805011608
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Cu (C7 H4 N O4)2 (C6 H7 N O)2]'
_chemical_formula_moiety         'C26 H22 Cu N4 O10'
_chemical_formula_sum            'C26 H22 Cu N4 O10'
_chemical_formula_weight         614.03
_chemical_name_systematic
;
Bis(3-nitrobenzoato)bis(3-pyridylmethanol-N,O)copper(II) complex
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                83.72(3)
_cell_angle_beta                 77.11(3)
_cell_angle_gamma                80.69(3)
_cell_formula_units_Z            1
_cell_length_a                   6.6920(13)
_cell_length_b                   7.6470(15)
_cell_length_c                   12.997(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      3.9
_cell_volume                     637.9(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2001)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2001)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Kuma KM-4 CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4407
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         3.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(COSABS99; Starynowicz, 1999)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             315
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.527
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0342P)²+0.2981P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0656
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                2663
_reflns_number_total             2788
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            sj6056.cif
_cod_data_source_block           I
_cod_database_code               2205801
_cod_database_fobs_code          2205801
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cu 0.0000 0.0000 0.0000 0.00992(8) Uani d S 1 Cu
O1 -0.20981(15) 0.02994(13) 0.13387(8) 0.0134(2) Uani d . 1 O
O2 -0.1009(2) 0.2434(2) 0.20548(9) 0.0255(3) Uani d . 1 O
O3 0.8099(2) -0.21625(13) -0.03357(9) 0.0141(2) Uani d . 1 O
O4 -0.4264(2) 0.3488(2) 0.57250(9) 0.0298(3) Uani d . 1 O
O5 -0.7544(2) 0.3383(2) 0.62520(11) 0.0432(4) Uani d . 1 O
N1 -0.5903(3) 0.3110(2) 0.56077(11) 0.0263(3) Uani d . 1 N
N2 0.1846(2) -0.17808(15) 0.07894(9) 0.0104(2) Uani d . 1 N
C1 -0.2230(2) 0.1375(2) 0.20391(11) 0.0137(3) Uani d . 1 C
C2 -0.4121(2) 0.1379(2) 0.29334(11) 0.0141(3) Uani d . 1 C
C3 -0.4140(2) 0.2193(2) 0.38455(11) 0.0160(3) Uani d . 1 C
C4 -0.5915(3) 0.2279(2) 0.46367(12) 0.0196(3) Uani d . 1 C
C5 -0.7680(3) 0.1638(2) 0.45455(13) 0.0246(3) Uani d . 1 C
C6 -0.7642(3) 0.0825(2) 0.36381(14) 0.0243(3) Uani d . 1 C
C7 -0.5856(2) 0.0673(2) 0.28352(12) 0.0185(3) Uani d . 1 C
C8 0.3891(2) -0.2106(2) 0.03762(11) 0.0106(3) Uani d . 1 C
C9 0.5250(2) -0.3321(2) 0.08491(11) 0.0112(3) Uani d . 1 C
C10 0.4468(2) -0.4207(2) 0.18103(12) 0.0161(3) Uani d . 1 C
C11 0.2363(2) -0.3887(2) 0.22432(12) 0.0182(3) Uani d . 1 C
C12 0.1101(2) -0.2670(2) 0.17124(11) 0.0137(3) Uani d . 1 C
C13 0.7501(2) -0.3687(2) 0.03120(12) 0.0134(3) Uani d . 1 C
H1 -0.303(3) 0.270(2) 0.3900(14) 0.017(4) Uiso d . 1 H
H2 -0.884(3) 0.174(3) 0.5109(17) 0.033(5) Uiso d . 1 H
H3 -0.880(3) 0.036(3) 0.3554(17) 0.031(5) Uiso d . 1 H
H4 -0.581(3) 0.014(2) 0.2206(15) 0.016(4) Uiso d . 1 H
H5 0.439(3) -0.142(2) -0.0258(14) 0.013(4) Uiso d . 1 H
H6 0.536(3) -0.500(3) 0.2169(15) 0.021(5) Uiso d . 1 H
H7 0.177(3) -0.448(3) 0.2883(16) 0.022(5) Uiso d . 1 H
H8 -0.035(3) -0.243(2) 0.2004(14) 0.016(4) Uiso d . 1 H
H9 0.769(3) -0.470(3) -0.0096(15) 0.020(5) Uiso d . 1 H
H10 0.830(3) -0.404(2) 0.0864(14) 0.016(4) Uiso d . 1 H
H11 0.888(4) -0.246(3) -0.085(2) 0.039(6) Uiso d . 1 H
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'
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
O1 Cu O1 . 2 180.0 ?
O1 Cu N2 . . 89.73(5) yes
O1 Cu N2 2 . 90.27(5) ?
O1 Cu N2 . 2 90.27(5) ?
O1 Cu N2 2 2 89.73(5) ?
N2 Cu N2 . 2 180.0 ?
O1 Cu O3 . 2_655 93.57(5) yes
O1 Cu O3 2 2_655 86.43(5) ?
N2 Cu O3 . 2_655 85.86(4) ?
N2 Cu O3 2 2_655 94.14(4) ?
O1 Cu O3 . 1_455 86.43(5) ?
O1 Cu O3 2 1_455 93.57(5) ?
N2 Cu O3 . 1_455 94.14(4) ?
N2 Cu O3 2 1_455 85.86(4) ?
O3 Cu O3 2_655 1_455 180.0 ?
C1 O1 Cu . . 128.33(9) ?
C13 O3 Cu . 1_655 129.04(9) ?
C13 O3 H11 . . 109.4(17) ?
Cu O3 H11 1_655 . 95.4(17) ?
O4 N1 O5 . . 123.7(2) ?
O4 N1 C4 . . 118.35(14) ?
O5 N1 C4 . . 118.0(2) ?
C12 N2 C8 . . 118.09(12) ?
C12 N2 Cu . . 122.56(9) ?
C8 N2 Cu . . 119.34(9) ?
O2 C1 O1 . . 127.23(13) ?
O2 C1 C2 . . 117.26(13) ?
O1 C1 C2 . . 115.50(13) ?
C7 C2 C3 . . 120.07(14) ?
C7 C2 C1 . . 121.27(13) ?
C3 C2 C1 . . 118.58(13) ?
C4 C3 C2 . . 118.37(15) ?
C4 C3 H1 . . 121.2(12) ?
C2 C3 H1 . . 120.4(12) ?
C5 C4 C3 . . 122.71(15) ?
C5 C4 N1 . . 119.36(14) ?
C3 C4 N1 . . 117.92(15) ?
C4 C5 C6 . . 118.44(14) ?
C4 C5 H2 . . 118.8(13) ?
C6 C5 H2 . . 122.7(13) ?
C5 C6 C7 . . 120.3(2) ?
C5 C6 H3 . . 120.8(13) ?
C7 C6 H3 . . 118.9(13) ?
C2 C7 C6 . . 120.03(15) ?
C2 C7 H4 . . 118.5(11) ?
C6 C7 H4 . . 121.4(11) ?
N2 C8 C9 . . 123.13(13) ?
N2 C8 H5 . . 116.4(10) ?
C9 C8 H5 . . 120.4(10) ?
C8 C9 C10 . . 118.19(13) ?
C8 C9 C13 . . 120.20(12) ?
C10 C9 C13 . . 121.60(13) ?
C11 C10 C9 . . 119.22(13) ?
C11 C10 H6 . . 120.5(12) ?
C9 C10 H6 . . 120.3(12) ?
C12 C11 C10 . . 119.05(13) ?
C12 C11 H7 . . 119.2(12) ?
C10 C11 H7 . . 121.7(12) ?
N2 C12 C11 . . 122.29(13) ?
N2 C12 H8 . . 117.7(11) ?
C11 C12 H8 . . 120.0(11) ?
O3 C13 C9 . . 109.73(11) ?
O3 C13 H9 . . 111.6(11) ?
C9 C13 H9 . . 108.3(11) ?
O3 C13 H10 . . 112.8(10) ?
C9 C13 H10 . . 107.5(11) ?
H9 C13 H10 . . 106.7(15) ?
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
Cu O1 . 1.9860(12) yes
Cu O1 2 1.9860(12) ?
Cu N2 . 2.0368(13) yes
Cu N2 2 2.0368(13) ?
Cu O3 2_655 2.3724(11) yes
Cu O3 1_455 2.3724(11) ?
O1 C1 . 1.272(2) ?
O2 C1 . 1.245(2) ?
O3 C13 . 1.419(2) ?
O3 Cu 1_655 2.3724(11) ?
O3 H11 . 0.78(2) ?
O4 N1 . 1.224(2) ?
O5 N1 . 1.226(2) ?
N1 C4 . 1.475(2) ?
N2 C12 . 1.347(2) ?
N2 C8 . 1.347(2) ?
C1 C2 . 1.515(2) ?
C2 C7 . 1.393(2) ?
C2 C3 . 1.395(2) ?
C3 C4 . 1.385(2) ?
C3 H1 . 0.91(2) ?
C4 C5 . 1.383(2) ?
C5 C6 . 1.386(3) ?
C5 H2 . 0.94(2) ?
C6 C7 . 1.398(2) ?
C6 H3 . 0.93(2) ?
C7 H4 . 0.95(2) ?
C8 C9 . 1.385(2) ?
C8 H5 . 0.95(2) ?
C9 C10 . 1.390(2) ?
C9 C13 . 1.507(2) ?
C10 C11 . 1.387(2) ?
C10 H6 . 0.94(2) ?
C11 C12 . 1.386(2) ?
C11 H7 . 0.94(2) ?
C12 H8 . 0.95(2) ?
C13 H9 . 0.96(2) ?
C13 H10 . 0.98(2) ?
