#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/70/7207018.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_7207018
loop_
_publ_author_name
'Wang, Xiu-Li'
'Mu, Bao'
'Lin, Hong-Yan'
'Liu, Guo-Cheng'
'Tian, Ai-Xiang'
'Yang, Song'
_publ_section_title
;
 Assembly and property of four 2D layer-like coordination polymers with
 different structural features derived from bis(3-pyridylformyl)piperazine
 ligand and aromatic dicarboxylic acids with nitro group
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              1001
_journal_paper_doi               10.1039/c1ce05824j
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C24 H21 Cu N5 O9'
_chemical_formula_sum            'C24 H21 Cu N5 O9'
_chemical_formula_weight         587
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.000(5)
_cell_angle_beta                 100.286(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   6.793(5)
_cell_length_b                   19.313(5)
_cell_length_c                   18.629(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2405(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15915
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bolck
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.8369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                3186
_reflns_number_total             4223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05824j.txt
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C24 H21 Cu N5 O9 '
_cod_database_code               7207018
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
Cu1 Cu 0.02838(6) 0.065063(18) 0.288116(19) 0.02543(13) Uani 1 1 d .
N1 N 0.0075(4) 0.06578(12) 0.17816(13) 0.0284(6) Uani 1 1 d .
O2 O -0.4501(4) 0.08335(12) -0.03456(12) 0.0474(6) Uani 1 1 d .
C16 C -0.1578(5) 0.08940(15) 0.13576(16) 0.0292(7) Uani 1 1 d .
H16A H -0.2672 0.1006 0.1572 0.035 Uiso 1 1 calc R
O6 O -0.1729(3) -0.34845(10) 0.20773(11) 0.0344(5) Uani 1 1 d .
O4 O -0.3808(3) 0.01119(10) 0.24275(12) 0.0351(5) Uani 1 1 d .
N3 N -0.6378(4) 0.29879(13) 0.07718(14) 0.0331(7) Uani 1 1 d .
O3 O -0.0769(3) -0.02973(10) 0.28549(11) 0.0305(5) Uani 1 1 d .
O8 O -0.8132(4) -0.25417(14) 0.10250(14) 0.0599(8) Uani 1 1 d .
O7 O -0.9054(4) -0.15438(13) 0.13667(13) 0.0500(7) Uani 1 1 d .
O1W O 0.3344(3) 0.01717(12) 0.32864(12) 0.0420(6) Uani 1 1 d .
H1WA H 0.4020 0.0194 0.2964 0.063 Uiso 1 1 calc R
C19 C -0.1949(5) -0.16564(15) 0.24797(15) 0.0261(7) Uani 1 1 d .
H19A H -0.0637 -0.1579 0.2711 0.031 Uiso 1 1 calc R
N4 N -1.0085(4) 0.41987(12) -0.10698(13) 0.0272(6) Uani 1 1 d .
O1 O -0.5573(4) 0.41158(12) 0.09401(13) 0.0468(6) Uani 1 1 d .
N2 N -0.4431(4) 0.18271(13) 0.03063(14) 0.0335(6) Uani 1 1 d .
C11 C -0.3660(5) 0.12121(16) 0.01446(16) 0.0318(8) Uani 1 1 d .
N5 N -0.7803(4) -0.20008(16) 0.13706(14) 0.0375(7) Uani 1 1 d .
C4 C -0.8599(5) 0.38712(14) 0.01414(15) 0.0260(7) Uani 1 1 d .
C21 C -0.1021(5) -0.29098(15) 0.23574(16) 0.0297(7) Uani 1 1 d .
C6 C -0.6719(5) 0.36642(16) 0.06545(15) 0.0289(7) Uani 1 1 d .
C14 C 0.1601(5) 0.05600(16) 0.07309(17) 0.0353(8) Uani 1 1 d .
H14A H 0.2712 0.0440 0.0530 0.042 Uiso 1 1 calc R
C18 C -0.3265(5) -0.11041(14) 0.23643(15) 0.0236(7) Uani 1 1 d .
C9 C -0.3264(5) 0.23851(16) 0.07119(17) 0.0347(8) Uani 1 1 d .
H9A H -0.2875 0.2717 0.0372 0.042 Uiso 1 1 calc R
H9B H -0.2056 0.2195 0.1002 0.042 Uiso 1 1 calc R
C20 C -0.2539(5) -0.23256(14) 0.22585(15) 0.0246(7) Uani 1 1 d .
C22 C -0.4490(5) -0.24396(16) 0.19136(15) 0.0289(7) Uani 1 1 d .
H22A H -0.4918 -0.2883 0.1764 0.035 Uiso 1 1 calc R
C7 C -0.7550(5) 0.24238(16) 0.03843(18) 0.0352(8) Uani 1 1 d .
H7A H -0.8770 0.2607 0.0097 0.042 Uiso 1 1 calc R
H7B H -0.7916 0.2097 0.0733 0.042 Uiso 1 1 calc R
O5 O 0.0692(4) -0.28082(11) 0.26715(13) 0.0463(6) Uani 1 1 d .
C23 C -0.5787(5) -0.18888(15) 0.17947(16) 0.0270(7) Uani 1 1 d .
C3 C -1.0351(5) 0.40401(16) 0.03879(17) 0.0342(8) Uani 1 1 d .
H3A H -1.0437 0.3993 0.0878 0.041 Uiso 1 1 calc R
C12 C -0.1741(5) 0.09809(15) 0.06081(16) 0.0289(7) Uani 1 1 d .
C17 C -0.2587(5) -0.03723(15) 0.25655(16) 0.0275(7) Uani 1 1 d .
C5 C -0.8537(5) 0.39550(15) -0.05890(16) 0.0288(7) Uani 1 1 d .
H5A H -0.7369 0.3837 -0.0755 0.035 Uiso 1 1 calc R
C13 C -0.0115(5) 0.08004(15) 0.02945(17) 0.0321(8) Uani 1 1 d .
H13A H -0.0180 0.0841 -0.0207 0.039 Uiso 1 1 calc R
C24 C -0.5228(5) -0.12233(15) 0.20176(15) 0.0288(7) Uani 1 1 d .
H24A H -0.6146 -0.0862 0.1938 0.035 Uiso 1 1 calc R
C10 C -0.4486(5) 0.27458(17) 0.12067(17) 0.0385(8) Uani 1 1 d .
H10A H -0.4756 0.2427 0.1580 0.046 Uiso 1 1 calc R
H10B H -0.3743 0.3136 0.1446 0.046 Uiso 1 1 calc R
C2 C -1.1952(5) 0.42769(17) -0.01059(18) 0.0382(8) Uani 1 1 d .
H2A H -1.3152 0.4384 0.0042 0.046 Uiso 1 1 calc R
C8 C -0.6342(5) 0.20600(17) -0.01101(17) 0.0369(8) Uani 1 1 d .
H8A H -0.7086 0.1665 -0.0338 0.044 Uiso 1 1 calc R
H8B H -0.6107 0.2374 -0.0492 0.044 Uiso 1 1 calc R
C1 C -1.1755(5) 0.43533(16) -0.08243(17) 0.0327(8) Uani 1 1 d .
H1A H -1.2841 0.4521 -0.1154 0.039 Uiso 1 1 calc R
C15 C 0.1643(5) 0.05006(15) 0.14676(17) 0.0335(8) Uani 1 1 d .
H15A H 0.2811 0.0344 0.1761 0.040 Uiso 1 1 calc R
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O6 Cu1 O3 170.98(9) 2 .
O6 Cu1 N1 88.74(9) 2 .
O3 Cu1 N1 91.24(9) . .
O6 Cu1 N4 89.24(9) 2 4_666
O3 Cu1 N4 92.90(9) . 4_666
N1 Cu1 N4 166.07(10) . 4_666
O6 Cu1 O1W 84.88(9) 2 .
O3 Cu1 O1W 86.35(9) . .
N1 Cu1 O1W 103.46(9) . .
N4 Cu1 O1W 90.09(9) 4_666 .
C16 N1 C15 118.1(3) . .
C16 N1 Cu1 120.0(2) . .
C15 N1 Cu1 121.5(2) . .
N1 C16 C12 122.9(3) . .
C21 O6 Cu1 125.5(2) . 2_545
C6 N3 C7 125.7(3) . .
C6 N3 C10 120.7(3) . .
C7 N3 C10 112.4(2) . .
C17 O3 Cu1 116.17(19) . .
C18 C19 C20 121.7(3) . .
C1 N4 C5 117.7(3) . .
C1 N4 Cu1 123.8(2) . 4_465
C5 N4 Cu1 118.4(2) . 4_465
C11 N2 C8 119.7(3) . .
C11 N2 C9 124.4(3) . .
C8 N2 C9 113.3(2) . .
O2 C11 N2 122.7(3) . .
O2 C11 C12 119.5(3) . .
N2 C11 C12 117.7(3) . .
O7 N5 O8 123.4(3) . .
O7 N5 C23 118.4(3) . .
O8 N5 C23 118.2(3) . .
C5 C4 C3 118.5(3) . .
C5 C4 C6 119.1(3) . .
C3 C4 C6 122.1(3) . .
O5 C21 O6 126.1(3) . .
O5 C21 C20 120.5(3) . .
O6 C21 C20 113.4(3) . .
O1 C6 N3 123.1(3) . .
O1 C6 C4 119.2(3) . .
N3 C6 C4 117.7(3) . .
C15 C14 C13 118.9(3) . .
C19 C18 C24 118.9(3) . .
C19 C18 C17 121.5(3) . .
C24 C18 C17 119.5(3) . .
N2 C9 C10 110.3(3) . .
C22 C20 C19 119.1(3) . .
C22 C20 C21 120.8(3) . .
C19 C20 C21 120.0(3) . .
C23 C22 C20 119.0(3) . .
N3 C7 C8 109.9(3) . .
C22 C23 C24 122.5(3) . .
C22 C23 N5 118.8(3) . .
C24 C23 N5 118.5(3) . .
C2 C3 C4 118.7(3) . .
C13 C12 C16 117.9(3) . .
C13 C12 C11 120.7(3) . .
C16 C12 C11 121.3(3) . .
O4 C17 O3 124.5(3) . .
O4 C17 C18 119.2(3) . .
O3 C17 C18 116.3(3) . .
N4 C5 C4 122.9(3) . .
C14 C13 C12 119.4(3) . .
C23 C24 C18 118.8(3) . .
N3 C10 C9 109.4(3) . .
C3 C2 C1 119.0(3) . .
N2 C8 C7 110.3(3) . .
N4 C1 C2 123.2(3) . .
N1 C15 C14 122.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O6 1.932(2) 2
Cu1 O3 1.963(2) .
Cu1 N1 2.028(3) .
Cu1 N4 2.035(2) 4_666
Cu1 O1W 2.277(3) .
N1 C16 1.333(4) .
N1 C15 1.339(4) .
O2 C11 1.228(4) .
C16 C12 1.391(4) .
O6 C21 1.283(3) .
O6 Cu1 1.932(2) 2_545
O4 C17 1.246(3) .
N3 C6 1.338(4) .
N3 C7 1.462(4) .
N3 C10 1.468(4) .
O3 C17 1.264(4) .
O8 N5 1.226(3) .
O7 N5 1.224(3) .
C19 C18 1.383(4) .
C19 C20 1.394(4) .
N4 C1 1.330(4) .
N4 C5 1.339(4) .
N4 Cu1 2.035(2) 4_465
O1 C6 1.225(4) .
N2 C11 1.354(4) .
N2 C8 1.460(4) .
N2 C9 1.465(4) .
C11 C12 1.497(4) .
N5 C23 1.470(4) .
C4 C5 1.378(4) .
C4 C3 1.389(4) .
C4 C6 1.506(4) .
C21 O5 1.222(4) .
C21 C20 1.517(4) .
C14 C15 1.372(4) .
C14 C13 1.377(4) .
C18 C24 1.393(4) .
C18 C17 1.513(4) .
C9 C10 1.516(4) .
C20 C22 1.384(4) .
C22 C23 1.374(4) .
C7 C8 1.512(4) .
C23 C24 1.383(4) .
C3 C2 1.371(4) .
C12 C13 1.383(4) .
C2 C1 1.377(4) .
