#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:27:03 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180435 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/04/7210483.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_7210483
loop_
_publ_author_name
'Wang, Xiu-Li'
'Lin, Hong-Yan'
'Mu, Bao'
'Tian, Ai-Xiang'
'Liu, Guo-Cheng'
'Hu, Ning-Hai'
_publ_section_title
;
 Copper(ii) metal--organic networks derived from
 bis(pyridylformyl)piperazine ligands and aromatic polycarboxylates: 2D
 layered structures and a novel 3,5-connected binodal 3D topology
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1990
_journal_paper_doi               10.1039/c0ce00400f
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C34 H28 Cu2 N4 O16'
_chemical_formula_weight         875.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 115.048(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.415(3)
_cell_length_b                   19.083(3)
_cell_length_c                   12.1863(16)
_cell_measurement_reflns_used    4287
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      1.84
_cell_volume                     4722.4(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and 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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11918
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.8851
_exptl_absorpt_correction_T_min  0.8458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4287
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0421
_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)+(0.0410P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                2637
_reflns_number_total             4287
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c0ce00400f.txt
_cod_data_source_block           compd3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4722.5(11)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7210483
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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 0.155256(18) 0.220055(18) 0.30745(4) 0.03441(14) Uani 1 1 d . . .
O1 O 0.15535(10) 0.12851(11) 0.3776(2) 0.0419(6) Uani 1 1 d . . .
O1W O 0.25165(9) 0.21274(10) 0.38293(19) 0.0423(6) Uani 1 1 d . . .
H1A H 0.2754 0.2475 0.3987 0.051 Uiso 1 1 d R . .
H1B H 0.2693 0.1845 0.4383 0.051 Uiso 1 1 d R . .
O2 O 0.15777(11) 0.18715(11) 0.5364(2) 0.0543(7) Uani 1 1 d . . .
O3 O 0.1860(2) 0.05783(18) 0.9060(3) 0.1131(14) Uani 1 1 d . . .
H3A H 0.1846 0.0510 0.9713 0.136 Uiso 0.50 1 calc PR . .
O4 O 0.16012(10) 0.31286(11) 0.2481(2) 0.0459(6) Uani 1 1 d . . .
O5 O 0.18418(13) 0.36921(12) 0.4225(3) 0.0605(8) Uani 1 1 d . . .
O6 O 0.1159(3) 0.44147(17) -0.1213(3) 0.165(2) Uani 1 1 d . . .
H6A H 0.1193 0.4467 -0.1852 0.198 Uiso 0.50 1 calc PR . .
O7 O 0.15435(11) 0.17295(13) 0.1250(2) 0.0490(7) Uani 1 1 d . A .
N1 N -0.05602(12) 0.21985(14) -0.2209(2) 0.0392(7) Uani 1 1 d . . .
C1 C 0.15777(15) 0.13085(16) 0.4828(4) 0.0371(9) Uani 1 1 d . . .
C2 C 0.16160(14) 0.06282(15) 0.5467(3) 0.0325(8) Uani 1 1 d . . .
C3 C 0.16922(16) 0.06204(18) 0.6654(3) 0.0447(10) Uani 1 1 d . . .
H3 H 0.1715 0.1042 0.7052 0.054 Uiso 1 1 calc R . .
C4 C 0.1735(2) 0.0000 0.7258(5) 0.0467(13) Uani 1 2 d S . .
C5 C 0.1816(4) 0.0000 0.8527(7) 0.086(2) Uani 1 2 d S . .
C6 C 0.15852(19) 0.0000 0.4887(4) 0.0296(11) Uani 1 2 d S . .
H6 H 0.1543 0.0000 0.4094 0.036 Uiso 1 2 calc SR . .
C7 C 0.17028(15) 0.36859(17) 0.3132(4) 0.0418(9) Uani 1 1 d . . .
C8 C 0.16243(16) 0.43652(16) 0.2460(3) 0.0397(9) Uani 1 1 d . . .
C9 C 0.1477(2) 0.43690(17) 0.1258(4) 0.0672(13) Uani 1 1 d . . .
H9 H 0.1426 0.3946 0.0849 0.081 Uiso 1 1 calc R . .
C10 C 0.1400(3) 0.5000 0.0626(5) 0.074(2) Uani 1 2 d S . .
C11 C 0.1238(5) 0.5000 -0.0676(7) 0.122(3) Uani 1 2 d S . .
C12 C 0.1713(2) 0.5000 0.3070(4) 0.0366(12) Uani 1 2 d S . .
H12 H 0.1833 0.5000 0.3900 0.044 Uiso 1 2 calc SR . .
C13 C 0.14660(17) 0.2031(2) 0.0321(4) 0.0558(11) Uani 1 1 d . . .
C14 C 0.07732(16) 0.2113(2) -0.0655(3) 0.0468(9) Uani 1 1 d . A .
C15 C 0.03967(17) 0.1526(2) -0.1053(4) 0.0689(14) Uani 1 1 d . . .
H15 H 0.0583 0.1085 -0.0804 0.083 Uiso 1 1 calc R A .
C16 C -0.02613(17) 0.15869(19) -0.1828(4) 0.0616(13) Uani 1 1 d . A .
H16 H -0.0508 0.1179 -0.2096 0.074 Uiso 1 1 calc R . .
C17 C -0.01858(18) 0.27635(19) -0.1831(4) 0.0650(13) Uani 1 1 d . A .
H17 H -0.0378 0.3200 -0.2097 0.078 Uiso 1 1 calc R . .
C18 C 0.04696(18) 0.2737(2) -0.1066(4) 0.0732(14) Uani 1 1 d . . .
H18 H 0.0710 0.3150 -0.0826 0.088 Uiso 1 1 calc R A .
N2A N 0.1929(3) 0.2519(4) 0.0245(6) 0.040(2) Uani 0.50 1 d PD A 1
C19A C 0.2594(3) 0.2543(5) 0.1241(6) 0.0416(19) Uani 0.50 1 d PD . 1
H19A H 0.2590 0.2317 0.1951 0.050 Uiso 0.50 1 calc PR . 1
H19B H 0.2726 0.3027 0.1447 0.050 Uiso 0.50 1 calc PR . 1
C20A C 0.1900(4) 0.2833(5) -0.0875(7) 0.043(2) Uani 0.50 1 d PD . 1
H20A H 0.2002 0.3329 -0.0752 0.051 Uiso 0.50 1 calc PR . 1
H20B H 0.1459 0.2783 -0.1517 0.051 Uiso 0.50 1 calc PR . 1
N2B N 0.1976(3) 0.2134(4) 0.0064(6) 0.046(2) Uani 0.50 1 d PD A 2
C19B C 0.2660(4) 0.2026(5) 0.0988(8) 0.051(2) Uani 0.50 1 d PD . 2
H19C H 0.2655 0.1911 0.1760 0.061 Uiso 0.50 1 calc PR . 2
H19D H 0.2857 0.1636 0.0750 0.061 Uiso 0.50 1 calc PR . 2
C20B C 0.1954(5) 0.2352(6) -0.1115(7) 0.057(3) Uani 0.50 1 d PD . 2
H20C H 0.2122 0.1977 -0.1443 0.069 Uiso 0.50 1 calc PR . 2
H20D H 0.1501 0.2441 -0.1680 0.069 Uiso 0.50 1 calc PR . 2
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
O4 Cu1 O1 176.06(10) . .
O4 Cu1 O1W 90.88(9) . .
O1 Cu1 O1W 86.21(9) . .
O4 Cu1 N1 91.76(10) . 2
O1 Cu1 N1 91.36(10) . 2
O1W Cu1 N1 174.82(10) . 2
O4 Cu1 O7 88.63(10) . .
O1 Cu1 O7 93.97(10) . .
O1W Cu1 O7 89.05(9) . .
N1 Cu1 O7 86.56(10) 2 .
C1 O1 Cu1 114.0(2) . .
Cu1 O1W H1A 121.9 . .
Cu1 O1W H1B 118.8 . .
H1A O1W H1B 107.5 . .
C5 O3 H3A 109.5 . .
C7 O4 Cu1 123.3(2) . .
C11 O6 H6A 109.5 . .
C13 O7 Cu1 129.1(3) . .
C17 N1 C16 116.3(3) . .
C17 N1 Cu1 125.2(2) . 2
C16 N1 Cu1 117.8(2) . 2
O2 C1 O1 123.3(3) . .
O2 C1 C2 118.9(4) . .
O1 C1 C2 117.8(3) . .
C6 C2 C3 119.0(3) . .
C6 C2 C1 120.5(3) . .
C3 C2 C1 120.5(3) . .
C2 C3 C4 121.2(3) . .
C2 C3 H3 119.4 . .
C4 C3 H3 119.4 . .
C3 C4 C3 118.8(5) . 6
C3 C4 C5 120.6(2) . .
C3 C4 C5 120.6(2) 6 .
O3 C5 O3 121.8(7) 6 .
O3 C5 C4 119.1(4) 6 .
O3 C5 C4 119.1(4) . .
C2 C6 C2 120.8(5) . 6
C2 C6 H6 119.6 . .
C2 C6 H6 119.6 6 .
O5 C7 O4 124.8(3) . .
O5 C7 C8 119.8(3) . .
O4 C7 C8 115.3(4) . .
C9 C8 C12 119.1(3) . .
C9 C8 C7 120.7(3) . .
C12 C8 C7 120.2(4) . .
C8 C9 C10 121.0(4) . .
C8 C9 H9 119.5 . .
C10 C9 H9 119.5 . .
C9 C10 C9 118.6(6) 6_565 .
C9 C10 C11 120.7(3) 6_565 .
C9 C10 C11 120.7(3) . .
O6 C11 O6 123.4(7) . 6_565
O6 C11 C10 118.3(4) . .
O6 C11 C10 118.3(4) 6_565 .
C8 C12 C8 121.1(5) 6_565 .
C8 C12 H12 119.4 6_565 .
C8 C12 H12 119.4 . .
O7 C13 N2B 119.6(4) . .
O7 C13 N2A 123.2(4) . .
O7 C13 C14 118.4(3) . .
N2B C13 C14 120.1(4) . .
N2A C13 C14 114.5(4) . .
C18 C14 C15 116.8(3) . .
C18 C14 C13 124.6(3) . .
C15 C14 C13 118.1(4) . .
C14 C15 C16 119.7(4) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
N1 C16 C15 123.3(3) . .
N1 C16 H16 118.3 . .
C15 C16 H16 118.3 . .
N1 C17 C18 123.2(3) . .
N1 C17 H17 118.4 . .
C18 C17 H17 118.4 . .
C14 C18 C17 120.7(3) . .
C14 C18 H18 119.7 . .
C17 C18 H18 119.7 . .
C13 N2A C20A 125.4(6) . .
C13 N2A C19A 118.5(6) . .
C20A N2A C19A 112.7(7) . .
N2A C19A C20A 110.9(7) . 7
N2A C19A H19A 109.5 . .
C20A C19A H19A 109.5 7 .
N2A C19A H19B 109.5 . .
C20A C19A H19B 109.5 7 .
H19A C19A H19B 108.1 . .
N2A C20A C19A 109.1(7) . 7
N2A C20A H20A 109.9 . .
C19A C20A H20A 109.9 7 .
N2A C20A H20B 109.9 . .
C19A C20A H20B 109.9 7 .
H20A C20A H20B 108.3 . .
C13 N2B C19B 121.3(6) . .
C13 N2B C20B 126.6(6) . .
C19B N2B C20B 112.1(8) . .
C20B C19B N2B 110.4(8) 7 .
C20B C19B H19C 109.6 7 .
N2B C19B H19C 109.6 . .
C20B C19B H19D 109.6 7 .
N2B C19B H19D 109.6 . .
H19C C19B H19D 108.1 . .
C19B C20B N2B 110.9(8) 7 .
C19B C20B H20C 109.5 7 .
N2B C20B H20C 109.5 . .
C19B C20B H20D 109.5 7 .
N2B C20B H20D 109.5 . .
H20C C20B H20D 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 1.934(2) .
Cu1 O1 1.945(2) .
Cu1 O1W 1.962(2) .
Cu1 N1 2.018(2) 2
Cu1 O7 2.390(3) .
O1 C1 1.260(4) .
O1W H1A 0.8203 .
O1W H1B 0.8221 .
O2 C1 1.257(4) .
O3 C5 1.263(4) .
O3 H3A 0.8200 .
O4 C7 1.288(4) .
O5 C7 1.234(4) .
O6 C11 1.269(5) .
O6 H6A 0.8200 .
O7 C13 1.216(4) .
N1 C17 1.324(4) .
N1 C16 1.328(4) .
N1 Cu1 2.018(2) 2
C1 C2 1.498(4) .
C2 C6 1.379(4) .
C2 C3 1.383(5) .
C3 C4 1.376(4) .
C3 H3 0.9300 .
C4 C3 1.376(4) 6
C4 C5 1.479(8) .
C5 O3 1.263(4) 6
C6 C2 1.379(4) 6
C6 H6 0.9300 .
C7 C8 1.503(5) .
C8 C9 1.358(5) .
C8 C12 1.391(4) .
C9 C10 1.400(5) .
C9 H9 0.9300 .
C10 C9 1.400(5) 6_565
C10 C11 1.470(9) .
C11 O6 1.269(5) 6_565
C12 C8 1.391(4) 6_565
C12 H12 0.9300 .
C13 N2B 1.321(8) .
C13 N2A 1.427(8) .
C13 C14 1.512(5) .
C14 C18 1.358(5) .
C14 C15 1.362(5) .
C15 C16 1.379(5) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 C18 1.367(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
N2A C20A 1.467(7) .
N2A C19A 1.471(7) .
C19A C20A 1.558(11) 7
C19A H19A 0.9700 .
C19A H19B 0.9700 .
C20A C19A 1.558(11) 7
C20A H20A 0.9700 .
C20A H20B 0.9700 .
N2B C19B 1.482(7) .
N2B C20B 1.477(8) .
C19B C20B 1.439(12) 7
C19B H19C 0.9700 .
C19B H19D 0.9700 .
C20B C19B 1.439(12) 7
C20B H20C 0.9700 .
C20B H20D 0.9700 .
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
O1W H1A O2 0.82 1.85 2.655(3) 167 7_556
O1W H1B O5 0.82 1.88 2.692(3) 172 7_556
