#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:00:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179088 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/50/4305005.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_4305005
loop_
_publ_author_name
'Feng-Qin Wang'
'Wei-Hua Mu'
'Xiang-Jun Zheng'
'Li-Cun Li'
'De-Cai Fang'
'Lin-Pei Jin'
_publ_section_title
;
Hydrothermal Reaction of Cu(II)/Pyrazine-2,3,5-tricarboxylic acid and
Characterization of the Copper(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5225
_journal_page_last               5233
_journal_paper_doi               10.1021/ic8001916
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C30 H18 Cu3 N8 O8'
_chemical_formula_weight         809.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6173(6)
_cell_length_b                   8.6173(6)
_cell_length_c                   37.986(5)
_cell_measurement_reflns_used    5784
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.60
_cell_volume                     2820.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            15925
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.313
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0375P)²+3.2324P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                2566
_reflns_number_total             2886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8001916-file003_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to
'constr' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4305005
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -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 0.39695(5) 0.60305(5) 0.7500 0.02455(16) Uani 1 2 d S . .
Cu2 Cu -0.08890(5) 0.89058(6) 0.701442(11) 0.02371(13) Uani 1 1 d . . .
O1 O 0.5969(3) 0.5925(3) 0.72653(7) 0.0291(6) Uani 1 1 d . . .
O2 O 0.7309(3) 0.6970(3) 0.68225(7) 0.0282(6) Uani 1 1 d . . .
O3 O 0.0428(3) 0.9171(4) 0.66033(7) 0.0281(6) Uani 1 1 d . . .
O4 O 0.0763(3) 0.7622(3) 0.71975(7) 0.0264(6) Uani 1 1 d . . .
N1 N 0.3359(4) 0.7231(4) 0.70900(8) 0.0211(7) Uani 1 1 d . . .
N2 N 0.2978(4) 0.8828(4) 0.64495(8) 0.0315(8) Uani 1 1 d . . .
N3 N -0.2367(4) 1.0535(4) 0.68687(9) 0.0252(7) Uani 1 1 d . . .
N4 N -0.2015(4) 0.9169(4) 0.74708(8) 0.0229(7) Uani 1 1 d . . .
C1 C 0.6070(4) 0.6759(4) 0.69831(10) 0.0221(8) Uani 1 1 d . . .
C2 C 0.4588(5) 0.7463(5) 0.68616(10) 0.0234(8) Uani 1 1 d . . .
C3 C 0.4374(4) 0.8227(5) 0.65548(10) 0.0282(10) Uani 1 1 d . . .
H3 H 0.5224 0.8351 0.6407 0.034 Uiso 1 1 calc R . .
C4 C 0.1803(5) 0.8631(5) 0.66653(10) 0.0239(9) Uani 1 1 d . . .
C5 C 0.1968(4) 0.7777(5) 0.70001(10) 0.0213(8) Uani 1 1 d . . .
C6 C -0.2451(5) 1.1163(5) 0.65487(11) 0.0330(10) Uani 1 1 d . . .
H6 H -0.1777 1.0813 0.6375 0.040 Uiso 1 1 calc R . .
C7 C -0.3500(5) 1.2314(6) 0.64668(12) 0.0373(11) Uani 1 1 d . . .
H7 H -0.3550 1.2718 0.6240 0.045 Uiso 1 1 calc R . .
C8 C -0.4472(5) 1.2853(6) 0.67264(13) 0.0425(12) Uani 1 1 d . . .
H8 H -0.5176 1.3642 0.6678 0.051 Uiso 1 1 calc R . .
C9 C -0.4395(5) 1.2214(5) 0.70606(11) 0.0334(10) Uani 1 1 d . . .
H9 H -0.5038 1.2570 0.7240 0.040 Uiso 1 1 calc R . .
C10 C -0.3338(4) 1.1031(5) 0.71216(10) 0.0250(8) Uani 1 1 d . . .
C11 C -0.3166(4) 1.0233(5) 0.74625(10) 0.0225(8) Uani 1 1 d . . .
C12 C -0.4091(5) 1.0492(5) 0.77567(11) 0.0350(10) Uani 1 1 d . . .
H12 H -0.4893 1.1213 0.7749 0.042 Uiso 1 1 calc R . .
C13 C -0.3797(6) 0.9657(6) 0.80613(11) 0.0398(11) Uani 1 1 d . . .
H13 H -0.4398 0.9822 0.8261 0.048 Uiso 1 1 calc R . .
C14 C -0.2624(6) 0.8593(6) 0.80678(11) 0.0379(11) Uani 1 1 d . . .
H14 H -0.2421 0.8025 0.8271 0.045 Uiso 1 1 calc R . .
C15 C -0.1742(5) 0.8372(5) 0.77680(11) 0.0313(9) Uani 1 1 d . . .
H15 H -0.0939 0.7652 0.7772 0.038 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
_geom_angle_publ_flag
O1 Cu1 N1 84.09(12) 8_666 8_666 ?
O1 Cu1 N1 148.55(13) 8_666 . ?
N1 Cu1 N1 110.77(18) 8_666 . ?
O1 Cu1 O1 97.35(16) 8_666 . ?
N1 Cu1 O1 148.56(13) 8_666 . ?
N1 Cu1 O1 84.08(12) . . ?
O4 Cu2 O3 85.78(11) . . ?
O4 Cu2 N3 169.44(13) . . ?
O3 Cu2 N3 93.88(13) . . ?
O4 Cu2 N4 96.33(12) . . ?
O3 Cu2 N4 165.12(13) . . ?
N3 Cu2 N4 81.35(13) . . ?
O4 Cu2 O2 100.87(11) . 1_455 ?
O3 Cu2 O2 102.47(11) . 1_455 ?
N3 Cu2 O2 89.52(12) . 1_455 ?
N4 Cu2 O2 91.63(12) . 1_455 ?
C1 O1 Cu1 114.5(2) . . ?
C1 O2 Cu2 120.7(3) . 1_655 ?
C4 O3 Cu2 110.2(2) . . ?
C5 O4 Cu2 109.0(2) . . ?
C5 N1 C2 118.5(3) . . ?
C5 N1 Cu1 129.6(3) . . ?
C2 N1 Cu1 111.9(2) . . ?
C4 N2 C3 116.5(3) . . ?
C6 N3 C10 119.3(3) . . ?
C6 N3 Cu2 125.4(3) . . ?
C10 N3 Cu2 115.3(3) . . ?
C15 N4 C11 119.7(4) . . ?
C15 N4 Cu2 125.9(3) . . ?
C11 N4 Cu2 114.4(3) . . ?
O2 C1 O1 123.1(3) . . ?
O2 C1 C2 121.7(3) . . ?
O1 C1 C2 115.2(3) . . ?
C3 C2 N1 120.5(3) . . ?
C3 C2 C1 125.7(3) . . ?
N1 C2 C1 113.8(3) . . ?
C2 C3 N2 123.8(3) . . ?
C2 C3 H3 118.1 . . ?
N2 C3 H3 118.1 . . ?
O3 C4 N2 123.1(3) . . ?
O3 C4 C5 115.1(3) . . ?
N2 C4 C5 121.9(3) . . ?
O4 C5 N1 122.6(3) . . ?
O4 C5 C4 118.4(3) . . ?
N1 C5 C4 118.9(3) . . ?
N3 C6 C7 122.3(4) . . ?
N3 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 C9 119.6(4) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C9 C10 118.4(4) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
N3 C10 C9 121.6(4) . . ?
N3 C10 C11 114.7(3) . . ?
C9 C10 C11 123.8(4) . . ?
N4 C11 C12 120.7(4) . . ?
N4 C11 C10 114.3(3) . . ?
C12 C11 C10 125.0(4) . . ?
C13 C12 C11 118.9(4) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C14 C13 C12 119.9(4) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 119.0(4) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
N4 C15 C14 121.8(4) . . ?
N4 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
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 O1 1.942(3) 8_666 ?
Cu1 N1 1.942(3) 8_666 ?
Cu1 N1 1.942(3) . ?
Cu1 O1 1.942(3) . ?
Cu2 O4 1.932(3) . ?
Cu2 O3 1.944(3) . ?
Cu2 N3 1.975(3) . ?
Cu2 N4 2.000(3) . ?
Cu2 O2 2.393(3) 1_455 ?
O1 C1 1.293(5) . ?
O2 C1 1.243(5) . ?
O2 Cu2 2.393(3) 1_655 ?
O3 C4 1.295(5) . ?
O4 C5 1.288(4) . ?
N1 C5 1.332(5) . ?
N1 C2 1.384(5) . ?
N2 C4 1.313(5) . ?
N2 C3 1.370(5) . ?
N3 C6 1.333(5) . ?
N3 C10 1.344(5) . ?
N4 C15 1.342(5) . ?
N4 C11 1.351(5) . ?
C1 C2 1.487(5) . ?
C2 C3 1.351(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.476(5) . ?
C6 C7 1.377(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.375(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.385(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.387(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.474(6) . ?
C11 C12 1.391(6) . ?
C12 C13 1.386(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.365(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.382(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Cu1 O1 C1 154.9(3) 8_666 . . . ?
N1 Cu1 O1 C1 -114.4(3) 8_666 . . . ?
N1 Cu1 O1 C1 6.5(3) . . . . ?
O4 Cu2 O3 C4 -10.5(3) . . . . ?
N3 Cu2 O3 C4 158.9(3) . . . . ?
N4 Cu2 O3 C4 88.3(5) . . . . ?
O2 Cu2 O3 C4 -110.7(3) 1_455 . . . ?
O3 Cu2 O4 C5 10.7(3) . . . . ?
N3 Cu2 O4 C5 -77.8(7) . . . . ?
N4 Cu2 O4 C5 -154.5(3) . . . . ?
O2 Cu2 O4 C5 112.6(3) 1_455 . . . ?
O1 Cu1 N1 C5 79.9(4) 8_666 . . . ?
N1 Cu1 N1 C5 -34.3(3) 8_666 . . . ?
O1 Cu1 N1 C5 174.3(4) . . . . ?
O1 Cu1 N1 C2 -97.4(3) 8_666 . . . ?
N1 Cu1 N1 C2 148.4(3) 8_666 . . . ?
O1 Cu1 N1 C2 -3.0(3) . . . . ?
O4 Cu2 N3 C6 102.0(7) . . . . ?
O3 Cu2 N3 C6 14.2(4) . . . . ?
N4 Cu2 N3 C6 -180.0(4) . . . . ?
O2 Cu2 N3 C6 -88.2(4) 1_455 . . . ?
O4 Cu2 N3 C10 -77.3(8) . . . . ?
O3 Cu2 N3 C10 -165.1(3) . . . . ?
N4 Cu2 N3 C10 0.7(3) . . . . ?
O2 Cu2 N3 C10 92.5(3) 1_455 . . . ?
O4 Cu2 N4 C15 -11.4(3) . . . . ?
O3 Cu2 N4 C15 -108.8(5) . . . . ?
N3 Cu2 N4 C15 179.0(3) . . . . ?
O2 Cu2 N4 C15 89.7(3) 1_455 . . . ?
O4 Cu2 N4 C11 170.3(3) . . . . ?
O3 Cu2 N4 C11 72.9(6) . . . . ?
N3 Cu2 N4 C11 0.7(3) . . . . ?
O2 Cu2 N4 C11 -88.6(3) 1_455 . . . ?
Cu2 O2 C1 O1 -82.1(4) 1_655 . . . ?
Cu2 O2 C1 C2 97.8(4) 1_655 . . . ?
Cu1 O1 C1 O2 171.6(3) . . . . ?
Cu1 O1 C1 C2 -8.3(4) . . . . ?
C5 N1 C2 C3 0.0(6) . . . . ?
Cu1 N1 C2 C3 177.6(3) . . . . ?
C5 N1 C2 C1 -178.1(4) . . . . ?
Cu1 N1 C2 C1 -0.4(4) . . . . ?
O2 C1 C2 C3 8.0(6) . . . . ?
O1 C1 C2 C3 -172.1(4) . . . . ?
O2 C1 C2 N1 -174.1(4) . . . . ?
O1 C1 C2 N1 5.8(5) . . . . ?
N1 C2 C3 N2 0.7(7) . . . . ?
C1 C2 C3 N2 178.5(4) . . . . ?
C4 N2 C3 C2 0.0(6) . . . . ?
Cu2 O3 C4 N2 -171.5(3) . . . . ?
Cu2 O3 C4 C5 8.2(4) . . . . ?
C3 N2 C4 O3 178.3(4) . . . . ?
C3 N2 C4 C5 -1.3(6) . . . . ?
Cu2 O4 C5 N1 169.1(3) . . . . ?
Cu2 O4 C5 C4 -9.2(4) . . . . ?
C2 N1 C5 O4 -179.6(4) . . . . ?
Cu1 N1 C5 O4 3.3(6) . . . . ?
C2 N1 C5 C4 -1.2(5) . . . . ?
Cu1 N1 C5 C4 -178.4(3) . . . . ?
O3 C4 C5 O4 0.8(5) . . . . ?
N2 C4 C5 O4 -179.6(4) . . . . ?
O3 C4 C5 N1 -177.7(4) . . . . ?
N2 C4 C5 N1 2.0(6) . . . . ?
C10 N3 C6 C7 0.2(7) . . . . ?
Cu2 N3 C6 C7 -179.1(4) . . . . ?
N3 C6 C7 C8 1.3(7) . . . . ?
C6 C7 C8 C9 -1.1(8) . . . . ?
C7 C8 C9 C10 -0.5(7) . . . . ?
C6 N3 C10 C9 -1.9(6) . . . . ?
Cu2 N3 C10 C9 177.4(3) . . . . ?
C6 N3 C10 C11 178.7(4) . . . . ?
Cu2 N3 C10 C11 -1.9(4) . . . . ?
C8 C9 C10 N3 2.1(7) . . . . ?
C8 C9 C10 C11 -178.6(4) . . . . ?
C15 N4 C11 C12 -1.2(6) . . . . ?
Cu2 N4 C11 C12 177.3(3) . . . . ?
C15 N4 C11 C10 179.7(3) . . . . ?
Cu2 N4 C11 C10 -1.9(5) . . . . ?
N3 C10 C11 N4 2.5(5) . . . . ?
C9 C10 C11 N4 -176.8(4) . . . . ?
N3 C10 C11 C12 -176.6(4) . . . . ?
C9 C10 C11 C12 4.1(7) . . . . ?
N4 C11 C12 C13 1.0(7) . . . . ?
C10 C11 C12 C13 -179.9(4) . . . . ?
C11 C12 C13 C14 -0.6(7) . . . . ?
C12 C13 C14 C15 0.2(8) . . . . ?
C11 N4 C15 C14 0.8(6) . . . . ?
Cu2 N4 C15 C14 -177.4(3) . . . . ?
C13 C14 C15 N4 -0.4(7) . . . . ?
