#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/77/4317779.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_4317779
loop_
_publ_author_name
'Xian-He Bu'
'He Liu'
'Miao Du'
'Lei Zhang'
'Ya-Mei Guo'
'Mitsuhiko Shionoya'
'Joan Ribas'
_publ_contact_author_address
;
   Department of Chemistry
   Nankai University
   Tianjin 300071, PR China
;
_publ_contact_author_email       buxh@nankai.edu.cn
_publ_contact_author_fax         86-22-23530850
_publ_contact_author_name        'Xian-He Bu'
_publ_contact_author_phone       86-22-23502809
_publ_section_title
;
 New Mononuclear, Cyclic Tetranuclear, and 1-D Helical-Chain Cu(II)
 Complexes Formed by Metal-Assisted Hydrolysis of
 3,6-Di-2-pyridyl-1,2,4,5-tetrazine (DPTZ): Crystal Structures and
 Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1855
_journal_page_last               1861
_journal_paper_doi               10.1021/ic010955y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C24 H16 N8 O2 Cu 2+, (Cl O4 1-)2, (H2 O)2'
_chemical_formula_sum            'C24 H20 Cl2 Cu N8 O12'
_chemical_formula_weight         746.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 103.24(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.399(3)
_cell_length_b                   10.974(2)
_cell_length_c                   13.618(4)
_cell_measurement_temperature    298.2
_cell_volume                     1512.8(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.8907
_diffrn_measured_fraction_theta_max 0.8907
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3180
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.378
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     214
_refine_ls_number_reflns         1546
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00176|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                1546
_reflns_number_total             3081
_reflns_threshold_expression     F²>3.0σ(F²)
_cod_data_source_file            ic010955y_2.cif
_cod_data_source_block           RGK400rax_Inst._of_Mol._Sc
_cod_original_cell_volume        1512.7(6)
_cod_original_formula_sum        'C24 H20 N8 O12 Cl2 Cu '
_cod_database_code               4317779
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu(1) Cu 0.5000 0.0000 0.5000 0.0442(3) Uani 0.50 d S . .
O(1) O 0.7003(4) -0.3093(4) 0.4869(3) 0.044(1) Uani 1.00 d . . .
N(1) N 0.4365(5) -0.1516(4) 0.5632(4) 0.044(2) Uani 1.00 d . . .
N(2) N 0.6324(6) -0.1193(5) 0.4736(4) 0.046(2) Uani 1.00 d . . .
N(3) N 0.7408(6) -0.1251(5) 0.4306(5) 0.049(2) Uani 1.00 d . . .
N(4) N 0.8861(7) -0.4148(6) 0.3967(6) 0.070(2) Uani 1.00 d . . .
C(1) C 0.3329(7) -0.1617(6) 0.6058(6) 0.051(2) Uani 1.00 d . . .
C(2) C 0.2986(8) -0.2724(7) 0.6420(6) 0.061(2) Uani 1.00 d . . .
C(3) C 0.3704(9) -0.3753(6) 0.6340(6) 0.060(2) Uani 1.00 d . . .
C(4) C 0.4780(8) -0.3652(6) 0.5895(6) 0.054(2) Uani 1.00 d . . .
C(5) C 0.5066(6) -0.2537(6) 0.5558(5) 0.043(2) Uani 1.00 d . . .
C(6) C 0.6132(7) -0.2275(5) 0.5058(5) 0.042(2) Uani 1.00 d . . .
C(7) C 0.7797(7) -0.2374(6) 0.4406(5) 0.047(2) Uani 1.00 d . . .
C(8) C 0.8929(7) -0.2934(6) 0.4108(5) 0.050(2) Uani 1.00 d . . .
C(9) C 0.9963(8) -0.2228(8) 0.4003(7) 0.070(3) Uani 1.00 d . . .
C(10) C 1.1017(9) -0.280(1) 0.3724(8) 0.088(4) Uani 1.00 d . . .
C(11) C 1.0984(9) -0.4024(10) 0.3605(8) 0.086(3) Uani 1.00 d . . .
C(12) C 0.9900(10) -0.4660(8) 0.3703(8) 0.080(3) Uani 1.00 d . . .
H(1) H 0.2817 -0.0914 0.6113 0.0611 Uiso 1.00 calc . . .
H(2) H 0.2252 -0.2769 0.6724 0.0735 Uiso 1.00 calc . . .
H(3) H 0.3474 -0.4515 0.6583 0.0723 Uiso 1.00 calc . . .
H(4) H 0.5302 -0.4344 0.5828 0.0653 Uiso 1.00 calc . . .
H(9) H 0.9965 -0.1374 0.4117 0.0836 Uiso 1.00 calc . . .
H(10) H 1.1746 -0.2338 0.3617 0.1062 Uiso 1.00 calc . . .
H(11) H 1.1719 -0.4438 0.3455 0.1036 Uiso 1.00 calc . . .
H(12) H 0.9877 -0.5512 0.3576 0.0963 Uiso 1.00 calc . . .
Cl(1) Cl 0.4324(2) -0.3360(2) 0.2288(2) 0.0592(6) Uani 1.00 d . . .
O(3) O 0.343(1) -0.2451(9) 0.1907(7) 0.178(4) Uani 1.00 d . . .
O(4) O 0.423(1) -0.3631(9) 0.3287(7) 0.162(4) Uani 1.00 d . . .
O(5) O 0.400(1) -0.433(1) 0.178(1) 0.257(7) Uani 1.00 d . . .
O(6) O 0.552(1) -0.305(2) 0.243(1) 0.308(9) Uani 1.00 d . . .
O(2) O 0.3531(6) -0.0539(5) 0.3493(5) 0.084(2) Uani 1.00 d . . .
H(2O) H 0.2833 0.0101 0.3322 0.1013 Uiso 1.00 calc . . .
H(2O') H 0.3595 -0.1297 0.2947 0.1013 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cu Cu 0.320 1.265
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N(1) Cu(1) N(1) 180.0 1_555 1_555 3_656 yes
N(1) Cu(1) N(2) 81.1(2) 1_555 1_555 1_555 yes
N(1) Cu(1) N(2) 98.9(2) 1_555 1_555 3_656 yes
N(1) Cu(1) N(2) 98.9(2) 3_656 1_555 1_555 yes
N(1) Cu(1) N(2) 81.1(2) 3_656 1_555 3_656 yes
N(2) Cu(1) N(2) 180.0 1_555 1_555 3_656 yes
C(6) O(1) C(7) 101.8(5) 1_555 1_555 1_555 yes
Cu(1) N(1) C(1) 128.1(4) 1_555 1_555 1_555 yes
Cu(1) N(1) C(5) 114.1(4) 1_555 1_555 1_555 yes
C(1) N(1) C(5) 117.7(5) 1_555 1_555 1_555 yes
Cu(1) N(2) N(3) 140.3(4) 1_555 1_555 1_555 yes
Cu(1) N(2) C(6) 112.0(4) 1_555 1_555 1_555 yes
N(3) N(2) C(6) 107.7(5) 1_555 1_555 1_555 yes
N(2) N(3) C(7) 105.3(5) 1_555 1_555 1_555 yes
C(8) N(4) C(12) 115.8(7) 1_555 1_555 1_555 yes
N(1) C(1) C(2) 121.6(6) 1_555 1_555 1_555 yes
C(1) C(2) C(3) 120.2(7) 1_555 1_555 1_555 yes
C(2) C(3) C(4) 118.4(6) 1_555 1_555 1_555 yes
C(3) C(4) C(5) 118.4(6) 1_555 1_555 1_555 yes
N(1) C(5) C(4) 123.7(6) 1_555 1_555 1_555 yes
N(1) C(5) C(6) 110.7(5) 1_555 1_555 1_555 yes
C(4) C(5) C(6) 125.6(6) 1_555 1_555 1_555 yes
O(1) C(6) N(2) 112.6(6) 1_555 1_555 1_555 yes
O(1) C(6) C(5) 125.3(5) 1_555 1_555 1_555 yes
N(2) C(6) C(5) 122.1(5) 1_555 1_555 1_555 yes
O(1) C(7) N(3) 112.5(6) 1_555 1_555 1_555 yes
O(1) C(7) C(8) 119.0(6) 1_555 1_555 1_555 yes
N(3) C(7) C(8) 128.4(7) 1_555 1_555 1_555 yes
N(4) C(8) C(7) 115.8(7) 1_555 1_555 1_555 yes
N(4) C(8) C(9) 124.5(7) 1_555 1_555 1_555 yes
C(7) C(8) C(9) 119.7(7) 1_555 1_555 1_555 yes
C(8) C(9) C(10) 117.7(8) 1_555 1_555 1_555 yes
C(9) C(10) C(11) 118.8(9) 1_555 1_555 1_555 yes
C(10) C(11) C(12) 119.8(9) 1_555 1_555 1_555 yes
N(4) C(12) C(11) 123.4(8) 1_555 1_555 1_555 yes
O(3) Cl(1) O(4) 108.7(6) 1_555 1_555 1_555 yes
O(3) Cl(1) O(5) 109.1(8) 1_555 1_555 1_555 yes
O(3) Cl(1) O(6) 114(1) 1_555 1_555 1_555 yes
O(4) Cl(1) O(5) 106.2(10) 1_555 1_555 1_555 yes
O(4) Cl(1) O(6) 101.3(9) 1_555 1_555 1_555 yes
O(5) Cl(1) O(6) 116(1) 1_555 1_555 1_555 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu(1) N(1) 2.051(5) . . yes
Cu(1) N(1) 2.051(5) . 3_656 yes
Cu(1) N(2) 1.991(5) . . yes
Cu(1) N(2) 1.991(5) . 3_656 yes
O(1) C(6) 1.341(7) . . yes
O(1) C(7) 1.393(8) . . yes
N(1) C(1) 1.339(9) . . yes
N(1) C(5) 1.352(8) . . yes
N(2) N(3) 1.386(8) . . yes
N(2) C(6) 1.297(8) . . yes
N(3) C(7) 1.295(8) . . yes
N(4) C(8) 1.345(9) . . yes
N(4) C(12) 1.34(1) . . yes
C(1) C(2) 1.389(10) . . yes
C(2) C(3) 1.37(1) . . yes
C(3) C(4) 1.39(1) . . yes
C(4) C(5) 1.364(9) . . yes
C(5) C(6) 1.456(9) . . yes
C(7) C(8) 1.464(10) . . yes
C(8) C(9) 1.36(1) . . yes
C(9) C(10) 1.39(1) . . yes
C(10) C(11) 1.35(1) . . yes
C(11) C(12) 1.36(1) . . yes
Cl(1) O(3) 1.383(9) . . yes
Cl(1) O(4) 1.419(10) . . yes
Cl(1) O(5) 1.270(10) . . yes
Cl(1) O(6) 1.26(1) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O(1) O(3) 2.893(10) . 4_545 ?
O(1) O(4) 3.24(1) . . ?
O(1) O(6) 3.33(2) . . ?
N(1) O(2) 3.039(8) . . ?
N(1) O(2) 3.178(8) . 3_656 ?
N(2) O(2) 3.047(8) . 3_656 ?
N(2) O(2) 3.092(8) . . ?
N(2) O(5) 3.50(1) . 4_545 ?
N(2) O(3) 3.57(1) . 4_545 ?
N(3) O(5) 3.46(2) . 4_545 ?
N(3) O(6) 3.46(2) . . ?
N(4) C(12) 3.40(1) . 3_746 ?
N(4) C(3) 3.48(1) . 3_646 ?
C(2) O(6) 3.29(1) . 4_445 ?
C(3) O(4) 3.55(1) . 3_646 ?
C(4) O(4) 3.27(1) . 3_646 ?
C(4) O(4) 3.47(1) . . ?
C(5) O(4) 3.24(1) . . ?
C(5) O(3) 3.56(1) . 4_545 ?
C(6) O(3) 3.06(1) . 4_545 ?
C(6) O(4) 3.12(1) . . ?
C(6) O(2) 3.584(9) . . ?
C(6) O(6) 3.59(2) . . ?
C(7) O(6) 3.24(2) . . ?
C(7) O(3) 3.32(1) . 4_545 ?
C(9) O(5) 3.60(1) . 2_655 ?
C(11) O(2) 3.44(1) . 2_645 ?
C(11) O(4) 3.52(2) . 1_655 ?
C(12) C(12) 3.57(2) . 3_746 ?
O(3) O(2) 3.00(1) . . ?
O(4) O(2) 3.49(1) . . ?
O(5) O(2) 2.90(2) . 2_545 ?
