#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:41:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179257 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/77/4317778.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_4317778
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_sum            'C30 H26 Cu4 N16 O18'
_chemical_formula_weight         1150.81
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.587(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3422(14)
_cell_length_b                   15.987(2)
_cell_length_c                   13.963(2)
_cell_measurement_temperature    298(2)
_cell_volume                     1976.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8103
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.224
_exptl_absorpt_correction_T_max  0.6063
_exptl_absorpt_correction_T_min  0.4699
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         3490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0427P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                2478
_reflns_number_total             3490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010955y_1.cif
_cod_data_source_block           complex3
_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 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1976.6(5)
_cod_database_code               4317778
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.03710(6) 0.04511(3) 0.64230(4) 0.02796(16) Uani 1 1 d . . .
Cu2 Cu 0.13949(6) 0.28169(3) 0.50271(4) 0.02965(16) Uani 1 1 d . . .
O1 O 0.1998(3) 0.03149(16) 0.4917(2) 0.0315(7) Uani 1 1 d . . .
O2 O -0.0391(3) 0.28409(16) 0.5478(2) 0.0331(7) Uani 1 1 d . . .
O3 O 0.2793(3) 0.33423(18) 0.6677(2) 0.0411(8) Uani 1 1 d . . .
O4 O 0.3554(5) 0.3169(2) 0.8294(3) 0.0755(13) Uani 1 1 d . . .
O5 O 0.2536(5) 0.2157(2) 0.7359(3) 0.0662(11) Uani 1 1 d . . .
O6 O -0.0866(3) -0.03829(17) 0.7348(2) 0.0353(7) Uani 1 1 d . . .
O7 O 0.0616(4) 0.0468(2) 0.8424(2) 0.0529(9) Uani 1 1 d . . .
O8 O -0.0335(4) -0.0602(2) 0.8958(2) 0.0471(9) Uani 1 1 d . . .
O9 O 0.1443(4) -0.0166(3) 0.6525(3) 0.0420(9) Uani 1 1 d . . .
N1 N 0.3041(4) 0.24039(19) 0.4493(3) 0.0272(8) Uani 1 1 d . . .
N2 N 0.1051(4) 0.39651(19) 0.4469(2) 0.0279(8) Uani 1 1 d . . .
N3 N 0.1252(4) 0.52703(19) 0.4029(3) 0.0313(9) Uani 1 1 d . . .
N4 N 0.1225(4) 0.16380(19) 0.5248(2) 0.0257(8) Uani 1 1 d . . .
N5 N 0.0085(4) 0.14229(19) 0.5652(2) 0.0245(8) Uani 1 1 d . . .
N8 N 0.2940(4) 0.2885(2) 0.7436(3) 0.0352(9) Uani 1 1 d . . .
N6 N -0.2004(4) 0.1212(2) 0.6516(2) 0.0289(8) Uani 1 1 d . . .
N7 N -0.0170(4) -0.0171(2) 0.8275(3) 0.0344(9) Uani 1 1 d . . .
C1 C 0.2032(4) 0.1110(2) 0.4925(3) 0.0244(9) Uani 1 1 d . . .
C2 C 0.3132(5) 0.1556(2) 0.4521(3) 0.0263(9) Uani 1 1 d . . .
C3 C 0.4207(5) 0.1141(3) 0.4225(3) 0.0348(11) Uani 1 1 d . . .
C4 C 0.5203(6) 0.1591(3) 0.3880(4) 0.0450(13) Uani 1 1 d . . .
C5 C 0.5113(5) 0.2446(3) 0.3844(4) 0.0435(13) Uani 1 1 d . . .
C6 C 0.4026(5) 0.2830(3) 0.4157(4) 0.0376(11) Uani 1 1 d . . .
C7 C -0.0384(6) 0.4265(3) 0.3895(4) 0.0410(12) Uani 1 1 d . . .
C8 C -0.0211(8) 0.5053(4) 0.3651(4) 0.0607(19) Uani 1 1 d . . .
C9 C 0.1921(6) 0.4591(3) 0.4501(4) 0.0422(12) Uani 1 1 d . . .
C10 C -0.0642(4) 0.2111(2) 0.5747(3) 0.0255(9) Uani 1 1 d . . .
C11 C -0.1851(4) 0.1994(2) 0.6210(3) 0.0252(9) Uani 1 1 d . . .
C12 C -0.2763(5) 0.2644(3) 0.6317(3) 0.0345(11) Uani 1 1 d . . .
C13 C -0.3905(6) 0.2471(3) 0.6717(4) 0.0438(13) Uani 1 1 d . . .
C14 C -0.4089(5) 0.1666(3) 0.6994(4) 0.0406(12) Uani 1 1 d . . .
C15 C -0.3126(5) 0.1060(3) 0.6899(3) 0.0351(11) Uani 1 1 d . . .
H1 H 0.169(6) -0.010(3) 0.599(4) 0.055(17) Uiso 1 1 d . . .
H2 H 0.591(5) 0.133(3) 0.373(3) 0.046(14) Uiso 1 1 d . . .
H3 H -0.456(5) 0.286(2) 0.679(3) 0.030(11) Uiso 1 1 d . . .
H4 H 0.416(4) 0.056(2) 0.425(3) 0.031(12) Uiso 1 1 d . . .
H5 H -0.309(4) 0.057(2) 0.712(3) 0.025(11) Uiso 1 1 d . . .
H6 H 0.299(5) 0.461(3) 0.482(3) 0.049(14) Uiso 1 1 d . . .
H7 H -0.263(5) 0.316(3) 0.611(3) 0.041(13) Uiso 1 1 d . . .
H8 H -0.497(6) 0.155(3) 0.728(4) 0.066(15) Uiso 1 1 d . . .
H9 H 0.394(4) 0.339(2) 0.417(3) 0.026(11) Uiso 1 1 d . . .
H10 H 0.580(5) 0.274(3) 0.363(3) 0.053(15) Uiso 1 1 d . . .
H11 H -0.071(6) 0.538(3) 0.335(4) 0.07(2) Uiso 1 1 d . . .
H12 H -0.120(5) 0.393(3) 0.381(3) 0.044(14) Uiso 1 1 d . . .
H14 H 0.136(6) -0.059(3) 0.648(4) 0.06(2) Uiso 1 1 d . . .
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
O9 Cu1 N6 169.74(16) . . ?
O9 Cu1 O6 89.41(15) . . ?
N6 Cu1 O6 91.45(13) . . ?
O9 Cu1 N5 95.97(16) . . ?
N6 Cu1 N5 81.96(13) . . ?
O6 Cu1 N5 170.93(12) . . ?
O9 Cu1 O1 97.03(14) . 3_556 ?
N6 Cu1 O1 93.23(12) . 3_556 ?
O6 Cu1 O1 86.74(11) . 3_556 ?
N5 Cu1 O1 99.79(11) . 3_556 ?
N4 Cu2 O2 81.14(12) . . ?
N4 Cu2 N2 163.66(14) . . ?
O2 Cu2 N2 93.47(12) . . ?
N4 Cu2 N1 81.40(13) . . ?
O2 Cu2 N1 161.64(12) . . ?
N2 Cu2 N1 101.79(13) . . ?
N4 Cu2 O3 103.64(12) . . ?
O2 Cu2 O3 86.78(11) . . ?
N2 Cu2 O3 91.36(12) . . ?
N1 Cu2 O3 102.84(12) . . ?
C1 O1 Cu1 122.5(2) . 3_556 ?
C10 O2 Cu2 109.4(2) . . ?
N8 O3 Cu2 118.9(3) . . ?
N7 O6 Cu1 108.9(2) . . ?
C6 N1 C2 118.2(4) . . ?
C6 N1 Cu2 130.5(3) . . ?
C2 N1 Cu2 111.3(3) . . ?
C9 N2 C7 103.4(4) . . ?
C9 N2 Cu2 133.6(3) . . ?
C7 N2 Cu2 123.0(3) . . ?
C9 N3 C8 104.1(4) . . ?
C1 N4 N5 125.4(3) . . ?
C1 N4 Cu2 119.5(3) . . ?
N5 N4 Cu2 114.7(2) . . ?
C10 N5 N4 108.5(3) . . ?
C10 N5 Cu1 112.7(2) . . ?
N4 N5 Cu1 136.4(2) . . ?
O5 N8 O4 118.1(4) . . ?
O5 N8 O3 122.2(4) . . ?
O4 N8 O3 119.7(4) . . ?
C15 N6 C11 118.1(4) . . ?
C15 N6 Cu1 128.9(3) . . ?
C11 N6 Cu1 112.8(2) . . ?
O8 N7 O7 123.3(4) . . ?
O8 N7 O6 118.9(4) . . ?
O7 N7 O6 117.8(4) . . ?
O1 C1 N4 129.4(4) . . ?
O1 C1 C2 119.4(3) . . ?
N4 C1 C2 111.3(3) . . ?
N1 C2 C3 121.3(4) . . ?
N1 C2 C1 116.2(3) . . ?
C3 C2 C1 122.5(4) . . ?
C2 C3 C4 119.5(4) . . ?
C5 C4 C3 119.6(4) . . ?
C4 C5 C6 118.5(5) . . ?
N1 C6 C5 122.9(5) . . ?
C8 C7 N2 107.3(5) . . ?
C7 C8 N3 109.7(5) . . ?
N2 C9 N3 115.6(5) . . ?
O2 C10 N5 125.8(3) . . ?
O2 C10 C11 118.9(3) . . ?
N5 C10 C11 115.3(3) . . ?
N6 C11 C12 122.3(4) . . ?
N6 C11 C10 115.4(3) . . ?
C12 C11 C10 122.3(4) . . ?
C13 C12 C11 118.3(4) . . ?
C14 C13 C12 119.1(4) . . ?
C15 C14 C13 119.7(4) . . ?
N6 C15 C14 122.4(4) . . ?
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 O9 1.927(3) . ?
Cu1 N6 1.987(3) . ?
Cu1 O6 2.010(3) . ?
Cu1 N5 2.011(3) . ?
Cu1 O1 2.345(3) 3_556 ?
Cu2 N4 1.924(3) . ?
Cu2 O2 1.962(3) . ?
Cu2 N2 1.980(3) . ?
Cu2 N1 2.022(3) . ?
Cu2 O3 2.409(3) . ?
O1 C1 1.272(4) . ?
O1 Cu1 2.345(3) 3_556 ?
O2 C10 1.271(4) . ?
O3 N8 1.258(4) . ?
O4 N8 1.237(4) . ?
O5 N8 1.219(4) . ?
O6 N7 1.295(4) . ?
O7 N7 1.236(4) . ?
O8 N7 1.225(4) . ?
N1 C6 1.344(5) . ?
N1 C2 1.357(5) . ?
N2 C9 1.281(5) . ?
N2 C7 1.408(5) . ?
N3 C9 1.319(6) . ?
N3 C8 1.345(7) . ?
N4 C1 1.303(5) . ?
N4 N5 1.398(4) . ?
N5 C10 1.321(5) . ?
N6 C15 1.342(5) . ?
N6 C11 1.344(5) . ?
C1 C2 1.501(5) . ?
C2 C3 1.373(6) . ?
C3 C4 1.378(6) . ?
C4 C5 1.371(7) . ?
C5 C6 1.372(6) . ?
C7 C8 1.329(7) . ?
C10 C11 1.481(5) . ?
C11 C12 1.381(6) . ?
C12 C13 1.381(6) . ?
C13 C14 1.370(6) . ?
C14 C15 1.358(6) . ?
