#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/05/4320569.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_4320569
loop_
_publ_author_name
'Bao-Qing Ma'
'Hao-Ling Sun'
'Song Gao'
'Guang-Xian Xu'
_publ_section_title
;
 Variable Dimensionality from Mononuclear and Trinuclear to One and Two
 Dimensions: A Series of Copper(II) Compounds with 4,4'-Dipyridine Dioxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6247
_journal_page_last               6253
_journal_paper_doi               10.1021/ic0104712
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H24 Cl Cu0.5 N6 O10'
_chemical_formula_weight         695.77
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.719(3)
_cell_angle_beta                 97.282(5)
_cell_angle_gamma                98.254(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9729(5)
_cell_length_b                   11.6632(11)
_cell_length_c                   14.3691(12)
_cell_measurement_temperature    293(2)
_cell_volume                     1418.3(2)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Denzo & Maxus'
_computing_molecular_graphics    'Siemens SHELXTL (1990)'
_computing_publication_material  'SIemens SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.71
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.1001
_diffrn_reflns_av_sigmaI/netI    0.0876
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21777
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            'organge red'
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             715
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         4973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0644
_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)+(0.0553P)²+1.8874P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                3314
_reflns_number_total             4973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0104712_2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_formula_sum        'C30 H24 Cl Cu0.50 N6 O10'
_cod_database_code               4320569
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.0000 0.0000 0.0000 0.0341(2) Uani 1 2 d S . .
Cl1 Cl 0.27221(16) 0.29714(13) -0.32107(9) 0.0581(4) Uani 1 1 d . . .
O1 O 0.2217(3) 0.0220(3) 0.0476(2) 0.0454(8) Uani 1 1 d . . .
O2 O 0.8225(4) -0.6081(3) -0.0738(3) 0.0585(10) Uani 1 1 d . . .
O3 O 0.0740(4) 0.0212(3) -0.1448(2) 0.0509(9) Uani 1 1 d . . .
O4 O -0.5659(4) 0.1464(4) -0.6926(3) 0.0652(11) Uani 1 1 d . . .
O5 O 0.0176(4) 0.1775(3) 0.0398(2) 0.0443(8) Uani 1 1 d . . .
O6 O 0.1966(5) 0.7285(4) 0.6880(3) 0.0687(11) Uani 1 1 d . . .
O7 O 0.3207(7) 0.2107(4) -0.2776(3) 0.1104(19) Uani 1 1 d . . .
O8 O 0.4057(6) 0.3676(5) -0.3376(4) 0.1030(16) Uani 1 1 d . . .
O9 O 0.2002(5) 0.3773(4) -0.2590(3) 0.0931(15) Uani 1 1 d . . .
O10 O 0.1791(5) 0.2406(4) -0.4144(3) 0.0859(14) Uani 1 1 d . . .
N1 N 0.3082(4) -0.0625(3) 0.0260(3) 0.0366(9) Uani 1 1 d . . .
N2 N 0.7459(4) -0.5189(3) -0.0589(3) 0.0425(10) Uani 1 1 d . . .
N3 N -0.0144(4) 0.0404(3) -0.2181(3) 0.0394(9) Uani 1 1 d . . .
N4 N -0.4795(4) 0.1310(4) -0.6180(3) 0.0462(10) Uani 1 1 d . . .
N5 N 0.0650(5) 0.2557(4) 0.1263(3) 0.0524(11) Uani 1 1 d . . .
N6 N 0.1933(6) 0.6587(4) 0.5969(4) 0.0646(13) Uani 1 1 d . . .
C1 C 0.4030(5) -0.0791(4) 0.1000(3) 0.0396(11) Uani 1 1 d . . .
H1A H 0.4066 -0.0327 0.1636 0.048 Uiso 1 1 calc R . .
C2 C 0.4934(5) -0.1635(4) 0.0821(3) 0.0412(11) Uani 1 1 d . . .
H2A H 0.5584 -0.1742 0.1338 0.049 Uiso 1 1 calc R . .
C3 C 0.4902(5) -0.2342(4) -0.0126(3) 0.0363(10) Uani 1 1 d . . .
C4 C 0.3948(5) -0.2116(4) -0.0870(3) 0.0414(11) Uani 1 1 d . . .
H4A H 0.3915 -0.2554 -0.1513 0.050 Uiso 1 1 calc R . .
C5 C 0.3050(5) -0.1253(4) -0.0671(3) 0.0411(11) Uani 1 1 d . . .
H5A H 0.2422 -0.1104 -0.1177 0.049 Uiso 1 1 calc R . .
C6 C 0.5825(5) -0.3313(4) -0.0303(3) 0.0339(10) Uani 1 1 d . . .
C7 C 0.7172(5) -0.3260(4) 0.0310(3) 0.0397(11) Uani 1 1 d . . .
H7B H 0.7545 -0.2578 0.0832 0.048 Uiso 1 1 calc R . .
C8 C 0.7962(5) -0.4188(4) 0.0162(3) 0.0424(12) Uani 1 1 d . . .
H8B H 0.8861 -0.4129 0.0586 0.051 Uiso 1 1 calc R . .
C9 C 0.6164(5) -0.5269(4) -0.1210(4) 0.0483(12) Uani 1 1 d . . .
H9B H 0.5827 -0.5953 -0.1736 0.058 Uiso 1 1 calc R . .
C10 C 0.5334(5) -0.4352(4) -0.1078(4) 0.0439(12) Uani 1 1 d . . .
H10B H 0.4437 -0.4428 -0.1510 0.053 Uiso 1 1 calc R . .
C11 C -0.0298(5) -0.0353(4) -0.3080(3) 0.0413(11) Uani 1 1 d . . .
H11A H 0.0211 -0.1003 -0.3174 0.050 Uiso 1 1 calc R . .
C12 C -0.1192(5) -0.0181(4) -0.3859(3) 0.0419(11) Uani 1 1 d . . .
H12A H -0.1285 -0.0717 -0.4474 0.050 Uiso 1 1 calc R . .
C13 C -0.1969(5) 0.0789(4) -0.3744(3) 0.0359(10) Uani 1 1 d . . .
C14 C -0.1774(5) 0.1543(4) -0.2805(3) 0.0414(11) Uani 1 1 d . . .
H14A H -0.2274 0.2199 -0.2694 0.050 Uiso 1 1 calc R . .
C15 C -0.0873(5) 0.1356(4) -0.2037(3) 0.0440(12) Uani 1 1 d . . .
H15A H -0.0760 0.1883 -0.1416 0.053 Uiso 1 1 calc R . .
C16 C -0.2938(5) 0.0978(4) -0.4580(3) 0.0376(11) Uani 1 1 d . . .
C17 C -0.2811(5) 0.0434(4) -0.5545(3) 0.0423(11) Uani 1 1 d . . .
H17A H -0.2091 -0.0061 -0.5664 0.051 Uiso 1 1 calc R . .
C18 C -0.3709(5) 0.0608(4) -0.6316(4) 0.0473(12) Uani 1 1 d . . .
H18A H -0.3579 0.0240 -0.6948 0.057 Uiso 1 1 calc R . .
C19 C -0.4947(5) 0.1835(5) -0.5258(4) 0.0484(13) Uani 1 1 d . . .
H19A H -0.5689 0.2313 -0.5155 0.058 Uiso 1 1 calc R . .
C20 C -0.4052(5) 0.1693(4) -0.4467(4) 0.0451(12) Uani 1 1 d . . .
H20A H -0.4190 0.2081 -0.3842 0.054 Uiso 1 1 calc R . .
C21 C 0.0025(6) 0.3632(5) 0.1432(4) 0.0532(13) Uani 1 1 d . . .
H21A H -0.0653 0.3765 0.0942 0.064 Uiso 1 1 calc R . .
C22 C 0.0416(7) 0.4427(5) 0.2284(4) 0.0614(15) Uani 1 1 d . . .
H22A H 0.0014 0.5132 0.2385 0.074 Uiso 1 1 calc R . .
C23 C 0.1427(6) 0.4265(5) 0.3062(4) 0.0522(13) Uani 1 1 d . . .
C24 C 0.2049(6) 0.3293(5) 0.2852(4) 0.0555(14) Uani 1 1 d . . .
H24A H 0.2781 0.3180 0.3323 0.067 Uiso 1 1 calc R . .
C25 C 0.1641(6) 0.2416(5) 0.1935(4) 0.0627(15) Uani 1 1 d . . .
H25A H 0.2092 0.1735 0.1817 0.075 Uiso 1 1 calc R . .
C26 C 0.1668(6) 0.5123(5) 0.4060(4) 0.0551(14) Uani 1 1 d . . .
C27 C 0.0797(6) 0.6014(5) 0.4316(4) 0.0596(15) Uani 1 1 d . . .
H27A H 0.0094 0.6133 0.3831 0.072 Uiso 1 1 calc R . .
C28 C 0.0926(6) 0.6686(5) 0.5205(4) 0.0566(14) Uani 1 1 d . . .
H28A H 0.0305 0.7262 0.5329 0.068 Uiso 1 1 calc R . .
C29 C 0.2814(7) 0.5802(6) 0.5745(4) 0.0699(17) Uani 1 1 d . . .
H29A H 0.3548 0.5754 0.6245 0.084 Uiso 1 1 calc R . .
C30 C 0.2759(7) 0.5059(5) 0.4861(4) 0.0663(16) Uani 1 1 d . . .
H30A H 0.3415 0.4507 0.4765 0.080 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'
Cl Cl 0.1484 0.1585 '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 O1 180.00(19) . 2 ?
O1 Cu1 O5 91.24(12) . 2 ?
O1 Cu1 O5 88.76(12) 2 2 ?
O1 Cu1 O5 88.76(12) . . ?
O1 Cu1 O5 91.24(12) 2 . ?
O5 Cu1 O5 180.00(5) 2 . ?
O1 Cu1 O3 84.71(12) . . ?
O1 Cu1 O3 95.29(12) 2 . ?
O5 Cu1 O3 93.44(13) 2 . ?
O5 Cu1 O3 86.56(13) . . ?
O1 Cu1 O3 95.29(12) . 2 ?
O1 Cu1 O3 84.71(12) 2 2 ?
O5 Cu1 O3 86.56(13) 2 2 ?
O5 Cu1 O3 93.44(13) . 2 ?
O3 Cu1 O3 180.0(3) . 2 ?
O7 Cl1 O9 111.9(3) . . ?
O7 Cl1 O10 110.9(3) . . ?
O9 Cl1 O10 112.5(3) . . ?
O7 Cl1 O8 107.6(3) . . ?
O9 Cl1 O8 106.9(3) . . ?
O10 Cl1 O8 106.8(3) . . ?
N1 O1 Cu1 125.4(2) . . ?
N3 O3 Cu1 125.7(2) . . ?
N5 O5 Cu1 130.0(3) . . ?
O1 N1 C5 121.1(4) . . ?
O1 N1 C1 117.8(4) . . ?
C5 N1 C1 121.1(4) . . ?
O2 N2 C8 121.2(4) . . ?
O2 N2 C9 119.4(4) . . ?
C8 N2 C9 119.4(4) . . ?
O3 N3 C11 119.1(4) . . ?
O3 N3 C15 120.8(4) . . ?
C11 N3 C15 120.1(4) . . ?
O4 N4 C19 121.4(4) . . ?
O4 N4 C18 120.7(4) . . ?
C19 N4 C18 117.9(4) . . ?
C25 N5 O5 124.4(5) . . ?
C25 N5 C21 119.5(5) . . ?
O5 N5 C21 116.1(4) . . ?
C29 N6 O6 124.4(5) . . ?
C29 N6 C28 115.7(5) . . ?
O6 N6 C28 119.9(5) . . ?
N1 C1 C2 120.2(4) . . ?
C1 C2 C3 121.0(4) . . ?
C4 C3 C2 117.0(4) . . ?
C4 C3 C6 122.7(4) . . ?
C2 C3 C6 120.3(4) . . ?
C5 C4 C3 120.9(4) . . ?
N1 C5 C4 119.8(4) . . ?
C7 C6 C10 116.7(4) . . ?
C7 C6 C3 122.3(4) . . ?
C10 C6 C3 121.0(4) . . ?
C8 C7 C6 121.3(4) . . ?
N2 C8 C7 121.0(4) . . ?
N2 C9 C10 121.0(5) . . ?
C9 C10 C6 120.5(4) . . ?
N3 C11 C12 120.9(4) . . ?
C11 C12 C13 121.0(4) . . ?
C14 C13 C12 115.9(4) . . ?
C14 C13 C16 122.8(4) . . ?
C12 C13 C16 121.2(4) . . ?
C15 C14 C13 122.1(4) . . ?
N3 C15 C14 119.9(4) . . ?
C20 C16 C17 115.3(4) . . ?
C20 C16 C13 122.6(4) . . ?
C17 C16 C13 122.1(4) . . ?
C18 C17 C16 122.0(4) . . ?
C17 C18 N4 121.2(5) . . ?
N4 C19 C20 122.4(4) . . ?
C19 C20 C16 121.1(5) . . ?
C22 C21 N5 119.1(5) . . ?
C21 C22 C23 123.0(5) . . ?
C24 C23 C22 115.6(5) . . ?
C24 C23 C26 123.8(5) . . ?
C22 C23 C26 120.5(5) . . ?
C23 C24 C25 122.3(5) . . ?
N5 C25 C24 120.3(5) . . ?
C27 C26 C30 113.6(5) . . ?
C27 C26 C23 123.2(5) . . ?
C30 C26 C23 123.1(5) . . ?
C28 C27 C26 122.6(6) . . ?
C27 C28 N6 123.1(6) . . ?
N6 C29 C30 125.8(6) . . ?
C29 C30 C26 119.0(6) . . ?
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 1.977(3) . ?
Cu1 O1 1.977(3) 2 ?
Cu1 O5 1.980(3) 2 ?
Cu1 O5 1.980(3) . ?
Cu1 O3 2.323(3) . ?
Cu1 O3 2.323(3) 2 ?
Cl1 O7 1.404(4) . ?
Cl1 O9 1.408(4) . ?
Cl1 O10 1.428(4) . ?
Cl1 O8 1.434(5) . ?
O1 N1 1.340(4) . ?
O2 N2 1.315(4) . ?
O3 N3 1.322(4) . ?
O4 N4 1.308(5) . ?
O5 N5 1.318(5) . ?
O6 N6 1.349(6) . ?
N1 C5 1.346(5) . ?
N1 C1 1.348(5) . ?
N2 C8 1.348(6) . ?
N2 C9 1.349(6) . ?
N3 C11 1.345(5) . ?
N3 C15 1.352(5) . ?
N4 C19 1.344(6) . ?
N4 C18 1.362(6) . ?
N5 C25 1.286(6) . ?
N5 C21 1.423(6) . ?
N6 C29 1.300(7) . ?
N6 C28 1.370(7) . ?
C1 C2 1.358(6) . ?
C2 C3 1.395(6) . ?
C3 C4 1.386(6) . ?
C3 C6 1.487(6) . ?
C4 C5 1.374(6) . ?
C6 C7 1.385(6) . ?
C6 C10 1.393(6) . ?
C7 C8 1.364(6) . ?
C9 C10 1.377(6) . ?
C11 C12 1.366(6) . ?
C12 C13 1.398(6) . ?
C13 C14 1.384(6) . ?
C13 C16 1.474(6) . ?
C14 C15 1.366(6) . ?
C16 C20 1.390(6) . ?
C16 C17 1.397(6) . ?
C17 C18 1.361(6) . ?
C19 C20 1.367(6) . ?
C21 C22 1.305(7) . ?
C22 C23 1.417(7) . ?
C23 C24 1.319(7) . ?
C23 C26 1.494(7) . ?
C24 C25 1.415(7) . ?
C26 C27 1.392(7) . ?
C26 C30 1.439(8) . ?
C27 C28 1.299(7) . ?
C29 C30 1.333(8) . ?
