#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:11:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179316 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/13/4321383.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_4321383
loop_
_publ_author_name
'Ming-Liang Tong'
'Hung Kay Lee'
'Ye-Xiang Tong'
'Xiao-Ming Chen'
'Thomas C. W. Mak'
_publ_contact_author
;
      Chen, Xiao-Ming
      School of Chemistry and Chemical Engineering
      Zhongshan University
      Guangzhou, 510275
      P. R. China
;
_publ_contact_author_email       cescxm@zsu.edu.cn
_publ_contact_author_fax         '86 20 84112245'
_publ_contact_author_phone       86-20-84113986
_publ_section_title
;
 An Octanuclear Copper(II) Complex Containing thegem-Diol Anionic Form of
 Di-2-pyridyl Ketone (dpd-2H) and 2-Hydroxypyridine: Synthesis, Crystal
 Structure, and Properties of [Cu8(dpd-2H)4(μ2-O2CMe)4{2-(OH)C5H4N}4]-
 (ClO4)4.4H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4666
_journal_page_last               4669
_journal_paper_doi               10.1021/ic000114b
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C72 H72 Cl4 Cu8 N12 O40'
_chemical_formula_weight         2395.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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            2
_cell_length_a                   17.205(2)
_cell_length_b                   17.205(2)
_cell_length_c                   14.822(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4387.5(11)
_computing_molecular_graphics    'SHELXTL v. 5 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku RAXIS-IIC diffractometer'
_diffrn_measurement_method       IP
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3871
_diffrn_reflns_theta_full        25.52
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    2.122
_exptl_absorpt_correction_T_max  1.009
_exptl_absorpt_correction_T_min  0.922
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3871
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0858P)²+1.7986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                3773
_reflns_number_total             3871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000114b.cif
_cod_data_source_block           cu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+1.7986P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+1.7986P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321383
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.24198(4) 0.01988(4) 0.12117(6) 0.0677(2) Uani 1 d . . .
Cu2 Cu 0.06684(3) -0.06852(4) 0.07801(4) 0.0511(2) Uani 1 d . . .
N1 N 0.0259(3) -0.0893(3) 0.2008(3) 0.0571(10) Uani 1 d . . .
N2 N -0.2297(3) -0.1343(3) 0.1083(4) 0.0644(12) Uani 1 d . . .
O1 O -0.0423(2) -0.0951(2) 0.0457(2) 0.0502(8) Uani 1 d . . .
O2 O -0.1328(2) -0.0210(2) 0.1214(3) 0.0570(8) Uani 1 d . . .
C1 C 0.0705(4) -0.0893(4) 0.2768(4) 0.0673(14) Uani 1 d . . .
H1A H 0.1245 -0.0755 0.2735 0.080 Uiso 1 d R . .
C2 C 0.0370(4) -0.1085(4) 0.3597(4) 0.0789(18) Uani 1 d . . .
H2A H 0.0683 -0.1098 0.4132 0.080 Uiso 1 d R . .
C3 C -0.0409(4) -0.1280(4) 0.3634(4) 0.0779(16) Uani 1 d . . .
H3A H -0.0640 -0.1410 0.4204 0.080 Uiso 1 d R . .
C4 C -0.0851(4) -0.1259(4) 0.2855(5) 0.0715(15) Uani 1 d . . .
H4A H -0.1392 -0.1395 0.2872 0.080 Uiso 1 d R . .
C5 C -0.0495(3) -0.1051(3) 0.2050(4) 0.0551(11) Uani 1 d . . .
C6 C -0.0947(3) -0.0939(3) 0.1163(4) 0.0537(12) Uani 1 d . . .
C7 C -0.1553(3) -0.1568(3) 0.1064(4) 0.0545(12) Uani 1 d . . .
C8 C -0.1353(4) -0.2346(4) 0.0965(5) 0.0729(16) Uani 1 d . . .
H8A H -0.0816 -0.2500 0.0960 0.080 Uiso 1 d R . .
C9 C -0.1929(5) -0.2893(4) 0.0872(6) 0.0828(18) Uani 1 d . . .
H9A H -0.1813 -0.3434 0.0788 0.080 Uiso 1 d R . .
C10 C -0.2691(4) -0.2641(4) 0.0886(7) 0.090(2) Uani 1 d . . .
H10A H -0.3110 -0.3008 0.0850 0.080 Uiso 1 d R . .
C11 C -0.2874(4) -0.1860(4) 0.0998(5) 0.0798(18) Uani 1 d . . .
H11A H -0.3405 -0.1688 0.1009 0.080 Uiso 1 d R . .
O3 O 0.3542(3) 0.0239(3) 0.1175(5) 0.1043(19) Uani 1 d . . .
H3B H 0.3755 0.0646 0.0961 0.080 Uiso 1 d R . .
N3 N 0.4403(5) -0.0812(6) 0.0893(6) 0.115(2) Uani 1 d . . .
C12 C 0.3978(4) -0.0295(5) 0.1448(7) 0.097(3) Uani 1 d . . .
C13 C 0.4085(4) -0.0424(5) 0.2339(5) 0.0794(17) Uani 1 d . . .
H13A H 0.3828 -0.0078 0.2751 0.080 Uiso 1 d R . .
C14 C 0.4537(5) -0.0988(6) 0.2691(7) 0.106(3) Uani 1 d . . .
H14A H 0.4560 -0.1040 0.3335 0.080 Uiso 1 d R . .
C15 C 0.4927(5) -0.1473(6) 0.2171(6) 0.104(3) Uani 1 d . . .
H15A H 0.5261 -0.1857 0.2437 0.080 Uiso 1 d R . .
C16 C 0.4850(5) -0.1410(6) 0.1235(7) 0.098(2) Uani 1 d . . .
H16A H 0.5111 -0.1766 0.0839 0.080 Uiso 1 d R . .
C17 C 0.2624(5) -0.2248(4) 0.1534(6) 0.093(2) Uani 1 d . . .
H17A H 0.2319 -0.2688 0.1410 0.080 Uiso 1 d R . .
H17B H 0.3109 -0.2279 0.1182 0.080 Uiso 1 d R . .
H17C H 0.2759 -0.2216 0.2156 0.080 Uiso 1 d R . .
C18 C 0.2181(3) -0.1525(3) 0.1288(5) 0.0679(14) Uani 1 d . . .
O4 O 0.2537(3) -0.0908(3) 0.1412(4) 0.0948(15) Uani 1 d . . .
O5 O 0.1497(3) -0.1584(2) 0.0990(3) 0.0678(11) Uani 1 d . . .
Cl1 Cl 0.26538(13) 0.02887(12) 0.39417(14) 0.0909(5) Uani 1 d . . .
O6 O 0.2549(6) 0.0466(6) 0.3021(5) 0.153(3) Uani 1 d U . .
O7 O 0.2379(7) 0.0882(5) 0.4492(5) 0.157(4) Uani 1 d U . .
O8 O 0.2217(8) -0.0363(5) 0.4137(10) 0.192(5) Uani 1 d U . .
O9 O 0.3441(5) 0.0104(8) 0.4072(8) 0.184(4) Uani 1 d U . .
O1W O 0.0539(5) -0.2894(5) 0.0751(7) 0.147(3) Uani 1 d . . .
H1WA H 0.0915 -0.2412 0.1061 0.120 Uiso 1 d R . .
H1WB H 0.0590 -0.3261 0.0372 0.120 Uiso 1 d 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
O2 Cu1 O3 176.9(2) 2 . ?
O2 Cu1 O4 96.6(2) 2 . ?
O3 Cu1 O4 86.3(2) . . ?
O2 Cu1 N2 83.31(18) 2 2 ?
O3 Cu1 N2 93.9(2) . 2 ?
O4 Cu1 N2 176.7(2) . 2 ?
O1 Cu2 N1 173.14(17) 4 . ?
O1 Cu2 O1 93.55(13) 4 . ?
N1 Cu2 O1 81.06(17) . . ?
O1 Cu2 O2 89.02(15) 4 2 ?
N1 Cu2 O2 92.56(18) . 2 ?
O1 Cu2 O2 141.42(14) . 2 ?
O1 Cu2 O5 97.97(16) 4 . ?
N1 Cu2 O5 88.44(18) . . ?
O1 Cu2 O5 120.02(15) . . ?
O2 Cu2 O5 97.60(15) 2 . ?
C5 N1 C1 120.7(5) . . ?
C5 N1 Cu2 115.3(4) . . ?
C1 N1 Cu2 124.0(4) . . ?
C11 N2 C7 121.0(5) . . ?
C11 N2 Cu1 126.0(4) . 2 ?
C7 N2 Cu1 113.0(4) . 2 ?
C6 O1 Cu2 123.9(3) . 3 ?
C6 O1 Cu2 115.4(3) . . ?
Cu2 O1 Cu2 112.77(16) 3 . ?
C6 O2 Cu1 118.2(3) . 2 ?
C6 O2 Cu2 113.5(3) . 2 ?
Cu1 O2 Cu2 123.58(19) 2 2 ?
N1 C1 C2 119.6(6) . . ?
C3 C2 C1 119.5(6) . . ?
C2 C3 C4 119.6(6) . . ?
C3 C4 C5 118.7(6) . . ?
N1 C5 C4 121.7(5) . . ?
N1 C5 C6 115.3(5) . . ?
C4 C5 C6 122.9(5) . . ?
O1 C6 O2 110.8(4) . . ?
O1 C6 C7 111.5(5) . . ?
O2 C6 C7 108.7(4) . . ?
O1 C6 C5 108.4(4) . . ?
O2 C6 C5 107.4(5) . . ?
C7 C6 C5 110.0(4) . . ?
N2 C7 C8 121.3(6) . . ?
N2 C7 C6 116.8(5) . . ?
C8 C7 C6 121.9(5) . . ?
C9 C8 C7 119.4(6) . . ?
C8 C9 C10 117.9(6) . . ?
C9 C10 C11 121.4(7) . . ?
N2 C11 C10 119.0(6) . . ?
C12 O3 Cu1 124.1(5) . . ?
C16 N3 C12 122.9(8) . . ?
O3 C12 C13 121.2(9) . . ?
O3 C12 N3 125.6(9) . . ?
C13 C12 N3 113.2(8) . . ?
C14 C13 C12 125.1(8) . . ?
C15 C14 C13 121.5(10) . . ?
C14 C15 C16 118.8(9) . . ?
N3 C16 C15 118.3(9) . . ?
O4 C18 O5 125.6(6) . . ?
O4 C18 C17 114.9(6) . . ?
O5 C18 C17 119.5(6) . . ?
C18 O4 Cu1 140.1(4) . . ?
C18 O5 Cu2 128.2(4) . . ?
O8 Cl1 O7 106.8(7) . . ?
O8 Cl1 O9 108.2(8) . . ?
O7 Cl1 O9 114.4(8) . . ?
O8 Cl1 O6 108.0(8) . . ?
O7 Cl1 O6 111.5(5) . . ?
O9 Cl1 O6 107.8(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 O2 1.879(4) 2 ?
Cu1 O3 1.934(5) . ?
Cu1 O4 1.938(5) . ?
Cu1 N2 1.989(5) 2 ?
Cu2 O1 1.950(3) 4 ?
Cu2 N1 1.984(4) . ?
Cu2 O1 1.991(3) . ?
Cu2 O2 2.018(4) 2 ?
Cu2 O5 2.127(5) . ?
N1 C5 1.328(7) . ?
N1 C1 1.362(8) . ?
N2 C11 1.338(8) . ?
N2 C7 1.337(7) . ?
N2 Cu1 1.989(5) 2 ?
O1 C6 1.381(7) . ?
O1 Cu2 1.950(3) 3 ?
O2 C6 1.416(6) . ?
O2 Cu1 1.879(4) 2 ?
O2 Cu2 2.018(4) 2 ?
C1 C2 1.397(9) . ?
C2 C3 1.381(10) . ?
C3 C4 1.383(10) . ?
C4 C5 1.388(8) . ?
C5 C6 1.539(7) . ?
C6 C7 1.511(8) . ?
C7 C8 1.390(8) . ?
C8 C9 1.374(10) . ?
C9 C10 1.382(11) . ?
C10 C11 1.390(11) . ?
O3 C12 1.254(9) . ?
N3 C16 1.380(13) . ?
N3 C12 1.415(12) . ?
C12 C13 1.351(12) . ?
C13 C14 1.348(11) . ?
C14 C15 1.320(13) . ?
C15 C16 1.398(13) . ?
C17 C18 1.503(9) . ?
C18 O4 1.239(8) . ?
C18 O5 1.261(7) . ?
Cl1 O8 1.380(11) . ?
Cl1 O7 1.390(7) . ?
Cl1 O9 1.404(9) . ?
Cl1 O6 1.410(7) . ?
