#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/27/2202775.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2202775
loop_
_publ_author_name
'Li, Chun Hui'
'Wang, Ru-Ji'
'Kou, Hui-Zhong'
'Li, Yadong'
_publ_section_title
;
 Heptapyridinebis(μ-dimethylglyoximato)tricopper(II) diperchlorate: a
 novel trinuclear copper complex bridged by glyoximate groups
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m608
_journal_page_last               m610
_journal_paper_doi               10.1107/S160053680301331X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu3 (C4 H6 N2 O2)2 (C5 H5 N)7] (Cl O4)2'
_chemical_formula_moiety         'C43 H47 Cu3 N11 O4 2+, 2Cl O4 1-'
_chemical_formula_structural     'Cu3 (C5 H5 N)7 (C4 H6 N2 O2)2 (Cl O4)2'
_chemical_formula_sum            'C43 H47 Cl2 Cu3 N11 O12'
_chemical_formula_weight         1171.47
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 104.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.615(5)
_cell_length_b                   8.3158(17)
_cell_length_c                   25.469(5)
_cell_measurement_reflns_used    3680
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.6
_cell_volume                     5047.7(19)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SMART (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '15\\times15 microns'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19837
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.428
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.639
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         7345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w = {exp[1.50(sinθ/λ)²]}/[σ²(Fo²)+(0.001P)²]
where P = (Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                2919
_reflns_number_total             7370
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ob6252.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202775
_cod_database_fobs_code          2202775
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 0.5000 0.27798(8) 0.2500 0.03695(17) Uani d S 1 . . Cu
Cu2 0.411147(18) 0.19183(6) 0.124310(18) 0.04841(15) Uani d . 1 . . Cu
Cl1 0.66856(6) -0.0917(2) 0.14861(6) 0.0784(4) Uani d . 1 . . Cl
O1 0.38765(9) 0.3306(3) 0.17468(9) 0.0488(7) Uani d . 1 . . O
O2 0.51937(10) 0.3049(3) 0.37100(9) 0.0565(8) Uani d . 1 . . O
O3 0.6535(4) 0.0183(8) 0.1751(3) 0.319(5) Uani d . 1 . . O
O4 0.6309(3) -0.1904(10) 0.1414(3) 0.318(5) Uani d . 1 . . O
O5 0.6745(4) -0.0386(10) 0.1057(3) 0.325(5) Uani d . 1 . . O
O6 0.7129(3) -0.1487(11) 0.1680(3) 0.351(6) Uani d . 1 . . O
N1 0.35001(14) 0.3280(4) 0.05632(13) 0.0604(10) Uani d . 1 . . N
N2 0.43487(14) 0.0347(4) 0.07239(13) 0.0530(9) Uani d . 1 . . N
N3 0.36047(13) 0.0113(4) 0.14329(13) 0.0538(9) Uani d . 1 . . N
N4 0.5000 0.0226(5) 0.2500 0.0425(11) Uani d S 1 . . N
N5 0.41851(11) 0.3259(3) 0.22596(11) 0.0379(7) Uani d . 1 . . N
N6 0.48431(12) 0.3182(4) 0.32218(11) 0.0409(8) Uani d . 1 . . N
C1 0.30521(19) 0.3961(6) 0.06513(17) 0.0693(14) Uani d . 1 . . C
H1A 0.2972 0.3767 0.0983 0.083 Uiso calc R 1 . . H
C2 0.2694(2) 0.4935(7) 0.0294(2) 0.0868(17) Uani d . 1 . . C
H2A 0.2389 0.5413 0.0386 0.104 Uiso calc R 1 . . H
C3 0.2793(2) 0.5184(7) -0.0192(2) 0.1012(19) Uani d . 1 . . C
H3A 0.2551 0.5818 -0.0449 0.121 Uiso calc R 1 . . H
C4 0.3248(3) 0.4500(8) -0.0304(2) 0.116(2) Uani d . 1 . . C
H4A 0.3324 0.4644 -0.0640 0.139 Uiso calc R 1 . . H
C5 0.3597(2) 0.3583(7) 0.0092(2) 0.0930(18) Uani d . 1 . . C
H5A 0.3920 0.3156 0.0019 0.112 Uiso calc R 1 . . H
C6 0.39805(18) -0.0334(6) 0.03109(17) 0.0700(14) Uani d . 1 . . C
H6A 0.3612 0.0038 0.0225 0.084 Uiso calc R 1 . . H
C7 0.4116(2) -0.1542(7) 0.00087(19) 0.103(2) Uani d . 1 . . C
H7A 0.3849 -0.1947 -0.0287 0.124 Uiso calc R 1 . . H
C8 0.4644(3) -0.2155(7) 0.0143(2) 0.121(2) Uani d . 1 . . C
H8A 0.4740 -0.3016 -0.0049 0.146 Uiso calc R 1 . . H
C9 0.5029(2) -0.1487(7) 0.0562(2) 0.1011(19) Uani d . 1 . . C
H9A 0.5396 -0.1868 0.0658 0.121 Uiso calc R 1 . . H
C10 0.48668(18) -0.0237(6) 0.08408(16) 0.0653(13) Uani d . 1 . . C
H10A 0.5133 0.0222 0.1126 0.078 Uiso calc R 1 . . H
C11 0.37271(19) -0.1439(6) 0.14398(18) 0.0719(14) Uani d . 1 . . C
H11A 0.4053 -0.1745 0.1344 0.086 Uiso calc R 1 . . H
C12 0.3401(2) -0.2620(6) 0.1580(2) 0.0924(17) Uani d . 1 . . C
H12A 0.3505 -0.3696 0.1581 0.111 Uiso calc R 1 . . H
C13 0.2924(2) -0.2185(8) 0.1715(2) 0.0977(19) Uani d . 1 . . C
H13A 0.2691 -0.2960 0.1807 0.117 Uiso calc R 1 . . H
C14 0.2790(2) -0.0605(8) 0.1716(2) 0.0938(18) Uani d . 1 . . C
H14A 0.2463 -0.0279 0.1805 0.113 Uiso calc R 1 . . H
C15 0.31472(19) 0.0511(6) 0.15829(17) 0.0744(15) Uani d . 1 . . C
H15A 0.3062 0.1596 0.1600 0.089 Uiso calc R 1 . . H
C16 0.53702(16) -0.0623(5) 0.23080(16) 0.0533(11) Uani d . 1 . . C
H16A 0.5636 -0.0069 0.2176 0.064 Uiso calc R 1 . . H
C17 0.5376(2) -0.2240(6) 0.2298(2) 0.0902(17) Uani d . 1 . . C
H17A 0.5635 -0.2787 0.2153 0.108 Uiso calc R 1 . . H
C18 0.5000 -0.3055(9) 0.2500 0.133(4) Uani d S 1 . . C
H18A 0.5000 -0.4174 0.2500 0.160 Uiso calc SR 1 . . H
C19 0.33500(14) 0.4091(5) 0.25580(15) 0.0645(13) Uani d . 1 . . C
H19A 0.3171 0.4053 0.2177 0.097 Uiso calc R 1 . . H
H19B 0.3321 0.5159 0.2692 0.097 Uiso calc R 1 . . H
H19C 0.3169 0.3347 0.2747 0.097 Uiso calc R 1 . . H
C20 0.39531(15) 0.3646(4) 0.26476(14) 0.0412(9) Uani d . 1 . . C
C21 0.43287(16) 0.3603(4) 0.31935(14) 0.0424(10) Uani d . 1 . . C
C22 0.41269(16) 0.3983(5) 0.36877(14) 0.0725(15) Uani d . 1 . . C
H22A 0.4433 0.3889 0.4005 0.109 Uiso calc R 1 . . H
H22B 0.3836 0.3242 0.3714 0.109 Uiso calc R 1 . . H
H22C 0.3982 0.5060 0.3662 0.109 Uiso calc R 1 . . H
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N5 Cu1 N5 . 2_655 156.84(17) yes
N5 Cu1 N6 . . 80.65(12) yes
N5 Cu1 N6 2_655 . 95.48(12) yes
N5 Cu1 N6 . 2_655 95.48(12) no
N5 Cu1 N6 2_655 2_655 80.65(12) no
N6 Cu1 N6 . 2_655 160.75(17) yes
N5 Cu1 N4 . . 101.58(8) yes
N5 Cu1 N4 2_655 . 101.58(8) no
N6 Cu1 N4 . . 99.62(9) yes
N6 Cu1 N4 2_655 . 99.62(9) no
O1 Cu2 O2 . 2_655 94.37(11) yes
O1 Cu2 N2 . . 177.23(12) no
O2 Cu2 N2 2_655 . 87.69(12) no
O1 Cu2 N3 . . 88.86(12) yes
O2 Cu2 N3 2_655 . 155.43(12) yes
N2 Cu2 N3 . . 88.50(13) yes
O1 Cu2 N1 . . 87.55(12) yes
O2 Cu2 N1 2_655 . 102.16(12) no
N2 Cu2 N1 . . 93.84(13) no
N3 Cu2 N1 . . 102.32(13) no
O6 Cl1 O4 . . 112.5(6) no
O6 Cl1 O5 . . 102.3(5) no
O4 Cl1 O5 . . 111.5(5) no
O6 Cl1 O3 . . 116.0(6) no
O4 Cl1 O3 . . 104.9(5) no
O5 Cl1 O3 . . 109.7(5) no
N5 O1 Cu2 . . 116.30(19) no
N6 O2 Cu2 . 2_655 117.17(19) no
C5 N1 C1 . . 115.5(4) no
C5 N1 Cu2 . . 123.6(3) no
C1 N1 Cu2 . . 120.5(3) no
C10 N2 C6 . . 116.6(4) no
C10 N2 Cu2 . . 120.2(3) no
C6 N2 Cu2 . . 122.3(3) no
C15 N3 C11 . . 116.7(4) no
C15 N3 Cu2 . . 119.4(3) no
C11 N3 Cu2 . . 123.9(3) no
C16 N4 C16 2_655 . 116.3(5) no
C16 N4 Cu1 2_655 . 121.9(2) no
C16 N4 Cu1 . . 121.9(2) no
C20 N5 O1 . . 119.0(3) no
C20 N5 Cu1 . . 114.7(2) no
O1 N5 Cu1 . . 126.18(19) no
C21 N6 O2 . . 118.1(3) no
C21 N6 Cu1 . . 113.8(2) no
O2 N6 Cu1 . . 128.1(2) no
N1 C1 C2 . . 125.0(5) no
C3 C2 C1 . . 118.3(5) no
C2 C3 C4 . . 118.9(6) no
C3 C4 C5 . . 118.5(5) no
N1 C5 C4 . . 123.7(5) no
N2 C6 C7 . . 123.3(4) no
C6 C7 C8 . . 119.3(5) no
C9 C8 C7 . . 118.7(5) no
C8 C9 C10 . . 118.8(5) no
N2 C10 C9 . . 123.2(4) no
N3 C11 C12 . . 123.8(5) no
C13 C12 C11 . . 118.4(5) no
C12 C13 C14 . . 119.1(5) no
C13 C14 C15 . . 118.9(5) no
N3 C15 C14 . . 123.1(5) no
N4 C16 C17 . . 123.1(4) no
C16 C17 C18 . . 118.9(5) no
C17 C18 C17 2_655 . 119.7(7) no
N5 C20 C21 . . 115.0(3) no
N5 C20 C19 . . 123.7(3) no
C21 C20 C19 . . 121.3(3) no
N6 C21 C20 . . 115.8(3) no
N6 C21 C22 . . 122.3(3) no
C20 C21 C22 . . 121.9(3) no
N1 C1 H1A . . 117.5 ?
C2 C1 H1A . . 117.5 ?
C3 C2 H2A . . 120.8 ?
C1 C2 H2A . . 120.8 ?
C2 C3 H3A . . 120.6 ?
C4 C3 H3A . . 120.6 ?
C3 C4 H4A . . 120.7 ?
C5 C4 H4A . . 120.7 ?
N1 C5 H5A . . 118.2 ?
C4 C5 H5A . . 118.2 ?
N2 C6 H6A . . 118.4 ?
C7 C6 H6A . . 118.4 ?
C6 C7 H7A . . 120.3 ?
C8 C7 H7A . . 120.3 ?
C9 C8 H8A . . 120.7 ?
C7 C8 H8A . . 120.7 ?
C8 C9 H9A . . 120.6 ?
C10 C9 H9A . . 120.6 ?
N2 C10 H10A . . 118.4 ?
C9 C10 H10A . . 118.4 ?
N3 C11 H11A . . 118.1 ?
C12 C11 H11A . . 118.1 ?
C13 C12 H12A . . 120.8 ?
C11 C12 H12A . . 120.8 ?
C12 C13 H13A . . 120.4 ?
C14 C13 H13A . . 120.4 ?
C13 C14 H14A . . 120.6 ?
C15 C14 H14A . . 120.6 ?
N3 C15 H15A . . 118.5 ?
C14 C15 H15A . . 118.5 ?
N4 C16 H16A . . 118.5 ?
C17 C16 H16A . . 118.5 ?
C16 C17 H17A . . 120.5 ?
C18 C17 H17A . . 120.5 ?
C17 C18 H18A . . 120.2 ?
C17 C18 H18A 2_655 . 120.2 ?
C20 C19 H19A . . 109.5 ?
C20 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
C20 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C21 C22 H22A . . 109.5 ?
C21 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N5 . 1.986(3) yes
Cu1 N5 2_655 1.986(3) no
Cu1 N6 . 1.999(3) yes
Cu1 N6 2_655 1.999(3) no
Cu1 N4 . 2.124(4) yes
Cu2 O1 . 1.919(2) yes
Cu2 O2 2_655 1.929(2) yes
Cu2 N2 . 2.045(3) yes
Cu2 N3 . 2.085(3) yes
Cu2 N1 . 2.290(3) yes
Cl1 O6 . 1.179(5) no
Cl1 O4 . 1.217(5) no
Cl1 O5 . 1.221(5) no
Cl1 O3 . 1.247(5) no
O1 N5 . 1.337(3) no
O2 N6 . 1.329(3) no
O2 Cu2 2_655 1.929(2) no
N1 C5 . 1.305(5) no
N1 C1 . 1.308(5) no
N2 C10 . 1.327(4) no
N2 C6 . 1.331(4) no
N3 C15 . 1.319(4) no
N3 C11 . 1.324(5) no
N4 C16 2_655 1.338(4) no
N4 C16 . 1.338(4) no
N5 C20 . 1.300(4) no
N6 C21 . 1.298(4) no
C1 C2 . 1.363(6) no
C2 C3 . 1.335(6) no
C3 C4 . 1.348(7) no
C4 C5 . 1.380(6) no
C6 C7 . 1.357(6) no
C7 C8 . 1.360(6) no
C8 C9 . 1.355(6) no
C9 C10 . 1.374(6) no
C11 C12 . 1.371(6) no
C12 C13 . 1.354(6) no
C13 C14 . 1.355(7) no
C14 C15 . 1.377(6) no
C16 C17 . 1.345(6) no
C17 C18 . 1.349(6) no
C18 C17 2_655 1.349(6) no
C19 C20 . 1.491(4) no
C20 C21 . 1.465(4) no
C21 C22 . 1.498(4) no
C1 H1A . 0.9300 ?
C2 H2A . 0.9300 ?
C3 H3A . 0.9300 ?
C4 H4A . 0.9300 ?
C5 H5A . 0.9300 ?
C6 H6A . 0.9300 ?
C7 H7A . 0.9300 ?
C8 H8A . 0.9300 ?
C9 H9A . 0.9300 ?
C10 H10A . 0.9300 ?
C11 H11A . 0.9300 ?
C12 H12A . 0.9300 ?
C13 H13A . 0.9300 ?
C14 H14A . 0.9300 ?
C15 H15A . 0.9300 ?
C16 H16A . 0.9300 ?
C17 H17A . 0.9300 ?
C18 H18A . 0.9300 ?
C19 H19A . 0.9600 ?
C19 H19B . 0.9600 ?
C19 H19C . 0.9600 ?
C22 H22A . 0.9600 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9600 ?
