#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:40:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179341 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/38/4323827.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_4323827
loop_
_publ_author_name
'Frank Zippel'
'Friedhelm Ahlers'
'Rüdiger Werner'
'Wolfgang Haase'
'Hans-Friedrich Nolting'
'Bernt Krebs'
_publ_contact_author
;
        Bernt Krebs
        Anorganisch-Chemisches Institut
        Westfälische Wilhelms-Universität
        Wilhelm Klemm Str. 8
        48149 Münster
        Bundesrepublik Deutschland
;
_publ_contact_author_email       KREBS@VNWZ01.UNI-MUENSTER.DE
_publ_contact_author_fax         '049 251 83-8366'
_publ_contact_author_phone       '049 251 83-3131'
_publ_section_title
;
 Structural and Functional Models for the Dinuclear Copper Active Site in
 Catechol Oxidases: Syntheses, X-ray Crystal Structures, Magnetic and
 Spectral Properties, and X-ray Absorption Spectroscopic Studies in Solid
 State and in Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3409
_journal_page_last               3419
_journal_paper_doi               10.1021/ic9513604
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C41 H50 Cl2 Cu2 N8 O13'
_chemical_formula_weight         1060.87
_chemical_name_common            '[Cu2bbpen2](ClO4)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.478(9)
_cell_length_b                   18.795(8)
_cell_length_c                   13.888(6)
_cell_measurement_temperature    150(2)
_cell_volume                     4562(4)
_computing_cell_refinement       'Siemens P3/V, Rel. 4.21'
_computing_data_collection       'Siemens P3/V, Rel. 4.21'
_computing_data_reduction        'SHELXTL PLUS, XDISK'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'SHELXL-93 (Sheldrick 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       omega-scan
_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    0.1578
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2445
_diffrn_reflns_theta_max         21.09
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       needles
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.807
_refine_ls_goodness_of_fit_obs   1.178
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         2444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.836
_refine_ls_restrained_S_obs      1.178
_refine_ls_R_factor_all          0.1566
_refine_ls_R_factor_obs          0.0651
_refine_ls_shift/esd_max         0.064
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0952P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1814
_refine_ls_wR_factor_obs         0.1472
_reflns_number_observed          996
_reflns_number_total             2445
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9513604_2.cif
_cod_data_source_block           clint
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+0.0000P] 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^)+(0.0952P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4562.2(36)
_cod_database_code               4323827
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu 0.17751(7) 0.20641(8) 0.12778(10) 0.0498(5) Uani 1 d . .
O1 O 0.2135(3) 0.3034(4) 0.1280(5) 0.050(2) Uani 1 d . .
N1 N 0.0693(5) 0.2297(5) 0.1559(7) 0.056(3) Uani 1 d . .
N2 N -0.0418(7) 0.2798(7) 0.1527(10) 0.096(5) Uani 1 d . .
H2 H -0.0791(7) 0.3092(7) 0.1377(10) 0.115 Uiso 1 calc R .
N3 N 0.1543(5) 0.1127(5) 0.0763(7) 0.053(3) Uani 1 d . .
N4 N 0.1601(5) -0.0030(5) 0.0403(7) 0.054(3) Uani 1 d . .
H4 H 0.1731(5) -0.0481(5) 0.0437(7) 0.065 Uiso 1 calc R .
C1 C 0.1709(10) 0.3590(9) 0.1784(13) 0.120(6) Uiso 1 d . .
H1 H 0.1378(10) 0.3364(9) 0.2285(13) 0.144 Uiso 1 calc R .
C2 C 0.1222(12) 0.3942(10) 0.1078(12) 0.183(11) Uani 1 d . .
H2A H 0.1551(12) 0.4211(10) 0.0627(12) 0.220 Uiso 1 calc R .
H2B H 0.0893(12) 0.4289(10) 0.1418(12) 0.220 Uiso 1 calc R .
C3 C 0.0673(12) 0.3406(8) 0.0451(12) 0.145(9) Uani 1 d . .
H3A H 0.0266(12) 0.3681(8) 0.0124(12) 0.174 Uiso 1 calc R .
H3B H 0.0979(12) 0.3157(8) -0.0045(12) 0.174 Uiso 1 calc R .
C4 C 0.0305(7) 0.2845(8) 0.1175(10) 0.071(4) Uani 1 d . .
C5 C 0.0211(7) 0.1879(8) 0.2167(10) 0.066(4) Uani 1 d . .
C6 C 0.0334(9) 0.1278(9) 0.2727(11) 0.086(5) Uani 1 d . .
H6 H 0.0819(9) 0.1050(9) 0.2740(11) 0.104 Uiso 1 calc R .
C7 C -0.0257(13) 0.1028(10) 0.3253(12) 0.116(7) Uani 1 d . .
H7 H -0.0191(13) 0.0626(10) 0.3658(12) 0.139 Uiso 1 calc R .
C8 C -0.0966(13) 0.1366(14) 0.3198(17) 0.143(11) Uani 1 d . .
H8 H -0.1370(13) 0.1167(14) 0.3568(17) 0.171 Uiso 1 calc R .
C9 C -0.1132(11) 0.1944(13) 0.2673(16) 0.139(9) Uani 1 d . .
H9 H -0.1630(11) 0.2146(13) 0.2649(16) 0.167 Uiso 1 calc R .
C10 C -0.0495(8) 0.2233(11) 0.2148(13) 0.093(5) Uani 1 d . .
C11 C 0.2755(10) 0.0849(9) 0.2281(15) 0.147(8) Uani 1 d . .
H11A H 0.3046(10) 0.0614(9) 0.2802(15) 0.176 Uiso 1 calc R .
H11B H 0.2323(10) 0.1106(9) 0.2584(15) 0.176 Uiso 1 calc R .
C12 C 0.2447(8) 0.0312(7) 0.1673(10) 0.081(5) Uani 1 d . .
H12A H 0.2230(8) -0.0064(7) 0.2091(10) 0.097 Uiso 1 calc R .
H12B H 0.2878(8) 0.0095(7) 0.1314(10) 0.097 Uiso 1 calc R .
C13 C 0.1859(6) 0.0510(8) 0.0970(8) 0.049(3) Uani 1 d . .
C14 C 0.1048(6) 0.0996(8) -0.0029(9) 0.048(3) Uani 1 d . .
C15 C 0.0586(6) 0.1446(7) -0.0520(9) 0.058(4) Uani 1 d . .
H15 H 0.0558(6) 0.1937(7) -0.0364(9) 0.070 Uiso 1 calc R .
C16 C 0.0159(6) 0.1160(8) -0.1256(11) 0.065(4) Uani 1 d . .
H16 H -0.0169(6) 0.1457(8) -0.1623(11) 0.078 Uiso 1 calc R .
C17 C 0.0207(7) 0.0422(9) -0.1469(9) 0.067(4) Uani 1 d . .
H17 H -0.0101(7) 0.0240(9) -0.1976(9) 0.081 Uiso 1 calc R .
C18 C 0.0671(7) -0.0038(7) -0.0988(9) 0.063(4) Uani 1 d . .
H18 H 0.0708(7) -0.0529(7) -0.1143(9) 0.076 Uiso 1 calc R .
C19 C 0.1086(6) 0.0280(8) -0.0244(9) 0.053(3) Uani 1 d . .
Cl1 Cl 0.1566(4) 0.5630(5) 0.8867(5) 0.157(3) Uani 1 d . .
O2 O 0.2136(11) 0.5221(15) 0.8916(11) 0.443(22) Uani 1 d . .
O3 O 0.1238(7) 0.5684(9) 0.8025(10) 0.215(9) Uani 1 d . .
O4 O 0.1553(7) 0.6248(8) 0.9446(12) 0.189(7) Uani 1 d . .
O5 O 0.1125(20) 0.5292(14) 0.9422(25) 0.415(22) Uani 1 d . .
O6 O 0.2085(6) -0.1452(6) 0.0546(10) 0.124(4) Uani 1 d . .
H6A H 0.2504(47) -0.1416(76) 0.0253(86) 0.186 Uiso 1 calc R .
C20 C 0.3341(9) 0.6938(9) 1.0125(16) 0.159(9) Uani 1 d . .
H20A H 0.3882(9) 0.6809(40) 1.0190(90) 0.239 Uiso 1 calc R .
H20B H 0.3251(60) 0.7400(18) 1.0430(66) 0.239 Uiso 1 calc R .
H20C H 0.3207(56) 0.6966(51) 0.9441(25) 0.239 Uiso 1 calc R .
C21 C 0.2500 0.2500 0.3819(20) 0.260(23) Uani 1 d S .
H21A H 0.2633 0.2908 0.3412(20) 0.391 Uiso 0.50 calc PR .
H21B H 0.2964 0.2230 0.3971(20) 0.391 Uiso 0.50 calc PR .
H21C H 0.2264 0.2669 0.4416(20) 0.391 Uiso 0.50 calc PR .
O7 O 0.1878(13) 0.1969(17) 0.3225(18) 0.204(14) Uani 0.50 d P .
H7A H 0.2098(13) 0.1786(17) 0.2747(18) 0.306 Uiso 0.50 calc PR .
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 76.5(3) 2 . ?
O1 Cu1 N3 97.0(3) 2 . ?
O1 Cu1 N3 157.7(4) . . ?
O1 Cu1 N1 166.3(3) 2 . ?
O1 Cu1 N1 95.9(3) . . ?
N3 Cu1 N1 94.2(4) . . ?
O1 Cu1 Cu1 38.4(2) 2 2 ?
O1 Cu1 Cu1 38.1(2) . 2 ?
N3 Cu1 Cu1 131.8(3) . 2 ?
N1 Cu1 Cu1 133.0(3) . 2 ?
C1 O1 Cu1 125.2(8) . 2 ?
C1 O1 Cu1 120.7(8) . . ?
Cu1 O1 Cu1 103.5(3) 2 . ?
C4 N1 C5 111.1(10) . . ?
C4 N1 Cu1 124.9(9) . . ?
C5 N1 Cu1 123.9(9) . . ?
C4 N2 C10 111.6(13) . . ?
C13 N3 C14 105.7(10) . . ?
C13 N3 Cu1 129.1(8) . . ?
C14 N3 Cu1 124.7(9) . . ?
C13 N4 C19 105.9(10) . . ?
C2 C1 O1 107.5(14) . . ?
C2 C1 C11 109.8(17) . 2 ?
O1 C1 C11 112.7(13) . 2 ?
C1 C2 C3 114.8(15) . . ?
C4 C3 C2 107.9(12) . . ?
N1 C4 N2 106.0(14) . . ?
N1 C4 C3 123.7(12) . . ?
N2 C4 C3 130.3(15) . . ?
C6 C5 C10 122.2(15) . . ?
C6 C5 N1 133.5(14) . . ?
C10 C5 N1 104.2(14) . . ?
C7 C6 C5 117.8(17) . . ?
C6 C7 C8 119.5(20) . . ?
C9 C8 C7 126.3(24) . . ?
C8 C9 C10 114.4(23) . . ?
N2 C10 C5 107.0(14) . . ?
N2 C10 C9 133.3(19) . . ?
C5 C10 C9 119.5(19) . . ?
C12 C11 C1 116.2(17) . 2 ?
C11 C12 C13 118.7(14) . . ?
N3 C13 N4 113.1(10) . . ?
N3 C13 C12 131.6(13) . . ?
N4 C13 C12 115.3(13) . . ?
C15 C14 C19 121.9(12) . . ?
C15 C14 N3 130.2(13) . . ?
C19 C14 N3 107.9(12) . . ?
C14 C15 C16 117.0(13) . . ?
C15 C16 C17 120.3(12) . . ?
C18 C17 C16 123.6(12) . . ?
C17 C18 C19 113.6(12) . . ?
C14 C19 C18 123.6(13) . . ?
C14 C19 N4 107.3(12) . . ?
C18 C19 N4 129.1(14) . . ?
O5 Cl1 O2 98.2(20) . . ?
O5 Cl1 O3 108.5(19) . . ?
O2 Cl1 O3 116.3(9) . . ?
O5 Cl1 O4 93.2(17) . . ?
O2 Cl1 O4 118.9(12) . . ?
O3 Cl1 O4 116.0(11) . . ?
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 1.913(6) 2 ?
Cu1 O1 1.928(7) . ?
Cu1 N3 1.943(10) . ?
Cu1 N1 1.981(9) . ?
Cu1 Cu1 3.017(3) 2 ?
O1 C1 1.46(2) . ?
O1 Cu1 1.913(6) 2 ?
N1 C4 1.343(14) . ?
N1 C5 1.428(14) . ?
N2 C4 1.36(2) . ?
N2 C10 1.37(2) . ?
N3 C13 1.316(14) . ?
N3 C14 1.421(13) . ?
N4 C13 1.361(13) . ?
N4 C19 1.399(13) . ?
C1 C2 1.46(2) . ?
C1 C11 1.57(2) 2 ?
C2 C3 1.64(2) . ?
C3 C4 1.59(2) . ?
C5 C6 1.39(2) . ?
C5 C10 1.40(2) . ?
C6 C7 1.35(2) . ?
C7 C8 1.39(2) . ?
C8 C9 1.34(2) . ?
C9 C10 1.44(2) . ?
C11 C12 1.42(2) . ?
C11 C1 1.57(2) 2 ?
C12 C13 1.47(2) . ?
C14 C15 1.354(15) . ?
C14 C19 1.380(15) . ?
C15 C16 1.375(15) . ?
C16 C17 1.42(2) . ?
C17 C18 1.36(2) . ?
C18 C19 1.397(15) . ?
Cl1 O5 1.26(3) . ?
Cl1 O2 1.261(12) . ?
Cl1 O3 1.306(12) . ?
Cl1 O4 1.413(14) . ?
O6 C20 1.32(2) 2_554 ?
C20 O6 1.32(2) 2_556 ?
C21 O7 1.69(3) . ?
