#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309151.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_4309151
loop_
_publ_author_name
'Janet L. Shaw'
'Gordon T. Yee'
'Guangbin Wang'
'David E. Benson'
'Cagil Gokdemir'
'Christopher J. Ziegler'
_publ_contact_author
;
Christopher J. Ziegler
University of Akron
Department of Chemistry
Akron, OH 44325-3601
;
_publ_contact_author_email       ziegler@uakron.edu
_publ_contact_author_fax         '1 330 972 7370'
_publ_contact_author_phone       '1 330 972 2531'
_publ_section_title
;
Magneto-Structural Relationships in a Series of Dinuclear Oxalato-Bridged
(Diphenyldipyrazolylmethane)copper(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5060
_journal_page_last               5067
_journal_paper_doi               10.1021/ic048229t
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C20 H16 Cu N5 O5'
_chemical_formula_weight         469.92
_chemical_name_common            JK065
_chemical_name_systematic
;
 u-oxalato-bis-[(diphenyldipyrazolylmethane)copper(II) nitrate]
;
_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                98.985(14)
_cell_angle_beta                 110.449(13)
_cell_angle_gamma                103.664(14)
_cell_formula_units_Z            2
_cell_length_a                   8.863(7)
_cell_length_b                   10.241(9)
_cell_length_c                   11.425(10)
_cell_measurement_reflns_used    1668
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.79
_cell_measurement_theta_min      2.49
_cell_volume                     911.1(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8205
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.9403
_exptl_absorpt_correction_T_min  0.7929
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0436P)²+0.7973P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                3445
_reflns_number_total             4254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048229tsi20041216_011457_2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_database_code               4309151
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
C1 C 0.3746(4) 0.7056(4) 0.8680(3) 0.0152(7) Uani 1 1 d . . .
C2 C 0.3106(4) 0.7149(4) 0.9758(3) 0.0163(7) Uani 1 1 d . . .
C3 C 0.3396(5) 0.8432(4) 1.0554(4) 0.0205(8) Uani 1 1 d . . .
C4 C 0.2994(5) 0.8494(5) 1.1621(4) 0.0268(9) Uani 1 1 d . . .
C5 C 0.2323(5) 0.7293(4) 1.1916(4) 0.0248(9) Uani 1 1 d . . .
C6 C 0.2019(5) 0.6029(4) 1.1121(4) 0.0209(8) Uani 1 1 d . . .
C7 C 0.2388(4) 0.5948(4) 1.0040(3) 0.0168(7) Uani 1 1 d . . .
C8 C 0.2987(4) 0.5610(4) 0.7726(3) 0.0145(7) Uani 1 1 d . . .
C9 C 0.1268(5) 0.5177(4) 0.6918(3) 0.0171(7) Uani 1 1 d . . .
C10 C 0.0532(5) 0.3880(4) 0.6051(3) 0.0201(8) Uani 1 1 d . . .
C11 C 0.1496(5) 0.3023(4) 0.5952(3) 0.0187(8) Uani 1 1 d . . .
C12 C 0.3182(5) 0.3448(4) 0.6748(4) 0.0195(8) Uani 1 1 d . . .
C13 C 0.3931(5) 0.4730(4) 0.7652(3) 0.0157(7) Uani 1 1 d . . .
C14 C 0.8166(5) 0.7834(4) 0.9468(4) 0.0192(8) Uani 1 1 d . . .
C15 C 0.8233(5) 0.7927(4) 1.0712(4) 0.0201(8) Uani 1 1 d . . .
C16 C 0.6596(5) 0.7672(4) 1.0578(3) 0.0169(7) Uani 1 1 d . . .
C17 C 0.3248(5) 0.8995(4) 0.6354(4) 0.0191(8) Uani 1 1 d . . .
C18 C 0.2128(5) 0.9367(4) 0.6824(4) 0.0207(8) Uani 1 1 d . . .
C19 C 0.2194(5) 0.8745(4) 0.7802(4) 0.0186(8) Uani 1 1 d . . .
C20 C 0.5866(4) 0.4946(4) 0.5419(3) 0.0153(7) Uani 1 1 d . . .
Cu1 Cu 0.55084(5) 0.72014(5) 0.67183(4) 0.01452(13) Uani 1 1 d . . .
H3 H 0.392(4) 0.918(4) 1.043(3) 0.002(8) Uiso 1 1 d . . .
H4 H 0.321(5) 0.933(4) 1.209(4) 0.021(11) Uiso 1 1 d . . .
H5 H 0.210(5) 0.738(4) 1.266(4) 0.018(10) Uiso 1 1 d . . .
H6 H 0.157(5) 0.530(4) 1.132(4) 0.021(11) Uiso 1 1 d . . .
H7 H 0.220(4) 0.516(4) 0.954(3) 0.004(8) Uiso 1 1 d . . .
H9 H 0.060(4) 0.579(4) 0.695(3) 0.004(8) Uiso 1 1 d . . .
H10 H -0.054(5) 0.363(4) 0.560(4) 0.017(10) Uiso 1 1 d . . .
H11 H 0.098(5) 0.214(5) 0.537(4) 0.025(11) Uiso 1 1 d . . .
H12 H 0.383(4) 0.291(4) 0.668(3) 0.005(8) Uiso 1 1 d . . .
H13 H 0.506(5) 0.506(4) 0.811(4) 0.014(9) Uiso 1 1 d . . .
H14 H 0.895(5) 0.795(4) 0.917(4) 0.013(10) Uiso 1 1 d . . .
H15 H 0.919(6) 0.820(5) 1.139(4) 0.031(12) Uiso 1 1 d . . .
H16 H 0.618(5) 0.762(4) 1.115(4) 0.015(10) Uiso 1 1 d . . .
H17 H 0.349(5) 0.921(4) 0.570(4) 0.022(11) Uiso 1 1 d . . .
H18 H 0.145(5) 0.989(4) 0.659(4) 0.024(11) Uiso 1 1 d . . .
H19 H 0.159(5) 0.870(4) 0.830(4) 0.026(11) Uiso 1 1 d . . .
N1 N 0.5612(4) 0.7447(3) 0.9322(3) 0.0147(6) Uani 1 1 d . . .
N2 N 0.6571(4) 0.7535(3) 0.8624(3) 0.0154(6) Uani 1 1 d . . .
N3 N 0.3355(4) 0.8068(3) 0.7928(3) 0.0148(6) Uani 1 1 d . . .
N4 N 0.3979(4) 0.8191(3) 0.7011(3) 0.0156(6) Uani 1 1 d . . .
N5 N 0.7955(4) 0.9350(3) 0.6414(3) 0.0168(6) Uani 1 1 d . . .
O1 O 0.6429(3) 0.8728(3) 0.5776(3) 0.0256(6) Uani 1 1 d . . .
O2 O 0.8735(4) 0.9057(3) 0.7432(3) 0.0281(6) Uani 1 1 d . . .
O3 O 0.8728(3) 1.0304(3) 0.6085(3) 0.0287(7) Uani 1 1 d . . .
O4 O 0.3727(3) 0.6061(3) 0.4970(2) 0.0171(5) Uani 1 1 d . . .
O5 O 0.6724(3) 0.5892(3) 0.6456(2) 0.0168(5) Uani 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
N3 C1 N1 107.1(3) . . ?
N3 C1 C2 111.5(3) . . ?
N1 C1 C2 106.4(3) . . ?
N3 C1 C8 107.4(3) . . ?
N1 C1 C8 111.3(3) . . ?
C2 C1 C8 112.9(3) . . ?
C7 C2 C3 119.0(3) . . ?
C7 C2 C1 120.1(3) . . ?
C3 C2 C1 120.5(3) . . ?
C4 C3 C2 119.8(4) . . ?
C5 C4 C3 120.8(4) . . ?
C6 C5 C4 119.3(4) . . ?
C5 C6 C7 120.7(4) . . ?
C6 C7 C2 120.4(4) . . ?
C13 C8 C9 119.4(3) . . ?
C13 C8 C1 122.6(3) . . ?
C9 C8 C1 117.9(3) . . ?
C10 C9 C8 119.8(3) . . ?
C9 C10 C11 120.5(4) . . ?
C12 C11 C10 119.6(4) . . ?
C11 C12 C13 120.7(4) . . ?
C8 C13 C12 119.9(3) . . ?
N2 C14 C15 110.3(3) . . ?
C16 C15 C14 105.1(3) . . ?
N1 C16 C15 108.3(3) . . ?
N4 C17 C18 110.5(3) . . ?
C19 C18 C17 105.7(3) . . ?
N3 C19 C18 107.6(3) . . ?
O4 C20 O5 126.2(3) 2_666 . ?
O4 C20 C20 117.8(4) 2_666 2_666 ?
O5 C20 C20 115.9(4) . 2_666 ?
O5 Cu1 N4 168.53(11) . . ?
O5 Cu1 N2 91.97(11) . . ?
N4 Cu1 N2 86.46(12) . . ?
O5 Cu1 O4 84.55(11) . . ?
N4 Cu1 O4 91.32(12) . . ?
N2 Cu1 O4 151.01(12) . . ?
O5 Cu1 O1 99.33(12) . . ?
N4 Cu1 O1 91.24(12) . . ?
N2 Cu1 O1 120.36(12) . . ?
O4 Cu1 O1 88.55(12) . . ?
C16 N1 N2 110.1(3) . . ?
C16 N1 C1 128.9(3) . . ?
N2 N1 C1 120.9(3) . . ?
C14 N2 N1 106.1(3) . . ?
C14 N2 Cu1 133.2(3) . . ?
N1 N2 Cu1 120.7(2) . . ?
C19 N3 N4 110.0(3) . . ?
C19 N3 C1 130.6(3) . . ?
N4 N3 C1 118.1(3) . . ?
C17 N4 N3 106.2(3) . . ?
C17 N4 Cu1 130.1(3) . . ?
N3 N4 Cu1 123.5(2) . . ?
O1 N5 O3 121.0(3) . . ?
O1 N5 O2 120.1(3) . . ?
O3 N5 O2 118.9(3) . . ?
N5 O1 Cu1 109.9(2) . . ?
C20 O4 Cu1 109.7(2) 2_666 . ?
C20 O5 Cu1 111.8(2) . . ?
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
C1 N3 1.474(4) . ?
C1 N1 1.477(4) . ?
C1 C2 1.524(5) . ?
C1 C8 1.532(5) . ?
C2 C7 1.386(5) . ?
C2 C3 1.387(5) . ?
C3 C4 1.381(5) . ?
C4 C5 1.380(6) . ?
C5 C6 1.367(6) . ?
C6 C7 1.379(5) . ?
C8 C13 1.379(5) . ?
C8 C9 1.393(5) . ?
C9 C10 1.378(5) . ?
C10 C11 1.380(5) . ?
C11 C12 1.367(5) . ?
C12 C13 1.384(5) . ?
C14 N2 1.331(5) . ?
C14 C15 1.390(5) . ?
C15 C16 1.360(5) . ?
C16 N1 1.342(4) . ?
C17 N4 1.329(5) . ?
C17 C18 1.380(5) . ?
C18 C19 1.362(5) . ?
C19 N3 1.351(4) . ?
C20 O4 1.239(4) 2_666 ?
C20 O5 1.259(4) . ?
C20 C20 1.540(7) 2_666 ?
Cu1 O5 1.957(3) . ?
Cu1 N4 1.959(3) . ?
Cu1 N2 1.982(3) . ?
Cu1 O4 2.011(3) . ?
Cu1 O1 2.192(3) . ?
N1 N2 1.351(4) . ?
N3 N4 1.353(4) . ?
N5 O1 1.235(4) . ?
N5 O3 1.243(4) . ?
N5 O2 1.251(4) . ?
O4 C20 1.239(4) 2_666 ?
