#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309150.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_4309150
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            'C40 H32 Cl2 Cu2 N8 O4'
_chemical_formula_weight         886.74
_chemical_name_common            JK107
_chemical_name_systematic
;
 u-oxalato-bis-[(diphenyldipyrazolylmethane)copper(II) chloride]
;
_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                95.535(2)
_cell_angle_beta                 110.303(2)
_cell_angle_gamma                106.111(2)
_cell_formula_units_Z            1
_cell_length_a                   8.6155(8)
_cell_length_b                   10.1435(9)
_cell_length_c                   11.3612(11)
_cell_measurement_temperature    100(2)
_cell_volume                     873.91(14)
_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 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0353
_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       -14
_diffrn_reflns_number            7782
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.428
_exptl_absorpt_correction_T_max  0.8703
_exptl_absorpt_correction_T_min  0.7541
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0365
_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)+(0.0532P)²+0.6656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                3611
_reflns_number_total             4046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048229tsi20041216_011457_1.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_original_cell_volume        873.90(14)
_cod_database_code               4309150
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 -0.06736(4) 0.27106(3) 0.33834(3) 0.01228(10) Uani 1 1 d . . .
Cl1 Cl -0.27853(8) 0.08090(6) 0.36777(6) 0.01732(14) Uani 1 1 d . . .
O1 O -0.1768(2) 0.41743(18) 0.35418(15) 0.0152(3) Uani 1 1 d . . .
O2 O 0.1121(2) 0.37977(18) 0.51159(16) 0.0156(3) Uani 1 1 d . . .
N3 N -0.0675(2) 0.2446(2) 0.07655(18) 0.0109(4) Uani 1 1 d . . .
N4 N -0.1693(3) 0.2368(2) 0.14632(18) 0.0135(4) Uani 1 1 d . . .
N1 N 0.1665(3) 0.1899(2) 0.22557(18) 0.0119(4) Uani 1 1 d . . .
N2 N 0.0963(3) 0.1748(2) 0.31641(18) 0.0127(4) Uani 1 1 d . . .
C20 C -0.0830(3) 0.5110(2) 0.4545(2) 0.0134(4) Uani 1 1 d . . .
C13 C 0.1034(3) 0.5222(2) 0.2289(2) 0.0141(5) Uani 1 1 d . . .
C8 C 0.2026(3) 0.4362(2) 0.2290(2) 0.0112(4) Uani 1 1 d . . .
C9 C 0.3800(3) 0.4829(3) 0.3103(2) 0.0141(5) Uani 1 1 d . . .
C10 C 0.4546(3) 0.6136(3) 0.3931(2) 0.0174(5) Uani 1 1 d . . .
C11 C 0.3528(3) 0.6975(3) 0.3967(2) 0.0173(5) Uani 1 1 d . . .
C12 C 0.1778(3) 0.6521(3) 0.3148(2) 0.0160(5) Uani 1 1 d . . .
C1 C 0.1269(3) 0.2897(2) 0.1421(2) 0.0106(4) Uani 1 1 d . . .
C2 C 0.1966(3) 0.2814(2) 0.0357(2) 0.0116(4) Uani 1 1 d . . .
C3 C 0.1737(3) 0.1515(3) -0.0349(2) 0.0152(5) Uani 1 1 d . . .
C4 C 0.2151(3) 0.1451(3) -0.1422(2) 0.0169(5) Uani 1 1 d . . .
C5 C 0.2746(3) 0.2667(3) -0.1825(2) 0.0187(5) Uani 1 1 d . . .
C6 C 0.2980(3) 0.3957(3) -0.1134(2) 0.0168(5) Uani 1 1 d . . .
C7 C 0.2608(3) 0.4034(3) -0.0036(2) 0.0142(5) Uani 1 1 d . . .
C17 C -0.3340(3) 0.1947(3) 0.0611(2) 0.0162(5) Uani 1 1 d . . .
C18 C -0.3407(3) 0.1764(3) -0.0642(2) 0.0174(5) Uani 1 1 d . . .
C19 C -0.1689(3) 0.2095(3) -0.0507(2) 0.0140(4) Uani 1 1 d . . .
C14 C 0.1675(3) 0.0934(3) 0.3868(2) 0.0155(5) Uani 1 1 d . . .
C15 C 0.2882(3) 0.0584(3) 0.3450(2) 0.0167(5) Uani 1 1 d . . .
C16 C 0.2873(3) 0.1235(2) 0.2451(2) 0.0146(5) Uani 1 1 d . . .
H11 H 0.395(4) 0.778(3) 0.452(3) 0.015(7) Uiso 1 1 d . . .
H13 H -0.007(4) 0.495(3) 0.177(3) 0.013(7) Uiso 1 1 d . . .
H6 H 0.335(4) 0.472(3) -0.140(3) 0.013(7) Uiso 1 1 d . . .
H3 H 0.133(4) 0.075(3) -0.012(3) 0.010(7) Uiso 1 1 d . . .
H15 H 0.353(4) 0.003(4) 0.375(3) 0.026(8) Uiso 1 1 d . . .
H4 H 0.197(4) 0.061(3) -0.187(3) 0.020(8) Uiso 1 1 d . . .
H14 H 0.140(4) 0.070(3) 0.456(3) 0.022(8) Uiso 1 1 d . . .
H19 H -0.124(4) 0.210(3) -0.109(3) 0.010(6) Uiso 1 1 d . . .
H16 H 0.350(4) 0.132(3) 0.201(3) 0.019(7) Uiso 1 1 d . . .
H17 H -0.433(4) 0.181(3) 0.091(3) 0.009(6) Uiso 1 1 d . . .
H7 H 0.280(3) 0.490(3) 0.043(2) 0.006(6) Uiso 1 1 d . . .
H9 H 0.448(4) 0.429(3) 0.312(3) 0.009(6) Uiso 1 1 d . . .
H10 H 0.572(4) 0.642(3) 0.447(3) 0.019(7) Uiso 1 1 d . . .
H18 H -0.435(4) 0.148(3) -0.141(3) 0.019(7) Uiso 1 1 d . . .
H12 H 0.106(4) 0.701(3) 0.316(3) 0.016(7) Uiso 1 1 d . . .
H5 H 0.294(4) 0.264(3) -0.247(3) 0.017(7) Uiso 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'
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'
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'
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
N2 Cu1 O1 162.21(8) . . ?
N2 Cu1 O2 90.25(7) . . ?
O1 Cu1 O2 83.78(7) . . ?
N2 Cu1 N4 85.39(8) . . ?
O1 Cu1 N4 92.15(7) . . ?
O2 Cu1 N4 152.39(8) . . ?
N2 Cu1 Cl1 100.14(6) . . ?
O1 Cu1 Cl1 97.64(5) . . ?
O2 Cu1 Cl1 108.27(5) . . ?
N4 Cu1 Cl1 99.33(6) . . ?
C20 O1 Cu1 111.31(15) . . ?
C20 O2 Cu1 111.15(15) 2_566 . ?
C19 N3 N4 110.34(19) . . ?
C19 N3 C1 129.13(19) . . ?
N4 N3 C1 120.52(18) . . ?
C17 N4 N3 105.90(19) . . ?
C17 N4 Cu1 131.88(17) . . ?
N3 N4 Cu1 122.05(15) . . ?
C16 N1 N2 109.55(19) . . ?
C16 N1 C1 131.01(19) . . ?
N2 N1 C1 118.44(18) . . ?
C14 N2 N1 106.33(19) . . ?
C14 N2 Cu1 129.36(16) . . ?
N1 N2 Cu1 124.19(15) . . ?
O2 C20 O1 126.5(2) 2_566 . ?
O2 C20 C20 116.7(3) 2_566 2_566 ?
O1 C20 C20 116.8(3) . 2_566 ?
C8 C13 C12 120.1(2) . . ?
C8 C13 H13 120.4(19) . . ?
C12 C13 H13 119.5(19) . . ?
C13 C8 C9 119.8(2) . . ?
C13 C8 C1 122.7(2) . . ?
C9 C8 C1 117.5(2) . . ?
C10 C9 C8 119.9(2) . . ?
C10 C9 H9 118.5(18) . . ?
C8 C9 H9 121.6(18) . . ?
C9 C10 C11 120.2(2) . . ?
C9 C10 H10 118.6(19) . . ?
C11 C10 H10 121.2(19) . . ?
C12 C11 C10 119.8(2) . . ?
C12 C11 H11 118.0(19) . . ?
C10 C11 H11 122.1(19) . . ?
C11 C12 C13 120.1(2) . . ?
C11 C12 H12 123.1(19) . . ?
C13 C12 H12 116.8(19) . . ?
N1 C1 N3 106.73(17) . . ?
N1 C1 C2 111.88(18) . . ?
N3 C1 C2 106.28(17) . . ?
N1 C1 C8 107.30(17) . . ?
N3 C1 C8 111.70(17) . . ?
C2 C1 C8 112.84(18) . . ?
C7 C2 C3 119.2(2) . . ?
C7 C2 C1 119.3(2) . . ?
C3 C2 C1 120.9(2) . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 H3 119.3(18) . . ?
C2 C3 H3 120.4(18) . . ?
C3 C4 C5 120.2(2) . . ?
C3 C4 H4 119(2) . . ?
C5 C4 H4 121(2) . . ?
C6 C5 C4 120.1(2) . . ?
C6 C5 H5 119(2) . . ?
C4 C5 H5 121(2) . . ?
C5 C6 C7 120.1(2) . . ?
C5 C6 H6 119.8(19) . . ?
C7 C6 H6 120.1(19) . . ?
C2 C7 C6 120.2(2) . . ?
C2 C7 H7 120.7(16) . . ?
C6 C7 H7 119.1(16) . . ?
N4 C17 C18 110.9(2) . . ?
N4 C17 H17 120.0(15) . . ?
C18 C17 H17 129.0(15) . . ?
C19 C18 C17 105.1(2) . . ?
C19 C18 H18 124.9(19) . . ?
C17 C18 H18 130.0(19) . . ?
N3 C19 C18 107.7(2) . . ?
N3 C19 H19 121.9(18) . . ?
C18 C19 H19 130.3(18) . . ?
N2 C14 C15 110.6(2) . . ?
N2 C14 H14 121.5(19) . . ?
C15 C14 H14 127.8(19) . . ?
C16 C15 C14 105.3(2) . . ?
C16 C15 H15 126(2) . . ?
C14 C15 H15 129(2) . . ?
N1 C16 C15 108.1(2) . . ?
N1 C16 H16 120(2) . . ?
C15 C16 H16 132(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
Cu1 N2 1.991(2) . ?
Cu1 O1 1.9921(17) . ?
Cu1 O2 2.0009(17) . ?
Cu1 N4 2.002(2) . ?
Cu1 Cl1 2.3961(7) . ?
O1 C20 1.257(3) . ?
O2 C20 1.256(3) 2_566 ?
N3 C19 1.353(3) . ?
N3 N4 1.363(3) . ?
N3 C1 1.487(3) . ?
N4 C17 1.329(3) . ?
N1 C16 1.357(3) . ?
N1 N2 1.366(3) . ?
N1 C1 1.481(3) . ?
N2 C14 1.329(3) . ?
C20 O2 1.256(3) 2_566 ?
C20 C20 1.535(5) 2_566 ?
C13 C8 1.380(3) . ?
C13 C12 1.396(3) . ?
C13 H13 0.87(3) . ?
C8 C9 1.396(3) . ?
C8 C1 1.530(3) . ?
C9 C10 1.387(3) . ?
C9 H9 0.90(3) . ?
C10 C11 1.388(4) . ?
C10 H10 0.93(3) . ?
C11 C12 1.381(4) . ?
C11 H11 0.88(3) . ?
C12 H12 0.90(3) . ?
C1 C2 1.530(3) . ?
C2 C7 1.390(3) . ?
C2 C3 1.401(3) . ?
C3 C4 1.384(3) . ?
C3 H3 0.86(3) . ?
C4 C5 1.384(4) . ?
C4 H4 0.89(3) . ?
C5 C6 1.383(4) . ?
C5 H5 0.80(3) . ?
C6 C7 1.393(3) . ?
C6 H6 0.88(3) . ?
C7 H7 0.92(3) . ?
C17 C18 1.397(3) . ?
C17 H17 1.00(3) . ?
C18 C19 1.372(3) . ?
C18 H18 0.91(3) . ?
C19 H19 0.88(3) . ?
C14 C15 1.396(3) . ?
C14 H14 0.93(3) . ?
C15 C16 1.366(4) . ?
C15 H15 0.90(3) . ?
C16 H16 0.85(3) . ?
