#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322309.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_4322309
loop_
_publ_author_name
'Raúl Chiozzone'
'Ricardo González'
'Carlos Kremer'
'Giovanni De Munno'
'Joan Cano'
'Francesc Lloret'
'Miguel Julve'
'Juan Faus'
_publ_section_title
;
 Synthesis, Crystal Structure, and Magnetic Properties of
 Tetraphenylarsonium Tetrachloro(oxalato)rhenate(IV) and
 Bis(2,2'-bipyridine)tetrachloro(μ-oxalato)copper(II)rhenium(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4745
_journal_page_last               4752
_journal_paper_doi               10.1021/ic990376h
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         '[ReCl4(m-ox)Cu(bipy)2]'
_chemical_formula_sum            'C22 H16 Cl4 Cu N4 O4 Re'
_chemical_formula_weight         791.9
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.
_cell_angle_beta                 93.97(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   9.421(2)
_cell_length_b                   16.909(4)
_cell_length_c                   16.179(4)
_cell_measurement_radiation      'Mo K\a'
_cell_measurement_temperature    295
_cell_measurement_wavelength     0.710730
_cell_volume                     2571.1(10)
_computing_cell_refinement       'Siemens P3/V'
_computing_data_collection       'Siemens P3/V,(VMS vers 4.21/V, 1990)'
_computing_data_reduction
'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens SHELXTL-PLUS and PARST'
_computing_structure_refinement  'Siemens SHELXTL-PLUS'
_computing_structure_solution    'Siemens SHELXTL-PLUS'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Siemens R3m/V diffractometer'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  'highly-oriented graphite crystal'
_diffrn_radiation_source         'fine-focus xray_tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710730
_diffrn_reflns_av_R_equivalents  3.83
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6019
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         1.5
_exptl_absorpt_coefficient_mu    59.84
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.36
_refine_diff_density_max         2.01
_refine_diff_density_min         -1.54
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.54
_refine_ls_hydrogen_treatment    '"riding model" with fixed isotropic U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          5.31
_refine_ls_R_factor_obs          4.37
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(σ²(F)+ 0.0010*F²))'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         6.13
_refine_ls_wR_factor_obs         6.52
_reflns_number_observed          4523
_reflns_number_total             5430
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            ic990376h_2.cif
_cod_data_source_block           (2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/(\s^2^(F)+ 0.0010*F^2^))' 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^(F)+
0.0010*F^2^))'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 2/m 1'
_cod_original_formula_sum        'C22 H16 Cl4 Cu1 N4 O4 Re1'
_cod_database_code               4322309
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_occupancy
_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_type_symbol
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_disorder_group
Re1 1.00 0.40437(3) 0.65920(2) 0.18973(2) 0.0311(1) Uani Re ? ? ?
Cl1 1.00 0.2278(2) 0.6101(1) 0.0956(1) 0.0545(7) Uani Cl ? ? ?
Cl2 1.00 0.4271(2) 0.7805(1) 0.1239(2) 0.0556(7) Uani Cl ? ? ?
Cl3 1.00 0.2396(2) 0.7102(1) 0.2774(1) 0.0531(7) Uani Cl ? ? ?
Cl4 1.00 0.5859(2) 0.6017(1) 0.1161(1) 0.0510(7) Uani Cl ? ? ?
O1 1.00 0.4090(5) 0.5577(3) 0.2596(3) 0.033(1) Uani O ? ? ?
O2 1.00 0.5612(5) 0.6871(3) 0.2781(3) 0.039(2) Uani O ? ? ?
C1 1.00 0.5131(7) 0.5523(4) 0.3165(4) 0.033(2) Uani C ? ? ?
C2 1.00 0.6080(7) 0.6278(5) 0.3265(4) 0.034(2) Uani C ? ? ?
O3 1.00 0.5346(6) 0.4960(3) 0.3604(3) 0.045(2) Uani O ? ? ?
O4 1.00 0.7103(6) 0.6301(4) 0.3742(3) 0.045(2) Uani O ? ? ?
Cu1 1.00 0.31577(9) 0.40585(5) 0.30935(5) 0.0347(3) Uani Cu ? ? ?
N1 1.00 0.2187(6) 0.4760(3) 0.3869(4) 0.033(2) Uani N ? ? ?
C3 1.00 0.2677(8) 0.4974(5) 0.4640(5) 0.041(2) Uani C ? ? ?
C4 1.00 0.205(1) 0.5561(5) 0.5078(5) 0.054(3) Uani C ? ? ?
C5 1.00 0.091(1) 0.5959(5) 0.4708(6) 0.059(3) Uani C ? ? ?
C6 1.00 0.0390(9) 0.5740(5) 0.3918(6) 0.052(3) Uani C ? ? ?
C7 1.00 0.1042(7) 0.5127(4) 0.3518(5) 0.036(2) Uani C ? ? ?
C8 1.00 0.0583(8) 0.4869(4) 0.2671(5) 0.038(2) Uani C ? ? ?
C9 1.00 -0.0606(9) 0.5135(6) 0.2218(7) 0.059(3) Uani C ? ? ?
C10 1.00 -0.096(1) 0.4821(7) 0.1430(7) 0.068(3) Uani C ? ? ?
C11 1.00 -0.011(1) 0.4258(6) 0.1119(6) 0.059(3) Uani C ? ? ?
C12 1.00 0.1091(9) 0.4022(5) 0.1599(5) 0.047(3) Uani C ? ? ?
N2 1.00 0.1447(6) 0.4326(3) 0.2344(4) 0.034(2) Uani N ? ? ?
N3 1.00 0.4503(6) 0.3760(3) 0.2254(4) 0.033(2) Uani N ? ? ?
C13 1.00 0.4513(9) 0.4031(5) 0.1478(5) 0.046(3) Uani C ? ? ?
C14 1.00 0.548(1) 0.3759(6) 0.0937(5) 0.055(3) Uani C ? ? ?
C15 1.00 0.646(1) 0.3228(6) 0.1199(6) 0.064(4) Uani C ? ? ?
C16 1.00 0.6529(9) 0.2971(5) 0.2024(6) 0.055(3) Uani C ? ? ?
C17 1.00 0.5532(8) 0.3248(4) 0.2533(5) 0.037(2) Uani C ? ? ?
C18 1.00 0.5479(7) 0.3024(4) 0.3410(5) 0.036(2) Uani C ? ? ?
C19 1.00 0.6499(9) 0.2560(5) 0.3822(6) 0.051(3) Uani C ? ? ?
C20 1.00 0.641(1) 0.2396(6) 0.4657(6) 0.059(4) Uani C ? ? ?
C21 1.00 0.526(1) 0.2687(5) 0.5049(6) 0.052(3) Uani C ? ? ?
C22 1.00 0.4250(8) 0.3146(4) 0.4605(5) 0.040(2) Uani C ? ? ?
N4 1.00 0.4374(6) 0.3317(3) 0.3803(4) 0.031(2) Uani N ? ? ?
H1W 1.00 0.289(4) 0.454(3) 0.729(5) 0.06 Uiso H ? O9 ?
H14 1.00 0.545(1) 0.3952(6) 0.0378(5) 0.06 Uiso H ? C14 ?
H3 1.00 0.3496(8) 0.4708(5) 0.4893(5) 0.06 Uiso H ? C3 ?
H15 1.00 0.711(1) 0.3022(6) 0.0822(6) 0.06 Uiso H ? C15 ?
H11 1.00 -0.035(1) 0.4030(6) 0.0583(6) 0.06 Uiso H ? C11 ?
H16 1.00 0.7258(9) 0.2611(5) 0.2229(6) 0.06 Uiso H ? C16 ?
H5 1.00 0.047(1) 0.6385(5) 0.4991(6) 0.06 Uiso H ? C5 ?
H12 1.00 0.1691(9) 0.3623(5) 0.1385(5) 0.06 Uiso H ? C12 ?
H4 1.00 0.240(1) 0.5689(5) 0.5633(5) 0.06 Uiso H ? C4 ?
H19 1.00 0.7270(9) 0.2349(5) 0.3532(6) 0.06 Uiso H ? C19 ?
H9 1.00 -0.1195(9) 0.5534(6) 0.2441(7) 0.06 Uiso H ? C9 ?
H20 1.00 0.713(1) 0.2087(6) 0.4957(6) 0.06 Uiso H ? C20 ?
H3 1.00 -0.0412(9) 0.6010(5) 0.3649(6) 0.06 Uiso H ? C6 ?
H21 1.00 0.516(1) 0.2573(5) 0.5624(6) 0.06 Uiso H ? C21 ?
H13 1.00 0.3830(9) 0.4424(5) 0.1290(5) 0.06 Uiso H ? C13 ?
H22 1.00 0.3449(8) 0.3344(4) 0.4877(5) 0.06 Uiso H ? C22 ?
H10 1.00 -0.179(1) 0.5004(7) 0.1110(7) 0.06 Uiso H ? C10 ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C Carbon 0 88 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1
H Hydrogen 0 64 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1
N Nitrogen 0 16 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1
O Oxygen 0 16 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1
Cl Chlorine 0 16 0.1320 0.1590 Internat_Tables_Vol_IV_Table_2.3.1
Cu Copper 0 4 0.2630 1.2660 Internat_Tables_Vol_IV_Table_2.3.1
Re Rhenium 0 4 -1.5980 7.2320 Internat_Tables_Vol_IV_Table_2.3.1
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cr1 O2 83.2(1) . . . .
O1 Re1 O2 79.7(2) . . . .
Cl4 Re1 O2 86.2(2) . . . .
Cl4 Re1 O1 86.8(1) . . . .
Cl3 Re1 O2 88.2(2) . . . .
Cl3 Re1 O1 87.9(1) . . . .
Cl3 Re1 Cl4 172.96(8) . . . .
Cl2 Re1 O2 91.9(2) . . . .
Cl2 Re1 O1 171.5(1) . . . .
Cl2 Re1 Cl4 92.24(8) . . . .
Cl2 Re1 Cl3 92.23(8) . . . .
Cl1 Re1 O2 172.3(2) . . . .
Cl1 Re1 O1 92.8(1) . . . .
Cl1 Re1 Cl4 91.90(7) . . . .
Cl1 Re1 Cl3 93.08(8) . . . .
Cl1 Re1 Cl2 95.67(8) . . . .
Re1 O1 C1 115.7(4) . . . .
Re1 O2 C2 115.7(4) . . . .
O1 C1 O3 124.3(6) . . . .
O1 C1 C2 114.5(6) . . . .
C2 C1 O3 121.1(6) . . . .
O2 C2 C1 113.1(6) . . . .
C1 C2 O4 121.7(6) . . . .
O2 C2 O4 125.2(7) . . . .
N3 Cu1 N4 82.3(2) . . . .
N2 Cu1 N4 153.2(2) . . . .
N2 Cu1 N3 99.7(2) . . . .
N1 Cu1 N4 106.3(2) . . . .
N1 Cu1 N3 157.5(2) . . . .
N1 Cu1 N2 82.1(2) . . . .
Cu1 N1 C7 113.6(4) . . . .
Cu1 N1 C3 126.8(5) . . . .
C3 N1 C7 118.9(6) . . . .
N1 C3 C4 122.5(7) . . . .
C3 C4 C5 118.7(8) . . . .
C4 C5 C6 119.1(9) . . . .
C5 C6 C7 119.4(8) . . . .
N1 C7 C6 121.3(7) . . . .
C6 C7 C8 122.9(7) . . . .
N1 C7 C8 115.8(6) . . . .
C7 C8 N2 114.6(6) . . . .
C7 C8 C9 125.1(7) . . . .
C9 C8 N2 120.3(7) . . . .
C8 C9 C10 119.6(9) . . . .
C9 C10 C11 120(1) . . . .
C10 C11 C12 118.1(9) . . . .
C11 C12 N2 122.7(8) . . . .
C8 N2 C12 119.5(6) . . . .
Cu1 N2 C12 127.1(5) . . . .
Cu1 N2 C8 113.3(5) . . . .
Cu1 N3 C17 114.3(5) . . . .
Cu1 N3 C13 127.0(5) . . . .
C13 N3 C17 118.7(6) . . . .
N3 C13 C14 121.9(7) . . . .
C13 C14 C15 119.5(9) . . . .
C14 C15 C16 119.9(9) . . . .
C15 C16 C17 118.4(8) . . . .
N3 C17 C16 121.5(7) . . . .
C16 C17 C18 124.1(7) . . . .
N3 C17 C18 114.5(6) . . . .
C17 C18 N4 116.0(6) . . . .
C17 C18 C19 122.9(7) . . . .
C19 C18 N4 121.1(7) . . . .
C18 C19 C20 119.8(8) . . . .
C19 C20 C21 118.6(9) . . . .
C2 C21 C22 119.5(8) . . . .
C21 C22 N4 121.2(7) . . . .
C18 N4 C22 119.8(6) . . . .
Cu1 N4 C22 127.2(5) . . . .
Cu1 N4 C18 112.9(4) . . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 Cl1 2.328(2) . . .
Re1 Cl2 2.328(2) . . .
Re1 Cl3 2.339(2) . . .
Re1 Cl4 2.360(2) . . .
Re1 O1 2.054(5) . . .
Re1 O2 2.039(5) . . .
O1 C1 1.302(8) . . .
O2 C2 1.328(9) . . .
C1 C2 1.56(1) . . .
C1 O3 1.195(9) . . .
C2 O4 1.194(8) . . .
Cu1 N1 1.995(6) . . .
Cu1 N2 2.001(6) . . .
Cu1 N3 1.985(6) . . .
Cu1 N4 2.005(6) . . .
N1 C3 1.35(1) . . .
N1 C7 1.336(9) . . .
C3 C4 1.38(1) . . .
C4 C5 1.37(1) . . .
C5 C6 1.39(1) . . .
C6 C7 1.39(1) . . .
C7 C8 1.48(1) . . .
C8 C9 1.37(1) . . .
C8 N2 1.358(9) . . .
C9 C10 1.40(2) . . .
C10 C11 1.36(1) . . .
C11 C12 1.39(1) . . .
C12 N2 1.33(1) . . .
N3 C13 1.34(1) . . .
N3 C17 1.353(9) . . .
C13 C14 1.39(1) . . .
C14 C15 1.33(1) . . .
C16 C17 1.37(1) . . .
C17 C18 1.47(1) . . .
C18 C19 1.38(1) . . .
C18 N4 1.351(9) . . .
C19 C20 1.39(1) . . .
C20 C21 1.38(1) . . .
C21 C22 1.39(1) . . .
C22 N4 1.34(1) . . .
