#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006196.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_2006196
loop_
_publ_author_name
'Cotton, F. A.'
'Daniels, L. M.'
'Lu, J.'
'Ren, T.'
_publ_section_title
;
 Tetrakis(\m-2-biphenylcarboxylato-<i>O</i>:<i>O</i>')bis[chlororhenium(III)]
 Bis(dichloromethane) Solvate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              714
_journal_page_last               716
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Re2 Cl2 (C13 H9 O2)4], 2CH2 Cl2'
_chemical_formula_moiety         'Re2Cl2(O2C13H9)4, 2(CH2Cl2)'
_chemical_formula_structural     'Re2Cl2(O2CPhPh)4, 2(CH2Cl2)'
_chemical_formula_sum            'C54 H40 Cl6 O8 Re2'
_chemical_formula_weight         1401.96
_chemical_name_common
;
Dichloro-tetrabiphenylcarboxylate-dirhenium
;
_chemical_name_systematic
;
Dichloro tetrakis(\m~2~-2-biphenylcarboxylato) dirhenium(III) -
dichloromethane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                76.13(2)
_cell_angle_beta                 89.66(3)
_cell_angle_gamma                65.21(2)
_cell_formula_units_Z            1
_cell_length_a                   11.364(3)
_cell_length_b                   11.372(3)
_cell_length_c                   11.668(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      28.5
_cell_volume                     1321.3(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1989)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1985)'
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC-5R'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3561
_diffrn_reflns_theta_max         57
_diffrn_reflns_theta_min         3.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.045
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type
'empirical via \y scan (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.764
_refine_diff_density_min         -1.881
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_obs          0.0314
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0524P)^2^+4.3865P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0842
_refine_ls_wR_factor_obs         0.0826
_reflns_number_observed          3370
_reflns_number_total             3561
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    bs1024.cif
_[local]_cod_data_source_block   re2biphoac4
_cod_original_cell_volume        1321.3(6)
_cod_database_code               2006196
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Re 0.0183(2) 0.0204(2) 0.0401(2) -0.01016(12) 0.00621(11) -0.01529(11)
Cl1 0.0586(11) 0.0597(11) 0.0646(11) -0.0402(9) 0.0270(9) -0.0193(9)
O1 0.031(2) 0.027(2) 0.052(2) -0.017(2) 0.013(2) -0.018(2)
O2 0.028(2) 0.025(2) 0.046(2) -0.012(2) 0.012(2) -0.015(2)
O3 0.023(2) 0.033(2) 0.047(2) -0.013(2) 0.003(2) -0.015(2)
O4 0.024(2) 0.034(2) 0.044(2) -0.016(2) 0.002(2) -0.013(2)
C1 0.025(3) 0.030(3) 0.048(3) -0.015(3) 0.006(3) -0.019(3)
C2 0.043(4) 0.025(3) 0.047(3) -0.018(3) 0.013(3) -0.020(3)
C3 0.063(5) 0.044(4) 0.064(4) -0.036(4) 0.023(4) -0.031(3)
C4 0.081(6) 0.045(4) 0.077(5) -0.046(4) 0.023(4) -0.035(4)
C5 0.087(6) 0.043(4) 0.076(5) -0.031(4) 0.023(5) -0.042(4)
C6 0.060(5) 0.041(4) 0.081(5) -0.019(4) 0.025(4) -0.040(4)
C7 0.047(4) 0.029(3) 0.051(4) -0.014(3) 0.008(3) -0.020(3)
C8 0.029(3) 0.030(3) 0.072(5) -0.007(3) 0.012(3) -0.026(3)
C9 0.060(5) 0.051(5) 0.078(6) -0.021(4) 0.000(4) -0.024(4)
C10 0.066(6) 0.070(6) 0.121(8) -0.032(5) -0.015(6) -0.041(6)
C11 0.056(6) 0.065(6) 0.158(11) -0.039(5) 0.026(6) -0.042(7)
C12 0.084(7) 0.106(8) 0.103(8) -0.066(7) 0.031(6) -0.038(6)
C13 0.074(6) 0.083(6) 0.082(6) -0.052(5) 0.029(5) -0.039(5)
C14 0.024(3) 0.029(3) 0.045(4) -0.010(3) 0.005(3) -0.023(3)
C15 0.023(3) 0.036(3) 0.053(4) -0.008(3) 0.002(3) -0.022(3)
C16 0.029(3) 0.051(4) 0.074(5) -0.019(3) 0.004(3) -0.026(4)
C17 0.028(4) 0.061(5) 0.096(6) -0.018(3) -0.006(4) -0.039(5)
C18 0.030(4) 0.068(5) 0.094(6) -0.008(4) -0.018(4) -0.039(5)
C19 0.040(4) 0.051(4) 0.058(4) -0.004(3) -0.010(3) -0.019(4)
C20 0.025(3) 0.042(4) 0.055(4) -0.004(3) -0.002(3) -0.024(3)
C21 0.032(4) 0.043(4) 0.056(4) -0.007(3) -0.007(3) -0.001(3)
C22 0.058(5) 0.126(9) 0.075(6) -0.050(6) 0.009(5) -0.020(6)
C23 0.075(7) 0.156(13) 0.094(8) -0.065(9) 0.014(6) 0.005(8)
C24 0.058(6) 0.078(7) 0.159(12) -0.037(6) -0.004(7) 0.019(8)
C25 0.072(7) 0.051(5) 0.177(12) -0.032(5) 0.012(7) -0.035(6)
C26 0.060(5) 0.051(5) 0.098(7) -0.024(4) 0.015(5) -0.026(5)
C101 0.135(11) 0.168(14) 0.102(9) -0.087(11) -0.004(8) -0.038(9)
Cl2 0.173(4) 0.303(7) 0.191(4) -0.168(5) 0.071(4) -0.126(5)
Cl3 0.145(3) 0.300(6) 0.109(3) -0.102(4) -0.008(2) -0.060(3)
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Re 0.04739(2) 0.54614(2) -0.06947(2) 0.02423(12) Uani d . 1 Re
Cl1 0.1474(2) 0.6495(2) -0.2284(2) 0.0553(4) Uani d . 1 Cl
O1 -0.0223(4) 0.7138(4) -0.0120(4) 0.0340(9) Uani d . 1 O
O2 -0.1164(4) 0.6219(4) 0.1258(4) 0.0315(9) Uani d . 1 O
O3 -0.1172(4) 0.6240(4) -0.1816(4) 0.0328(9) Uani d . 1 O
O4 -0.2108(4) 0.5316(4) -0.0438(4) 0.0320(9) Uani d . 1 O
C1 -0.0927(5) 0.7205(6) 0.0759(5) 0.0316(13) Uani d . 1 C
C2 -0.1428(6) 0.8433(6) 0.1164(5) 0.0353(14) Uani d . 1 C
C3 -0.0657(7) 0.9124(7) 0.1082(6) 0.049(2) Uani d . 1 C
H3A 0.0105(7) 0.8845(7) 0.0714(6) 0.059 Uiso calc R 1 H
C4 -0.1015(8) 1.0220(7) 0.1544(7) 0.057(2) Uani d . 1 C
H4A -0.0488(8) 1.0668(7) 0.1505(7) 0.069 Uiso calc R 1 H
C5 -0.2161(9) 1.0646(7) 0.2064(7) 0.062(2) Uani d . 1 C
H5A -0.2410(9) 1.1384(7) 0.2377(7) 0.075 Uiso calc R 1 H
C6 -0.2935(8) 0.9979(7) 0.2120(7) 0.057(2) Uani d . 1 C
H6A -0.3707(8) 1.0283(7) 0.2469(7) 0.069 Uiso calc R 1 H
C7 -0.2607(6) 0.8876(6) 0.1677(6) 0.041(2) Uani d . 1 C
C8 -0.3529(6) 0.8255(6) 0.1706(7) 0.043(2) Uani d . 1 C
C9 -0.4075(8) 0.8234(8) 0.0656(8) 0.062(2) Uani d . 1 C
H9A -0.3833(8) 0.8565(8) -0.0070(8) 0.075 Uiso calc R 1 H
C10 -0.4994(9) 0.7708(9) 0.0702(10) 0.081(3) Uani d . 1 C
H10A -0.5369(9) 0.7694(9) 0.0002(10) 0.097 Uiso calc R 1 H
C11 -0.5343(9) 0.7214(10) 0.1770(12) 0.086(3) Uani d . 1 C
H11A -0.5959(9) 0.6873(10) 0.1788(12) 0.104 Uiso calc R 1 H
C12 -0.4809(10) 0.7216(11) 0.2793(10) 0.086(3) Uani d . 1 C
H12A -0.5035(10) 0.6862(11) 0.3518(10) 0.104 Uiso calc R 1 H
C13 -0.3916(9) 0.7756(9) 0.2748(8) 0.069(2) Uani d . 1 C
H13A -0.3566(9) 0.7780(9) 0.3455(8) 0.083 Uiso calc R 1 H
C14 -0.2158(5) 0.6038(6) -0.1474(5) 0.0305(13) Uani d . 1 C
C15 -0.3350(6) 0.6598(6) -0.2291(6) 0.0366(14) Uani d . 1 C
C16 -0.4187(6) 0.5968(7) -0.2051(7) 0.049(2) Uani d . 1 C
H16A -0.4008(6) 0.5277(7) -0.1365(7) 0.058 Uiso calc R 1 H
C17 -0.5269(7) 0.6369(8) -0.2824(8) 0.059(2) Uani d . 1 C
H17A -0.5824(7) 0.5951(8) -0.2663(8) 0.070 Uiso calc R 1 H
C18 -0.5530(7) 0.7378(9) -0.3828(8) 0.065(2) Uani d . 1 C
H18A -0.6255(7) 0.7636(9) -0.4358(8) 0.078 Uiso calc R 1 H
C19 -0.4726(7) 0.8024(8) -0.4067(7) 0.054(2) Uani d . 1 C
H19A -0.4921(7) 0.8711(8) -0.4758(7) 0.065 Uiso calc R 1 H
C20 -0.3635(6) 0.7666(7) -0.3296(6) 0.042(2) Uani d . 1 C
C21 -0.2865(6) 0.8467(7) -0.3547(6) 0.049(2) Uani d . 1 C
C22 -0.2138(9) 0.8428(12) -0.4500(8) 0.083(3) Uani d . 1 C
H22A -0.2112(9) 0.7884(12) -0.4990(8) 0.100 Uiso calc R 1 H
C23 -0.1457(11) 0.9190(16) -0.4723(11) 0.111(4) Uani d . 1 C
H23A -0.0968(11) 0.9155(16) -0.5366(11) 0.133 Uiso calc R 1 H
C24 -0.1480(10) 0.9989(12) -0.4032(14) 0.105(4) Uani d . 1 C
H24A -0.1022(10) 1.0511(12) -0.4210(14) 0.126 Uiso calc R 1 H
C25 -0.2185(10) 1.0038(9) -0.3054(13) 0.098(4) Uani d . 1 C
H25A -0.2182(10) 1.0563(9) -0.2554(13) 0.117 Uiso calc R 1 H
C26 -0.2894(8) 0.9281(8) -0.2843(9) 0.068(2) Uani d . 1 C
H26A -0.3399(8) 0.9328(8) -0.2210(9) 0.082 Uiso calc R 1 H
C101 -0.8435(14) 0.5755(16) -0.5124(11) 0.127(5) Uani d . 1 C
H10B -0.8881(14) 0.6392(16) -0.4665(11) 0.152 Uiso calc R 1 H
H10C -0.8174(14) 0.4863(16) -0.4603(11) 0.152 Uiso calc R 1 H
Cl2 -0.7113(5) 0.5923(7) -0.5506(5) 0.188(2) Uani d . 1 Cl
Cl3 -0.9528(4) 0.5979(6) -0.6249(4) 0.180(2) Uani d . 1 Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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
Re Re Cl1 2_565 . 178.23(5) y
O2 Re Re 2_565 2_565 89.39(11) y
O1 Re Re . 2_565 90.17(11) y
O4 Re Re 2_565 2_565 90.20(11) y
O3 Re Re . 2_565 89.35(12) y
O2 Re O1 2_565 . 179.56(14) y
O2 Re O4 2_565 2_565 89.5(2) y
O1 Re O4 . 2_565 90.4(2) y
O2 Re O3 2_565 . 90.7(2) y
O1 Re O3 . . 89.3(2) y
O4 Re O3 2_565 . 179.49(14) y
O2 Re Cl1 2_565 . 90.11(12) y
O1 Re Cl1 . . 90.33(12) y
O4 Re Cl1 2_565 . 91.50(12) y
O3 Re Cl1 . . 88.95(12) y
C1 O1 Re . . 119.3(3) ?
C1 O2 Re . 2_565 120.9(4) ?
C14 O3 Re . . 120.1(4) ?
C14 O4 Re . 2_565 119.5(3) ?
O2 C1 O1 . . 120.2(5) ?
O2 C1 C2 . . 121.2(5) ?
O1 C1 C2 . . 118.6(5) ?
C3 C2 C7 . . 120.3(5) ?
C3 C2 C1 . . 117.4(5) ?
C7 C2 C1 . . 122.2(5) ?
C4 C3 C2 . . 120.4(7) ?
C5 C4 C3 . . 119.5(7) ?
C6 C5 C4 . . 120.0(6) ?
C5 C6 C7 . . 122.3(7) ?
C6 C7 C2 . . 117.5(6) ?
C6 C7 C8 . . 119.2(6) ?
C2 C7 C8 . . 123.2(5) ?
C13 C8 C9 . . 118.1(7) ?
C13 C8 C7 . . 121.7(7) ?
C9 C8 C7 . . 120.1(7) ?
C8 C9 C10 . . 119.1(9) ?
C11 C10 C9 . . 120.4(9) ?
C12 C11 C10 . . 120.9(9) ?
C11 C12 C13 . . 118.7(10) ?
C8 C13 C12 . . 122.7(9) ?
O4 C14 O3 . . 120.8(5) ?
O4 C14 C15 . . 119.1(5) ?
O3 C14 C15 . . 120.0(6) ?
C20 C15 C16 . . 120.3(6) ?
C20 C15 C14 . . 122.8(6) ?
C16 C15 C14 . . 116.8(6) ?
C17 C16 C15 . . 120.2(7) ?
C18 C17 C16 . . 119.9(7) ?
C17 C18 C19 . . 120.7(7) ?
C18 C19 C20 . . 121.3(8) ?
C19 C20 C15 . . 117.6(7) ?
C19 C20 C21 . . 119.0(7) ?
C15 C20 C21 . . 123.3(6) ?
C26 C21 C22 . . 118.9(8) ?
C26 C21 C20 . . 120.0(7) ?
C22 C21 C20 . . 121.1(8) ?
C23 C22 C21 . . 119.9(11) ?
C24 C23 C22 . . 121.4(12) ?
C23 C24 C25 . . 120.2(10) ?
C24 C25 C26 . . 118.2(11) ?
C21 C26 C25 . . 121.3(10) ?
Cl2 C101 Cl3 . . 116.9(8) ?
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
Re Re 2_565 2.2363(7) y
Re Cl1 . 2.482(2) y
Re O1 . 2.013(4) y
Re O2 2_565 2.009(4) y
Re O3 . 2.019(4) y
Re O4 2_565 2.017(4) y
O1 C1 . 1.294(7) y
O2 C1 . 1.268(7) y
O3 C14 . 1.279(7) y
O4 C14 . 1.275(7) y
C1 C2 . 1.465(8) ?
C2 C3 . 1.391(9) ?
C2 C7 . 1.405(9) ?
C3 C4 . 1.380(9) ?
C4 C5 . 1.379(11) ?
C5 C6 . 1.374(11) ?
C6 C7 . 1.376(9) ?
C7 C8 . 1.486(9) ?
C8 C13 . 1.365(11) ?
C8 C9 . 1.387(11) ?
C9 C10 . 1.400(12) ?
C10 C11 . 1.368(15) ?
C11 C12 . 1.343(15) ?
C12 C13 . 1.384(12) ?
C14 C15 . 1.466(8) ?
C15 C20 . 1.396(9) ?
C15 C16 . 1.404(9) ?
C16 C17 . 1.371(10) ?
C17 C18 . 1.361(12) ?
C18 C19 . 1.382(11) ?
C19 C20 . 1.388(9) ?
C20 C21 . 1.491(10) ?
C21 C26 . 1.368(11) ?
C21 C22 . 1.378(12) ?
C22 C23 . 1.37(2) ?
C23 C24 . 1.35(2) ?
C24 C25 . 1.39(2) ?
C25 C26 . 1.389(12) ?
C101 Cl2 . 1.638(13) ?
C101 Cl3 . 1.710(12) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_3
_geom_torsion
O1 Re Re O2 2_565 0.03(15)
O3 Re Re O4 2_565 0.24(14)