#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:52:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179310 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/07/4320718.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_4320718
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'Marina A. Petrukhina'
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 10. Redox
 Reactions of an Edge-Sharing Dirhenium(III) Non-metal-Metal-Bonded
 Complex, Re2(μ-Cl)2Cl4(PMe3)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6825
_journal_page_last               6831
_journal_paper_doi               10.1021/ic010653w
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Re2 Cl5 (P (C H3)3)4'
_chemical_formula_structural     Re2(\m-Cl)3Cl2(PMe3)4
_chemical_formula_sum            'C12 H36 Cl5 P4 Re2'
_chemical_formula_weight         853.94
_chemical_melting_point          ?
_chemical_name_systematic
; 
Tris-(mu-chloro)-bis-chloro-tetrakis-trimethylphosphine- 
di-rhenium(II,III) 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 94.65(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.377(2)
_cell_length_b                   13.071(2)
_cell_length_c                   10.818(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     1321.6(4)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4128
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         2.77
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    9.896
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.320
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.049
_refine_diff_density_min         -2.255
_refine_diff_density_rms         0.326
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2946
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.037
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_obs          0.0630
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1390P)²+12.9800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1642
_refine_ls_wR_factor_obs         0.1625
_reflns_number_observed          2895
_reflns_number_total             2946
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010653w_2.cif
_cod_data_source_block           Re2Cl5(PMe3)4_(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1390P)^2^+12.9800P] 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^)+(0.1390P)^2^+12.9800P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320718
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re1 Re 0.73393(9) 0.51604(6) 0.31461(7) 0.0195(3) Uani 1 d . .
Re2 Re 0.76723(8) 0.42778(5) 0.09460(6) 0.0179(3) Uani 1 d . .
P1 P 0.5834(7) 0.4393(5) 0.4548(5) 0.0308(14) Uani 1 d . .
P2 P 0.9313(7) 0.5451(5) 0.4582(5) 0.0307(14) Uani 1 d . .
P3 P 0.6501(7) 0.2752(4) 0.0191(5) 0.0288(13) Uani 1 d . .
P4 P 0.9983(6) 0.3761(4) 0.0526(5) 0.0247(13) Uani 1 d . .
Cl1 Cl 0.5361(6) 0.5043(4) 0.1464(4) 0.0255(12) Uani 1 d . .
Cl2 Cl 0.8099(7) 0.3405(4) 0.2917(4) 0.0331(14) Uani 1 d . .
Cl3 Cl 0.8553(6) 0.6019(4) 0.1491(4) 0.0265(11) Uani 1 d . .
Cl4 Cl 0.6530(8) 0.6836(4) 0.3647(5) 0.044(2) Uani 1 d . .
Cl5 Cl 0.7180(7) 0.4903(5) -0.1101(5) 0.036(2) Uani 1 d . .
C1 C 0.6611(30) 0.3509(26) 0.5727(22) 0.048(7) Uani 1 d . .
H1A H 0.7423(30) 0.3832(26) 0.6184(22) 0.071 Uiso 1 calc R .
H1B H 0.6924(30) 0.2893(26) 0.5330(22) 0.071 Uiso 1 calc R .
H1C H 0.5898(30) 0.3335(26) 0.6294(22) 0.071 Uiso 1 calc R .
C2 C 0.4902(46) 0.5294(29) 0.5533(36) 0.082(12) Uani 1 d . .
H2A H 0.5595(46) 0.5750(29) 0.5957(36) 0.123 Uiso 1 calc R .
H2B H 0.4411(46) 0.4911(29) 0.6140(36) 0.123 Uiso 1 calc R .
H2C H 0.4211(46) 0.5691(29) 0.5018(36) 0.123 Uiso 1 calc R .
C3 C 0.4407(38) 0.3636(31) 0.3863(31) 0.071(11) Uani 1 d . .
H3A H 0.3889(38) 0.4021(31) 0.3204(31) 0.107 Uiso 1 calc R .
H3B H 0.3763(38) 0.3458(31) 0.4488(31) 0.107 Uiso 1 calc R .
H3C H 0.4789(38) 0.3016(31) 0.3524(31) 0.107 Uiso 1 calc R .
C4 C 1.0467(25) 0.4361(19) 0.5138(23) 0.036(5) Uani 1 d U .
H4A H 0.9875(25) 0.3813(19) 0.5420(23) 0.054 Uiso 1 calc R .
H4B H 1.1130(25) 0.4586(19) 0.5818(23) 0.054 Uiso 1 calc R .
H4C H 1.0999(25) 0.4114(19) 0.4465(23) 0.054 Uiso 1 calc R .
C5 C 1.0592(34) 0.6361(20) 0.4113(27) 0.051(7) Uani 1 d U .
H5A H 1.0892(34) 0.6169(20) 0.3307(27) 0.076 Uiso 1 calc R .
H5B H 1.1417(34) 0.6370(20) 0.4715(27) 0.076 Uiso 1 calc R .
H5C H 1.0160(34) 0.7035(20) 0.4062(27) 0.076 Uiso 1 calc R .
C6 C 0.8988(31) 0.6014(21) 0.6066(22) 0.043(6) Uani 1 d U .
H6A H 0.8294(31) 0.5603(21) 0.6462(22) 0.065 Uiso 1 calc R .
H6B H 0.8620(31) 0.6702(21) 0.5937(22) 0.065 Uiso 1 calc R .
H6C H 0.9877(31) 0.6037(21) 0.6591(22) 0.065 Uiso 1 calc R .
C7 C 0.6523(34) 0.1650(21) 0.1155(22) 0.046(7) Uani 1 d U .
H7A H 0.7502(34) 0.1490(21) 0.1449(22) 0.069 Uiso 1 calc R .
H7B H 0.6109(34) 0.1076(21) 0.0685(22) 0.069 Uiso 1 calc R .
H7C H 0.5970(34) 0.1784(21) 0.1858(22) 0.069 Uiso 1 calc R .
C8 C 0.4675(37) 0.2917(27) -0.0241(32) 0.065(9) Uani 1 d U .
H8A H 0.4543(37) 0.3510(27) -0.0779(32) 0.097 Uiso 1 calc R .
H8B H 0.4167(37) 0.3021(27) 0.0494(32) 0.097 Uiso 1 calc R .
H8C H 0.4305(37) 0.2314(27) -0.0679(32) 0.097 Uiso 1 calc R .
C9 C 0.7122(28) 0.2250(19) -0.1228(20) 0.033(6) Uani 1 d . .
H9A H 0.8143(28) 0.2122(19) -0.1111(20) 0.050 Uiso 1 calc R .
H9B H 0.6930(28) 0.2743(19) -0.1891(20) 0.050 Uiso 1 calc R .
H9C H 0.6625(28) 0.1616(19) -0.1444(20) 0.050 Uiso 1 calc R .
C10 C 1.0571(29) 0.2515(24) 0.1047(26) 0.047(7) Uani 1 d . .
H10A H 0.9901(29) 0.2003(24) 0.0706(26) 0.070 Uiso 1 calc R .
H10B H 1.0618(29) 0.2489(24) 0.1946(26) 0.070 Uiso 1 calc R .
H10C H 1.1511(29) 0.2379(24) 0.0771(26) 0.070 Uiso 1 calc R .
C11 C 1.0453(37) 0.3802(25) -0.1088(25) 0.053(8) Uani 1 d . .
H11A H 1.0171(37) 0.4458(25) -0.1451(25) 0.080 Uiso 1 calc R .
H11B H 0.9958(37) 0.3258(25) -0.1556(25) 0.080 Uiso 1 calc R .
H11C H 1.1478(37) 0.3714(25) -0.1109(25) 0.080 Uiso 1 calc R .
C12 C 1.1374(31) 0.4582(24) 0.1267(26) 0.048(7) Uani 1 d U .
H12A H 1.1168(31) 0.5290(24) 0.1049(26) 0.071 Uiso 1 calc R .
H12B H 1.2294(31) 0.4392(24) 0.0985(26) 0.071 Uiso 1 calc R .
H12C H 1.1401(31) 0.4503(24) 0.2160(26) 0.071 Uiso 1 calc R .
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'
P P 0.1023 0.0942 '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'
Re Re -1.0185 7.2310 '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
P2 Re1 P1 97.1(2) . . y
P2 Re1 Cl4 87.1(2) . . y
P1 Re1 Cl4 91.5(2) . . y
P2 Re1 Cl2 89.9(2) . . y
P1 Re1 Cl2 81.9(2) . . y
Cl4 Re1 Cl2 172.4(2) . . y
P2 Re1 Cl3 91.2(2) . . y
P1 Re1 Cl3 171.0(2) . . y
Cl4 Re1 Cl3 85.5(2) . . y
Cl2 Re1 Cl3 101.5(2) . . y
P2 Re1 Cl1 172.5(2) . . y
P1 Re1 Cl1 89.7(2) . . y
Cl4 Re1 Cl1 89.5(2) . . y
Cl2 Re1 Cl1 94.3(2) . . y
Cl3 Re1 Cl1 81.9(2) . . y
P2 Re1 Re2 120.9(2) . . y
P1 Re1 Re2 120.1(2) . . y
Cl4 Re1 Re2 130.94(15) . . y
Cl2 Re1 Re2 56.36(12) . . y
Cl3 Re1 Re2 57.25(12) . . y
Cl1 Re1 Re2 57.36(12) . . y
P4 Re2 Cl5 91.8(2) . . y
P4 Re2 P3 95.7(2) . . y
Cl5 Re2 P3 85.4(2) . . y
P4 Re2 Cl2 86.9(2) . . y
Cl5 Re2 Cl2 172.0(2) . . y
P3 Re2 Cl2 86.9(2) . . y
P4 Re2 Cl3 90.9(2) . . y
Cl5 Re2 Cl3 86.6(2) . . y
P3 Re2 Cl3 169.8(2) . . y
Cl2 Re2 Cl3 101.2(2) . . y
P4 Re2 Cl1 172.7(2) . . y
Cl5 Re2 Cl1 88.0(2) . . y
P3 Re2 Cl1 91.6(2) . . y
Cl2 Re2 Cl1 94.3(2) . . y
Cl3 Re2 Cl1 81.8(2) . . y
P4 Re2 Re1 118.05(14) . . y
Cl5 Re2 Re1 130.68(15) . . y
P3 Re2 Re1 125.34(15) . . y
Cl2 Re2 Re1 56.29(13) . . y
Cl3 Re2 Re1 56.94(12) . . y
Cl1 Re2 Re1 57.48(11) . . y
C3 P1 C1 100.6(15) . . n
C3 P1 C2 102.6(21) . . n
C1 P1 C2 100.3(15) . . n
C3 P1 Re1 115.8(11) . . n
C1 P1 Re1 119.2(10) . . n
C2 P1 Re1 115.5(13) . . n
C5 P2 C6 98.4(12) . . n
C5 P2 C4 102.4(13) . . n
C6 P2 C4 99.2(12) . . n
C5 P2 Re1 115.4(10) . . n
C6 P2 Re1 118.1(9) . . n
C4 P2 Re1 119.8(9) . . n
C8 P3 C7 102.8(16) . . n
C8 P3 C9 101.1(14) . . n
C7 P3 C9 102.4(12) . . n
C8 P3 Re2 113.6(11) . . n
C7 P3 Re2 119.5(8) . . n
C9 P3 Re2 115.0(8) . . n
C10 P4 C12 101.9(14) . . n
C10 P4 C11 103.5(13) . . n
C12 P4 C11 100.5(14) . . n
C10 P4 Re2 117.7(10) . . n
C12 P4 Re2 112.6(10) . . n
C11 P4 Re2 118.1(10) . . n
Re2 Cl1 Re1 65.16(13) . . y
Re1 Cl2 Re2 67.36(14) . . y
Re1 Cl3 Re2 65.81(14) . . y
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
Re1 P2 2.349(6) . y
Re1 P1 2.376(6) . y
Re1 Cl4 2.394(5) . y
Re1 Cl2 2.421(5) . y
Re1 Cl3 2.468(5) . y
Re1 Cl1 2.496(5) . y
Re1 Re2 2.6858(11) . y
Re2 P4 2.349(6) . y
Re2 Cl5 2.371(5) . y
Re2 P3 2.389(6) . y
Re2 Cl2 2.423(5) . y
Re2 Cl3 2.476(5) . y
Re2 Cl1 2.492(5) . y
P1 C3 1.78(3) . n
P1 C1 1.83(3) . n
P1 C2 1.85(3) . n
P2 C5 1.79(3) . n
P2 C6 1.81(3) . n
P2 C4 1.86(2) . n
P3 C8 1.75(3) . n
P3 C7 1.78(3) . n
P3 C9 1.81(2) . n
P4 C10 1.80(3) . n
P4 C12 1.82(3) . n
P4 C11 1.84(3) . n
