#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/74/2007416.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_2007416
loop_
_publ_author_name
'Harben, Spencer M.'
'Smith, Paul D.'
'Beddoes, Roy L.'
'Helliwell, Madeleine'
'Collison, David'
'Garner, C. David'
_publ_section_title
;
 Mixed-halide Complex trans-Tetrahalobis(triphenylphosphine
 oxide)rhenium(IV)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              941
_journal_page_last               943
_journal_paper_doi               10.1107/S0108270197018027
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Re1 Br2.5 Cl1.5 (C18 H15 O1 P1)2]'
_chemical_formula_sum            'C36 H30 Br2.5 Cl1.5 O2 P2 Re'
_chemical_formula_weight         995.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                108.59(2)
_cell_angle_beta                 93.55(2)
_cell_angle_gamma                102.414(15)
_cell_formula_units_Z            1
_cell_length_a                   9.728(2)
_cell_length_b                   10.556(2)
_cell_length_c                   9.499(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      14.7
_cell_volume                     893.9(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC-5R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2822
_diffrn_reflns_theta_max         60.07
_diffrn_reflns_theta_min         4.56
_diffrn_standards_decay_%        1.35
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.046
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_type   '\DF (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tabular
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.414
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.095
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_obs          .052
_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)+(0.0756P)²+7.75P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.148
_refine_ls_wR_factor_obs         .1411
_reflns_number_observed          2538
_reflns_number_total             2640
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            cf1176.cif
_cod_data_source_block           s365
_cod_depositor_comments
;
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^)+(0.0756P)^2^+7.75P] 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^)+(0.0756P)^2^+7.75P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        894.0(3)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C36 H30 Br2.50 Cl1.50 O2 P2 Re'
_cod_database_code               2007416
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_disorder_group
_atom_site_type_symbol
Re1 0 0 0 .0305(2) Uani d S 1 . Re
Br1 -.0605(2) .1375(2) -.1476(2) .0619(4) Uani d P .63 . Br
Br2 -.1395(2) .1024(2) .1876(2) .0658(5) Uani d P .63 . Br
Cl1 -.0605(2) .1375(2) -.1476(2) .0619(4) Uani d P .38 . Cl
Cl2 -.1395(2) .1024(2) .1876(2) .0658(5) Uani d P .38 . Cl
P1 .2726(3) .2616(3) .2312(3) .0430(6) Uani d . 1 . P
O1 .1753(7) .1539(7) .1067(9) .053(2) Uani d . 1 . O
C1 .3123(12) .2057(12) .3863(12) .051(3) Uani d . 1 . C
C2 .4463(13) .2082(14) .4366(15) .065(3) Uani d . 1 . C
H2 .5210(13) .2368(14) .3883(15) .078 Uiso calc R 1 . H
C3 .4737(16) .1689(17) .5579(18) .083(4) Uani d . 1 . C
H3 .5662(16) .1718(17) .5929(18) .100 Uiso calc R 1 . H
C4 .3609(17) .1249(16) .6274(16) .080(4) Uani d . 1 . C
H4 .3783(17) .0990(16) .7103(16) .095 Uiso calc R 1 . H
C5 .2257(16) .1191(15) .5766(15) .073(4) Uani d . 1 . C
H5 .1508(16) .0873(15) .6227(15) .087 Uiso calc R 1 . H
C6 .1999(14) .1609(13) .4553(14) .062(3) Uani d . 1 . C
H6 .1077(14) .1588(13) .4206(14) .075 Uiso calc R 1 . H
C7 .1999(11) .4085(10) .3013(12) .048(2) Uani d . 1 . C
C8 .1202(14) .4421(12) .1979(15) .063(3) Uani d . 1 . C
H8 .0998(14) .3866(12) .0973(15) .075 Uiso calc R 1 . H
C9 .0722(15) .5616(13) .2504(19) .075(4) Uani d . 1 . C
H9 .0185(15) .5858(13) .1834(19) .091 Uiso calc R 1 . H
C10 .1018(15) .6435(14) .3969(18) .075(4) Uani d . 1 . C
H10 .0711(15) .7243(14) .4289(18) .090 Uiso calc R 1 . H
C11 .1776(16) .6059(15) .4977(18) .081(4) Uani d . 1 . C
H11 .1961(16) .6602(15) .5987(18) .098 Uiso calc R 1 . H
C12 .2267(14) .4868(14) .4485(15) .068(3) Uani d . 1 . C
H12 .2776(14) .4612(14) .5164(15) .082 Uiso calc R 1 . H
C13 .4335(11) .3107(12) .1597(12) .050(3) Uani d . 1 . C
C14 .4808(13) .2039(14) .0597(15) .063(3) Uani d . 1 . C
H14 .4281(13) .1128(14) .0301(15) .076 Uiso calc R 1 . H
C15 .6080(14) .2382(17) .0068(17) .077(4) Uani d . 1 . C
H15 .6410(14) .1688(17) -.0591(17) .093 Uiso calc R 1 . H
C16 .6840(15) .368(2) .0480(18) .087(5) Uani d . 1 . C
H16 .7702(15) .388(2) .0124(18) .105 Uiso calc R 1 . H
C17 .6365(16) .4763(17) .1444(19) .086(4) Uani d . 1 . C
H17 .6898(16) .5669(17) .1703(19) .104 Uiso calc R 1 . H
C18 .5097(14) .4475(14) .2007(15) .067(3) Uani d . 1 . C
H18 .4766(14) .5180(14) .2645(15) .080 Uiso calc R 1 . H
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'
Br Br -0.6763 1.2805 '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'
P P 0.2955 0.4335 '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'
Cl Cl 0.3639 0.7018 '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
O1 Re1 O1 . 2 180.0 no
O1 Re1 Cl2 . 2 89.4(2) yes
O1 Re1 Cl2 2 2 90.6(2) no
O1 Re1 Br2 . 2 89.4(2) no
O1 Re1 Br2 2 2 90.6(2) no
Cl2 Re1 Br2 2 2 0.0(2) ?
O1 Re1 Br2 . . 90.6(2) ?
O1 Re1 Br2 2 . 89.4(2) ?
Cl2 Re1 Br2 2 . 180.0 ?
Br2 Re1 Br2 2 . 180.0 no
O1 Re1 Cl2 . . 90.6(2) ?
O1 Re1 Cl2 2 . 89.4(2) ?
Cl2 Re1 Cl2 2 . 180.0 ?
Br2 Re1 Cl2 2 . 180.0 ?
Br2 Re1 Cl2 . . 0.0(2) ?
O1 Re1 Cl1 . 2 90.6(2) yes
O1 Re1 Cl1 2 2 89.4(2) no
Cl2 Re1 Cl1 2 2 89.65(6) yes
Br2 Re1 Cl1 2 2 89.65(6) no
Br2 Re1 Cl1 . 2 90.35(6) no
Cl2 Re1 Cl1 . 2 90.35(6) no
O1 Re1 Br1 . 2 90.6(2) no
O1 Re1 Br1 2 2 89.4(2) no
Cl2 Re1 Br1 2 2 89.65(6) no
Br2 Re1 Br1 2 2 89.65(6) no
Br2 Re1 Br1 . 2 90.35(6) no
Cl2 Re1 Br1 . 2 90.35(6) no
Cl1 Re1 Br1 2 2 0.00(14) ?
O1 Re1 Br1 . . 89.4(2) ?
O1 Re1 Br1 2 . 90.6(2) ?
Cl2 Re1 Br1 2 . 90.35(6) ?
Br2 Re1 Br1 2 . 90.35(6) ?
Br2 Re1 Br1 . . 89.65(6) ?
Cl2 Re1 Br1 . . 89.65(6) ?
Cl1 Re1 Br1 2 . 180.0 yes
Br1 Re1 Br1 2 . 180.0 yes
O1 Re1 Cl1 . . 89.4(2) ?
O1 Re1 Cl1 2 . 90.6(2) ?
Cl2 Re1 Cl1 2 . 90.35(6) ?
Br2 Re1 Cl1 2 . 90.35(6) ?
Br2 Re1 Cl1 . . 89.65(6) ?
Cl2 Re1 Cl1 . . 89.65(6) ?
Cl1 Re1 Cl1 2 . 180.0 ?
Br1 Re1 Cl1 2 . 180.0 ?
Br1 Re1 Cl1 . . 0.00(14) ?
O1 P1 C13 . . 106.9(5) ?
O1 P1 C7 . . 110.7(5) ?
C13 P1 C7 . . 109.4(5) ?
O1 P1 C1 . . 113.2(5) ?
C13 P1 C1 . . 109.0(5) ?
C7 P1 C1 . . 107.6(5) ?
P1 O1 Re1 . . 158.1(5) yes
C2 C1 C6 . . 120.1(11) ?
C2 C1 P1 . . 122.3(9) ?
C6 C1 P1 . . 117.6(9) ?
C1 C2 C3 . . 120.9(12) ?
C1 C2 H2 . . 119.5(7) ?
C3 C2 H2 . . 119.5(8) ?
C2 C3 C4 . . 118.7(13) ?
C2 C3 H3 . . 120.6(8) ?
C4 C3 H3 . . 120.6(8) ?
C5 C4 C3 . . 121.1(12) ?
C5 C4 H4 . . 119.4(8) ?
C3 C4 H4 . . 119.4(8) ?
C4 C5 C6 . . 119.5(13) ?
C4 C5 H5 . . 120.3(8) ?
C6 C5 H5 . . 120.3(8) ?
C1 C6 C5 . . 119.6(12) ?
C1 C6 H6 . . 120.2(7) ?
C5 C6 H6 . . 120.2(8) ?
C12 C7 C8 . . 121.4(11) ?
C12 C7 P1 . . 121.0(9) ?
C8 C7 P1 . . 117.6(9) ?
C7 C8 C9 . . 117.6(13) ?
C7 C8 H8 . . 121.2(7) ?
C9 C8 H8 . . 121.2(9) ?
C10 C9 C8 . . 121.7(14) ?
C10 C9 H9 . . 119.1(8) ?
C8 C9 H9 . . 119.1(9) ?
C9 C10 C11 . . 119.4(12) ?
C9 C10 H10 . . 120.3(8) ?
C11 C10 H10 . . 120.3(8) ?
C10 C11 C12 . . 120.1(13) ?
C10 C11 H11 . . 120.0(8) ?
C12 C11 H11 . . 120.0(9) ?
C7 C12 C11 . . 119.7(13) ?
C7 C12 H12 . . 120.1(7) ?
C11 C12 H12 . . 120.1(9) ?
C18 C13 C14 . . 121.1(11) ?
C18 C13 P1 . . 122.1(9) ?
C14 C13 P1 . . 116.8(9) ?
C15 C14 C13 . . 118.1(13) ?
C15 C14 H14 . . 120.9(9) ?
C13 C14 H14 . . 120.9(7) ?
C16 C15 C14 . . 121.4(14) ?
C16 C15 H15 . . 119.3(9) ?
C14 C15 H15 . . 119.3(9) ?
C15 C16 C17 . . 121.2(13) ?
C15 C16 H16 . . 119.4(9) ?
C17 C16 H16 . . 119.4(9) ?
C18 C17 C16 . . 119.7(14) ?
C18 C17 H17 . . 120.2(9) ?
C16 C17 H17 . . 120.2(9) ?
C17 C18 C13 . . 118.4(13) ?
C17 C18 H18 . . 120.8(9) ?
C13 C18 H18 . . 120.8(7) ?
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
Re1 O1 . 2.030(7) yes
Re1 O1 2 2.030(7) ?
Re1 Cl2 2 2.426(2) yes
Re1 Br2 2 2.426(2) no
Re1 Br2 . 2.426(2) ?
Re1 Cl2 . 2.426(2) ?
Re1 Cl1 2 2.445(2) yes
Re1 Br1 2 2.445(2) no
Re1 Br1 . 2.445(2) ?
Re1 Cl1 . 2.445(2) ?
P1 O1 . 1.459(8) yes
P1 C13 . 1.785(11) ?
P1 C7 . 1.795(10) ?
P1 C1 . 1.803(11) ?
C1 C2 . 1.35(2) ?
C1 C6 . 1.38(2) ?
C2 C3 . 1.37(2) ?
C2 H2 . .93 ?
C3 C4 . 1.39(2) ?
C3 H3 . .93 ?
C4 C5 . 1.35(2) ?
C4 H4 . .93 ?
C5 C6 . 1.39(2) ?
C5 H5 . .93 ?
C6 H6 . .93 ?
C7 C12 . 1.35(2) ?
C7 C8 . 1.39(2) ?
C8 C9 . 1.39(2) ?
C8 H8 . .93 ?
C9 C10 . 1.36(2) ?
C9 H9 . .93 ?
C10 C11 . 1.38(2) ?
C10 H10 . .93 ?
C11 C12 . 1.39(2) ?
C11 H11 . .93 ?
C12 H12 . .93 ?
C13 C18 . 1.39(2) ?
C13 C14 . 1.41(2) ?
C14 C15 . 1.38(2) ?
C14 H14 . .93 ?
C15 C16 . 1.33(2) ?
C15 H15 . .93 ?
C16 C17 . 1.40(2) ?
C16 H16 . .93 ?
C17 C18 . 1.39(2) ?
C17 H17 . .93 ?
C18 H18 . .93 ?
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_1
_geom_torsion
C13 P1 O1 Re1 . 169.2(12)
C7 P1 O1 Re1 . -71.7(14)
C1 P1 O1 Re1 . 49.2(14)
O1 Re1 O1 P1 2 -178.(16)
Cl2 Re1 O1 P1 2 -149.6(13)
Br2 Re1 O1 P1 2 -149.6(13)
Br2 Re1 O1 P1 . 30.4(13)
Cl2 Re1 O1 P1 . 30.4(13)
Cl1 Re1 O1 P1 2 -60.0(13)
Br1 Re1 O1 P1 2 -60.0(13)
Br1 Re1 O1 P1 . 120.0(13)
Cl1 Re1 O1 P1 . 120.0(13)
O1 P1 C1 C2 . 120.7(11)
C13 P1 C1 C2 . 1.9(12)
C7 P1 C1 C2 . -116.6(11)
O1 P1 C1 C6 . -60.1(11)
C13 P1 C1 C6 . -178.8(10)
C7 P1 C1 C6 . 62.6(11)
C6 C1 C2 C3 . -1.(2)
P1 C1 C2 C3 . 178.0(12)
C1 C2 C3 C4 . 1.(2)
C2 C3 C4 C5 . 1.(3)
C3 C4 C5 C6 . -2.(3)
C2 C1 C6 C5 . 0.(2)
P1 C1 C6 C5 . -179.0(10)
C4 C5 C6 C1 . 1.(2)
O1 P1 C7 C12 . 147.1(10)
C13 P1 C7 C12 . -95.4(11)
C1 P1 C7 C12 . 22.9(12)
O1 P1 C7 C8 . -35.5(10)
C13 P1 C7 C8 . 82.0(10)
C1 P1 C7 C8 . -159.7(9)
C12 C7 C8 C9 . 1.8(19)
P1 C7 C8 C9 . -175.6(10)
C7 C8 C9 C10 . 0.(2)
C8 C9 C10 C11 . -2.(2)
C9 C10 C11 C12 . 2.(2)
C8 C7 C12 C11 . -2.(2)
P1 C7 C12 C11 . 175.3(11)
C10 C11 C12 C7 . 0.(2)
O1 P1 C13 C18 . 139.7(10)
C7 P1 C13 C18 . 19.8(12)
C1 P1 C13 C18 . -97.6(11)
O1 P1 C13 C14 . -40.7(10)
C7 P1 C13 C14 . -160.6(9)
C1 P1 C13 C14 . 82.0(10)
C18 C13 C14 C15 . 2.0(19)
P1 C13 C14 C15 . -177.6(10)
C13 C14 C15 C16 . -0.(2)
C14 C15 C16 C17 . -2.(3)
C15 C16 C17 C18 . 2.(3)
C16 C17 C18 C13 . 0.(2)
C14 C13 C18 C17 . -2.0(19)
P1 C13 C18 C17 . 177.6(11)
