#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2009060.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_2009060
loop_
_publ_author_name
'Fl\"orke, U.'
_publ_section_title
;
 Di-\m-chloro-bis[tricarbonyl(dicyclohexylphosphine)rhenium]
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900119
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Re2 Cl2 (C12 H23 P1)2 (C1 O1)6]'
_chemical_formula_moiety         'C30 H46 Cl2 O6 P2 Re2'
_chemical_formula_sum            'C30 H46 Cl2 O6 P2 Re2'
_chemical_formula_weight         1007.91
_chemical_name_systematic
;
bis[\m-chloro-tricarbonyl(dicyclohexylphosphine)rhenium]
;
_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'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.
_cell_angle_beta                 118.35(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   10.112(2)
_cell_length_b                   19.144(7)
_cell_length_c                   10.511(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      10
_cell_volume                     1790.7(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker P4'
_diffrn_measurement_method       \w
_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  0.021
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4340
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        8
_diffrn_standards_interval_count 397
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.030
_exptl_absorpt_correction_T_max  0.401
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(XPREP; Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.579
_refine_ls_extinction_coef       0.00291(16)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4129
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0272P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.054
_reflns_number_gt                3207
_reflns_number_total             4129
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    qa0171.cif
_[local]_cod_data_source_block   1
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_original_cell_volume        1790.7(9)
_cod_database_code               2009060
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Re1 0.515890(17) 0.101630(8) 0.987662(17) 0.03473(7) Uani d . 1 Re
P1 0.49173(12) 0.08010(6) 0.74463(12) 0.0360(2) Uani d . 1 P
Cl1 0.32090(11) 0.00666(5) 0.93382(12) 0.0428(2) Uani d . 1 Cl
C1 0.6725(5) 0.1678(2) 1.0387(4) 0.0438(10) Uani d . 1 C
O1 0.7657(4) 0.20947(18) 1.0731(4) 0.0665(9) Uani d . 1 O
C2 0.3793(5) 0.1782(2) 0.9150(5) 0.0441(10) Uani d . 1 C
O2 0.2992(4) 0.22470(18) 0.8718(4) 0.0706(10) Uani d . 1 O
C3 0.5376(6) 0.1162(2) 1.1806(5) 0.0516(11) Uani d . 1 C
O3 0.5506(5) 0.1292(2) 1.2909(4) 0.0857(13) Uani d . 1 O
C11 0.3164(4) 0.1075(2) 0.5849(4) 0.0440(10) Uani d D 1 C
H11 0.3148 0.1587 0.5853 0.053 Uiso calc R 1 H
C12 0.3109(6) 0.0854(3) 0.4436(5) 0.0629(14) Uani d D 1 C
H12A 0.3177 0.0349 0.4413 0.076 Uiso calc R 1 H
H12B 0.3964 0.1050 0.4380 0.076 Uiso calc R 1 H
C13 0.1664(6) 0.1097(3) 0.3142(5) 0.0809(18) Uani d D 1 C
H13A 0.1656 0.1604 0.3101 0.097 Uiso calc R 1 H
H13B 0.1631 0.0922 0.2262 0.097 Uiso calc R 1 H
C14 0.0284(6) 0.0845(3) 0.3229(6) 0.086(2) Uani d D 1 C
H14A -0.0614 0.1029 0.2417 0.103 Uiso calc R 1 H
H14B 0.0236 0.0339 0.3175 0.103 Uiso calc R 1 H
C15 0.0345(5) 0.1081(3) 0.4610(6) 0.0777(17) Uani d D 1 C
H15A -0.0525 0.0902 0.4664 0.093 Uiso calc R 1 H
H15B 0.0307 0.1587 0.4622 0.093 Uiso calc R 1 H
C16 0.1769(5) 0.0829(3) 0.5920(5) 0.0575(13) Uani d D 1 C
H16A 0.1792 0.1006 0.6795 0.069 Uiso calc R 1 H
H16B 0.1766 0.0323 0.5958 0.069 Uiso calc R 1 H
C21 0.6452(4) 0.1111(2) 0.7104(5) 0.0451(10) Uani d D 1 C
H21 0.6276 0.0911 0.6179 0.054 Uiso calc R 1 H
C22 0.6421(5) 0.1907(2) 0.6943(5) 0.0538(11) Uani d D 1 C
H22A 0.5461 0.2049 0.6152 0.065 Uiso calc R 1 H
H22B 0.6529 0.2124 0.7821 0.065 Uiso calc R 1 H
C23 0.7689(5) 0.2154(3) 0.6649(6) 0.0715(15) Uani d D 1 C
H23A 0.7521 0.1974 0.5722 0.086 Uiso calc R 1 H
H23B 0.7677 0.2660 0.6598 0.086 Uiso calc R 1 H
C24 0.9192(6) 0.1916(3) 0.7799(7) 0.092(2) Uani d D 1 C
H24A 0.9401 0.2129 0.8713 0.110 Uiso calc R 1 H
H24B 0.9962 0.2067 0.7558 0.110 Uiso calc R 1 H
C25 0.9241(6) 0.1122(3) 0.7949(8) 0.090(2) Uani d D 1 C
H25A 1.0209 0.0983 0.8732 0.108 Uiso calc R 1 H
H25B 0.9133 0.0912 0.7065 0.108 Uiso calc R 1 H
C26 0.7985(5) 0.0849(3) 0.8255(6) 0.0618(14) Uani d D 1 C
H26A 0.7993 0.0343 0.8260 0.074 Uiso calc R 1 H
H26B 0.8165 0.1008 0.9200 0.074 Uiso calc R 1 H
H1 0.493(6) 0.011(2) 0.723(5) 0.080 Uiso d . 1 H
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
Re1 0.04013(9) 0.03005(9) 0.03891(9) -0.00345(8) 0.02277(7) -0.00153(8)
P1 0.0403(5) 0.0317(5) 0.0414(6) -0.0015(4) 0.0238(5) -0.0010(4)
Cl1 0.0359(5) 0.0381(6) 0.0539(6) -0.0025(4) 0.0209(5) 0.0068(5)
C1 0.052(2) 0.040(2) 0.045(2) -0.005(2) 0.027(2) -0.003(2)
O1 0.069(2) 0.051(2) 0.078(2) -0.0241(18) 0.0329(19) -0.0113(18)
C2 0.055(3) 0.035(2) 0.049(2) 0.001(2) 0.031(2) -0.0033(19)
O2 0.077(2) 0.053(2) 0.088(3) 0.0189(19) 0.045(2) 0.0055(19)
C3 0.073(3) 0.037(3) 0.058(3) -0.009(2) 0.042(3) -0.001(2)
O3 0.145(4) 0.074(3) 0.059(2) -0.014(3) 0.065(3) -0.013(2)
C11 0.045(2) 0.038(2) 0.044(2) 0.0002(19) 0.017(2) 0.002(2)
C12 0.071(3) 0.071(4) 0.042(3) -0.004(3) 0.023(3) -0.001(2)
C13 0.104(5) 0.071(4) 0.042(3) -0.005(3) 0.014(3) 0.006(3)
C14 0.076(4) 0.070(4) 0.061(4) 0.002(3) -0.008(3) 0.008(3)
C15 0.046(3) 0.072(4) 0.091(4) 0.003(3) 0.013(3) 0.010(3)
C16 0.046(2) 0.060(3) 0.059(3) -0.006(2) 0.019(2) 0.005(2)
C21 0.047(2) 0.052(3) 0.052(2) -0.004(2) 0.036(2) -0.004(2)
C22 0.062(3) 0.050(3) 0.066(3) -0.009(2) 0.044(3) 0.001(2)
C23 0.078(4) 0.068(4) 0.097(4) -0.023(3) 0.064(3) -0.004(3)
C24 0.072(4) 0.089(5) 0.140(6) -0.027(4) 0.071(4) -0.010(4)
C25 0.060(3) 0.104(5) 0.128(6) 0.000(3) 0.062(4) -0.007(4)
C26 0.051(3) 0.067(3) 0.082(4) 0.005(2) 0.044(3) -0.005(3)
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'
O O 0.0106 0.0060 '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'
Re Re -1.0185 7.2310 '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'
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
C1 Re1 C2 . . 87.06(19)
C1 Re1 C3 . . 86.79(18)
C2 Re1 C3 . . 90.51(18)
C1 Re1 P1 . . 93.60(12)
C2 Re1 P1 . . 90.95(13)
C3 Re1 P1 . . 178.51(13)
C1 Re1 Cl1 . 3_657 97.30(13)
C2 Re1 Cl1 . 3_657 174.81(13)
C3 Re1 Cl1 . 3_657 92.54(14)
P1 Re1 Cl1 . 3_657 85.98(4)
C1 Re1 Cl1 . . 175.56(13)
C2 Re1 Cl1 . . 97.06(13)
C3 Re1 Cl1 . . 91.50(13)
P1 Re1 Cl1 . . 88.01(4)
Cl1 Re1 Cl1 3_657 . 78.67(4)
C11 P1 C21 . . 105.31(19)
C11 P1 Re1 . . 118.13(14)
C21 P1 Re1 . . 117.73(14)
Re1 Cl1 Re1 3_657 . 101.33(4)
O1 C1 Re1 . . 177.2(4)
O2 C2 Re1 . . 179.0(4)
O3 C3 Re1 . . 175.5(4)
C12 C11 C16 . . 110.9(4)
C12 C11 P1 . . 112.5(3)
C16 C11 P1 . . 112.3(3)
C11 C12 C13 . . 111.2(4)
C14 C13 C12 . . 111.6(4)
C15 C14 C13 . . 110.3(5)
C14 C15 C16 . . 111.6(5)
C11 C16 C15 . . 111.0(4)
C26 C21 C22 . . 111.9(4)
C26 C21 P1 . . 111.8(3)
C22 C21 P1 . . 111.4(3)
C23 C22 C21 . . 110.8(4)
C24 C23 C22 . . 111.8(4)
C23 C24 C25 . . 110.9(5)
C24 C25 C26 . . 111.7(4)
C21 C26 C25 . . 110.6(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Re1 C1 . 1.895(4)
Re1 C2 . 1.907(4)
Re1 C3 . 1.954(5)
Re1 P1 . 2.4824(13)
Re1 Cl1 3_657 2.5316(12)
Re1 Cl1 . 2.5404(11)
P1 C11 . 1.847(4)
P1 C21 . 1.849(4)
Cl1 Re1 3_657 2.5317(12)
C1 O1 . 1.154(5)
C2 O2 . 1.143(5)
C3 O3 . 1.130(5)
C11 C12 . 1.519(6)
C11 C16 . 1.522(5)
C12 C13 . 1.521(6)
C13 C14 . 1.520(7)
C14 C15 . 1.493(7)
C15 C16 . 1.523(6)
C21 C26 . 1.528(6)
C21 C22 . 1.533(5)
C22 C23 . 1.530(5)
C23 C24 . 1.494(7)
C24 C25 . 1.527(7)
C25 C26 . 1.541(6)