#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007267.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_2007267
loop_
_publ_author_name
'Flörke, Ulrich'
_publ_section_title
μ-Chloro-(μ-dicyclohexylphosphanido)bis[tricarbonyl(triphenylphosphine)rhenium]
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800017
_journal_paper_doi               10.1107/S0108270198099703
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '[Re2 Cl (C12 H22 P )(C18 H15 P )2 (C O )6 ]'
_chemical_formula_sum            'C54 H52 Cl O6 P3 Re2'
_chemical_formula_weight         1297.72
_chemical_name_systematic
;
 (μ-dicyclohexyl)(μ-chloro)bis(triphenylphosphane-tricarbonyl-rhenium)
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 114.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.228(4)
_cell_length_b                   25.010(9)
_cell_length_c                   10.823(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      8
_cell_volume                     2517.5(19)
_computing_structure_refinement  'SHELXTL V5 (Siemens 1995)'
_computing_structure_solution    'SHELXTL V5 (Siemens 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3'
_diffrn_measurement_method       omega
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5807
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.002
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.372
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SHELXTL (Siemens, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.924
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_restrained_S_obs      1.023
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_obs          .0469
_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)+(0.0367P)²+16.3787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1347
_refine_ls_wR_factor_obs         .0903
_reflns_number_observed          3670
_reflns_number_total             5559
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            qa0036.cif
_cod_data_source_block           s401
_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^)+(0.0367P)^2^+16.3787P] 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^)+(0.0367P)^2^+16.3787P] 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        2517.5(18)
_cod_original_sg_symbol_Hall     '-P 2y1'
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2007267
_cod_database_fobs_code          2007267
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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 .02248(3) .171788(15) .16439(3) .02791(11) Uani d . 1 . Re
Cl1 .1943(3) .2500 .2770(3) .0367(8) Uani d S 1 . Cl
P1 -.1306(3) .2500 .0470(3) .0287(7) Uani d S 1 . P
P2 .1893(3) .10124(11) .2913(3) .0352(6) Uani d . 1 . P
C1 -.1128(10) .1192(4) .0717(9) .038(2) Uani d . 1 . C
O1 -.1975(8) .0869(3) .0106(7) .052(2) Uani d . 1 . O
C2 .0943(9) .1703(4) .0202(9) .036(2) Uani d . 1 . C
O2 .1294(8) .1699(3) -.0668(7) .058(2) Uani d . 1 . O
C3 -.0494(10) .1756(5) .3079(10) .047(3) Uani d . 1 . C
O3 -.0917(11) .1760(4) .3901(9) .084(3) Uani d . 1 . O
C11 -.1706(14) .2500 -.1385(12) .039(3) Uani d S 1 . C
H11A -.0763(14) .2500 -.1417(12) .047 Uiso calc SR 1 . H
C12 -.2472(11) .2995(5) -.2188(9) .054(3) Uani d . 1 . C
H12A -.1976(11) .3314(5) -.1716(9) .064 Uiso calc R 1 . H
H12B -.3448(11) .3007(5) -.2256(9) .064 Uiso calc R 1 . H
C13 -.2505(16) .2983(5) -.3622(10) .075(4) Uani d . 1 . C
H13A -.3004(16) .3298(5) -.4117(10) .090 Uiso calc R 1 . H
H13B -.1527(16) .2996(5) -.3548(10) .090 Uiso calc R 1 . H
C14 -.323(3) .2500 -.4393(17) .095(7) Uani d S 1 . C
H14A -.423(3) .2500 -.4542(17) .113 Uiso calc SR 1 . H
H14B -.319(3) .2500 -.5272(17) .113 Uiso calc SR 1 . H
C21 -.3127(16) .2500 .053(2) .062(5) Uani d S 1 . C
C24 -.572(3) .2500 .096(3) .127(9) Uiso d S 1 . C
C22 -.3877(15) .2008(6) .0278(16) .034(4) Uiso d P .59(2) 1 C
H22A -.3294(15) .1749(6) .0949(16) .080 Uiso calc PR .59(2) 1 H
H22B -.4003(15) .1877(6) -.0608(16) .080 Uiso calc PR .59(2) 1 H
C23 -.532(3) .2040(12) .032(3) .101(10) Uiso d P .59(2) 1 C
H23A -.604(3) .2019(12) -.061(3) .080 Uiso calc PR .59(2) 1 H
H23B -.543(3) .1719(12) .077(3) .080 Uiso calc PR .59(2) 1 H
C25 -.343(3) .2122(14) .139(4) .080(12) Uiso d P .41(2) 2 C
H25A -.281(3) .2210(14) .232(4) .080 Uiso calc PR .41(2) 2 H
H25B -.314(3) .1770(14) .121(4) .080 Uiso calc PR .41(2) 2 H
C26 -.499(2) .2083(9) .125(2) .033(6) Uiso d P .41(2) 2 C
H26A -.548(2) .1818(9) .056(2) .080 Uiso calc PR .41(2) 2 H
H26B -.495(2) .1950(9) .211(2) .080 Uiso calc PR .41(2) 2 H
C31 .1019(10) .0360(4) .2843(10) .044(2) Uani d . 1 . C
C32 -.0137(12) .0344(5) .3175(11) .055(3) Uani d . 1 . C
H32 -.0476(12) .0663(5) .3375(11) .066 Uiso calc R 1 . H
C33 -.0807(12) -.0123(5) .3221(12) .063(3) Uani d . 1 . C
H33 -.1586(12) -.0117(5) .3455(12) .075 Uiso calc R 1 . H
C34 -.0348(17) -.0590(5) .2932(14) .078(4) Uani d . 1 . C
H34 -.0797(17) -.0910(5) .2961(14) .094 Uiso calc R 1 . H
C35 .0781(19) -.0580(6) .2599(17) .097(5) Uani d . 1 . C
H35 .1108(19) -.0901(6) .2399(17) .117 Uiso calc R 1 . H
C36 .1478(14) -.0112(5) .2540(14) .073(4) Uani d . 1 . C
H36 .2249(14) -.0120(5) .2297(14) .088 Uiso calc R 1 . H
C41 .2889(10) .1086(5) .4762(10) .047(3) Uani d . 1 . C
C42 .2843(12) .1539(6) .5422(10) .065(4) Uani d . 1 . C
H42 .2326(12) .1832(6) .4931(10) .077 Uiso calc R 1 . H
C43 .3566(15) .1571(6) .6840(11) .086(5) Uani d . 1 . C
H43 .3521(15) .1881(6) .7298(11) .104 Uiso calc R 1 . H
C44 .4348(15) .1134(8) .7542(13) .093(6) Uani d . 1 . C
H44 .4846(15) .1153(8) .8482(13) .112 Uiso calc R 1 . H
C45 .4404(15) .0681(7) .6898(14) .087(5) Uani d . 1 . C
H45 .4941(15) .0392(7) .7391(14) .105 Uiso calc R 1 . H
C46 .3672(11) .0646(5) .5518(12) .060(3) Uani d . 1 . C
H46 .3693(11) .0329(5) .5077(12) .072 Uiso calc R 1 . H
C51 .3311(10) .0849(4) .2345(11) .044(3) Uani d . 1 . C
C52 .2924(13) .0646(5) .1043(11) .054(3) Uani d . 1 . C
H52 .1961(13) .0585(5) .0481(11) .065 Uiso calc R 1 . H
C53 .3966(15) .0536(5) .0588(14) .067(4) Uani d . 1 . C
H53 .3709(15) .0387(5) -.0269(14) .081 Uiso calc R 1 . H
C54 .5373(15) .0645(5) .1388(17) .073(4) Uani d . 1 . C
H54 .6066(15) .0582(5) .1059(17) .088 Uiso calc R 1 . H
C55 .5777(13) .0847(5) .2673(16) .072(4) Uani d . 1 . C
H55 .6740(13) .0918(5) .3215(16) .086 Uiso calc R 1 . H
C56 .4755(12) .0942(5) .3154(13) .058(3) Uani d . 1 . C
H56 .5031(12) .1070(5) .4033(13) .070 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 0.0033 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 C3 . . 91.3(4)
C1 Re1 C2 . . 89.9(4)
C3 Re1 C2 . . 178.3(4)
C1 Re1 P2 . . 88.9(3)
C3 Re1 P2 . . 89.7(3)
C2 Re1 P2 . . 91.6(3)
C1 Re1 P1 . . 96.4(3)
C3 Re1 P1 . . 90.1(3)
C2 Re1 P1 . . 88.5(3)
P2 Re1 P1 . . 174.71(9)
C1 Re1 Cl1 . . 175.1(3)
C3 Re1 Cl1 . . 89.7(3)
C2 Re1 Cl1 . . 89.1(3)
P2 Re1 Cl1 . . 95.93(8)
P1 Re1 Cl1 . . 78.78(8)
Re1 Cl1 Re1 . 4_565 99.00(11)
C11 P1 C21 . . 104.8(7)
C11 P1 Re1 . 4_565 110.9(2)
C21 P1 Re1 . 4_565 113.6(3)
C11 P1 Re1 . . 110.9(2)
C21 P1 Re1 . . 113.6(3)
Re1 P1 Re1 4_565 . 103.13(12)
C41 P2 C51 . . 103.2(5)
C41 P2 C31 . . 99.9(5)
C51 P2 C31 . . 103.0(5)
C41 P2 Re1 . . 118.8(4)
C51 P2 Re1 . . 115.8(3)
C31 P2 Re1 . . 113.7(3)
O1 C1 Re1 . . 178.2(8)
O2 C2 Re1 . . 176.9(7)
O3 C3 Re1 . . 177.6(11)
C12 C11 C12 4_565 . 108.2(11)
C12 C11 P1 4_565 . 116.2(7)
C12 C11 P1 . . 116.2(7)
C11 C12 C13 . . 110.4(10)
C14 C13 C12 . . 112.4(12)
C13 C14 C13 4_565 . 109.5(15)
C22 C21 C22 . 4_565 120.8(16)
C25 C21 C25 . 4_565 82.(3)
C22 C21 P1 . . 117.2(8)
C22 C21 P1 4_565 . 117.2(8)
C25 C21 P1 . . 119.7(15)
C25 C21 P1 4_565 . 119.7(15)
C26 C24 C26 . 4_565 113.(3)
C23 C24 C23 . 4_565 102.(3)
C21 C22 C23 . . 114.2(16)
C24 C23 C22 . . 121.(2)
C21 C25 C26 . . 118.(2)
C21 C25 C25 . 4_565 49.1(15)
C26 C25 C25 . 4_565 93.6(16)
C24 C26 C25 . . 118.(3)
C36 C31 C32 . . 117.4(10)
C36 C31 P2 . . 124.5(8)
C32 C31 P2 . . 118.0(9)
C33 C32 C31 . . 122.3(11)
C34 C33 C32 . . 120.3(11)
C33 C34 C35 . . 118.0(13)
C34 C35 C36 . . 122.9(13)
C31 C36 C35 . . 119.1(11)
C42 C41 C46 . . 119.0(10)
C42 C41 P2 . . 122.2(8)
C46 C41 P2 . . 118.7(10)
C41 C42 C43 . . 120.6(13)
C44 C43 C42 . . 118.5(15)
C45 C44 C43 . . 121.4(13)
C44 C45 C46 . . 120.0(14)
C45 C46 C41 . . 120.4(14)
C56 C51 C52 . . 118.7(9)
C56 C51 P2 . . 122.1(9)
C52 C51 P2 . . 119.1(8)
C53 C52 C51 . . 120.0(11)
C54 C53 C52 . . 120.2(13)
C53 C54 C55 . . 120.7(10)
C56 C55 C54 . . 119.6(12)
C55 C56 C51 . . 120.8(12)
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 C1 . 1.870(10) ?
Re1 C3 . 1.978(10) ?
Re1 C2 . 1.983(9) ?
Re1 P2 . 2.441(3) ?
Re1 P1 . 2.497(2) ?
Re1 Cl1 . 2.572(2) ?
Cl1 Re1 4_565 2.572(2) ?
P1 C11 . 1.874(12) ?
P1 C21 . 1.890(14) ?
P1 Re1 4_565 2.497(2) ?
P2 C41 . 1.839(10) ?
P2 C51 . 1.841(9) ?
P2 C31 . 1.848(11) ?
C1 O1 . 1.168(11) ?
C2 O2 . 1.138(10) ?
C3 O3 . 1.140(11) ?
C11 C12 4_565 1.529(12) ?
C11 C12 . 1.529(12) ?
C12 C13 . 1.538(14) ?
C13 C14 . 1.48(2) ?
C14 C13 4_565 1.48(2) ?
C21 C22 . 1.42(2) ?
C21 C22 4_565 1.42(2) ?
C21 C25 . 1.44(3) ?
C21 C25 4_565 1.44(3) ?
C24 C26 . 1.25(2) ?
C24 C26 4_565 1.25(2) ?
C24 C23 . 1.49(3) ?
C24 C23 4_565 1.49(3) ?
C22 C23 . 1.50(3) ?
C25 C26 . 1.54(4) ?
C25 C25 4_565 1.89(7) ?
C31 C36 . 1.36(2) ?
C31 C32 . 1.371(13) ?
C32 C33 . 1.365(15) ?
C33 C34 . 1.34(2) ?
C34 C35 . 1.35(2) ?
C35 C36 . 1.39(2) ?
C41 C42 . 1.35(2) ?
C41 C46 . 1.405(15) ?
C42 C43 . 1.401(14) ?
C43 C44 . 1.38(2) ?
C44 C45 . 1.34(2) ?
C45 C46 . 1.37(2) ?
C51 C56 . 1.387(14) ?
C51 C52 . 1.391(15) ?
C52 C53 . 1.375(14) ?
C53 C54 . 1.36(2) ?
C54 C55 . 1.37(2) ?
C55 C56 . 1.37(2) ?
