#------------------------------------------------------------------------------
#$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $
#$Revision: 91933 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007266.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_2007266
loop_
_publ_author_name
'Fl\"orke, Ulrich'
_publ_section_title
;
 Octacarbonylbis(\m-cyclohexylphosphanido)manganeserhenium
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800016
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '[Mn Re (C6 H12 P )2 (C O )8 ]'
_chemical_formula_sum            'C20 H24 Mn O8 P2 Re'
_chemical_formula_weight         695.47
_chemical_name_systematic
;
 Bis(\m-cyclohexylphosphido)-octacarbonyl-manganese-rhenium
;
_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                66.16(2)
_cell_angle_beta                 87.77(2)
_cell_angle_gamma                75.19(2)
_cell_formula_units_Z            2
_cell_length_a                   9.722(2)
_cell_length_b                   11.360(2)
_cell_length_c                   13.123(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      9
_cell_volume                     1278.2(5)
_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-2theta
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6439
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        insignificant
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.389
_exptl_absorpt_correction_T_max  0.306
_exptl_absorpt_correction_T_min  0.196
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SHELXTL (Siemens, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.641
_refine_ls_extinction_coef       0.0006(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         6181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.166
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_obs          .0394
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+1.2095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_obs         .0848
_reflns_number_observed          4528
_reflns_number_total             6181
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    qa0035.cif
_[local]_cod_data_source_block   s388
_cod_database_code               2007266
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 .15910(3) .15592(3) .29910(2) .04049(12) Uani d P .6064(9) . Re
Mn1 .15910(3) .15592(3) .29910(2) .04049(12) Uani d P .3936(9) . Mn
Mn2 .50882(4) .23174(4) .18535(3) .0434(2) Uani d P .6064(9) . Mn
Re2 .50882(4) .23174(4) .18535(3) .0434(2) Uani d P .3936(9) . Re
P1 .34516(14) .25298(13) .32402(11) .0375(3) Uani d . 1 . P
P2 .32008(14) .14437(13) .15253(11) .0395(3) Uani d . 1 . P
C1 .0565(6) .3320(6) .1952(5) .0480(12) Uani d . 1 . C
O1 -.0028(5) .4348(4) .1327(4) .0808(14) Uani d . 1 . O
C2 .0301(6) .0756(6) .2646(5) .0568(15) Uani d . 1 . C
O2 -.0545(6) .0306(5) .2487(4) .090(2) Uani d . 1 . O
C3 .0558(6) .1707(6) .4186(5) .0567(14) Uani d . 1 . C
O3 -.0127(6) .1767(5) .4920(4) .094(2) Uani d . 1 . O
C4 .2770(6) -.0152(6) .3953(5) .0550(14) Uani d . 1 . C
O4 .3452(5) -.1139(4) .4539(4) .0804(14) Uani d . 1 . O
C5 .5924(6) .0590(6) .2943(5) .0543(14) Uani d . 1 . C
O5 .6410(5) -.0425(5) .3615(4) .0824(15) Uani d . 1 . O
C6 .6400(6) .2994(6) .2300(5) .0582(15) Uani d . 1 . C
O6 .7234(5) .3371(6) .2561(4) .087(2) Uani d . 1 . O
C7 .6253(6) .2039(6) .0768(5) .0571(14) Uani d . 1 . C
O7 .7027(5) .1879(5) .0124(4) .0843(15) Uani d . 1 . O
C8 .3968(6) .4004(6) .0863(5) .0492(13) Uani d . 1 . C
O8 .3249(5) .4985(4) .0276(4) .0723(13) Uani d . 1 . O
C11 .2843(6) .4176(6) .3344(5) .0581(14) Uani d . 1 . C
H11 .2074(6) .4728(6) .2757(5) .070 Uiso calc R 1 . H
C12 .2192(8) .4004(7) .4447(6) .078(2) Uani d . 1 . C
H12A .1374(8) .3649(7) .4491(6) .094 Uiso calc R 1 . H
H12B .2886(8) .3364(7) .5054(6) .094 Uiso calc R 1 . H
C13 .1728(9) .5305(8) .4587(8) .104(3) Uani d . 1 . C
H13A .0888(9) .5867(8) .4087(8) .125 Uiso calc R 1 . H
H13B .1459(9) .5118(8) .5345(8) .125 Uiso calc R 1 . H
C14 .2803(10) .6030(10) .4365(10) .130(4) Uani d . 1 . C
H14A .3577(10) .5539(10) .4943(10) .156 Uiso calc R 1 . H
H14B .2395(10) .6887(10) .4396(10) .156 Uiso calc R 1 . H
C15 .3381(10) .6247(8) .3261(9) .115(3) Uani d . 1 . C
H15A .4149(10) .6675(8) .3175(9) .138 Uiso calc R 1 . H
H15B .2638(10) .6834(8) .2675(9) .138 Uiso calc R 1 . H
C16 .3947(8) .4911(7) .3143(7) .086(2) Uani d . 1 . C
H16A .4261(8) .5084(7) .2398(7) .103 Uiso calc R 1 . H
H16B .4764(8) .4366(7) .3673(7) .103 Uiso calc R 1 . H
C21 .2375(6) .2181(5) .0072(4) .0460(12) Uani d . 1 . C
H21 .1910(6) .3123(5) -.0111(4) .055 Uiso calc R 1 . H
C22 .3467(7) .2138(8) -.0781(5) .072(2) Uani d . 1 . C
H22A .4007(7) .1222(8) -.0584(5) .087 Uiso calc R 1 . H
H22B .4128(7) .2640(8) -.0759(5) .087 Uiso calc R 1 . H
C23 .2772(8) .2715(8) -.1963(5) .082(2) Uani d . 1 . C
H23A .2320(8) .3658(8) -.2192(5) .099 Uiso calc R 1 . H
H23B .3500(8) .2622(8) -.2472(5) .099 Uiso calc R 1 . H
C24 .1681(8) .2022(8) -.2029(5) .079(2) Uani d . 1 . C
H24A .1241(8) .2423(8) -.2785(5) .095 Uiso calc R 1 . H
H24B .2143(8) .1090(8) -.1852(5) .095 Uiso calc R 1 . H
C25 .0566(8) .2119(9) -.1239(6) .085(2) Uani d . 1 . C
H25A -.0109(8) .1637(9) -.1275(6) .102 Uiso calc R 1 . H
H25B .0051(8) .3047(9) -.1456(6) .102 Uiso calc R 1 . H
C26 .1226(7) .1543(7) -.0038(5) .070(2) Uani d . 1 . C
H26A .0480(7) .1675(7) .0448(5) .085 Uiso calc R 1 . H
H26B .1635(7) .0590(7) .0208(5) .085 Uiso calc R 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 .0366(2) .0413(2) .0427(2) -.01486(12) .00359(11) -.01360(12)
Mn1 .0366(2) .0413(2) .0427(2) -.01486(12) .00359(11) -.01360(12)
Mn2 .0374(2) .0458(3) .0437(2) -.0131(2) .0061(2) -.0139(2)
Re2 .0374(2) .0458(3) .0437(2) -.0131(2) .0061(2) -.0139(2)
P1 .0371(6) .0379(7) .0372(7) -.0115(5) .0021(5) -.0140(5)
P2 .0434(7) .0353(6) .0390(7) -.0090(5) .0025(5) -.0151(5)
C1 .044(3) .050(3) .049(3) -.013(3) .004(2) -.020(3)
O1 .078(3) .055(3) .079(3) .000(2) -.010(3) -.007(2)
C2 .050(3) .065(4) .057(3) -.027(3) .006(3) -.020(3)
O2 .092(4) .109(4) .093(4) -.066(3) .001(3) -.041(3)
C3 .047(3) .065(4) .060(4) -.020(3) .013(3) -.026(3)
O3 .110(4) .099(4) .082(3) -.040(3) .047(3) -.040(3)
C4 .054(3) .053(3) .061(4) -.029(3) .003(3) -.018(3)
O4 .068(3) .051(3) .098(4) -.013(2) -.022(3) -.006(2)
C5 .049(3) .055(4) .050(3) -.008(3) .009(3) -.016(3)
O5 .077(3) .068(3) .067(3) -.001(2) .012(2) -.004(2)
C6 .039(3) .068(4) .064(4) -.019(3) .011(3) -.021(3)
O6 .053(3) .124(4) .105(4) -.041(3) .006(3) -.056(3)
C7 .054(3) .051(3) .057(3) -.014(3) .007(3) -.013(3)
O7 .081(3) .094(4) .067(3) -.012(3) .031(3) -.031(3)
C8 .044(3) .051(3) .052(3) -.022(3) .005(2) -.016(3)
O8 .070(3) .052(2) .070(3) -.019(2) -.006(2) .003(2)
C11 .061(4) .055(3) .068(4) -.018(3) .004(3) -.033(3)
C12 .089(5) .079(5) .096(5) -.037(4) .040(4) -.058(4)
C13 .098(6) .115(7) .152(8) -.042(5) .049(6) -.102(7)
C14 .100(7) .165(10) .222(12) -.060(7) .061(7) -.166(10)
C15 .112(7) .088(6) .200(11) -.064(5) .057(7) -.095(7)
C16 .082(5) .090(5) .125(7) -.049(4) .041(5) -.070(5)
C21 .056(3) .047(3) .038(3) -.013(2) -.004(2) -.020(2)
C22 .065(4) .108(5) .048(3) -.031(4) .009(3) -.031(4)
C23 .099(5) .115(6) .043(3) -.044(5) .010(3) -.032(4)
C24 .100(5) .103(6) .053(4) -.033(4) .000(4) -.046(4)
C25 .088(5) .124(6) .063(4) -.047(5) -.002(4) -.047(4)
C26 .081(4) .101(5) .051(3) -.048(4) .011(3) -.039(4)
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
M1 C3 . 1.870(6) ?
M1 C2 . 1.890(6) ?
M1 C4 . 1.917(6) ?
M1 C1 . 1.933(6) ?
M1 P1 . 2.4396(13) ?
M1 P2 . 2.4558(15) ?
M2 C7 . 1.862(6) ?
M2 C6 . 1.866(6) ?
M2 C5 . 1.887(6) ?
M2 C8 . 1.891(6) ?
M2 P1 . 2.4155(15) ?
M2 P2 . 2.4240(14) ?
P1 C11 . 1.870(6) ?
P2 C21 . 1.862(5) ?
C1 O1 . 1.135(6) ?
C2 O2 . 1.139(7) ?
C3 O3 . 1.165(7) ?
C4 O4 . 1.118(7) ?
C5 O5 . 1.123(6) ?
C6 O6 . 1.130(7) ?
C7 O7 . 1.149(7) ?
C8 O8 . 1.129(6) ?
C11 C16 . 1.476(8) ?
C11 C12 . 1.516(8) ?
C12 C13 . 1.514(9) ?
C13 C14 . 1.441(10) ?
C14 C15 . 1.482(12) ?
C15 C16 . 1.544(9) ?
C21 C26 . 1.519(8) ?
C21 C22 . 1.519(8) ?
C22 C23 . 1.525(8) ?
C23 C24 . 1.498(10) ?
C24 C25 . 1.485(10) ?
C25 C26 . 1.534(8) ?
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'
Mn Mn 0.3368 0.7283 '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
C3 M1 C2 91.5(3)
C3 M1 C4 91.2(3)
C2 M1 C4 91.1(2)
C3 M1 C1 93.0(2)
C2 M1 C1 92.3(2)
C4 M1 C1 174.6(2)
C3 M1 P1 96.3(2)
C2 M1 P1 172.1(2)
C4 M1 P1 87.8(2)
C1 M1 P1 88.2(2)
C3 M1 P2 172.2(2)
C2 M1 P2 96.1(2)
C4 M1 P2 87.1(2)
C1 M1 P2 88.3(2)
P1 M1 P2 76.02(5)
C7 M2 C6 91.3(3)
C7 M2 C5 92.7(2)
C6 M2 C5 90.7(3)
C7 M2 C8 94.5(2)
C6 M2 C8 95.0(2)
C5 M2 C8 170.7(2)
C7 M2 P1 174.2(2)
C6 M2 P1 94.3(2)
C5 M2 P1 85.6(2)
C8 M2 P1 86.6(2)
C7 M2 P2 97.4(2)
C6 M2 P2 171.2(2)
C5 M2 P2 87.4(2)
C8 M2 P2 85.8(2)
P1 M2 P2 77.06(5)
C11 P1 M2 118.9(2)
C11 P1 M1 116.6(2)
M1 P1 M2 103.77(5)
C21 P2 M2 116.9(2)
C21 P2 M1 116.7(2)
M1 P2 M2 103.04(5)
O1 C1 M1 178.7(5)
O2 C2 M1 174.9(6)
O3 C3 M1 176.7(6)
O4 C4 M1 178.0(6)
O5 C5 M2 178.0(6)
O6 C6 M2 177.4(6)
O7 C7 M2 176.4(6)
O8 C8 M2 176.8(5)
C16 C11 C12 111.9(6)
C16 C11 P1 114.3(5)
C12 C11 P1 110.2(4)
C13 C12 C11 112.2(6)
C14 C13 C12 114.1(7)
C13 C14 C15 112.6(7)
C14 C15 C16 110.9(7)
C11 C16 C15 111.6(6)
C26 C21 C22 110.2(5)
C26 C21 P2 112.3(4)
C22 C21 P2 112.7(4)
C21 C22 C23 112.1(5)
C24 C23 C22 111.4(6)
C25 C24 C23 110.7(6)
C24 C25 C26 111.1(6)
C21 C26 C25 112.6(5)
_journal_paper_doi 10.1107/S0108270198099715