##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Bis(μ-diphenylphosphido)bis{trans-tricarbonylbis[1-(4-
ethoxybutoxy)pentylidene]rhenium}
;
_chemical_formula_moiety     'C52 H64 O10 P2 Re2'
_chemical_formula_sum     'C52 H64 O10 P2 Re2'
_chemical_formula_iupac     '[Re2 (C11 H22 O2)2 (C12 H10 P)2 (C O)6]'
_chemical_formula_weight     1283.37
_symmetry_cell_setting     triclinic
_symmetry_space_group_name_H-M     'P -1'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, -z'
_cell_length_a     10.294(6)
_cell_length_b     12.102(5)
_cell_length_c     12.230(6)
_cell_angle_alpha     69.86(2)
_cell_angle_beta     86.58(2)
_cell_angle_gamma     66.39(2)
_cell_volume     1305.3(11)
_cell_formula_units_Z     1
_cell_measurement_reflns_used     25
_cell_measurement_theta_min     8
_cell_measurement_theta_max     15
_cell_measurement_temperature     293(2)
_exptl_crystal_description     prism
_exptl_crystal_colour     yellow
_exptl_crystal_size_max      .49
_exptl_crystal_size_mid      .41
_exptl_crystal_size_min      .20
_exptl_crystal_density_diffrn     1.633
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     636
_exptl_absorpt_coefficient_mu     4.749
_exptl_absorpt_correction_type     '\y scan'
_exptl_absorpt_process_details     '(North et al., 1968)'
_exptl_absorpt_correction_T_min      .150
_exptl_absorpt_correction_T_max      .409
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker P4'
_diffrn_measurement_method     ω
_diffrn_reflns_number     5891
_diffrn_reflns_av_R_equivalents      .0258
_diffrn_reflns_av_sigmaI/netI      .0246
_diffrn_reflns_theta_min     2.55
_diffrn_reflns_theta_max     27.56
_diffrn_reflns_theta_full     27.56
_diffrn_measured_fraction_theta_max      .932
_diffrn_measured_fraction_theta_full      .932
_diffrn_reflns_limit_h_min     -13
_diffrn_reflns_limit_h_max     13
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     15
_diffrn_reflns_limit_l_min     0
_diffrn_reflns_limit_l_max     15
_diffrn_standards_number     2
_diffrn_standards_interval_count     400
_diffrn_standards_decay_%     '<1'
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     5615
_reflns_number_gt     4907
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0367
_refine_ls_R_factor_gt      .0281
_refine_ls_wR_factor_ref      .0656
_refine_ls_goodness_of_fit_ref     1.040
_refine_ls_restrained_S_all     1.040
_refine_ls_number_reflns     5615
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
     'calc w = 1/[σ²(Fo²)+(0.0371P)²+0.5044P] where P = (Fo²+2Fc²)/3'
_refine_ls_shift/su_max      .001
_refine_ls_shift/su_mean      .000
_refine_diff_density_max     1.001
_refine_diff_density_min      -.869
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef      .0081(4)
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'P' 'P'  .1023  .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'
_computing_data_collection     'XSCANS (Bruker, 1996)'
_computing_cell_refinement     'XSCANS'
_computing_data_reduction     'SHELXTL (Bruker, 1998)'
_computing_structure_solution     'SHELXTL'
_computing_structure_refinement     'SHELXTL'
_computing_molecular_graphics     'SHELXTL'
_computing_publication_material     'SHELXTL'
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_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Re1 1.125433(15)  .055541(15)  .381509(13)  .04152(7) Uani d . 1 . . Re
    P1  .99320(10)  -.09052(10)  .43864(8)  .0401(2) Uani d . 1 . . P
    C1 1.2072(5)  .0222(4)  .2442(4)  .0561(10) Uani d . 1 . . C
    O1 1.2602(4)  .0074(4)  .1614(3)  .0853(11) Uani d . 1 . . O
    C2 1.2184(5)  .1713(5)  .3601(4)  .0600(11) Uani d . 1 . . C
    O2 1.2764(5)  .2377(4)  .3453(4)  .0929(13) Uani d . 1 . . O
    C3 1.2991(5)  -.0869(5)  .4764(4)  .0565(10) Uani d . 1 . . C
    O3 1.4052(4)  -.1641(4)  .5222(4)  .0861(12) Uani d . 1 . . O
    C11 1.1079(4)  -.2625(4)  .4633(4)  .0470(9) Uani d . 1 . . C
    C12 1.2311(5)  -.2983(5)  .4089(5)  .0694(13) Uani d . 1 . . C
    H12 1.2601  -.2356  .3606  .083 Uiso calc R 1 . . H
    C13 1.3125(7)  -.4273(6)  .4257(6)  .0884(18) Uani d . 1 . . C
    H13 1.3957  -.4494  .3886  .106 Uiso calc R 1 . . H
    C14 1.2741(6)  -.5208(5)  .4943(6)  .0816(16) Uani d . 1 . . C
    H14 1.3296  -.6067  .5045  .098 Uiso calc R 1 . . H
    C15 1.1522(7)  -.4875(5)  .5486(6)  .0854(17) Uani d . 1 . . C
    H15 1.1243  -.5511  .5967  .102 Uiso calc R 1 . . H
    C16 1.0698(6)  -.3594(5)  .5326(5)  .0711(13) Uani d . 1 . . C
    H16  .9864  -.3383  .5697  .085 Uiso calc R 1 . . H
    C21  .8686(4)  -.0639(4)  .3195(3)  .0454(9) Uani d . 1 . . C
    C22  .7432(5)  -.0799(5)  .3417(5)  .0659(12) Uani d . 1 . . C
    H22  .7176  -.1022  .4179  .079 Uiso calc R 1 . . H
    C23  .6548(7)  -.0626(6)  .2496(6)  .0857(18) Uani d . 1 . . C
    H23  .5697  -.0725  .2651  .103 Uiso calc R 1 . . H
    C24  .6906(7)  -.0316(5)  .1374(5)  .0813(17) Uani d . 1 . . C
    H24  .6312  -.0211  .0768  .098 Uiso calc R 1 . . H
    C25  .8139(7)  -.0164(5)  .1156(5)  .0789(16) Uani d . 1 . . C
    H25  .8391  .0051  .0392  .095 Uiso calc R 1 . . H
    C26  .9033(5)  -.0326(4)  .2051(4)  .0596(11) Uani d . 1 . . C
    H26  .9878  -.0222  .1881  .071 Uiso calc R 1 . . H
    C4  .9463(4)  .2108(4)  .2761(4)  .0459(9) Uani d . 1 . . C
    O4  .8191(3)  .2241(3)  .3075(2)  .0495(6) Uani d . 1 . . O
    C31  .6835(4)  .3317(4)  .2490(4)  .0570(10) Uani d . 1 . . C
    H31A  .7021  .4002  .1903  .068 Uiso calc R 1 . . H
    H31B  .6278  .3658  .3057  .068 Uiso calc R 1 . . H
    C32  .6024(5)  .2832(4)  .1925(4)  .0562(11) Uani d . 1 . . C
    H32A  .6022  .2035  .2477  .067 Uiso calc R 1 . . H
    H32B  .6494  .2654  .1256  .067 Uiso calc R 1 . . H
    C33  .4500(5)  .3813(4)  .1530(4)  .0586(11) Uani d . 1 . . C
    H33A  .3992  .3906  .2208  .070 Uiso calc R 1 . . H
    H33B  .4499  .4643  .1060  .070 Uiso calc R 1 . . H
    C34  .3754(5)  .3400(5)  .0824(5)  .0696(13) Uani d . 1 . . C
    H34A  .3903  .2509  .1228  .084 Uiso calc R 1 . . H
    H34B  .2739  .3927  .0718  .084 Uiso calc R 1 . . H
    O5  .4311(5)  .3543(4)  -.0259(3)  .0843(11) Uani d . 1 . . O
    C36  .4003(8)  .2918(7)  -.0906(6)  .0954(19) Uani d . 1 . . C
    H36A  .2989  .3314  -.1142  .114 Uiso calc R 1 . . H
    H36B  .4253  .2023  -.0426  .114 Uiso calc R 1 . . H
    C37  .4792(10)  .2991(8)  -.1940(8)  .124(3) Uani d . 1 . . C
    H37A  .4573  .2551  -.2374  .187 Uiso calc R 1 . . H
    H37B  .5794  .2594  -.1704  .187 Uiso calc R 1 . . H
    H37C  .4528  .3877  -.2422  .187 Uiso calc R 1 . . H
    C38  .9572(5)  .3110(5)  .1647(4)  .0604(11) Uani d . 1 . . C
    H38A 1.0543  .3045  .1631  .073 Uiso calc R 1 . . H
    H38B  .8961  .3959  .1658  .073 Uiso calc R 1 . . H
    C39  .9159(6)  .2981(5)  .0533(4)  .0728(14) Uani d . 1 . . C
    H39A  .9441  .2076  .0660  .087 Uiso calc R 1 . . H
    H39B  .8132  .3405  .0369  .087 Uiso calc R 1 . . H
    C40  .9831(7)  .3548(7)  -.0508(5)  .0912(18) Uani d . 1 . . C
    H40A 1.0854  .3056  -.0379  .109 Uiso calc R 1 . . H
    H40B  .9645  .4422  -.0576  .109 Uiso calc R 1 . . H
    C41  .9306(8)  .3570(7)  -.1642(6)  .113(3) Uani d . 1 . . C
    H41A  .9788  .3931  -.2268  .170 Uiso calc R 1 . . H
    H41B  .8299  .4084  -.1795  .170 Uiso calc R 1 . . H
    H41C  .9494  .2707  -.1587  .170 Uiso calc R 1 . . H
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 . 1.929(5) ?
    Re1 C2 . 1.933(5) ?
    Re1 C3 . 1.979(5) ?
    Re1 C4 . 2.105(4) y
    Re1 P1 2_756 2.5328(15) y
    Re1 P1 . 2.5355(14) y
    P1 C21 . 1.855(4) ?
    P1 C11 . 1.860(4) ?
    P1 Re1 2_756 2.5328(15) ?
    C1 O1 . 1.156(5) ?
    C2 O2 . 1.144(5) ?
    C3 O3 . 1.130(5) ?
    C11 C16 . 1.376(6) ?
    C11 C12 . 1.377(6) ?
    C12 C13 . 1.391(7) ?
    C13 C14 . 1.345(8) ?
    C14 C15 . 1.362(8) ?
    C15 C16 . 1.386(7) ?
    C21 C22 . 1.378(6) ?
    C21 C26 . 1.382(6) ?
    C22 C23 . 1.396(7) ?
    C23 C24 . 1.362(9) ?
    C24 C25 . 1.353(8) ?
    C25 C26 . 1.383(6) ?
    C4 O4 . 1.304(5) y
    C4 C38 . 1.514(6) y
    O4 C31 . 1.476(5) ?
    C31 C32 . 1.502(6) ?
    C32 C33 . 1.519(6) ?
    C33 C34 . 1.507(7) ?
    C34 O5 . 1.394(7) ?
    O5 C36 . 1.390(7) ?
    C36 C37 . 1.458(10) ?
    C38 C39 . 1.528(7) ?
    C39 C40 . 1.498(7) ?
    C40 C41 . 1.507(9) ?
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
    C1 Re1 C2 . . 88.2(2) ?
    C1 Re1 C3 . . 88.57(19) ?
    C2 Re1 C3 . . 88.7(2) ?
    C1 Re1 C4 . . 90.03(17) ?
    C2 Re1 C4 . . 89.22(19) ?
    C3 Re1 C4 . . 177.52(16) ?
    C1 Re1 P1 . 2_756 175.74(14) ?
    C2 Re1 P1 . 2_756 95.94(15) ?
    C3 Re1 P1 . 2_756 92.29(14) ?
    C4 Re1 P1 . 2_756 89.27(12) ?
    C1 Re1 P1 . . 100.42(14) ?
    C2 Re1 P1 . . 171.27(14) ?
    C3 Re1 P1 . . 90.47(14) ?
    C4 Re1 P1 . . 91.79(11) ?
    P1 Re1 P1 2_756 . 75.40(4) y
    C21 P1 C11 . . 97.52(17) ?
    C21 P1 Re1 . 2_756 113.96(14) ?
    C11 P1 Re1 . 2_756 113.00(14) ?
    C21 P1 Re1 . . 114.08(14) ?
    C11 P1 Re1 . . 114.05(14) ?
    Re1 P1 Re1 2_756 . 104.60(4) y
    O1 C1 Re1 . . 175.7(4) ?
    O2 C2 Re1 . . 177.8(5) ?
    O3 C3 Re1 . . 173.4(4) ?
    C16 C11 C12 . . 117.0(4) ?
    C16 C11 P1 . . 121.3(3) ?
    C12 C11 P1 . . 121.6(3) ?
    C11 C12 C13 . . 120.5(5) ?
    C14 C13 C12 . . 121.7(6) ?
    C13 C14 C15 . . 118.8(5) ?
    C14 C15 C16 . . 120.3(5) ?
    C11 C16 C15 . . 121.7(5) ?
    C22 C21 C26 . . 118.0(4) ?
    C22 C21 P1 . . 121.8(3) ?
    C26 C21 P1 . . 120.1(3) ?
    C21 C22 C23 . . 119.9(5) ?
    C24 C23 C22 . . 121.3(6) ?
    C25 C24 C23 . . 118.9(5) ?
    C24 C25 C26 . . 121.0(6) ?
    C21 C26 C25 . . 120.9(5) ?
    O4 C4 C38 . . 117.4(4) ?
    O4 C4 Re1 . . 119.5(3) y
    C38 C4 Re1 . . 123.0(3) ?
    C4 O4 C31 . . 126.6(3) ?
    O4 C31 C32 . . 108.9(3) ?
    C31 C32 C33 . . 111.1(4) ?
    C34 C33 C32 . . 110.8(4) ?
    O5 C34 C33 . . 108.2(4) ?
    C36 O5 C34 . . 115.5(4) ?
    O5 C36 C37 . . 110.5(6) ?
    C4 C38 C39 . . 113.8(4) ?
    C40 C39 C38 . . 113.0(5) ?
    C39 C40 C41 . . 113.8(6) ?
data_global
_journal_date_recd_electronic     2001-05-08
_journal_date_accepted     2001-05-10
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2001
_journal_volume     57
_journal_issue      6
_journal_page_first     m237
_journal_page_last     m238
_journal_paper_category     EM
_publ_contact_author_name     'Dr Ulrich Florke'
_publ_contact_author_address
;
Anorganische und Analytische Chemie
Universitat Paderborn
Warburgerstrasse 100
D-33098 Paderborn
Germany
;
_publ_contact_author_email     uf@chemie.uni-paderborn.de
_publ_contact_author_fax     '+49 5251 60 3423'
_publ_contact_author_phone     '+49 5251 60 2496'
_publ_section_title
;
Bis(μ-diphenylphosphido)bis{trans-tricarbonylbis[1-(4-
ethoxybutoxy)pentylidene]rhenium}
;
loop_
    _publ_author_name
    _publ_author_address
    'Flörke, Ulrich'
;Fachbereich Chemie und Chemietechnik
 Universität-GH Paderborn
 Warburgerstraße 100
 D-33098 Paderborn
Germany
;
    'Petters, Dina'
;Fachbereich Chemie und Chemietechnik
 Universität-GH Paderborn
 Warburgerstraße 100
 D-33098 Paderborn
Germany
;
