Heterometallic bromo-bridged complexes with a Re(CO)3 fragment
da Silva, Ana C.; Piotrowski, Holger; Mayer, Peter; Polborn, Kurt; Severin, Kay; Journal of the Chemical Society, Dalton Transactions  (2000) 2960–; doi:10.1039/b004262p

data_7009902
_publ_section_title
;
 Heterometallic bromo-bridged complexes with a Re(CO)3 fragment
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2960
_journal_paper_doi               10.1039/b004262p
_journal_year                    2000
_chemical_compound_source
;

;
_chemical_formula_moiety         'Re2, Br3, 6(C O), Ru2, Br3, 2(C12 H18)'
_chemical_formula_sum            'C30 H36 Br6 O6 Re2 Ru2'
_chemical_formula_weight         1546.58
_chemical_name_common            Re2Br3(CO)6+Ru2Br3(C12H18)2
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Re2_Ru2_Br_CO_(C12H18)_e094_Beck
_audit_creation_date             16-Apr-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 91.680(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3340(11)
_cell_length_b                   15.1881(9)
_cell_length_c                   17.0439(10)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.2
_cell_volume                     3967.7(4)
_computing_cell_refinement       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_collection       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_reduction        'Stoe IPDS software (Darmstadt, Germany)'
_computing_molecular_graphics
;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
 Plot Program for Crystal Structure Illustrations, Oak Ridge National
 Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
 Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
 Germany, 1995).
;
_computing_publication_material
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
--- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)
;
_diffrn_ambient_temperature      200(3)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'image-plate area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36602
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.21
_diffrn_source_current           50_mA
_diffrn_source_power             2.75_kW
_diffrn_source_type              'Spellman DF4 Series'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    12.908
_exptl_absorpt_correction_T_max  0.3495
_exptl_absorpt_correction_T_min  0.1950
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.5891(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.723
_refine_diff_density_min         -1.541
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         9483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                6927
_reflns_number_total             9483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004262p.txt
_cod_data_source_block           e094
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7009902
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 194.0
_kl_diffrn_detector_area_phi_incr 1.0
_kl_diffrn_detector_area_expos_time 2.00_min
_kl_diffrn_detector_area_plate_dist 60.0_mm
_kl_diffrn_detector_area_eff_mos_spread 0.006
_kl_diffrn_detector_area_profile_funct dynamic
_kl_diffrn_detector_area_profile_min 9
_kl_diffrn_detector_area_profile_max 21
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
TITL  e094 in P 21/n
CELL  0.71073   15.3340   15.1881   17.0439    90.000    91.680    90.000
ZERR  4          0.0011    0.0009    0.0010     0.000     0.008     0.000
LATT  1
SYMM   .50000-X,  .50000+Y,  .50000-Z
SFAC    C   H   O   BR  RU  RE
UNIT   120 144  24  24   8   8
L.S.      14
TEMP -73
ACTA
BOND $H
CONF
FMAP      2
PLAN     -25
WGHT    0.030000
FVAR       0.10396
C111  1    0.945258    0.177201    0.807003    11.00000    0.04086    0.02221 =
         0.03116   -0.00160    0.00032   -0.00204
O111  3    0.998526    0.190459    0.762254    11.00000    0.05124    0.04728 =
         0.05011    0.00252    0.02704   -0.01483
C211  1    0.934860    0.182059    0.964107    11.00000    0.03015    0.02563 =
         0.03921   -0.00271    0.00178    0.00128
O211  3    0.982248    0.200091    1.015492    11.00000    0.03541    0.05359 =
         0.04355   -0.01389   -0.01493   -0.00091
C311  1    0.895516    0.034575    0.885150    11.00000    0.02445    0.03377 =
         0.02888   -0.00351    0.00333    0.00023
O311  3    0.918822   -0.037597    0.889476    11.00000    0.03977    0.03071 =
         0.05236   -0.00222    0.00628    0.00832
REM     ------------------------------------------------------------------------
RE1   6    0.857340    0.152478    0.879467    11.00000    0.02199    0.02206 =
         0.01923   -0.00123    0.00102   -0.00031
REM     ------------------------------------------------------------------------
BR11  4    0.784395    0.310176    0.871588    11.00000    0.03504    0.02289 =
         0.02966   -0.00061   -0.00183   -0.00120
BR21  4    0.725080    0.120785    0.970497    11.00000    0.03414    0.03561 =
         0.02282    0.00639    0.00558    0.00597
BR31  4    0.738045    0.120056    0.769595    11.00000    0.03489    0.03360 =
         0.02334   -0.00411   -0.00137   -0.00037
REM     ------------------------------------------------------------------------
RE2   6    0.640134    0.213705    0.862550    11.00000    0.02404    0.02074 =
         0.02398    0.00231    0.00081    0.00208
REM     ------------------------------------------------------------------------
C121  1    0.586762    0.278221    0.778748    11.00000    0.03010    0.03263 =
         0.03151   -0.00014   -0.00256   -0.00421
O121  3    0.552071    0.313913    0.727858    11.00000    0.04658    0.05424 =
         0.04716    0.02079   -0.01943    0.00276
C221  1    0.542015    0.137066    0.856293    11.00000    0.04052    0.02505 =
         0.04352    0.00294    0.00380    0.00488
O221  3    0.480824    0.094786    0.851332    11.00000    0.04003    0.03462 =
         0.10409   -0.00426    0.00226   -0.01431
C321  1    0.580681    0.281021    0.937454    11.00000    0.03978    0.02574 =
         0.03359    0.00600    0.00625   -0.00126
O321  3    0.543990    0.319139    0.985211    11.00000    0.07015    0.03530 =
         0.05890   -0.00606    0.03435    0.01157
REM     ------------------------------------------------------------------------
REM     ------------------------------------------------------------------------
C112  1    0.762213    0.241848    0.569523    11.00000    0.01997    0.02491 =
         0.01439   -0.00233    0.00073    0.00005
C11A  1    0.775315    0.339015    0.569498    11.00000    0.03017    0.02241 =
         0.02845   -0.00165   -0.00150    0.00316
AFIX  23
H11A  2    0.723306    0.368206    0.545549    11.00000   -1.20000
H11B  2    0.826330    0.354008    0.537818    11.00000   -1.20000
AFIX   0
C11B  1    0.790234    0.371878    0.653395    11.00000    0.04551    0.02814 =
         0.03106   -0.01175    0.00352   -0.00544
AFIX 137
H11C  2    0.740699    0.354826    0.685117    11.00000   -1.50000
H11D  2    0.795734    0.436162    0.653199    11.00000   -1.50000
H11E  2    0.843852    0.345757    0.675768    11.00000   -1.50000
AFIX   0
C212  1    0.835706    0.183424    0.570586    11.00000    0.01745    0.02418 =
         0.01544   -0.00232   -0.00294   -0.00065
AFIX  43
H212  2    0.893051    0.207155    0.572458    11.00000   -1.20000
AFIX   0
C312  1    0.824262    0.091600    0.568903    11.00000    0.03065    0.02203 =
         0.01691    0.00315    0.00250    0.00166
C31A  1    0.901805    0.030150    0.568604    11.00000    0.03049    0.02872 =
         0.03992    0.00412    0.00686    0.00989
AFIX  23
H31A  2    0.952949    0.061521    0.548111    11.00000   -1.20000
H31B  2    0.888656   -0.020494    0.533654    11.00000   -1.20000
AFIX   0
C31B  1    0.922897   -0.002700    0.650879    11.00000    0.04348    0.03786 =
         0.04111   -0.00347   -0.01234    0.01556
AFIX 137
H31C  2    0.939226    0.047202    0.684670    11.00000   -1.50000
H31D  2    0.971529   -0.044485    0.649511    11.00000   -1.50000
H31E  2    0.871587   -0.032077    0.671697    11.00000   -1.50000
AFIX   0
C412  1    0.738533    0.056723    0.566706    11.00000    0.03457    0.02112 =
         0.01833    0.00010    0.00397   -0.00520
AFIX  43
H412  2    0.730681   -0.005314    0.565596    11.00000   -1.20000
AFIX   0
C512  1    0.664945    0.111671    0.566132    11.00000    0.02454    0.03165 =
         0.01350   -0.00267    0.00405   -0.00528
C51A  1    0.574965    0.073046    0.563976    11.00000    0.02301    0.05208 =
         0.02972   -0.00214    0.00051   -0.01269
AFIX  23
H51A  2    0.575272    0.016511    0.535075    11.00000   -1.20000
H51B  2    0.534359    0.113594    0.535796    11.00000   -1.20000
AFIX   0
C51B  1    0.543790    0.057728    0.646146    11.00000    0.02996    0.08759 =
         0.04025    0.00744    0.00473   -0.02987
AFIX 137
H51C  2    0.585468    0.019829    0.674826    11.00000   -1.50000
H51D  2    0.486486    0.029136    0.643510    11.00000   -1.50000
H51E  2    0.539197    0.114284    0.673394    11.00000   -1.50000
AFIX   0
C612  1    0.677470    0.204565    0.568011    11.00000    0.02202    0.02804 =
         0.01754   -0.00479    0.00111    0.00114
AFIX  43
H612  2    0.628048    0.242272    0.568255    11.00000   -1.20000
AFIX   0
REM     ------------------------------------------------------------------------
RU1   5    0.749224    0.150051    0.471282    11.00000    0.02027    0.01905 =
         0.01477   -0.00135    0.00206   -0.00171
REM     ------------------------------------------------------------------------
BR12  4    0.623681    0.134859    0.370557    11.00000    0.02448    0.06989 =
         0.02104    0.00164    0.00107   -0.00269
BR22  4    0.795937    0.266378    0.371673    11.00000    0.08381    0.03164 =
         0.01903   -0.00281    0.00593   -0.02760
BR32  4    0.825179    0.051502    0.372792    11.00000    0.04706    0.04932 =
         0.02315   -0.00483    0.00087    0.01949
REM     ------------------------------------------------------------------------
RU2   5    0.745126    0.149020    0.271902    11.00000    0.02201    0.02120 =
         0.01487   -0.00204    0.00214   -0.00225
REM     ------------------------------------------------------------------------
C122  1    0.774751    0.234953    0.174178    11.00000    0.03072    0.02618 =
         0.01641   -0.00046    0.00096   -0.00491
C12A  1    0.807945    0.327939    0.173562    11.00000    0.04245    0.03057 =
         0.02503   -0.00008    0.00113   -0.01016
AFIX  23
H12A  2    0.865308    0.330965    0.201637    11.00000   -1.20000
H12B  2    0.766906    0.366780    0.201008    11.00000   -1.20000
AFIX   0
C12B  1    0.817075    0.359364    0.088801    11.00000    0.06514    0.03265 =
         0.03309    0.00863    0.01144   -0.00937
AFIX 137
H12C  2    0.860526    0.323118    0.062817    11.00000   -1.50000
H12D  2    0.835831    0.421047    0.088769    11.00000   -1.50000
H12E  2    0.760711    0.354032    0.060588    11.00000   -1.50000
AFIX   0
C222  1    0.683457    0.218409    0.173347    11.00000    0.02658    0.02332 =
         0.01966   -0.00090   -0.00131    0.00250
AFIX  43
H222  2    0.643773    0.266456    0.172171    11.00000   -1.20000
AFIX   0
C322  1    0.650868    0.130734    0.174256    11.00000    0.02421    0.02824 =
         0.01624   -0.00520   -0.00192   -0.00208
C32A  1    0.554526    0.113610    0.173083    11.00000    0.02323    0.03309 =
         0.03263   -0.00537    0.00377    0.00130
AFIX  23
H32A  2    0.524045    0.164020    0.196868    11.00000   -1.20000
H32B  2    0.542264    0.060336    0.204359    11.00000   -1.20000
AFIX   0
C32B  1    0.521258    0.100583    0.089134    11.00000    0.02703    0.05474 =
         0.04163    0.01061   -0.01017   -0.00568
AFIX 137
H32C  2    0.521256    0.157191    0.061538    11.00000   -1.50000
H32D  2    0.461740    0.077082    0.089220    11.00000   -1.50000
H32E  2    0.559297    0.059066    0.062440    11.00000   -1.50000
AFIX   0
C422  1    0.710835    0.059551    0.176191    11.00000    0.02644    0.02058 =
         0.02003   -0.00614    0.00067   -0.00166
AFIX  43
H422  2    0.689639    0.000806    0.177397    11.00000   -1.20000
AFIX   0
C522  1    0.802637    0.075187    0.176346    11.00000    0.02792    0.03092 =
         0.01093   -0.00260    0.00208    0.00001
C52A  1    0.863293   -0.001727    0.178065    11.00000    0.03059    0.03983 =
         0.02642   -0.00547    0.00252    0.00869
AFIX  23
H52A  2    0.839833   -0.048675    0.211776    11.00000   -1.20000
H52B  2    0.920882    0.016393    0.200346    11.00000   -1.20000
AFIX   0
C52B  1    0.873462   -0.036432    0.095288    11.00000    0.04039    0.05126 =
         0.03351   -0.01879   -0.00310    0.01945
AFIX 137
H52C  2    0.816050   -0.052335    0.072806    11.00000   -1.50000
H52D  2    0.911161   -0.088544    0.096749    11.00000   -1.50000
H52E  2    0.899737    0.009184    0.062884    11.00000   -1.50000
AFIX   0
C622  1    0.832941    0.162865    0.174568    11.00000    0.02222    0.03995 =
         0.01406   -0.00167    0.00531   -0.00474
AFIX  43
H622  2    0.893925    0.173660    0.173610    11.00000   -1.20000

HKLF      4
END
;
_kl_archive_schakal_comment      'release 99 for Win32 systems'