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_7009903
_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         'Re1, Rh1, Br3, (C O)3, (C10 H15)'
_chemical_formula_sum            'C13 H15 Br3 O3 Re Rh'
_chemical_formula_weight         748.081
_chemical_name_common            cp(Me)5-Rh-Br3-Re-(CO)3
_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                Re_Rh_(CO)3_C10H15_Br3_e117_beck
_audit_creation_date             16-May-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 90.434(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6576(8)
_cell_length_b                   14.8986(17)
_cell_length_c                   12.3070(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                     1770.7(3)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16749
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.15
_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    14.535
_exptl_absorpt_correction_T_max  0.5046
_exptl_absorpt_correction_T_min  0.1416
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.8062(5)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.788
_refine_diff_density_min         -2.038
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                3398
_reflns_number_total             4233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004262p.txt
_cod_data_source_block           e117
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7009903
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 200.2
_kl_diffrn_detector_area_phi_incr 1.4
_kl_diffrn_detector_area_expos_time 4.00_min
_kl_diffrn_detector_area_plate_dist 60.0_mm
_kl_diffrn_detector_area_eff_mos_spread 0.008
_kl_diffrn_detector_area_profile_funct dynamic
_kl_diffrn_detector_area_profile_min 11
_kl_diffrn_detector_area_profile_max 21
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
TITL  e117 in P21/n
CELL  0.71073    9.6576   14.8986   12.3070    90.000    90.434    90.000
ZERR  4          0.0008    0.0017    0.0010     0.000     0.010     0.000
LATT  1
SYMM   .50000-X,  .50000+Y,  .50000-Z
SFAC    C   H   O   BR  RE  RH
UNIT    52  60  12  12   4   4
L.S.      12
FMAP      2
PLAN     -25

TEMP  -73
BOND  $H
CONF
ACTA

WGHT    0.027300
FVAR       0.19723
RH    6    0.363593    0.181593    0.248537    11.00000    0.01132    0.01220 =
         0.01418   -0.00043    0.00175    0.00082
RE    5    0.620793    0.027393    0.240005    11.00000    0.01212    0.01378 =
         0.02501    0.00112    0.00271    0.00094
BR1   4    0.627181    0.203557    0.267758    11.00000    0.01546    0.01812 =
         0.03023   -0.00491   -0.00172   -0.00179
BR2   4    0.429317    0.073841    0.097440    11.00000    0.02131    0.02958 =
         0.02757   -0.01401   -0.00419    0.00691
BR3   4    0.410377    0.046517    0.373182    11.00000    0.02472    0.03391 =
         0.03803    0.02186    0.01554    0.01132
O1    3    0.854509    0.022002    0.075725    11.00000    0.02687    0.03789 =
         0.03039   -0.00219    0.00915    0.00488
C1    1    0.764765    0.025058    0.136487    11.00000    0.01501    0.02039 =
         0.02696   -0.00332    0.00149    0.00164
O2    3    0.835944   -0.026454    0.410065    11.00000    0.03106    0.04121 =
         0.02998    0.00881   -0.00103    0.00969
C2    1    0.752058   -0.004254    0.348323    11.00000    0.02108    0.02284 =
         0.02712    0.00445    0.00793    0.00166
O3    3    0.575494   -0.170894    0.195402    11.00000    0.02926    0.01790 =
         0.13802   -0.00622   -0.00693   -0.00632
C3    1    0.591538   -0.096687    0.212609    11.00000    0.01553    0.02617 =
         0.05864   -0.00126   -0.00170    0.00132
C4    1    0.304917    0.318163    0.282700    11.00000    0.01618    0.01110 =
         0.02188   -0.00188    0.00150    0.00045
C5    1    0.225690    0.257210    0.348241    11.00000    0.01282    0.01610 =
         0.01639   -0.00057    0.00330    0.00469
C6    1    0.148900    0.199890    0.277350    11.00000    0.01101    0.01578 =
         0.02443   -0.00201    0.00161    0.00367
C7    1    0.277481    0.296241    0.170062    11.00000    0.01795    0.01238 =
         0.02144    0.00254    0.00314    0.00664
C8    1    0.177832    0.224839    0.167886    11.00000    0.01497    0.02101 =
         0.02176   -0.00394   -0.00190    0.00713
C9    1    0.395171    0.392499    0.321636    11.00000    0.02535    0.01711 =
         0.03223   -0.00544    0.00242   -0.00501
AFIX  33
H9A   2    0.437406    0.422469    0.259228    11.00000   -1.50000
H9B   2    0.468057    0.368197    0.369019    11.00000   -1.50000
H9C   2    0.339551    0.435840    0.362332    11.00000   -1.50000
AFIX   0
C10   1    0.217890    0.258644    0.469563    11.00000    0.02752    0.03393 =
         0.01883   -0.00535    0.00576    0.00164
AFIX  33
H10A  2    0.156274    0.210623    0.494169    11.00000   -1.50000
H10B  2    0.181680    0.316766    0.493488    11.00000   -1.50000
H10C  2    0.310607    0.249482    0.500521    11.00000   -1.50000
AFIX   0
C11   1    0.048705    0.129136    0.311655    11.00000    0.01896    0.01452 =
         0.04254    0.00084    0.00684   -0.00005
AFIX  33
H11A  2    0.012950    0.097757    0.247328    11.00000   -1.50000
H11B  2   -0.028259    0.157097    0.350538    11.00000   -1.50000
H11C  2    0.095700    0.086143    0.359600    11.00000   -1.50000
AFIX   0
C12   1    0.113876    0.186540    0.067287    11.00000    0.02819    0.03518 =
         0.02918   -0.00769   -0.01241    0.00362
AFIX  33
H12A  2    0.047686    0.139555    0.087092    11.00000   -1.50000
H12B  2    0.186365    0.160781    0.021535    11.00000   -1.50000
H12C  2    0.065590    0.234140    0.027191    11.00000   -1.50000
AFIX   0
C13   1    0.335759    0.343551    0.073390    11.00000    0.04208    0.02881 =
         0.02698    0.01188    0.00902    0.00852
AFIX  33
H13A  2    0.403061    0.388661    0.097656    11.00000   -1.50000
H13B  2    0.260695    0.373054    0.032998    11.00000   -1.50000
H13C  2    0.381687    0.299920    0.026206    11.00000   -1.50000
HKLF      4

REM   e117 in P21/n
REM R1 =  0.0257 for   3398 Fo > 4sig(Fo)  and  0.0374 for all   4233 data
REM    190 parameters refined using      0 restraints

END
;