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_7009904
_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 Ir1 Br3 O3 C13 H15'
_chemical_formula_sum            'C13 H15 Br3 Ir O3 Re'
_chemical_formula_weight         837.392
_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_Ir_(CO)3_C10H15_Br3_e105_beck
_audit_creation_date             30-Apr-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 90.574(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7123(7)
_cell_length_b                   14.9342(10)
_cell_length_c                   12.2606(10)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.1
_cell_volume                     1778.3(2)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1013
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11649
_diffrn_reflns_theta_full        25.92
_diffrn_reflns_theta_max         25.92
_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    21.022
_exptl_absorpt_correction_T_max  0.4960
_exptl_absorpt_correction_T_min  0.2626
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.1278(4)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.152
_refine_diff_density_min         -2.678
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0286
_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          0.0715
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                2939
_reflns_number_total             3421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004262p.txt
_cod_data_source_block           e105
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7009904
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 170.0
_kl_diffrn_detector_area_phi_incr 1.0
_kl_diffrn_detector_area_expos_time 4.00_min
_kl_diffrn_detector_area_plate_dist 70.0_mm
_kl_diffrn_detector_area_eff_mos_spread 0.007
_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   e105 in P21/n (14), sir97
CELL  0.71073    9.7123   14.9342   12.2606    90.000    90.574    90.000
ZERR  4          0.0007    0.0010    0.0010     0.000     0.010     0.000
LATT  1
SYMM   .50000-X,  .50000+Y,  .50000-Z
SFAC    C   H   O   BR  RE  IR
UNIT    52  60  12  12   4   4
L.S.      8
FMAP      2
PLAN     -25

TEMP  -73
BOND  $H
CONF
ACTA

WGHT    0.031000
FVAR       0.16754
IR    6    0.362330    0.181001    0.248349    11.00000    0.01279    0.01343 =
         0.01124   -0.00037   -0.00035    0.00062
RE    5    0.622762    0.025408    0.240424    11.00000    0.01378    0.01509 =
         0.02258    0.00089    0.00078    0.00107
BR1   4    0.624546    0.201290    0.267532    11.00000    0.01670    0.01998 =
         0.02686   -0.00415   -0.00305   -0.00209
BR2   4    0.430946    0.072196    0.099121    11.00000    0.02355    0.03143 =
         0.02590   -0.01346   -0.00575    0.00678
BR3   4    0.412433    0.046210    0.372551    11.00000    0.02534    0.03404 =
         0.03452    0.02019    0.01319    0.01053
O1    3    0.854863    0.021634    0.076118    11.00000    0.02660    0.04534 =
         0.02939   -0.00215    0.00547    0.00197
C1    1    0.766549    0.023160    0.137256    11.00000    0.02064    0.01892 =
         0.01979   -0.00134   -0.00367   -0.00149
O2    3    0.837544   -0.028192    0.411334    11.00000    0.02029    0.05262 =
         0.02726    0.01553   -0.00418    0.01255
C2    1    0.752944   -0.005265    0.348492    11.00000    0.02130    0.01949 =
         0.02846   -0.00029    0.01070   -0.00573
O3    3    0.580097   -0.173278    0.198645    11.00000    0.03127    0.02091 =
         0.13228   -0.00926   -0.00505   -0.00543
C3    1    0.596900   -0.098411    0.214182    11.00000    0.01408    0.02124 =
         0.06349    0.00546   -0.00078   -0.00223
C4    1    0.304066    0.316891    0.282936    11.00000    0.02081    0.01306 =
         0.01527    0.00058   -0.00101    0.00440
C5    1    0.225183    0.257747    0.347404    11.00000    0.02153    0.01822 =
         0.01355   -0.00319    0.00444    0.00230
C6    1    0.148402    0.198510    0.277861    11.00000    0.00904    0.01766 =
         0.01999    0.00257   -0.00026   -0.00070
C7    1    0.274348    0.295816    0.168789    11.00000    0.02434    0.01441 =
         0.01433    0.00235   -0.00204    0.00805
C8    1    0.177817    0.224231    0.165996    11.00000    0.01918    0.01583 =
         0.01650   -0.00044   -0.00206    0.00501
C9    1    0.393304    0.391008    0.320615    11.00000    0.03535    0.01485 =
         0.02900   -0.00462   -0.00420   -0.00345
AFIX  33
H9A   2    0.434848    0.420377    0.257492    11.00000   -1.50000
H9B   2    0.466126    0.367260    0.368362    11.00000   -1.50000
H9C   2    0.338147    0.434560    0.360991    11.00000   -1.50000
AFIX   0
C10   1    0.215508    0.259265    0.470769    11.00000    0.03470    0.03088 =
         0.00994   -0.00463    0.00287   -0.00326
AFIX  33
H10A  2    0.153998    0.211307    0.494829    11.00000   -1.50000
H10B  2    0.178999    0.317224    0.494324    11.00000   -1.50000
H10C  2    0.307274    0.250245    0.502873    11.00000   -1.50000
AFIX   0
C11   1    0.047933    0.128568    0.312075    11.00000    0.01939    0.01852 =
         0.03493   -0.00462    0.00659   -0.00211
AFIX  33
H11A  2    0.012304    0.097256    0.247466    11.00000   -1.50000
H11B  2   -0.028454    0.156933    0.350637    11.00000   -1.50000
H11C  2    0.093975    0.085589    0.360587    11.00000   -1.50000
AFIX   0
C12   1    0.115727    0.184197    0.067109    11.00000    0.01716    0.04254 =
         0.02564   -0.00481   -0.01636   -0.00251
AFIX  33
H12A  2    0.050164    0.137553    0.088123    11.00000   -1.50000
H12B  2    0.188224    0.157770    0.022351    11.00000   -1.50000
H12C  2    0.067549    0.230675    0.025163    11.00000   -1.50000
AFIX   0
C13   1    0.331437    0.342476    0.071004    11.00000    0.03879    0.02771 =
         0.02348    0.00450    0.00279    0.00551
AFIX  33
H13A  2    0.398686    0.387557    0.094692    11.00000   -1.50000
H13B  2    0.256437    0.371747    0.030554    11.00000   -1.50000
H13C  2    0.376538    0.298652    0.023789    11.00000   -1.50000
HKLF      4

REM    e105 in P21/n (14), sir97
REM R1 =  0.0286 for   2939 Fo > 4sig(Fo)  and  0.0341 for all   3421 data
REM    190 parameters refined using      0 restraints

END

WGHT      0.0310      0.0000
REM Highest difference peak  1.152,  deepest hole -2.678,  1-sigma level  0.262
Q1    1   0.6249  0.0847  0.2399  11.00000  0.05    1.15
Q2    1   0.4248  0.2362  0.1939  11.00000  0.05    1.05
Q3    1   0.6251 -0.0332  0.2439  11.00000  0.05    1.04
Q4    1   0.2846  0.1401  0.2953  11.00000  0.05    1.03
Q5    1   0.2879  0.2283  0.3006  11.00000  0.05    1.02
Q6    1   0.3669  0.1189  0.2800  11.00000  0.05    1.02
;