Bis(μ~3~-4-bromophenylimido)tris(tricarbonylruthenium)(2 <i>Ru{—</i>Ru})
Anthony C. Willis; Waleed K. Mahdi; Mark G. Humphrey; Acta Crystallographica Section E 61 (2005) m2335–m2337; doi:10.1107/S1600536805032885

data_2207232
_publ_section_title
;
 Bis(\m~3~-4-bromophenylimido)tris(tricarbonylruthenium)(2
 <i>Ru{---</i>Ru})
;
_journal_coeditor_code           HB6277
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2335
_journal_page_last               m2337
_journal_paper_doi               10.1107/S1600536805032885
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ru3 (C6 H4 Br N)2 (C O)9]'
_chemical_formula_moiety         'C21 H8 Br2 N2 O9 Ru3'
_chemical_formula_sum            'C21 H8 Br2 N2 O9 Ru3'
_chemical_formula_weight         895.32
_chemical_melting_point          431
_chemical_name_systematic
;
Bis(\m~3~-4-bromophenylimido)tris(tricarbonylruthenium)(2 Ru---Ru)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                100.9819(9)
_cell_angle_beta                 112.3150(8)
_cell_angle_gamma                98.9674(8)
_cell_formula_units_Z            4
_cell_length_a                   13.0136(2)
_cell_length_b                   14.6979(2)
_cell_length_c                   15.8864(2)
_cell_measurement_reflns_used    36343
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2671.05(7)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_molecular_graphics
;
ORTEPII (Johnson 1976) in TEXSAN (Molecular Structure Corporation,
1997)
;
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Watkin et al., 2001)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58882
_diffrn_reflns_theta_full        27.494
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.637
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.717
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.284
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in MAXUS (Mackay et al.,
2000)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_description       plate
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.03
_refine_diff_density_min         -1.01
_refine_ls_extinction_coef       100(8)
_refine_ls_extinction_method     'Larson (1970), eq 22'
_refine_ls_goodness_of_fit_ref   1.0652
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         8846
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.001710
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994; Prince, 1982)
w = 1/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)],  where A~i~ are the
Chebychev coefficients listed below and x = F~calc~/F~max~  Method = robust
weighting (Prince, 1982);  W = w[1-(\dF/6\sF)^2^]^2^;  A~i~ are 1.71
0.166 1.45
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0345
_refine_ls_wR_factor_gt          0.0299
_refine_ls_wR_factor_ref         0.0299
_reflns_number_gt                8846
_reflns_number_total             12233
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            hb6277.cif
_cod_data_source_block           I
_cod_database_code               2207232
_cod_database_fobs_code          2207232