One-Pot Synthesis of Ruthenium Metallacycles via Oxidative Addition of Diaryldichalcogen and Halogen across a Ru‒Ru Bond
Nagarajaprakash, R.; Ramakrishna, Buthanapalli; Mahesh, K.; Mobin, Shaikh M.; Manimaran, Bala.; Organometallics 32 (2013) 7292–; doi:10.1021/om400686q

data_4082070
_publ_section_title
;
 One-Pot Synthesis of Ruthenium Metallacycles via Oxidative Addition of
 Diaryldichalcogen and Halogen across a Ru--Ru Bond
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7292
_journal_paper_doi               10.1021/om400686q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C18 H10 Br2 O6 Ru2 S2'
_chemical_formula_sum            'C18 H10 Br2 O6 Ru2 S2'
_chemical_formula_weight         748.34
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-31
_audit_creation_method
;
  Olex2 1.1
  (compiled Sep  7 2011 21:07:27, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.662(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9194(3)
_cell_length_b                   18.5213(5)
_cell_length_c                   11.7728(3)
_cell_measurement_reflns_used    3324
_cell_measurement_temperature    300
_cell_measurement_theta_max      29.1356
_cell_measurement_theta_min      2.6259
_cell_volume                     2359.69(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -45.00   41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   77.0000  -90.0000 86

  2 omega   49.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803   77.0000 -180.0000 26

  3 omega   -9.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803   77.0000   60.0000 98

  4 omega  -53.00    9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803  -37.0000   90.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0097182000
_diffrn_orient_matrix_UB_12      -0.0362547000
_diffrn_orient_matrix_UB_13      0.0184287000
_diffrn_orient_matrix_UB_21      0.0120726000
_diffrn_orient_matrix_UB_22      -0.0098719000
_diffrn_orient_matrix_UB_23      -0.0556543000
_diffrn_orient_matrix_UB_31      0.0636892000
_diffrn_orient_matrix_UB_32      0.0073853000
_diffrn_orient_matrix_UB_33      0.0160875000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5528
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.63
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.472
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                1801
_reflns_number_total             2076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400686q_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        2359.68(10)
_cod_database_code               4082070
_chemical_oxdiff_formula         'C18 H10 Br2 O6 Ru2 S2'
_chemical_oxdiff_usercomment     '300 K, COLORLESS, BLOCK'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32