Facile η5-η1 Ring Slippage of the Cycloolefin Ligands in Osmocene and Bis(η5-indenyl)ruthenium(II)
Wai-Man Cheung; Enrique Kwan Huang; Jun Zhu; Xiao-Yi Yi; Herman H. Y. Sung; Ian D. Williams; Wa-Hung Leung; Inorganic Chemistry 52 (2013) 10449–10455; doi:10.1021/ic401289k

data_4335952
_publ_contact_author_name
;
;
_publ_section_title
;
 Facile \h5-\h1 Ring Slippage of the Cycloolefin Ligands in Osmocene and
 Bis(\h5-indenyl)ruthenium(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10449
_journal_page_last               10455
_journal_paper_doi               10.1021/ic401289k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C44 H60 Cl4 Co2 N2 O18 Os P6 Ru2, 2(C2 O0.5)'
_chemical_formula_sum            'C48 H88 Cl4 Co2 N2 O19 Os P6 Ru2'
_chemical_formula_weight         1835.02
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-12
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Mar 20 2012 17:37:33, GUI svn.r4124)
;
_cell_angle_alpha                99.384(2)
_cell_angle_beta                 96.206(2)
_cell_angle_gamma                113.4960(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2605(15)
_cell_length_b                   15.9640(18)
_cell_length_c                   19.194(2)
_cell_measurement_reflns_used    7336
_cell_measurement_temperature    298
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     3608.5(7)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0602
_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       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37311
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.59
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.956
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.875361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2004/1 (Bruker,2004) was used for absorption correction.
 R(int) was 0.0480 before and 0.0241 after correction.
 The Ratio of minimum to maximum transmission is 0.875361.
 The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       needle
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         14072
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                10341
_reflns_number_total             14072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401289k_si_002_1.cif
_cod_data_source_block           wai109
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_source_target' value 'MO' changed to 'Mo' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3608.6(7)
_cod_database_code               4335952