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_4335953
_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
'C52 H84 Cl4 Co2 N2 O18 P6 Ru3, C H2 Cl2, 0.75(C6H14)'
_chemical_formula_sum            'C57.5 H96.5 Cl6 Co2 N2 O18 P6 Ru3'
_chemical_formula_weight         1923.46
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_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_creation_date             2012-05-14
_audit_creation_method
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  Olex2 1.2-beta
  (compiled May  2 2012 11:17:23, GUI svn.r4217)
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_cell_angle_alpha                90.00
_cell_angle_beta                 97.010(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3744(3)
_cell_length_b                   18.0585(3)
_cell_length_c                   31.6395(7)
_cell_measurement_reflns_used    10301
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      28.2648
_cell_measurement_theta_min      2.9985
_cell_volume                     8151.6(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
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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
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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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega -113.00  -62.00   0.6000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.9642 -178.0000 -180.0000 85

  2 omega  -50.00   37.00   0.6000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.9642   57.0000 -120.0000 145

  3 omega  -45.00   12.00   0.6000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.9642  -77.0000   90.0000 95

  4 omega -107.00   -5.60   0.6000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.9642  -19.0000  -60.0000 169

  5 omega  -99.00  -63.00   0.6000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.9642  -57.0000 -150.0000 60
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0178790000
_diffrn_orient_matrix_UB_12      -0.0326340000
_diffrn_orient_matrix_UB_13      0.0085444000
_diffrn_orient_matrix_UB_21      0.0110289000
_diffrn_orient_matrix_UB_22      -0.0203736000
_diffrn_orient_matrix_UB_23      -0.0178947000
_diffrn_orient_matrix_UB_31      0.0450521000
_diffrn_orient_matrix_UB_32      -0.0079441000
_diffrn_orient_matrix_UB_33      0.0108153000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            37436
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           40
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             3910
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         14954
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0728
_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^)+(0.0980P)^2^+13.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                12600
_reflns_number_total             14954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401289k_si_002_2.cif
_cod_data_source_block           wai119molt
_cod_original_formula_sum        'C57.50 H96.50 Cl6 Co2 N2 O18 P6 Ru3'
_cod_database_code               4335953
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32