Selective Photochemistry at Stereogenic Metal and Ligand Centers of cis-[Ru(diphosphine)2(H)2]: Preparative, NMR, Solid State, and Laser Flash Studies
Marius V. Câmpian; Robin N. Perutz; Barbara Procacci; Robert J. Thatcher; Olga Torres; Adrian C. Whitwood; Journal of the American Chemical Society 134 (2012) 3480–3497; doi:10.1021/ja210568t

data_4117511
_publ_contact_author_address
;Department of Chemistry,
University of York,
Heslington,
York
YO10 5DD
UK
;
_publ_contact_author_email       robin.perutz@york.ac.uk
_publ_contact_author_fax         '+44 1904 432516'
_publ_contact_author_name        'Professor Robin N Perutz'
_publ_contact_author_phone       '+44 1904 432549'
_publ_section_title
;
 Selective Photochemistry at Stereogenic Metal and Ligand Centers of
 cis-[Ru(diphosphine)2(H)2]: Preparative, NMR, Solid State, and Laser
 Flash Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3480
_journal_page_last               3497
_journal_paper_doi               10.1021/ja210568t
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H64 P4 Ru Si'
_chemical_formula_sum            'C34 H64 P4 Ru Si'
_chemical_formula_weight         725.89
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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  Olex2 1.1
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_cell_length_a                   10.8954(6)
_cell_length_b                   18.2414(9)
_cell_length_c                   18.2696(9)
_cell_measurement_reflns_used    12524
_cell_measurement_temperature    110.0(2)
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
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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
;
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.
;
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olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
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;
  1 omega  -54.00  -25.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9830   96.0000  157.0000 29

  2 omega  -90.00   -9.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9830  -77.0000   60.0000 81

  3 omega  -40.00   -7.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6138   77.0000   30.0000 33

  4 omega   -7.00   20.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8638   77.0000    0.0000 27

  5 omega   13.00   44.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8638   77.0000  150.0000 31

  6 omega    8.00   85.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8638   77.0000 -150.0000 77
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
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_diffrn_orient_matrix_UB_11      -0.0621651000
_diffrn_orient_matrix_UB_12      0.0081251000
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_diffrn_orient_matrix_UB_21      -0.0074646000
_diffrn_orient_matrix_UB_22      -0.0353563000
_diffrn_orient_matrix_UB_23      -0.0154743000
_diffrn_orient_matrix_UB_31      -0.0176540000
_diffrn_orient_matrix_UB_32      -0.0138825000
_diffrn_orient_matrix_UB_33      0.0347740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20656
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.4200
_diffrn_reflns_theta_min         2.9067
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94453
_exptl_absorpt_correction_type   multi-scan
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;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier
;
;
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       needle
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.1797
_exptl_crystal_size_mid          0.0986
_exptl_crystal_size_min          0.0367
_refine_diff_density_max         0.383
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_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0213P)^2^+1.0241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                7680
_reflns_number_total             8153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210568t_si_002_05.cif
_cod_data_source_block           L-R,R-Ru1(PhSiH2)(H)
_cod_database_code               4117511