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_4117509
_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         'C36 H58 P4 Ru, C6 H14'
_chemical_formula_sum            'C42 H72 P4 Ru'
_chemical_formula_weight         801.95
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-08-18
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.12 svn.r1921, GUI svn.r3809)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4162(13)
_cell_length_b                   14.9533(9)
_cell_length_c                   26.769(11)
_cell_measurement_reflns_used    7529
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.3141
_cell_measurement_theta_min      2.8215
_cell_volume                     4169.4(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -27.00   -1.00   1.0000  215.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6164  -60.0000 -150.0000 26

  2 omega    6.00   91.00   1.0000  215.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8664   77.0000 -150.0000 85

  3 omega  -39.00   33.00   1.0000  215.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8664  -77.0000   90.0000 72
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0251678000
_diffrn_orient_matrix_UB_12      0.0052113000
_diffrn_orient_matrix_UB_13      0.0245569000
_diffrn_orient_matrix_UB_21      0.0427013000
_diffrn_orient_matrix_UB_22      -0.0334372000
_diffrn_orient_matrix_UB_23      0.0088298000
_diffrn_orient_matrix_UB_31      0.0467040000
_diffrn_orient_matrix_UB_32      0.0331140000
_diffrn_orient_matrix_UB_33      0.0050104000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14373
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dull colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.1941
_exptl_crystal_size_mid          0.0698
_exptl_crystal_size_min          0.0191
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8493
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0402P)^2^+4.8219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                8071
_reflns_number_total             8493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210568t_si_002_03.cif
_cod_data_source_block           D-S,S-Ru2H2
_cod_database_code               4117509