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_4117514
_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 H69 B O2 P4 Ru'
_chemical_formula_sum            'C34 H69 B O2 P4 Ru'
_chemical_formula_weight         745.65
_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
;
'Wed Jan 12 11:48:33 2011'
;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
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;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.09766(17)
_cell_length_b                   18.0979(3)
_cell_length_c                   20.9211(3)
_cell_measurement_reflns_used    19302
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.5562
_cell_measurement_theta_min      2.9705
_cell_volume                     3823.26(11)
_computing_cell_refinement
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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
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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CrysAlisPro, Oxford Diffraction Ltd.,
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_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
;
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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_details
;
  1 omega  -48.00   45.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.5802   77.0000  120.0000 93

  2 omega   -5.00   84.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8302   77.0000    0.0000 89

  3 omega  -46.00   43.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8302  -70.0000  -60.0000 89

  4 omega    0.00   89.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8302   77.0000  150.0000 89
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
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_diffrn_orient_matrix_UB_11      -0.0431539000
_diffrn_orient_matrix_UB_12      0.0033776000
_diffrn_orient_matrix_UB_13      0.0266037000
_diffrn_orient_matrix_UB_21      -0.0026061000
_diffrn_orient_matrix_UB_22      -0.0390381000
_diffrn_orient_matrix_UB_23      0.0026883000
_diffrn_orient_matrix_UB_31      0.0553386000
_diffrn_orient_matrix_UB_32      0.0007308000
_diffrn_orient_matrix_UB_33      0.0208709000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31688
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.5562
_diffrn_reflns_theta_min         2.9705
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
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empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.2161
_exptl_crystal_size_mid          0.1531
_exptl_crystal_size_min          0.0264
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.040(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         10702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.5914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                9972
_reflns_number_total             10702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210568t_si_002_08.cif
_cod_data_source_block           L-R,R-Ru1(Bpin)(H)
_cod_original_cell_volume        3823.25(10)
_cod_database_code               4117514