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_4117518
_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         'C28 H56 Cl2 P4 Ru'
_chemical_formula_sum            'C28 H56 Cl2 P4 Ru'
_chemical_formula_weight         688.58
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-18
_audit_creation_method
;
  Olex2 1.1
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;
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.60235(14)
_cell_length_b                   13.80119(14)
_cell_length_c                   19.8946(2)
_cell_measurement_reflns_used    9081
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.5068
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_cell_volume                     3185.65(6)
_computing_cell_refinement
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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.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
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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
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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
;
A short history of SHELX (Sheldrick, 2007)/Bruker
;
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 16.145
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
1 omega  -24.00   39.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
-       26.4172  -37.0000  -90.0000 63

2 omega   31.00   96.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
-       26.4172   37.0000  -90.0000 65

3 omega  -45.00   52.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
-       26.4172  -37.0000  120.0000 97
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0477883
_diffrn_orient_matrix_UB_12      -0.0170433
_diffrn_orient_matrix_UB_13      -0.018844
_diffrn_orient_matrix_UB_21      0.0378656
_diffrn_orient_matrix_UB_22      0.0263825
_diffrn_orient_matrix_UB_23      0.0211612
_diffrn_orient_matrix_UB_31      0.0046003
_diffrn_orient_matrix_UB_32      -0.0406872
_diffrn_orient_matrix_UB_33      0.0216204
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16563
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.99122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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_primary    yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.2364
_exptl_crystal_size_mid          0.1258
_exptl_crystal_size_min          0.0361
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         8917
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                8256
_reflns_number_total             8917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210568t_si_002_12.cif
_cod_data_source_block           trans-R,R-Ru1(Cl)2
_cod_database_code               4117518