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_4117515
_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         'C38 H60 P4 Ru'
_chemical_formula_sum            'C38 H60 P4 Ru'
_chemical_formula_weight         741.81
_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             2011-10-18
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  Olex2 1.1
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_cell_formula_units_Z            4
_cell_length_a                   10.2481(3)
_cell_length_b                   17.7037(5)
_cell_length_c                   19.8698(5)
_cell_measurement_reflns_used    16888
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      32.0554
_cell_measurement_theta_min      3.0348
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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)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
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;
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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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
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;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.0
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_diffrn_measured_fraction_theta_full 0.998
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;
  1 omega  -42.00  -16.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0110  151.0000   22.0000 26

  2 omega  -67.00  -29.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0110  106.0000  -39.0000 38

  3 omega    7.00   92.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   37.0000 -120.0000 85

  4 omega    1.00   92.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   37.0000  -30.0000 91

  5 omega  -14.00   21.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172 -106.0000 -140.0000 35

  6 omega   -4.00   97.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   77.0000   60.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0688375000
_diffrn_orient_matrix_UB_12      -0.0007922000
_diffrn_orient_matrix_UB_13      -0.0035540000
_diffrn_orient_matrix_UB_21      0.0002196000
_diffrn_orient_matrix_UB_22      -0.0388814000
_diffrn_orient_matrix_UB_23      0.0085885000
_diffrn_orient_matrix_UB_31      -0.0069085000
_diffrn_orient_matrix_UB_32      -0.0095493000
_diffrn_orient_matrix_UB_33      -0.0345051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33778
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         32.13
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91440
_exptl_absorpt_correction_type   multi-scan
_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)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            '? yellow'
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_recrystallization_method hexane
_exptl_crystal_size_max          0.2387
_exptl_crystal_size_mid          0.1264
_exptl_crystal_size_min          0.0575
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.034(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         11534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.4276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                10927
_reflns_number_total             11534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210568t_si_002_09.cif
_cod_data_source_block           L-S,S-Ru2(C2H4)
_cod_original_cell_volume        3604.96(16)
_cod_database_code               4117515