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_4117507
_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 H58 P4 Ru'
_chemical_formula_sum            'C28 H58 P4 Ru'
_chemical_formula_weight         619.69
_chemical_name_systematic
;
?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-18
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.5462(3)
_cell_length_b                   10.5462(3)
_cell_length_c                   24.2854(16)
_cell_measurement_reflns_used    6842
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.23
_cell_volume                     2339.20(18)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35612
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.922239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0646 before and 0.0334 after correction.
The Ratio of minimum to maximum transmission is 0.9222.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       Shard
_exptl_crystal_F_000             990
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         9030
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0595
_reflns_number_gt                8611
_reflns_number_total             9030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210568t_si_002_01.cif
_cod_data_source_block           L-R,R-Ru1H2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_source_target' value 'MO' changed to 'Mo' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4117507