Probing Highly Selective H/D Exchange Processes with a Ruthenium Complex through Neutron Diffraction and Multinuclear NMR Studies.
Mary Grellier; Sax A. Mason; Alberto Albinati; Silvia C. Capelli; Silvia Rizzato; Christian Bijani; Yannick Coppel; Sylviane Sabo-Etienne; Inorganic Chemistry 52 (2013) 7329–7337; doi:10.1021/ic302307m

data_4335308
_publ_contact_author_address
;
 Laboratoire de Chimie de Coordination
 205 Route de Narbonne
 31077 Toulouse Cedex 04
;
_publ_contact_author_email       sabo@lcc-toulouse.fr
_publ_contact_author_name        'Sylviane Sabo-Etienne'
_publ_section_title
;
 Probing Highly Selective H/D Exchange Processes with a Ruthenium Complex
 through Neutron Diffraction and Multinuclear NMR Studies.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7329
_journal_page_last               7337
_journal_paper_doi               10.1021/ic302307m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C30 H54 D6 P2 Ru'
_chemical_formula_weight         589.84
_chemical_name_common            '[Ru(D)2(D2)2(P(C5H9)3)2]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.3836(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.82920(10)
_cell_length_b                   9.42600(10)
_cell_length_c                   21.6700(2)
_cell_measurement_reflns_used    11259
_cell_measurement_temperature    20(1)
_cell_measurement_theta_max      61.26
_cell_measurement_theta_min      3.17
_cell_volume                     2920.51(5)
_computing_cell_refinement       'ILL RAFD9'
_computing_data_collection       'ILL HKLGEN, MAD'
_computing_data_reduction        'ILL Retreat'
_computing_molecular_graphics
;     
 ORTEP for Windows v1.074 (L.J. Farrugia 1997)
 Mercury CSD 2.4.5 (Build RC3), CCDC, Cambridge (2011)
;
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia, J. Appl. Cryst.,1999,32, 837)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.,2008,A64,112)'
_diffrn_ambient_temperature      20(1)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type
'D19 position-sensitive detector diffractometer'
_diffrn_measurement_method       'omega step-scans'
_diffrn_radiation_monochromator  'Cu (311)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL High Flux Reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.1675
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27791
_diffrn_reflns_theta_full        61.27
_diffrn_reflns_theta_max         61.27
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  240
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.6425
_exptl_absorpt_correction_T_min  0.4643
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 An absorption correction for the cans used in the low T set up has also 
 been applied to the data set. T_min = 0.8182 and T-max = 0.9003.
 The corrections were carried out by using the ILL program D19abscan.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             219
_exptl_crystal_size_max          3.2
_exptl_crystal_size_mid          2.1
_exptl_crystal_size_min          1.8
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         9339
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+6.7203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                8035
_reflns_number_total             9339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302307m_si_002_1.cif
_cod_data_source_block           shelxl
_cod_database_code               4335308