Coordinatively Diverse ortho-Phosphinoaniline Complexes of Ruthenium and Isolation of a Putative Intermediate in Ketone Transfer Hydrogenation Catalysis
Lindsay J. Hounjet; Matthias Bierenstiel; Michael J. Ferguson; Robert McDonald; Martin Cowie; Inorganic Chemistry 49 (2010) 4288–4300; doi:10.1021/ic100165t

data_4315407
_publ_section_title
;
 Coordinatively Diverse ortho-Phosphinoaniline Complexes of Ruthenium and
 Isolation of a Putative Intermediate in Ketone Transfer Hydrogenation
 Catalysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4288
_journal_page_last               4300
_journal_paper_doi               10.1021/ic100165t
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'C39 H34 N4 O10 P2 Ru3, 0.5(C5 H12), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C42 H41 Cl N4 O10 P2 Ru3'
_chemical_formula_weight         1162.39
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.7770(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7363(5)
_cell_length_b                   12.7680(3)
_cell_length_c                   21.6124(6)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.47
_cell_volume                     4877.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42128
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  0.8818
_exptl_absorpt_correction_T_min  0.6846
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         11166
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+5.1261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                9664
_reflns_number_total             11166
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100165t_si_001_8.cif
_cod_data_source_block           7.0.5C5H12.0.5CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4315407