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_4315404
_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         'C43 H56 Cl N4 P2 Ru, Cl'
_chemical_formula_sum            'C43 H56 Cl2 N4 P2 Ru'
_chemical_formula_weight         862.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.0666(14)
_cell_length_b                   10.3284(4)
_cell_length_c                   22.7085(9)
_cell_measurement_reflns_used    9719
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.26
_cell_volume                     8459.1(6)
_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    'SIR-97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71812
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.9187
_exptl_absorpt_correction_T_min  0.8275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881. 9428 Friedel pairs'
_refine_ls_abs_structure_Flack   0.298(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         19378
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+1.9568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                17974
_reflns_number_total             19378
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100165t_si_001_5.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_cell_volume        8459.2(6)
_cod_database_code               4315404