Synthesis and Crystal Structures of Ru(II) Complexes Containing Chelating (Phosphinomethyl)oxazoline P,N-Type Ligands and Asymmetric Catalytic Transfer Hydrogenation of Acetophenone in Propan-2-ol
Pierre Braunstein; Claudia Graiff; Frédéric Naud; Andreas Pfaltz; Antonio Tiripicchio; Inorganic Chemistry 39 (2000) 4468–4475; doi:10.1021/ic0000754

data_4321379
_publ_section_title
;
 Synthesis and Crystal Structures of Ru(II) Complexes Containing Chelating
 (Phosphinomethyl)oxazoline P,N-Type Ligands and Asymmetric Catalytic
 Transfer Hydrogenation of Acetophenone in Propan-2-ol
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4468
_journal_page_last               4475
_journal_paper_doi               10.1021/ic0000754
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C32 H32 Cl2 N2 O2 P2 Ru'
_chemical_formula_sum            'C32 H32 Cl2 N2 O2 P2 Ru'
_chemical_formula_weight         710.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.44(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.427(4)
_cell_length_b                   17.487(3)
_cell_length_c                   22.422(5)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.83
_cell_measurement_theta_min      11.21
_cell_volume                     6629(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Siemens AED'
_diffrn_measurement_method       '\q/2\q 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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.1392
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16367
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         3.06
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.029
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         15987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.354
_refine_ls_shift/su_mean         0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.2142
_reflns_number_gt                5385
_reflns_number_total             15987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0000754_1.cif
_cod_data_source_block           fn31h
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6629(2)
_cod_database_code               4321379