Upgrading ethanol to 1-butanol with a homogeneous air-stable ruthenium catalyst.
Tseng, Kuei-Nin T; Lin, Steve; Kampf, Jeff W.; Szymczak, Nathaniel K.; Chemical communications (Cambridge, England) 52 (2016) 2901–2904; doi:10.1039/c5cc09913g

data_7118257
_publ_section_title
;
 Upgrading ethanol to 1-butanol with a homogeneous air-stable ruthenium
 catalyst.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2901
_journal_page_last               2904
_journal_paper_doi               10.1039/c5cc09913g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C39 H31 Cl N5 O3 P Ru'
_chemical_formula_sum            'C39 H31 Cl N5 O3 P Ru'
_chemical_formula_weight         785.18
_chemical_name_systematic        Ru(b4OMepi)(PPh3)(Cl)(CO)
_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
_audit_update_record
;
2015-12-01 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.709(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1333(3)
_cell_length_b                   12.4950(4)
_cell_length_c                   16.9891(5)
_cell_measurement_reflns_used    7770
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.7060
_cell_measurement_theta_min      2.7580
_cell_volume                     3385.27(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      85(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1288
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50930
_diffrn_reflns_theta_full        69.52
_diffrn_reflns_theta_max         69.52
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    5.308
_exptl_absorpt_correction_T_max  0.8570
_exptl_absorpt_correction_T_min  0.6466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/pentane'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.099
_refine_diff_density_min         -2.258
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0841
_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^)+(0.1459P)^2^+4.8742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2443
_reflns_number_gt                5229
_reflns_number_total             6297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc09913g2.cif
_cod_data_source_block           kt3190
_cod_depositor_comments
'Adding full bibliography for 7118256--7118257.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7118257