Highly Efficient Process for Production of Biofuel from Ethanol Catalyzed by Ruthenium Pincer Complexes.
Xie, Yinjun; Ben-David, Yehoshoa; Shimon, Linda J. W.; Milstein, David; Journal of the American Chemical Society 138 (2016) 9077–9080; doi:10.1021/jacs.6b05433

data_4130634
_publ_section_title
;
 Highly Efficient Process for Production of Biofuel from Ethanol Catalyzed
 by Ruthenium Pincer Complexes.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9077
_journal_page_last               9080
_journal_paper_doi               10.1021/jacs.6b05433
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C29 H41 N O2 P2 Ru'
_chemical_formula_sum            'C29 H41 N O2 P2 Ru'
_chemical_formula_weight         598.64
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.3890(6)
_cell_length_b                   26.3890(6)
_cell_length_c                   8.1302(2)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.40
_cell_measurement_theta_min      2.44
_cell_volume                     5661.7(2)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker KappaApexII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27122
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.698
_diffrn_reflns_theta_min         2.183
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 3042 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.015(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+1.3773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0533
_reflns_Friedel_coverage         0.842
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                6857
_reflns_number_total             7150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05433_si_002.cif
_cod_data_source_block           m1809
_cod_original_cell_volume        5661.7(3)
_cod_database_code               4130634
_shelx_estimated_absorpt_t_min   0.769
_shelx_estimated_absorpt_t_max   0.874
_shelxl_version_number           2013-4
_shelx_res_checksum              31111
_shelx_hkl_checksum              33958