Hydrogenation of carbon dioxide to methanol using a homogeneous ruthenium‒Triphos catalyst: from mechanistic investigations to multiphase catalysis
Wesselbaum, Sebastian; Moha, Verena; Meuresch, Markus; Brosinski, Sandra; Thenert, Katharina M.; Kothe, Jens; Stein, Thorsten vom; Englert, Ulli; Hölscher, Markus; Klankermayer, Jürgen; Leitner, Walter; Chem. Sci. 6 (2015) 693–; doi:10.1039/C4SC02087A

data_1517459
_publ_section_title
;
 Hydrogenation of carbon dioxide to methanol using a homogeneous
 ruthenium--Triphos catalyst: from mechanistic investigations to
 multiphase catalysis
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              693
_journal_paper_doi               10.1039/C4SC02087A
_journal_volume                  6
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C43 H42 O3 P3 Ru, C2 F6 N O4 S2, C H2 Cl2'
_chemical_formula_sum            'C46 H44 Cl2 F6 N O7 P3 Ru S2'
_chemical_formula_weight         1165.82
_chemical_name_common            'compound 4a'
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 109.038(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.731(2)
_cell_length_b                   15.301(3)
_cell_length_c                   13.247(2)
_cell_measurement_reflns_used    1561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.91
_cell_measurement_theta_min      2.34
_cell_volume                     2439.3(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_sigmaI/netI    0.1087
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26352
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         8701
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                6795
_reflns_number_total             8701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc02087a2.cif
_cod_data_source_block           4a
_cod_depositor_comments          'Adding full bibliography for 1517459.cif.'
_cod_original_cell_volume        2439.4(7)
_cod_database_code               1517459