A local proton source in a [Mn(bpy-R)(CO)3Br]-type redox catalyst enables CO2 reduction even in the absence of Bronsted acids
Federico Franco; Claudio Cometto; Federico Ferrero Vallana; Fabrizio Sordello; Emanuele Priola; Claudio Minero; Carlo Nervi; Roberto Gobetto; Chem.Commun. 50 (2014) 14670–; doi:10.1039/C4cc05563B

data_7115954
_publ_section_title
;
 A local proton source in a [Mn(bpy-R)(CO)3Br]-type redox catalyst enables
 CO2 reduction even in the absence of Bronsted acids
;
_journal_name_full               Chem.Commun.
_journal_page_first              14670
_journal_paper_doi               10.1039/C4cc05563B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'Mn1 Br1 O6 N2 C29 H26'
_chemical_formula_sum            'C4.14 H3.71 Br0.14 Mn0.14 N0.29 O0.86'
_chemical_formula_weight         90.48
_chemical_name_systematic
'fac-bromo-tricarbonyl-((4-phenyl-6-(1,3-dihydroxybenzen-2-yl)-2,2'-bipyridine)-manganese. Et2O'
_chemical_properties_physical    'Light-sensitive, Photo-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.684(4)
_cell_angle_beta                 69.151(4)
_cell_angle_gamma                79.227(4)
_cell_formula_units_Z            14
_cell_length_a                   11.3412(5)
_cell_length_b                   11.5546(5)
_cell_length_c                   12.4448(6)
_cell_measurement_reflns_used    6465
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.3560
_cell_measurement_theta_min      4.0500
_cell_volume                     1441.62(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.2890
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12327
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         36.15
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         12433
_exptl_absorpt_coefficient_mu    1.851
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_recrystallization_method 'slow evaporation from dierthyl ether'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         3085
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+2.1789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                2724
_reflns_number_total             3085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05563b2.cif
_cod_data_source_block           preex
_cod_original_cell_volume        1441.62(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115954