Hydrogen production from formic acid catalyzed by a phosphine free manganese complex: investigation and mechanistic insights
Léval, Alexander; Agapova, Anastasiya; Steinlechner, Christoph; Alberico, Elisabetta; Junge, Henrik; Beller, Matthias; Green Chemistry 22 (2020) 913–920; doi:10.1039/C9GC02453K

data_7239784
_publ_section_title
;
 Hydrogen production from formic acid catalyzed by a phosphine free
 manganese complex: investigation and mechanistic insights
;
_journal_issue                   3
_journal_name_full               'Green Chemistry'
_journal_page_first              913
_journal_page_last               920
_journal_paper_doi               10.1039/C9GC02453K
_journal_volume                  22
_journal_year                    2020
_chemical_formula_sum            'C12 H10 Mn N3 O5'
_chemical_formula_weight         331.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-11 deposited with the CCDC.	2019-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                97.266(3)
_cell_angle_beta                 95.849(3)
_cell_angle_gamma                95.577(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5940(14)
_cell_length_b                   8.5623(16)
_cell_length_c                   13.088(3)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.41
_cell_volume                     834.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33103
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.994
_diffrn_reflns_theta_min         1.579
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4438
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+0.3778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4009
_reflns_number_total             4438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9gc02453k2.cif
_cod_data_source_block           ax1527_sq
_cod_depositor_comments
;Adding full bibliography for 7239784--7239785.cif.

 Adding full bibliography for 7239784--7239785.cif.
;
_cod_database_code               7239784
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              50828
_shelx_fab_checksum              51777