Carbon Dioxide Promoted H(+) Reduction Using a Bis(imino)pyridine Manganese Electrocatalyst.
Mukhopadhyay, Tufan K.; MacLean, Nicholas L.; Gan, Lu; Ashley, Daniel C.; Groy, Thomas L.; Baik, Mu-Hyun; Jones, Anne K.; Trovitch, Ryan J.; Inorganic chemistry 54 (2015) 4475–4482; doi:10.1021/acs.inorgchem.5b00315

data_4343239
_publ_section_title
;
 Carbon Dioxide Promoted H(+) Reduction Using a Bis(imino)pyridine
 Manganese Electrocatalyst.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4475
_journal_page_last               4482
_journal_paper_doi               10.1021/acs.inorgchem.5b00315
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C40 H41 Mn N3 O P2, Br'
_chemical_formula_sum            'C40 H41 Br Mn N3 O P2'
_chemical_formula_weight         776.55
_chemical_name_common            MacLean_NLM_1_045
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.9017(11)
_cell_length_b                   15.6536(8)
_cell_length_c                   21.5227(11)
_cell_measurement_reflns_used    9511
_cell_measurement_temperature    123.(2)
_cell_measurement_theta_max      24.4249
_cell_measurement_theta_min      2.1664
_cell_volume                     7041.9(6)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2013.6-2 (Bruker-AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123.(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55593
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.433
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.354(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         12413
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                9622
_reflns_number_total             12413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00315_si_003.cif
_cod_data_source_block           Ph2PPrPDIMnCO
_cod_database_code               4343239
_shelx_res_checksum              664
_shelx_hkl_checksum              19446