Electrocatalytic Reduction of Dioxygen to Hydrogen Peroxide by a Molecular Manganese Complex with a Bipyridine-Containing Schiff Base Ligand.
Hooe, Shelby; Rheingold, Arnold L.; Machan, Charles W.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09027

data_4126958
_publ_section_title
;
 Electrocatalytic Reduction of Dioxygen to Hydrogen Peroxide by a
 Molecular Manganese Complex with a Bipyridine-Containing Schiff Base
 Ligand.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09027
_journal_year                    2017
_chemical_formula_moiety         'C38 H46 Cl Mn N2 O2, C4 H8 O'
_chemical_formula_sum            'C42 H54 Cl Mn N2 O3'
_chemical_formula_weight         725.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                73.599(8)
_cell_angle_beta                 80.485(11)
_cell_angle_gamma                88.031(8)
_cell_formula_units_Z            2
_cell_length_a                   9.4021(17)
_cell_length_b                   12.198(3)
_cell_length_c                   16.984(4)
_cell_measurement_reflns_used    7782
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.601
_cell_measurement_theta_min      2.410
_cell_volume                     1842.7(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26716
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.978
_diffrn_reflns_theta_max         25.978
_diffrn_reflns_theta_min         1.740
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.2593
_exptl_absorpt_correction_T_min  0.2319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0898 before and 0.0461 after correction. The Ratio of minimum to maximum transmission is 0.8943. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       needle
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0324P)^2^+1.6445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5483
_reflns_number_total             7142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09027_si_002.cif
_cod_data_source_block           machan01_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1842.8(7)
_cod_database_code               4126958
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H42A(0.5) H42B(0.5) H42C(0.5) H42D(0.5) H40A(0.5) H40B(0.5)
 H40C(0.5) H40D(0.5) C41(0.5) H41A(0.5) H41B(0.5) C41A(0.5) H41C(0.5) H41D(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C42(H42C,H42D), C39(H39A,H39B), C40(H40A,H40B), C40(H40C,
 H40D), C41(H41A,H41B), C41A(H41C,H41D)
3.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C4(H4), C3(H3), C8(H8), C9(H9), C7(H7), C14(H14), C2(H2), C26(H26),
 C12(H12)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C23(H23A,H23B,H23C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C), C33(H33A,H33B,H33C), C18(H18A,H18B,H18C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C22(H22A,H22B,H22C),
 C37(H37A,H37B,H37C)
;
_shelx_res_checksum              45005
_shelx_hkl_checksum              8654
_olex2_submission_special_instructions 'No special instructions were received'