Electrocatalytic Generation of H2 from Neutral Water in Acetonitrile Using Manganese Polypyridyl Complexes with Ligand Assistance
Richeson, Darrin; Rao, Gyandshwar Kumar; Jamshidi, Mohammad Parsa; Dawkins, Jeremy; Pell, Wendy; Korobkov, Ilia; Dalton Trans.  (2017) –; doi:10.1039/C7DT01039G

data_7042809
_publ_section_title
;
 Electrocatalytic Generation of H2 from Neutral Water in Acetonitrile
 Using Manganese Polypyridyl Complexes with Ligand Assistance
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01039G
_journal_year                    2017
_chemical_formula_sum            'C44 H38 F6 N8 O13 Re2 S2'
_chemical_formula_weight         1437.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1np4gy
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-22 deposited with the CCDC.
2017-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8249(14)
_cell_length_b                   24.919(2)
_cell_length_c                   12.1149(10)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.56
_cell_volume                     5079.3(7)
_computing_cell_refinement       'APEX II, Bruker (2012)'
_computing_data_collection       'APEX II, Bruker (2012)'
_computing_data_reduction        'XPREP, Bruker (2012)'
_computing_molecular_graphics    'SHELXTL, Bruker (2015)'
_computing_publication_material  'SHELXTL, Bruker (2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            60571
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.263
_diffrn_reflns_theta_min         1.869
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.936
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
; 
 Flack x determined using 4590 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.035(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         12489
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+1.6182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                11071
_reflns_number_total             12489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01039g2.cif
_cod_data_source_block           dr133a
_cod_original_cell_volume        5079.2(7)
_cod_database_code               7042809
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.384
_shelx_estimated_absorpt_t_max   0.506
_shelx_res_checksum              37192