Control of Ligand pKa Values Tunes the Electrocatalytic Dihydrogen Evolution Mechanism in a Redox-Active Aluminum(III) Complex
Sherbow, Tobias J.; Fettinger, James C.; Berben, Louise A.; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00230

data_4345683
_publ_section_title
;
 Control of Ligand pKa Values Tunes the Electrocatalytic Dihydrogen
 Evolution Mechanism in a Redox-Active Aluminum(III) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00230
_journal_year                    2017
_chemical_formula_moiety         'C29 H45 Al Cl2 N5 O, Al Cl4'
_chemical_formula_sum            'C29 H45 Al2 Cl6 N5 O'
_chemical_formula_weight         746.36
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                67.2772(14)
_cell_angle_beta                 72.3121(15)
_cell_angle_gamma                87.9924(19)
_cell_formula_units_Z            2
_cell_length_a                   11.7181(5)
_cell_length_b                   13.3674(5)
_cell_length_c                   13.6225(6)
_cell_measurement_reflns_used    9793
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      68.35
_cell_measurement_theta_min      3.71
_cell_volume                     1866.92(14)
_computing_cell_refinement       'SAINT (8.34a) (Bruker, 2013)'
_computing_data_collection       'Apex2 (2013.10-2) (Bruker, 2013)'
_computing_data_reduction        'SAINT (8.34a) (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12828
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.358
_diffrn_reflns_theta_min         3.706
_exptl_absorpt_coefficient_mu    4.894
_exptl_absorpt_correction_T_max  0.2999
_exptl_absorpt_correction_T_min  0.1565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       Block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.631
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.341
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         6574
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0467P)^2^+1.7761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6126
_reflns_number_total             6574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00230_si_002.cif
_cod_data_source_block           TJS31FMI
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_database_code               4345683
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.148
_shelx_estimated_absorpt_t_max   0.286
_shelx_res_checksum              7368
_shelx_hkl_checksum              80019