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_4345681
_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         'C25 H38 Al Cl2 N5, 3(C25 H39 Al Cl1 N5)'
_chemical_formula_sum            'C25 H38.75 Al Cl1.25 N5'
_chemical_formula_weight         480.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.6075(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2050(5)
_cell_length_b                   13.0203(5)
_cell_length_c                   15.6075(6)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      70.09
_cell_measurement_theta_min      5.42
_cell_volume                     2674.77(18)
_computing_cell_refinement       'SAINT (8.34a) (Bruker, 2013)'
_computing_data_collection       'Apex2 (2014.9-1) (Bruker, 2014)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12805
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.156
_diffrn_reflns_theta_min         4.777
_exptl_absorpt_coefficient_mu    1.968
_exptl_absorpt_correction_T_max  0.7304
_exptl_absorpt_correction_T_min  0.6452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/3 (Sheldrick, 2014)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5049
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0487P)^2^+0.8680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4695
_reflns_number_total             5049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00230_si_002.cif
_cod_data_source_block           TJS1FMI
_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               4345681
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.524
_shelx_estimated_absorpt_t_max   0.790
_shelx_res_checksum              30670
_shelx_hkl_checksum              63829