Electrocatalytic H<sub>2</sub>O Reduction with f-Elements: Mechanistic Insight and Overpotential Tuning in a Series of Lanthanide Complexes.
Halter, Dominik P.; Palumbo, Chad T.; Ziller, Joseph W.; Gembicky, Milan; Rheingold, Arnold L.; Evans, William J.; Meyer, Karsten; Journal of the American Chemical Society 140 (2018) 2587–2594; doi:10.1021/jacs.7b11532

data_4131831
_publ_section_title
;
 Electrocatalytic H<sub>2</sub>O Reduction with f-Elements: Mechanistic
 Insight and Overpotential Tuning in a Series of Lanthanide Complexes.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2587
_journal_page_last               2594
_journal_paper_doi               10.1021/jacs.7b11532
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_sum            'C81 H112 K N2 Nd O10'
_chemical_formula_weight         1457.06
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.894(3)
_cell_length_b                   19.894(3)
_cell_length_c                   19.894(3)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      22.14
_cell_measurement_theta_min      2.29
_cell_volume                     7873(2)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 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  0.1027
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78006
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.339
_diffrn_reflns_theta_max         25.339
_diffrn_reflns_theta_min         1.448
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.8012
_exptl_absorpt_correction_T_min  0.6523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3084
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
; 
 Flack x determined using 1796 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.018(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+4.5396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4270
_reflns_number_total             4826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11532_si_003.cif
_cod_data_source_block           ctp68
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        7873(3)
_cod_database_code               4131831
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.807
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              5940
_shelx_hkl_checksum              96277
_shelx_fab_checksum              98773