Mimicking of Tunichlorin: Deciphering the Importance of a β-Hydroxyl Substituent on Boosting the Hydrogen Evolution Reaction
Wu, Zhuo-Yan; Xue, Haozong; Wang, Teng; Guo, Yanru; Meng, Yin-Shan; Li, Xingguo; Zheng, Jie; Brückner, Christian; Rao, Guodong; Britt, R. David; Zhang, Jun-Long; ACS Catalysis  (2020) 2177–2188; doi:10.1021/acscatal.9b03985

data_4517324
_publ_section_title
;
 Mimicking of Tunichlorin: Deciphering the Importance of a \b-Hydroxyl
 Substituent on Boosting the Hydrogen Evolution Reaction
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              2177
_journal_page_last               2188
_journal_paper_doi               10.1021/acscatal.9b03985
_journal_year                    2020
_chemical_formula_sum            'C43 H10 F20 N4 Ni O2'
_chemical_formula_weight         1053.26
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_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                   15.3766(3)
_cell_length_b                   15.3766(3)
_cell_length_c                   15.4761(5)
_cell_measurement_reflns_used    10137
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      25.8390
_cell_measurement_theta_min      3.6960
_cell_volume                     3659.17(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180.01(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29373
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.231
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 696 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1868
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+3.1077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1693
_reflns_number_total             1868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b03985_si_003.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4517324--4517325.cif.'
_cod_original_cell_volume        3659.17(19)
_cod_database_code               4517324
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              99646
_shelx_hkl_checksum              85070