Synthetic β-Barrel by Metal-Induced Folding and Assembly.
Yamagami, Motoya; Sawada, Tomohisa; Fujita, Makoto; Journal of the American Chemical Society 140 (2018) 8644–8647; doi:10.1021/jacs.8b04284

data_4132497
_publ_section_title
;
 Synthetic \b-Barrel by Metal-Induced Folding and Assembly.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8644
_journal_page_last               8647
_journal_paper_doi               10.1021/jacs.8b04284
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_sum            'C174 H201.88 Cl6 N33 O30.5 Zn3'
_chemical_formula_weight         3652.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_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            8
_cell_length_a                   28.3964(3)
_cell_length_b                   28.3964(3)
_cell_length_c                   84.3978(18)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.8170
_cell_measurement_theta_min      1.5780
_cell_volume                     68054.6(18)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.837
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_device_type  'Rayonix MX225HE'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     1.000
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.837
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            149670
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        27.597
_diffrn_reflns_theta_max         27.597
_diffrn_reflns_theta_min         1.580
_diffrn_source                   'SPring-8 BL38B1'
_exptl_absorpt_coefficient_mu    0.740
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.713
_exptl_crystal_description       plate
_exptl_crystal_F_000             15303
_exptl_crystal_size_max          250
_exptl_crystal_size_mid          200
_exptl_crystal_size_min          100
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details
;
 Flack x determined using 3018 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.899(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         23716
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.949
_refine_ls_R_factor_all          0.3474
_refine_ls_R_factor_gt           0.2744
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5541
_refine_ls_wR_factor_ref         0.5938
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.837
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                11143
_reflns_number_total             23716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04284_si_004.cif
_cod_data_source_block           p41212
_cod_original_cell_volume        68055(2)
_cod_original_formula_sum        'C174 H201.88 Cl6 N33 O30.50 Zn3'
_cod_database_code               4132497
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              94021
_shelx_hkl_checksum              52190