Face-selective adsorption of a prochiral compound on the chiral pore-surface of a metal-macrocycle framework (MMF) directed towards stereoselective reactions.
Tashiro, Shohei; Umeki, Tsutomu; Kubota, Ryou; Shionoya, Mitsuhiko; Faraday discussions 225 (2021) 197–209; doi:10.1039/d0fd00019a

data_1557773
_publ_section_title
;
 Face-selective adsorption of a prochiral compound on the chiral
 pore-surface of a metal-macrocycle framework (MMF) directed towards
 stereoselective reactions.
;
_journal_name_full               'Faraday discussions'
_journal_page_first              197
_journal_page_last               209
_journal_paper_doi               10.1039/d0fd00019a
_journal_volume                  225
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C42 H42 Cl6 N6 Pd3), 0.401(C6 H7 O6), 0.5(C O), 7.224(O)'
_chemical_formula_sum            'C86.9 H86.8 Cl12 N12 O10.13 Pd6'
_chemical_formula_weight         2525.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-12-27 deposited with the CCDC.	2020-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.1321(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.1814(3)
_cell_length_b                   52.5455(10)
_cell_length_c                   19.8435(4)
_cell_measurement_reflns_used    111430
_cell_measurement_temperature    95
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      1.63
_cell_volume                     14783.9(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      95
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -67
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            145572
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.513
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5012.96
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.30
_refine_diff_density_min         -1.32
_refine_ls_abs_structure_details
;
 Flack x determined using 18528 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     2189
_refine_ls_number_reflns         67276
_refine_ls_number_restraints     264
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1532P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2227
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                49578
_reflns_number_total             67276
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d0fd00019a1.cif
_cod_data_source_block           mannose@MMF
_cod_depositor_comments
'Adding full bibliography for 1557771--1557774.cif.'
_cod_original_cell_volume        14783.8(5)
_cod_database_code               1557773
_shelx_res_checksum              1962