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_1557774
_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), 0.301(C8 H8 Cl O), 0.25(C7 H4 Cl O), 0.25(C7), 0.5(C8 H7 O2), 1.399(O), 2.25(C2 H3 N)'
_chemical_formula_sum            'C98.4 H97.66 Cl12.55 N14.25 O2.95 Pd6'
_chemical_formula_weight         2610.44
_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                 90.7890(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.3380(3)
_cell_length_b                   52.9530(10)
_cell_length_c                   19.7623(4)
_cell_measurement_reflns_used    139619
_cell_measurement_temperature    98
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      1.62
_cell_volume                     15002.9(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      98
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0754
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            245595
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.615
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5203.04
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.96
_refine_diff_density_min         -1.79
_refine_ls_abs_structure_details
;
 Flack x determined using 16096 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.068(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     2293
_refine_ls_number_reflns         68909
_refine_ls_number_restraints     512
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1798P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2253
_refine_ls_wR_factor_ref         0.2658
_reflns_Friedel_coverage         0.978
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                44483
_reflns_number_total             68909
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d0fd00019a1.cif
_cod_data_source_block           HAPCPE@MMF
_cod_depositor_comments
'Adding full bibliography for 1557771--1557774.cif.'
_cod_database_code               1557774
_shelx_res_checksum              97248