Chiral metal‒macrocycle frameworks: supramolecular chirality induction and helicity inversion of the helical macrocyclic structures
Kubota, Ryou; Tashiro, Shohei; Shionoya, Mitsuhiko; Chem. Sci. 7 (2016) 2217–; doi:10.1039/C5SC04570C

data_1542254
_publ_section_title
;
 Chiral metal--macrocycle frameworks: supramolecular chirality induction
 and helicity inversion of the helical macrocyclic structures
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2217
_journal_paper_doi               10.1039/C5SC04570C
_journal_volume                  7
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C42 H42 N6 Pd3 Cl6), 4.77(C H2 Cl2), 4.92(H2 O)'
_chemical_formula_sum            'C88.77 H103.38 Cl21.54 N12 O4.92 Pd6'
_chemical_formula_weight         2819.27
_space_group_IT_number           199
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      199
_symmetry_space_group_name_Hall  'I 2b 2c 3'
_symmetry_space_group_name_H-M   'I 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2014-02-27 deposited with the CCDC.
2015-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   31.4950(7)
_cell_length_b                   31.4950(7)
_cell_length_c                   31.4950(7)
_cell_measurement_reflns_used    72327
_cell_measurement_temperature    97
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.04
_cell_volume                     31241.0(12)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      97
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_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_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            136000
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11212.32
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.640
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  5643 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.07(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     397
_refine_ls_number_reflns         11931
_refine_ls_number_restraints     9
_refine_ls_R_factor_gt           0.0917
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1642P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2429
_reflns_number_gt                8758
_reflns_number_total             11931
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5sc04570c2.cif
_cod_data_source_block           P-MMF-2
_cod_depositor_comments
'Adding full bibliography for 1542253--1542262.cif.'
_cod_original_cell_volume        31240.9(12)
_cod_database_code               1542254