Polymorphs of layered assemblies of hydrogen-bonded hexagonal networks caused by conformational frustration
Ichiro Hisaki; Nobuaki Ikenaka; Norimitsu Tohnai; Mikiji Miyata; Chem.Commun. 52 (2016) 300–; doi:

data_7118399
_publ_section_title
;
 Polymorphs of layered assemblies of hydrogen-bonded hexagonal networks
 caused by conformational frustration
;
_journal_name_full               Chem.Commun.
_journal_page_first              300
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         '2(C60 H36 O12), 5(C8 H8 O2)'
_chemical_formula_sum            'C160 H112 O34'
_chemical_formula_weight         2578.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-10-16 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                93.295(3)
_cell_angle_beta                 93.991(3)
_cell_angle_gamma                102.380(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8218(9)
_cell_length_b                   15.8756(11)
_cell_length_c                   38.6736(18)
_cell_measurement_temperature    213
_cell_volume                     7649.3(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       DENZO
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'CrystalStructure 4.1.1'
_computing_publication_material  'CrystalStructure 4.1.1 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD Version 2013/2 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'CCD (MX225HE Rayonix)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_laue_measured_fraction_full 0.862
_diffrn_reflns_laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            42603
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        28.067
_diffrn_reflns_theta_max         28.067
_diffrn_reflns_theta_min         1.482
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2688.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-dimethylformamide, methyl benzoate'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1752
_refine_ls_number_reflns         22464
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1592
_refine_ls_R_factor_gt           0.1075
_refine_ls_shift/su_max          0.000
_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          0.3173
_refine_ls_wR_factor_ref         0.3604
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                13044
_reflns_number_total             22464
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5cc07690k2.cif
_cod_data_source_block           1_2D4
_cod_database_code               7118399
_shelx_res_checksum              76727
_platon_squeeze_void_probe_radius 1.20