Metal-Organic Nanotube with Helical and Propeller-Chiral Motifs Composed of a C10-Symmetric Double-Decker Nanoring.
Yamagishi, Hiroshi; Fukino, Takahiro; Hashizume, Daisuke; Mori, Tadashi; Inoue, Yoshihisa; Hikima, Takaaki; Takata, Masaki; Aida, Takuzo; Journal of the American Chemical Society 137 (2015) 7628–7631; doi:10.1021/jacs.5b04386

data_4123820
_publ_section_title
;
 Metal-Organic Nanotube with Helical and Propeller-Chiral Motifs Composed
 of a C10-Symmetric Double-Decker Nanoring.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7628
_journal_page_last               7631
_journal_paper_doi               10.1021/jacs.5b04386
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration adrm
_chemical_formula_moiety         'C102 H123 Ag2 Fe2 N4 O20 S, B F4, C4 H8 O'
_chemical_formula_sum            'C106 H131 Ag2 B F4 Fe2 N4 O21 S'
_chemical_formula_weight         2243.45
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5851(13)
_cell_length_b                   26.924(3)
_cell_length_c                   27.669(3)
_cell_measurement_reflns_used    116094
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      1.51
_cell_volume                     10120.4(18)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    SV
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR2011
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1368
_diffrn_reflns_av_unetI/netI     0.1327
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            115856
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.636
_diffrn_reflns_theta_min         1.513
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.91595
_exptl_absorpt_correction_T_min  0.80916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 [c.f. R.H. Blessing, Acta Cryst. (1995), A51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plate
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.455
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 2561 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         18060
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1854
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1586P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2821
_reflns_Friedel_coverage         0.750
_reflns_friedel_fraction_full    0.891
_reflns_friedel_fraction_max     0.887
_reflns_number_gt                8740
_reflns_number_total             18060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04386_si_002.cif
_cod_data_source_block           Fc-tri2
_cod_depositor_comments          'Adding full bibliography for 4123820.cif.'
_cod_original_cell_volume        10120.2(18)
_cod_database_code               4123820
_shelx_estimated_absorpt_t_min   0.844
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2014-3
_shelx_res_checksum              52281
_shelx_hkl_checksum              92469