Bottom-up synthesis and structures of π-lengthened tubular macrocycles
Matsuno, Taisuke; Kamata, Sho; Hitosugi, Shunpei; Isobe, Hiroyuki; Chemical Science 4 (2013) 3179–; doi:10.1039/c3sc50645b

data_1514765
_publ_section_title
;
 Bottom-up synthesis and structures of \p-lengthened tubular macrocycles
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              3179
_journal_paper_doi               10.1039/c3sc50645b
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C200 H256 Si8'
_chemical_formula_weight         2884.77
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-03-04 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.835(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.179(7)
_cell_length_b                   17.461(8)
_cell_length_c                   32.012(15)
_cell_measurement_reflns_used    4581
_cell_measurement_temperature    100
_cell_measurement_theta_max      16.01
_cell_measurement_theta_min      2.19
_cell_volume                     8997(7)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29996
_diffrn_reflns_theta_full        16.06
_diffrn_reflns_theta_max         16.06
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_correction_T_min  0.9891
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.929
_refine_ls_R_factor_all          0.1715
_refine_ls_R_factor_gt           0.1535
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4279
_refine_ls_wR_factor_ref         0.4429
_reflns_number_gt                3516
_reflns_number_total             4437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc50645b.txt
_cod_data_source_block           6,12-TIPSe[4]CA
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               1514765