Highly Strained Nonclassical Nanotube End-caps. A Single-Step Solution Synthesis from Strain-Free, Non-Macrocyclic Precursors.
Myśliwiec, Damian; Kondratowicz, Mateusz; Lis, Tadeusz; Chmielewski, Piotr J.; Stępień, Marcin; Journal of the American Chemical Society 137 (2015) 1643–1649; doi:10.1021/ja511951x

data_4123321
_publ_section_title
;
 Highly Strained Nonclassical Nanotube End-caps. A Single-Step Solution
 Synthesis from Strain-Free, Non-Macrocyclic Precursors.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1643
_journal_page_last               1649
_journal_paper_doi               10.1021/ja511951x
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C45 H27 N3, 2(C2 H4 Cl2)'
_chemical_formula_sum            'C49 H35 Cl4 N3'
_chemical_formula_weight         807.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                88.70(3)
_cell_angle_beta                 89.12(3)
_cell_angle_gamma                62.52(4)
_cell_formula_units_Z            6
_cell_length_a                   17.754(6)
_cell_length_b                   19.033(7)
_cell_length_c                   19.752(7)
_cell_measurement_reflns_used    10253
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     5920(4)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Xcalibur R kappa-geometry diffractometer with a Ruby CCD detector
;
_diffrn_measurement_method       w/
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59504
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a
multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.79
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1640
_refine_ls_number_reflns         23353
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1915
_refine_ls_R_factor_gt           0.1293
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1630P)^2^+20.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3508
_refine_ls_wR_factor_ref         0.3890
_reflns_number_gt                13161
_reflns_number_total             23353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja511951x_si_003.cif
_cod_data_source_block           dste17ma
_cod_depositor_comments
'Adding full bibliography for 4123320--4123321.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4123321