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_4123320
_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         'C51 H27 N3, 2.125(C H2 Cl2)'
_chemical_formula_sum            'C53.12 H31.25 Cl4.25 N3'
_chemical_formula_weight         862.22
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.59(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   72.75(4)
_cell_length_b                   11.847(5)
_cell_length_c                   19.475(9)
_cell_measurement_reflns_used    1475
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      2
_cell_volume                     16244(14)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type
;
Xcalibur O kappa-geometry diffractometer with a Onyx CCD detector
;
_diffrn_measurement_method       w/
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.2073
_diffrn_reflns_av_unetI/netI     0.2587
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       87
_diffrn_reflns_limit_h_min       -74
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37336
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         68.635
_diffrn_reflns_theta_min         2.510
_exptl_absorpt_coefficient_mu    3.136
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.696
_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-yellow'
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       needle
_exptl_crystal_F_000             7092
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.304
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         14259
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.3452
_refine_ls_R_factor_gt           0.1988
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0900P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3894
_refine_ls_wR_factor_ref         0.4670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4277
_reflns_number_total             14259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja511951x_si_002.cif
_cod_data_source_block           dst16a
_cod_depositor_comments
'Adding full bibliography for 4123320--4123321.cif.'
_cod_database_code               4123320
_shelx_estimated_absorpt_t_min   0.618
_shelx_estimated_absorpt_t_max   0.744
_shelxl_version_number           2013-2
_shelx_res_checksum              46572
_shelx_hkl_checksum              78214