Switching intermolecular interactions by confinement in carbon nanotubes
T. W. Chamberlain; M. A. Lebedeva; W. Abuajwa; M. Suyetin; W. Lewis; E. Bichoutskaia; M. Schroder; A.; N.; Khlobystov'; Chem.Commun. 51 (2015) 648–; doi:10.1039/C4cc08029G

data_7116398
_publ_section_title
;
 Switching intermolecular interactions by confinement in carbon nanotubes
;
_journal_name_full               Chem.Commun.
_journal_page_first              648
_journal_paper_doi               10.1039/C4cc08029G
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C81 H19 N'
_chemical_formula_sum            'C81 H19 N'
_chemical_formula_weight         1005.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.499(2)
_cell_length_b                   27.568(4)
_cell_length_c                   9.7851(15)
_cell_measurement_reflns_used    3026
_cell_measurement_temperature    293
_cell_measurement_theta_max      68.6
_cell_measurement_theta_min      21.5
_cell_volume                     4180.9(10)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 22.2222
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -130.0000 - 50.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 60.0000
                 Phi: 180.0000
                 XTD: 41.0648
              2theta: -39.7919
scan:
    Number of images: 120
               Slice: -130.0000 - -10.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 60.0000
                 Phi: 0.0000
                 XTD: 41.0648
              2theta: -39.7919
scan:
    Number of images: 30
               Slice: -60.0000 - -30.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 50.0000
                 Phi: 135.0000
                 XTD: 41.0648
              2theta: -39.7919
scan:
    Number of images: 180
               Slice: -180.0000 - 0.0000
         Image width: 1.0000
            Exp time: 45.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 50.0000
                 Phi: 135.0000
                 XTD: 41.0648
              2theta: -89.7919
scan:
    Number of images: 180
               Slice: -180.0000 - 0.0000
         Image width: 1.0000
            Exp time: 45.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 60.0000
                 Phi: 180.0000
                 XTD: 41.0648
              2theta: -89.7919
scan:
    Number of images: 180
               Slice: -180.0000 - 0.0000
         Image width: 1.0000
            Exp time: 45.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 60.0000
                 Phi: 315.0000
                 XTD: 41.0648
              2theta: -89.7919
scan:
    Number of images: 180
               Slice: -180.0000 - 0.0000
         Image width: 1.0000
            Exp time: 45.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 20.0000
                 Phi: 135.0000
                 XTD: 41.0648
              2theta: -89.7919
scan:
    Number of images: 180
               Slice: -180.0000 - 0.0000
         Image width: 1.0000
            Exp time: 45.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 60.0000
                 Phi: 225.0000
                 XTD: 41.0648
              2theta: -89.7919
scan:
    Number of images: 150
               Slice: -180.0000 - -30.0000
         Image width: 1.0000
            Exp time: 45.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 30.0000
                 Phi: 225.0000
                 XTD: 41.0648
              2theta: -89.7919
scan:
    Number of images: 105
               Slice: -153.0000 - -48.0000
         Image width: 1.0000
            Exp time: 45.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 60.0000
                 Phi: 0.0000
                 XTD: 41.0648
              2theta: -89.7919
scan:
    Number of images: 39
               Slice: -170.0000 - -131.0000
         Image width: 1.0000
            Exp time: 45.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 60.0000
                 Phi: 45.0000
                 XTD: 41.0648
              2theta: -89.7919
;
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn944+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.064338
_diffrn_orient_matrix_UB_12      0.004441
_diffrn_orient_matrix_UB_13      -0.001886
_diffrn_orient_matrix_UB_21      -0.001018
_diffrn_orient_matrix_UB_22      -0.025638
_diffrn_orient_matrix_UB_23      -0.025640
_diffrn_orient_matrix_UB_31      -0.007083
_diffrn_orient_matrix_UB_32      -0.071952
_diffrn_orient_matrix_UB_33      0.072227
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18720
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.572
_diffrn_reflns_theta_min         3.206
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1683 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0775P)^2^+1.6189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                3755
_reflns_number_total             3786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08029g2.cif
_cod_data_source_block           1
_cod_original_cell_volume        4181.1(11)
_cod_database_code               7116398
_nottingham_internal_coll_name   C60WBQ
_nottingham_internal_coll_number 10919
_nottingham_internal_coll_client WA/ANK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '10, 45'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_date   07/11/2013
_nottingham_internal_coll_location SOTON
_nottingham_internal_ncs_number  2011ncs0496
_nottingham_internal_process_date 09/01/2014
_nottingham_internal_process_user WA
_nottingham_internal_solution_date 9/1/2014
_nottingham_internal_solution_user WA/WL
_nottingham_internal_refinement_date 19/8/2014
_nottingham_internal_refinement_user WA/WL
_nottingham_internal_validation_date 19/8/2014
_nottingham_internal_validation_user WL
_nottingham_internal_archive_date 19/8/2014
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44)
;
_olex2_submission_special_instructions 'No special instructions were received'