Cofacial Organic Click Cage to Intercalate Polycyclic Aromatic Hydrocarbons.
Samanta, Jayanta; Natarajan, Ramalingam; Organic letters 18 (2016) 3394–3397; doi:10.1021/acs.orglett.6b01554

data_1555615
_publ_section_title
;
 Cofacial Organic Click Cage to Intercalate Polycyclic Aromatic
 Hydrocarbons.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3394
_journal_page_last               3397
_journal_paper_doi               10.1021/acs.orglett.6b01554
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C54 H39 N15 O3, C14 H10, 3.5(C H Cl3)'
_chemical_formula_sum            'C71.5 H52.5 Cl10.5 N15 O3'
_chemical_formula_weight         1542.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.96(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.420(14)
_cell_length_b                   13.581(11)
_cell_length_c                   32.38(3)
_cell_measurement_reflns_used    4786
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.78
_cell_measurement_theta_min      2.47
_cell_volume                     7211(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1310
_diffrn_reflns_av_unetI/netI     0.2414
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            55200
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.426
_diffrn_reflns_theta_min         1.363
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1160 before and 0.0770 after correction.
The Ratio of minimum to maximum transmission is 0.8653.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         15592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.2592
_refine_ls_R_factor_gt           0.0853
_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^)+(0.1386P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2148
_refine_ls_wR_factor_ref         0.2908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4594
_reflns_number_total             15592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01554_si_005.cif
_cod_data_source_block           rn_js_200_an_0m_a
_cod_original_cell_volume        7210(10)
_cod_original_formula_sum        'C71.50 H52.50 Cl10.50 N15 O3'
_cod_database_code               1555615
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) Cl3(0.5) C1(0.5) H1(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C1(H1), C1(H1), C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C17(H17A,H17B), C24(H24A,H24B), C34(H34A,H34B), C43(H43A,
 H43B), C52(H52A,H52B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15), C16(H16),
 C19(H19), C20(H20), C22(H22), C23(H23), C29(H29), C30(H30), C32(H32), C33(H33),
  C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C45(H45), C47(H47),
 C48(H48), C50(H50), C51(H51), C54(H54), C1(H1), C2(H2), C3(H3), C6(H6), C7(H7),
  C8(H8), C10(H10), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              62090
_shelx_hkl_checksum              92500
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'