Synthesis of a photoresponsive cryptand and its complexations with paraquat and 2,7-diazapyrenium.
Xu, Jiang-Fei; Chen, Yu-Zhe; Wu, Li-Zhu; Tung, Chen-Ho; Yang, Qing-Zheng; Organic letters 16 (2014) 684–687; doi:10.1021/ol403343s

data_1513495
_publ_section_title
;
 Synthesis of a photoresponsive cryptand and its complexations with
 paraquat and 2,7-diazapyrenium.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              684
_journal_page_last               687
_journal_paper_doi               10.1021/ol403343s
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C64 H76 F12 N4 O12 P2'
_chemical_formula_weight         1383.23
_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                98.940(3)
_cell_angle_beta                 99.394(3)
_cell_angle_gamma                105.091(2)
_cell_formula_units_Z            2
_cell_length_a                   11.875(3)
_cell_length_b                   12.513(3)
_cell_length_c                   23.689(5)
_cell_measurement_reflns_used    10317
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4784
_cell_measurement_theta_min      1.7232
_cell_volume                     3279.9(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
;
 Mercury: visualization and analysis of crystal structures, C. F. Macrae,
 P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
 M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43795
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         14976
_refine_ls_number_restraints     888
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+3.5411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2022
_reflns_number_gt                12108
_reflns_number_total             14976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol403343s_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        3279.7(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1513495