Synthesis of a naphthalenediimide-based cyclophane for controlling anion–arene interactions
Li, Yongjun; Zhao, Yingjie; Jiang, Runsheng; Liu, Huibiao; Li, Yuliang; Inorg. Chem. Front. 1 (2014) 661–; doi:10.1039/C4QI00095A

data_4348265
_publ_section_title
;
 Synthesis of a naphthalenediimide-based cyclophane for controlling
 anion--arene interactions
;
_journal_issue                   9
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              661
_journal_paper_doi               10.1039/C4QI00095A
_journal_volume                  1
_journal_year                    2014
_chemical_formula_moiety         'C36 H28 N8 O4, 2(F6 P), 3(C2 H3 N)'
_chemical_formula_sum            'C42 H37 F12 N11 O4 P2'
_chemical_formula_weight         1049.77
_chemical_name_systematic        nabp-Me22+2PF6
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.173(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.697(2)
_cell_length_b                   23.188(3)
_cell_length_c                   14.177(2)
_cell_measurement_reflns_used    727
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.17
_cell_volume                     4484.4(11)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30215
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.9301
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ether, dichloromethane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         7890
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+5.7138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.1939
_reflns_number_gt                7481
_reflns_number_total             7890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00095a2.cif
_cod_data_source_block           sa742
_cod_original_cell_volume        4484.3(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4348265