Synthesis and structural analysis of dehydrophenylalanine cyclophanes
Gibson (née Thomas), Susan E.; Jones, Jerome O.; Kalindjian, S. Barret; Knight, Jamie D.; Steed, Jonathan W.; Tozer, Matthew J.; Chemical Communications  (2002) 1938–; doi:10.1039/b205752m

data_7114503
_publ_section_title
;
 Synthesis and structural analysis of dehydrophenylalanine cyclophanes
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1938
_journal_paper_doi               10.1039/b205752m
_journal_year                    2002
_chemical_formula_sum            'C52 H78.1 Cl3.9 N2 O8.7'
_chemical_formula_weight         1008.72
_chemical_name_systematic        ?
_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                101.52(4)
_cell_angle_beta                 91.999(4)
_cell_angle_gamma                113.079(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1987(4)
_cell_length_b                   8.8260(6)
_cell_length_c                   20.8707(13)
_cell_measurement_temperature    100(2)
_cell_volume                     1350.6(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_sigmaI/netI    0.1472
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7441
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9737
_exptl_absorpt_correction_T_min  0.9484
_exptl_absorpt_correction_type   Scalepack
_exptl_absorpt_process_details   'Otwinowski & Minor, 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.011(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4708
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1836
_refine_ls_R_factor_gt           0.1299
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+10.5529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2724
_refine_ls_wR_factor_ref         0.2976
_reflns_number_gt                3141
_reflns_number_total             4708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205752m.txt
_cod_data_source_block           jk150a
_cod_original_cell_volume        1350.58(14)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52 H78.10 Cl3.90 N2 O8.70'
_cod_database_code               7114503