Shape-Persistant Macrocycles with Terpyridine Units: Synthesis, Characterization, and Structure in the Crystal
Christian Grave; Dieter Lentz; Andreas Schäfer; Paolo Samorì; Jürgen P. Rabe; Peter Franke; A. Dieter Schlüter; Journal of the American Chemical Society 125 (2003) 6907–6918; doi:10.1021/ja034029p

data_4113788
_publ_section_title
;
 Shape-Persistant Macrocycles with Terpyridine Units: Synthesis,
 Characterization, and Structure in the Crystal
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6907
_journal_page_last               6918
_journal_paper_doi               10.1021/ja034029p
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C117 H115 N3 O5'
_chemical_formula_weight         1643.12
_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                107.173(2)
_cell_angle_beta                 105.122(2)
_cell_angle_gamma                93.121(3)
_cell_formula_units_Z            2
_cell_length_a                   14.6610(16)
_cell_length_b                   14.9087(16)
_cell_length_c                   23.734(3)
_cell_measurement_reflns_used    3484
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      2.6
_cell_volume                     4735.9(9)
_computing_cell_refinement       'SAINT (BRUKER AXS)'
_computing_data_collection       'SMART (BRUKER AXS)'
_computing_data_reduction        'SAINT (BRUKER AXS)'
_computing_molecular_graphics    'ORTEP for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR 92 (Altomare, A.; Cascarano, G.; Giacovazzo, C.; Guagliardi, 1993)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'BRUKER AXS SMART 1000 CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.102
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            36482
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         12205
_refine_ls_number_restraints     1164
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1617
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          5.391
_refine_ls_shift/su_mean         0.045
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2869
_reflns_number_gt                5840
_reflns_number_total             12205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034029psi20030328_021920.cif
_cod_data_source_block           1grave
_cod_database_code               4113788