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_4113790
_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 H121 N3 O5'
_chemical_formula_weight         1649.17
_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                97.097(7)
_cell_angle_beta                 100.914(7)
_cell_angle_gamma                112.715(5)
_cell_formula_units_Z            2
_cell_length_a                   14.493(4)
_cell_length_b                   17.862(5)
_cell_length_c                   20.588(6)
_cell_measurement_reflns_used    1934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2.35
_cell_volume                     4712(2)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'SMART (Bruker-AXS)'
_computing_data_reduction        'SAINT (Bruker-AXS)'
_computing_molecular_graphics
;
PLUTON (Spek)
ORTEP for Windows (Farrugia, 1997)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 92 ( A. Altomare, et al.,1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1712
_diffrn_reflns_av_sigmaI/netI    0.1793
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31122
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.070
_exptl_crystal_colour            'pale Yellow'
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       platelett
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0011(3)
_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   1.428
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         12331
_refine_ls_number_restraints     343
_refine_ls_restrained_S_all      1.452
_refine_ls_R_factor_all          0.3139
_refine_ls_R_factor_gt           0.1274
_refine_ls_shift/su_max          1.013
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2463
_refine_ls_wR_factor_ref         0.2748
_reflns_number_gt                3097
_reflns_number_total             12331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034029psi20030328_022017.cif
_cod_data_source_block           grava
_cod_database_code               4113790