Hydrogen Bonding-Directed Multicomponent Dynamic Covalent Assembly of Mono- and Bimacrocycles. Self-Sorting and Macrocycle Exchange
Jian-Bin Lin; Xiao-Na Xu; Xi-Kui Jiang; Zhan-Ting Li; Journal of Organic Chemistry 73 (2008) 9403–9410; doi:10.1021/jo801972s

data_4023910
_publ_section_title
;
 Hydrogen Bonding-Directed Multicomponent Dynamic Covalent Assembly
 of Mono- and Bimacrocycles. Self-Sorting and Macrocycle Exchange
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9403
_journal_page_last               9410
_journal_paper_doi               10.1021/jo801972s
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C36 H50 N4 O6'
_chemical_formula_weight         634.80
_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                67.745(2)
_cell_angle_beta                 71.964(2)
_cell_angle_gamma                80.985(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5622(13)
_cell_length_b                   12.7845(14)
_cell_length_c                   13.3244(15)
_cell_measurement_reflns_used    1921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.038
_cell_measurement_theta_min      4.948
_cell_volume                     1731.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9138
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78435
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.427
_exptl_crystal_size_min          0.192
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0017(12)
_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   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6328
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1897
_reflns_number_gt                3461
_reflns_number_total             6328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo801972s_si_001_2.cif
_cod_data_source_block           cd2757
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4023910