Hydrazide-Based Quadruply Hydrogen-Bonded Heterodimers. Structure, Assembling Selectivity, and Supramolecular Substitution
Xin Zhao; Xiao-Zhong Wang; Xi-Kui Jiang; Ying-Qi Chen; Zhan-Ting Li; Guang-Ju Chen; Journal of the American Chemical Society 125 (2003) 15128–15139; doi:10.1021/ja037312x

data_4114463
_publ_section_title
;
 Hydrazide-Based Quadruply Hydrogen-Bonded Heterodimers. Structure,
 Assembling Selectivity, and Supramolecular Substitution
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15128
_journal_page_last               15139
_journal_paper_doi               10.1021/ja037312x
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C31 H46 N4 O5'
_chemical_formula_weight         554.72
_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                76.966(3)
_cell_angle_beta                 78.834(3)
_cell_angle_gamma                74.785(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3928(13)
_cell_length_b                   9.5527(14)
_cell_length_c                   18.941(3)
_cell_measurement_reflns_used    653
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.619
_cell_measurement_theta_min      4.764
_cell_volume                     1581.3(4)
_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 0.891
_diffrn_measured_fraction_theta_max 0.891
_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  0.0975
_diffrn_reflns_av_sigmaI/netI    0.2407
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9677
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76895
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0007(9)
_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   0.662
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6982
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.745
_refine_ls_R_factor_all          0.2172
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                1674
_reflns_number_total             6982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037312xsi20031001_114700.cif
_cod_data_source_block           cd22325
_cod_database_code               4114463