Dynamic Equilibrium of a Supramolecular Dimeric Rhomboid and Trimeric Hexagon and Determination of Its Thermodynamic Constants
Takuya Yamamoto; Atta M. Arif; Peter J. Stang; Journal of the American Chemical Society 125 (2003) 12309–12317; doi:10.1021/ja0302984

data_4114216
_publ_section_title
;
 Dynamic Equilibrium of a Supramolecular Dimeric Rhomboid and Trimeric
 Hexagon and Determination of Its Thermodynamic Constants
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12309
_journal_page_last               12317
_journal_paper_doi               10.1021/ja0302984
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C19 H11 N3'
_chemical_formula_weight         281.31
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.6781(26)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   34.5261(22)
_cell_length_b                   6.0759(4)
_cell_length_c                   10.5382(9)
_cell_measurement_reflns_used    2924
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      1.018
_cell_volume                     2164.9(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi plus Omega scan'
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.1022
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5692
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.9969
_exptl_absorpt_correction_T_min  0.9692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(5)
_refine_ls_extinction_coef       0.0067(10)
_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   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3536
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0360P)^2^+2.5111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                2477
_reflns_number_total             3536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0302984_1.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4114216