AAA-DDD Triple Hydrogen Bond Complexes
Barry A. Blight; Amaya Camara-Campos; Smilja Djurdjevic; Martin Kaller; David A. Leigh; Fiona M. McMillan; Hamish McNab; Alexandra M. Z. Slawin; Journal of the American Chemical Society 131 (2009) 14116–14122; doi:10.1021/ja906061v

data_4105089
_publ_section_title
;
 AAA-DDD Triple Hydrogen Bond Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14116
_journal_page_last               14122
_journal_paper_doi               10.1021/ja906061v
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety
'3[(C19 H11 N3),(C5 H8 N3),(C24 H20 B)],5(C2 H3 N)'
_chemical_formula_sum            'C154 H132 B3 N23'
_chemical_formula_weight         2337.26
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 99.372(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   36.323(12)
_cell_length_b                   10.166(3)
_cell_length_c                   34.552(10)
_cell_measurement_reflns_used    5121
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.3933
_cell_measurement_theta_min      21.3413
_cell_volume                     12588(7)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            79150
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.26
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4928
_exptl_crystal_size_max          0.1500
_exptl_crystal_size_mid          0.0500
_exptl_crystal_size_min          0.0500
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(5)
_refine_ls_extinction_coef       0.00087(7)
_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   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1643
_refine_ls_number_reflns         21718
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0884
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2417
_refine_ls_wR_factor_ref         0.2881
_reflns_number_gt                16054
_reflns_number_total             21718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906061v_si_002.cif
_cod_data_source_block           6.10
_cod_original_cell_volume        12588(6)
_cod_database_code               4105089