AAAA-DDDD Quadruple Hydrogen-Bond Arrays Featuring NH...N and CH...N Hydrogen Bonds
David A. Leigh; Craig C. Robertson; Alexandra M. Z. Slawin; Patrick I. T. Thomson; Journal of the American Chemical Society 135 (2013) 9939–9943; doi:10.1021/ja404504m

data_4120052
_publ_section_title
;
 AAAA-DDDD Quadruple Hydrogen-Bond Arrays Featuring NH...N and CH...N
 Hydrogen Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9939
_journal_page_last               9943
_journal_paper_doi               10.1021/ja404504m
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'C30 H28  N4,C15 H14 N7,C32 H12 B F24,0.25(C H4 O)'
_chemical_formula_sum            'C77.25 H55 B F24 N11 O0.25'
_chemical_formula_weight         1608.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.749(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.156(3)
_cell_length_b                   32.885(11)
_cell_length_c                   27.081(9)
_cell_measurement_reflns_used    4156
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.4
_cell_measurement_theta_min      21.3
_cell_volume                     8145(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.2520
_diffrn_reflns_av_sigmaI/netI    0.1190
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            107989
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.69
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3274
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.584
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1062
_refine_ls_number_reflns         14892
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.579
_refine_ls_R_factor_all          0.2981
_refine_ls_R_factor_gt           0.2181
_refine_ls_shift/su_max          0.163
_refine_ls_shift/su_mean         0.009
_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          0.4941
_refine_ls_wR_factor_ref         0.5297
_reflns_number_gt                7781
_reflns_number_total             14892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404504m_si_002.cif
_cod_data_source_block           5.4
_cod_database_code               4120052