Hünlich base: (re)discovery, synthesis, and structure elucidation after a century.
Rigol, Stephan; Beyer, Lothar; Hennig, Lothar; Sieler, Joachim; Giannis, Athanassios; Organic letters 15 (2013) 1418–1420; doi:10.1021/ol400357t

data_1556146
_publ_section_title
;
 H\"unlich base: (re)discovery, synthesis, and structure elucidation after
 a century.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1418
_journal_page_last               1420
_journal_paper_doi               10.1021/ol400357t
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C17 H20 N4, 3(H2 O1)'
_chemical_formula_sum            'C17 H26 N4 O3'
_chemical_formula_weight         334.42
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C c c 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.754(3)
_cell_length_b                   22.060(4)
_cell_length_c                   5.1460(10)
_cell_measurement_reflns_used    584
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1674.9(6)
_computing_cell_refinement       'IPDS1 software /Fa.STOE)'
_computing_data_collection       'IPDS1 software /Fa.STOE)'
_computing_data_reduction        'IPDS1 software /Fa.STOE)'
_computing_molecular_graphics    'Ortep3 for Windows  (L.J. Farrujia)'
_computing_publication_material  'WINGX (L.J.Farrugia)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  PDS1(Fa.STOE)
_diffrn_measurement_method       Omega-sans
_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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3871
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.9728
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1869
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                1124
_reflns_number_total             1869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol400357t_si_002.cif
_cod_data_source_block           ip1_1540
_cod_original_sg_symbol_H-M      Ccc2
_cod_database_code               1556146