Synthesis, characterization, and catalytic reactivity of a highly basic macrotricyclic aminopyridine.
Uchida, Natsuko; Taketoshi, Ayako; Kuwabara, Junpei; Yamamoto, Toshihide; Inoue, Yoshiaki; Watanabe, Yu; Kanbara, Takaki; Organic letters 12 (2010) 5242–5245; doi:10.1021/ol102236f

data_1503289
_publ_section_title
;
 Synthesis, characterization, and catalytic reactivity of a highly basic
 macrotricyclic aminopyridine.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5242
_journal_page_last               5245
_journal_paper_doi               10.1021/ol102236f
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C50 H56 Br Cl4 N9 '
_chemical_formula_sum            'C50 H56 Br Cl4 N9'
_chemical_formula_weight         1004.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.958(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.3682(14)
_cell_length_b                   16.537(2)
_cell_length_c                   28.698(4)
_cell_measurement_reflns_used    4391
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.42
_cell_volume                     4919.8(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            27172
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2088.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.11
_refine_diff_density_min         -1.99
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.361
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     573
_refine_ls_number_reflns         10767
_refine_ls_R_factor_gt           0.1019
_refine_ls_shift/su_max          0.0040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3464
_reflns_number_gt                6862
_reflns_number_total             10767
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol102236f_si_002.cif
_cod_data_source_block           '_ucd312b'
_cod_original_cell_volume        4919.9(12)
_cod_original_formula_sum        'C50 H56 Br Cl4 N9 '
_cod_database_code               1503289