Selective Formylation of Azacalixpyridine Macrocycles and Their Transformation to Molecular Semicages.
Ren, Wen-Sheng; Zhao, Liang; Wang, Mei-Xiang; The Journal of organic chemistry 80 (2015) 9272–9278; doi:10.1021/acs.joc.5b01722

data_4036358
_publ_section_title
;
 Selective Formylation of Azacalixpyridine Macrocycles and Their
 Transformation to Molecular Semicages.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9272
_journal_page_last               9278
_journal_paper_doi               10.1021/acs.joc.5b01722
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C28 H24 N8 O4, C H Cl3'
_chemical_formula_sum            'C29 H25 Cl3 N8 O4'
_chemical_formula_weight         655.92
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                82.779(12)
_cell_angle_beta                 83.587(14)
_cell_angle_gamma                81.730(11)
_cell_formula_units_Z            2
_cell_length_a                   9.641(3)
_cell_length_b                   11.263(4)
_cell_length_c                   13.731(5)
_cell_measurement_reflns_used    5244
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.24
_cell_volume                     1457.1(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 ver 1.1'
_computing_publication_material  'SHELX97 (Sheldrick, 2008)'
_computing_structure_refinement  'Olex2 ver 1.1'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19278
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6656
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+1.0438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                6087
_reflns_number_total             6656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b01722_si_004.cif
_cod_data_source_block           sa2784
_cod_original_cell_volume        1457.0(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4036358