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_4036359
_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 H26 N6 O2'
_chemical_formula_sum            'C30 H26 N4 O2'
_chemical_formula_weight         474.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
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Olex2 1.2
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_cell_length_c                   13.7280(14)
_cell_measurement_reflns_used    1240
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      25.4870
_cell_measurement_theta_min      3.5670
_cell_volume                     1184.8(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
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  1 omega  -56.00   39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -57.0000  150.0000 95

  2 omega  -12.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017   57.0000  -60.0000 93

  3 omega  -20.00   53.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -99.0000   60.0000 73
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0527441000
_diffrn_orient_matrix_UB_12      0.0276679000
_diffrn_orient_matrix_UB_13      0.0364455000
_diffrn_orient_matrix_UB_21      -0.0520856000
_diffrn_orient_matrix_UB_22      -0.0033748000
_diffrn_orient_matrix_UB_23      -0.0405927000
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_diffrn_orient_matrix_UB_33      -0.0022194000
_diffrn_radiation_monochromator  mirror
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_diffrn_reflns_limit_l_max       14
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_diffrn_reflns_number            7027
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_diffrn_source                   'SuperNova (Mo) X-ray Source'
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour
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_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description
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_exptl_crystal_F_000             500
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.0279P] where P=(Fo^2^+2Fc^2^)/3'
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_cod_data_source_block           exp_5525
_cod_database_code               4036359
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C28H26N6O2
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_reflns_odcompleteness_iscentric 1
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C24(H24), C20(H20), C19(H19), C10(H10), C26(H26), C7(H7), C29(H29),
 C30(H30), C32(H32), C28(H28), C31(H31), C33(H33), C21(H21)
2.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C23(H23A,H23B,
 H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'