New 2+2, 3+3 and 4+4 macrocycles derived from 1,2-diaminocyclohexane and 2,6-diformylpyridine.
Gregoliński, Janusz; Lisowski, Jerzy; Lis, Tadeusz; Organic & biomolecular chemistry 3 (2005) 3161–3166; doi:10.1039/b505909g

data_7150197
_publ_section_title
;
 New 2+2, 3+3 and 4+4 macrocycles derived from 1,2-diaminocyclohexane
 and 2,6-diformylpyridine.
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3161
_journal_page_last               3166
_journal_paper_doi               10.1039/b505909g
_journal_volume                  3
_journal_year                    2005
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C52 H60 N12'
_chemical_formula_sum            'C52 H60 N12'
_chemical_formula_weight         853.13
_chemical_melting_point          340
_chemical_name_common            imine
_chemical_name_systematic
;
8(R),13(R),23(S),28(S),38(R),43(R),53(S),58(S)-
7,14,22,29,37,44,52,59,61,62,63,64-dodecaazananocyclo
[55.3.1.1^16,20^.1^31,35^.1^46,50^.0^8,13^.0^23,28^.0^38,43^.0^53,58^]
-tetrahexaconta-
1(61),2,4,6,14,16(62),17,19,21,29,31(63),32,34,44,46(64),47,49,51,59
-eicosaene
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            2
_cell_length_a                   15.577(4)
_cell_length_b                   30.563(9)
_cell_length_c                   5.460(3)
_cell_measurement_reflns_used    6668
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     2599.4(18)
_computing_cell_refinement       'CrysAlis Red (Oxford Diffraction, 1995-2003)'
_computing_data_collection       'CrysAlis Red (Oxford Diffraction, 1995-2003)'
_computing_data_reduction        'CrysAlis Red (Oxford Diffraction, 1995-2003)'
_computing_molecular_graphics    'XP (Bruker, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type
'Xcalibur PX \k-geometry diffractometer CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_sigmaI/netI    0.0923
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            16367
_diffrn_reflns_theta_full        76.03
_diffrn_reflns_theta_max         76.03
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   'CrysAlis Red (Oxford Diffraction, 1995-2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillars
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(9)
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0860P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                2357
_reflns_number_total             4441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b505909g.txt
_cod_data_source_block           tekst
_cod_original_sg_symbol_H-M      P21212
_cod_database_code               7150197