#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:13:32 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180417 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/86/7208680.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7208680
loop_
_publ_author_name
'Konar, Anita Dutt'
_publ_section_title
;
 mABA inserted supramolecular triple helix formation in the solid state in
 synthetic tripeptides containing β-cyanoalanine and Aib as corner
 residues
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6689
_journal_paper_doi               10.1039/c2ce25527h
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C21 H28 N4 O6'
_chemical_formula_sum            'C21 H28 N4 O6'
_chemical_formula_weight         432.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   6.0152(11)
_cell_length_b                   12.442(2)
_cell_length_c                   29.838(6)
_cell_measurement_temperature    120(2)
_cell_volume                     2233.1(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.614
_diffrn_measured_fraction_theta_max 0.614
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0765
_diffrn_reflns_av_sigmaI/netI    0.1484
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            4001
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   'Empirical''Bruker SADABS V2.10'
_exptl_absorpt_process_details   'Bruker SADABS V2.10'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.799
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0559
_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/[σ²(Fo²)+(0.0487P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                1628
_reflns_number_total             3136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25527h.txt
_cod_data_source_block           as1f
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7208680
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
H1A H 0.007(11) 0.786(3) 0.1444(14) 0.017(12) Uiso 1 1 d .
H2A H 0.321(11) 0.635(3) 0.1369(12) 0.012(11) Uiso 1 1 d .
O6 O 0.0823(10) 1.1575(2) 0.18337(11) 0.0410(17) Uani 1 1 d .
O1 O 0.3641(8) 0.97301(18) 0.03348(8) 0.0268(12) Uani 1 1 d .
O2 O 0.2671(8) 0.8860(2) 0.09847(9) 0.0331(13) Uani 1 1 d .
N2 N 0.1435(10) 0.6355(2) 0.12233(11) 0.0207(14) Uani 1 1 d .
O3 O -0.0493(8) 0.6895(2) 0.06056(11) 0.0244(12) Uani 1 1 d .
C8 C 0.1286(14) 0.6760(3) 0.08045(14) 0.022(2) Uani 1 1 d .
N1 N 0.3616(9) 0.7957(2) 0.03546(11) 0.0239(14) Uani 1 1 d .
H1 H 0.3854 0.7991 0.0071 0.029 Uiso 1 1 calc R
C10 C 0.0482(11) 0.5564(3) 0.19232(14) 0.030(2) Uani 1 1 d .
H10A H 0.1621 0.5035 0.1878 0.045 Uiso 1 1 calc R
H10B H -0.0685 0.5264 0.2103 0.045 Uiso 1 1 calc R
H10C H 0.1102 0.6178 0.2073 0.045 Uiso 1 1 calc R
O4 O -0.4154(9) 0.6497(3) 0.16459(11) 0.0346(16) Uani 1 1 d .
C5 C 0.3532(11) 0.6936(3) 0.05844(14) 0.0232(17) Uani 1 1 d .
H5 H 0.4695 0.6916 0.0814 0.028 Uiso 1 1 calc R
C17 C -0.2368(13) 1.0556(3) 0.20013(15) 0.029(2) Uani 1 1 d .
N3 N -0.1463(10) 0.7790(3) 0.16150(13) 0.0278(16) Uani 1 1 d .
C4 C 0.3310(11) 0.8856(3) 0.05999(15) 0.0252(18) Uani 1 1 d .
C14 C -0.4564(13) 0.8596(4) 0.20258(15) 0.031(2) Uani 1 1 d .
H14 H -0.5303 0.7940 0.2034 0.038 Uiso 1 1 calc R
C6 C 0.3943(12) 0.6028(3) 0.02446(13) 0.0272(19) Uani 1 1 d .
H6A H 0.2844 0.6070 0.0007 0.033 Uiso 1 1 calc R
H6B H 0.5400 0.6118 0.0111 0.033 Uiso 1 1 calc R
O5 O -0.2129(11) 1.2441(2) 0.21226(12) 0.065(2) Uani 1 1 d .
C7 C 0.3811(12) 0.4969(3) 0.04615(14) 0.0260(18) Uani 1 1 d .
C13 C -0.2545(12) 0.8675(3) 0.18094(14) 0.0220(17) Uani 1 1 d .
C19 C -0.1264(15) 1.1618(3) 0.19925(16) 0.031(2) Uani 1 1 d .
C12 C -0.2223(14) 0.6754(4) 0.15728(15) 0.026(2) Uani 1 1 d .
C11 C -0.1460(13) 0.4956(3) 0.12195(15) 0.033(2) Uani 1 1 d .
H11A H -0.2155 0.5202 0.0949 0.049 Uiso 1 1 calc R
H11B H -0.2548 0.4612 0.1406 0.049 Uiso 1 1 calc R
H11C H -0.0304 0.4453 0.1147 0.049 Uiso 1 1 calc R
C18 C -0.1430(11) 0.9660(3) 0.17914(13) 0.0244(17) Uani 1 1 d .
H18 H -0.0079 0.9718 0.1642 0.029 Uiso 1 1 calc R
C9 C -0.0466(11) 0.5910(3) 0.14681(14) 0.0184(18) Uani 1 1 d .
C16 C -0.4433(13) 1.0476(4) 0.22162(16) 0.032(2) Uani 1 1 d .
H16 H -0.5076 1.1080 0.2347 0.039 Uiso 1 1 calc R
N7 N 0.3710(10) 0.4156(3) 0.06392(13) 0.0388(18) Uani 1 1 d .
C3 C 0.4148(13) 1.1516(3) 0.01246(14) 0.037(2) Uani 1 1 d .
H3A H 0.5616 1.1300 0.0036 0.056 Uiso 1 1 calc R
H3B H 0.4166 1.2259 0.0210 0.056 Uiso 1 1 calc R
H3C H 0.3141 1.1417 -0.0122 0.056 Uiso 1 1 calc R
C15 C -0.5509(13) 0.9496(4) 0.22332(16) 0.042(2) Uani 1 1 d .
H15 H -0.6861 0.9434 0.2382 0.050 Uiso 1 1 calc R
C28 C 0.3394(13) 1.0838(3) 0.05187(14) 0.027(2) Uani 1 1 d .
C2 C 0.4986(12) 1.0977(3) 0.09147(17) 0.035(2) Uani 1 1 d .
H2B H 0.4404 1.0606 0.1171 0.053 Uiso 1 1 calc R
H2C H 0.5140 1.1727 0.0983 0.053 Uiso 1 1 calc R
H2D H 0.6413 1.0684 0.0838 0.053 Uiso 1 1 calc R
C20 C 0.2025(14) 1.2573(3) 0.18236(17) 0.056(3) Uani 1 1 d .
H20A H 0.1304 1.3062 0.1621 0.084 Uiso 1 1 calc R
H20B H 0.3519 1.2445 0.1724 0.084 Uiso 1 1 calc R
H20C H 0.2053 1.2880 0.2119 0.084 Uiso 1 1 calc R
C1 C 0.1029(13) 1.1056(3) 0.06451(15) 0.0292(19) Uani 1 1 d .
H1B H 0.0082 1.0913 0.0393 0.044 Uiso 1 1 calc R
H1C H 0.0875 1.1794 0.0733 0.044 Uiso 1 1 calc R
H1D H 0.0612 1.0599 0.0891 0.044 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C19 O6 C20 116.3(4)
C4 O1 C28 120.7(3)
C8 N2 C9 123.4(6)
O3 C8 N2 123.6(7)
O3 C8 C5 122.9(4)
N2 C8 C5 113.3(6)
C4 N1 C5 117.8(3)
N1 C5 C8 111.3(4)
N1 C5 C6 109.1(3)
C8 C5 C6 108.8(4)
C18 C17 C16 120.4(5)
C18 C17 C19 121.6(6)
C16 C17 C19 118.0(5)
C12 N3 C13 128.3(6)
O2 C4 N1 124.1(4)
O2 C4 O1 126.5(4)
N1 C4 O1 109.1(4)
C13 C14 C15 120.6(6)
C7 C6 C5 111.1(3)
N7 C7 C6 178.5(4)
C14 C13 C18 120.2(5)
C14 C13 N3 123.1(5)
C18 C13 N3 116.7(6)
O5 C19 O6 123.2(6)
O5 C19 C17 123.8(7)
O6 C19 C17 113.0(5)
O4 C12 N3 123.0(6)
O4 C12 C9 121.0(5)
N3 C12 C9 115.8(7)
C13 C18 C17 119.2(6)
N2 C9 C11 111.0(4)
N2 C9 C12 112.5(4)
C11 C9 C12 111.4(5)
N2 C9 C10 104.9(5)
C11 C9 C10 111.1(3)
C12 C9 C10 105.6(4)
C15 C16 C17 119.6(5)
C16 C15 C14 120.0(7)
O1 C28 C1 110.8(4)
O1 C28 C3 101.5(3)
C1 C28 C3 112.3(5)
O1 C28 C2 109.0(4)
C1 C28 C2 112.3(4)
C3 C28 C2 110.4(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O6 C19 1.343(9)
O6 C20 1.437(7)
O1 C4 1.359(4)
O1 C28 1.491(4)
O2 C4 1.211(5)
N2 C8 1.350(5)
N2 C9 1.466(7)
O3 C8 1.235(8)
C8 C5 1.518(9)
N1 C4 1.349(5)
N1 C5 1.445(4)
C10 C9 1.534(6)
O4 C12 1.224(8)
C5 C6 1.538(5)
C17 C18 1.398(6)
C17 C16 1.402(10)
C17 C19 1.479(7)
N3 C12 1.374(6)
N3 C13 1.404(6)
C14 C13 1.379(9)
C14 C15 1.400(7)
C6 C7 1.470(5)
O5 C19 1.212(6)
C7 N7 1.144(5)
C13 C18 1.398(7)
C12 C9 1.523(8)
C11 C9 1.521(6)
C16 C15 1.382(8)
C3 C28 1.517(6)
C28 C1 1.497(9)
C28 C2 1.531(8)
