#------------------------------------------------------------------------------
#$Date: 2019-07-09 10:59:47 +0300 (Tue, 09 Jul 2019) $
#$Revision: 216877 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552059.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_1552059
loop_
_publ_author_name
'C. Marti-Gastaldo'
'D. Antypov'
'J. E. Warren'
'M. E. Briggs'
'P. A. Chater'
'P. V. Wiper'
'G. J. Miller'
'Y. Z. Khimyak'
'G. R. Darling'
'N. G. Berry'
'M. J. Rosseinsky'
_publ_section_title
;
 Side-chain control of porosity closure in single- and
 multiple-peptide-based porous materials by cooperative folding
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              343
_journal_page_last               351
_journal_paper_doi               10.1038/nchem.1871
_journal_volume                  6
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.5(C21 H36 N8 O13 Zn2), C O, 0.5(O)'
_chemical_formula_sum            'C11.5 H18 N4 O8 Zn'
_chemical_formula_weight         405.67
_chemical_name_systematic        'Zn[(GlyAla)0.5(GlyThr)0.5]2 H2O MeOH'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6542(6)
_cell_length_b                   14.8585(6)
_cell_length_c                   4.7251(2)
_cell_measurement_temperature    100.15
_cell_volume                     958.63(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
Bruker SAINT (Bruker, 2008)'
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            17834
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.05
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1120 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.6587.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             418
_exptl_crystal_recrystallization_method
'Crystallised directly from synthesis reaction in methanol.'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.813
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2798
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0478
_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/[σ²(Fo²)+(0.0875P)²+0.6298P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                2613
_reflns_number_total             2798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.1871-s4.cif
_cod_data_source_block           b00122-sr
_cod_original_formula_sum        'C11.50 H18 N4 O8 Zn'
_cod_database_code               1552059
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N5-H5A = N5-H5B
 0.91 with sigma of 0.02
 C14-O15
 1.43 with sigma of 0.02
 C8-O10
 1.43 with sigma of 0.02
 C7-C9 = C7-C8 = C8-C11
 1.52 with sigma of 0.02
 H5A-H5B
 1.45 with sigma of 0.04
 C4-H5A = C4-H5B
 1.95 with sigma of 0.04
 C7-O10
 2.4 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O10) = Uanis(C11)
4. Others
 Fixed Sof: H7B(0.5) H7A(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) O10(0.25)
 H10(0.25) C8(0.5) H8(0.5) C11(0.25) H11A(0.25) H11B(0.25) H11C(0.25) O15(0.5)
 C14(0.5) O16(0.25)
5.a Riding coordinates:
 O10(H10)
5.b Ternary CH refined with riding coordinates:
 C7(H7B), C7(H7A), C8(H8)
5.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
5.d Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
5.e Aromatic/amide H refined with riding coordinates:
 N6(H6)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z'
3 'x+1/2, -y+1/2, -z'
4 '-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.0000 0.5000 0.39567(8) 0.02271(14) Uani 1 2 d S . 1
O12 O 0.8662(3) 0.6429(4) 0.3637(10) 0.0908(19) Uani 1 1 d . . 2
C7 C 0.7547(3) 0.6215(2) 0.7541(8) 0.0386(8) Uani 1 1 d D . .
H7B H 0.7705 0.6277 0.9598 0.046 Uiso 0.50 1 calc PR A 2
H7A H 0.7793 0.6383 0.9463 0.046 Uiso 0.50 1 calc PR A 1
C3 C 0.6708(3) 0.7661(2) 0.8079(7) 0.0373(8) Uani 1 1 d . . .
N6 N 0.7081(2) 0.70269(19) 0.6441(6) 0.0322(6) Uani 1 1 d . B .
H6 H 0.7046 0.7098 0.4595 0.039 Uiso 1 1 calc R . .
O2 O 0.6712(4) 0.7632(3) 1.0681(6) 0.0832(16) Uani 1 1 d U B .
C9 C 0.6834(12) 0.5401(9) 0.700(3) 0.045(3) Uani 0.50 1 d PD B 2
H9A H 0.7136 0.4845 0.7689 0.067 Uiso 0.50 1 calc PR B 2
H9B H 0.6705 0.5348 0.4966 0.067 Uiso 0.50 1 calc PR B 2
H9C H 0.6216 0.5504 0.8005 0.067 Uiso 0.50 1 calc PR B 2
O10 O 0.7377(8) 0.4742(8) 0.934(3) 0.054(3) Uani 0.25 1 d PDU B 1
H10 H 0.7359 0.4278 0.8329 0.082 Uiso 0.25 1 d PR B 1
C4 C 0.6251(3) 0.8448(2) 0.6520(8) 0.0324(7) Uani 1 1 d D B .
H4A H 0.6776 0.8791 0.5561 0.039 Uiso 1 1 calc R . .
H4B H 0.5806 0.8211 0.5040 0.039 Uiso 1 1 calc R . .
N5 N 0.5701(2) 0.90575(17) 0.8338(6) 0.0268(5) Uani 1 1 d D . .
C1 C 0.8460(3) 0.6004(2) 0.5815(7) 0.0340(7) Uani 1 1 d . . .
O13 O 0.9017(2) 0.53998(18) 0.6786(6) 0.0413(6) Uani 1 1 d . . .
C8 C 0.6848(13) 0.5426(11) 0.803(4) 0.060(5) Uani 0.50 1 d PD B 1
H8 H 0.6306 0.5623 0.9314 0.072 Uiso 0.50 1 calc PR B 1
H5A H 0.521(2) 0.877(2) 0.916(8) 0.037(12) Uiso 1 1 d D . .
H5B H 0.613(3) 0.932(4) 0.945(11) 0.11(3) Uiso 1 1 d D . .
C11 C 0.6432(13) 0.5234(11) 0.510(4) 0.054(3) Uani 0.25 1 d PD B 1
H11A H 0.6131 0.5781 0.4346 0.082 Uiso 0.25 1 calc PR B 1
H11B H 0.5938 0.4758 0.5239 0.082 Uiso 0.25 1 calc PR B 1
H11C H 0.6961 0.5038 0.3843 0.082 Uiso 0.25 1 calc PR B 1
O15 O 0.5650(6) 0.3260(6) 1.137(2) 0.075(2) Uiso 0.50 1 d PD C 1
C14 C 0.5605(10) 0.2556(9) 0.950(3) 0.077(3) Uiso 0.50 1 d PD C 1
O16 O 0.6077(15) 0.3257(14) 0.898(5) 0.086(5) Uiso 0.25 1 d P . .
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'
Zn Zn 0.2839 1.4301 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N5 Zn1 N5 114.83(15) 4_646 3_566
O13 Zn1 N5 118.43(11) . 3_566
O13 Zn1 N5 104.43(12) 2_765 3_566
O13 Zn1 N5 104.43(12) . 4_646
O13 Zn1 N5 118.43(11) 2_765 4_646
O13 Zn1 O13 95.34(17) 2_765 .
H7B C7 H7A 11.9 . .
N6 C7 H7B 111.3 . .
N6 C7 H7A 105.3 . .
N6 C7 C9 107.9(7) . .
N6 C7 C1 109.7(3) . .
N6 C7 C8 114.5(7) . .
C9 C7 H7B 111.3 . .
C9 C7 H7A 123.2 . .
C1 C7 H7B 111.3 . .
C1 C7 H7A 105.3 . .
C1 C7 C9 105.2(7) . .
C1 C7 C8 115.7(8) . .
C8 C7 H7B 93.3 . .
C8 C7 H7A 105.3 . .
C8 C7 C9 18.1(9) . .
N6 C3 C4 115.1(3) . .
O2 C3 N6 124.0(3) . .
O2 C3 C4 120.9(3) . .
C7 N6 H6 118.4 . .
C3 N6 C7 123.3(3) . .
C3 N6 H6 118.4 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 O10 H10 109.4 . .
C3 C4 H4A 108.8 . .
C3 C4 H4B 108.8 . .
H4A C4 H4B 107.7 . .
N5 C4 C3 113.9(3) . .
N5 C4 H4A 108.8 . .
N5 C4 H4B 108.8 . .
Zn1 N5 H5A 102(3) 3_466 .
Zn1 N5 H5B 109(4) 3_466 .
C4 N5 Zn1 111.1(2) . 3_466
C4 N5 H5A 111(2) . .
C4 N5 H5B 107(3) . .
H5A N5 H5B 118(4) . .
O12 C1 C7 121.5(3) . .
O12 C1 O13 122.1(3) . .
O13 C1 C7 116.4(3) . .
C1 O13 Zn1 112.0(2) . .
C7 C8 H8 109.2 . .
O10 C8 C7 107.7(12) . .
O10 C8 H8 109.2 . .
O10 C8 C11 117.4(15) . .
C11 C8 C7 103.8(11) . .
C11 C8 H8 109.2 . .
C8 C11 H11A 109.5 . .
C8 C11 H11B 109.5 . .
C8 C11 H11C 109.5 . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N5 2.014(3) 3_566
Zn1 N5 2.014(3) 4_646
Zn1 O13 1.985(3) .
Zn1 O13 1.985(3) 2_765
O12 C1 1.238(6) .
C7 H7B 1.0000 .
C7 H7A 1.0000 .
C7 N6 1.460(4) .
C7 C9 1.574(13) .
C7 C1 1.523(5) .
C7 C8 1.529(15) .
C3 N6 1.321(4) .
C3 O2 1.230(4) .
C3 C4 1.517(4) .
N6 H6 0.8800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
O10 H10 0.8399 .
O10 C8 1.391(16) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C4 N5 1.457(4) .
N5 Zn1 2.014(3) 3_466
N5 H5A 0.880(18) .
N5 H5B 0.885(19) .
C1 O13 1.262(4) .
C8 H8 1.0000 .
C8 C11 1.523(17) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
O15 C14 1.371(13) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O12 C1 O13 Zn1 -15.8(6) . . . .
C7 C1 O13 Zn1 167.1(3) . . . .
C3 C4 N5 Zn1 -173.8(3) . . . 3_466
N6 C7 C1 O12 -7.5(6) . . . .
N6 C7 C1 O13 169.7(3) . . . .
N6 C7 C8 O10 -174.0(10) . . . .
N6 C7 C8 C11 60.9(13) . . . .
N6 C3 C4 N5 170.1(3) . . . .
O2 C3 N6 C7 -0.3(7) . . . .
O2 C3 C4 N5 -9.3(7) . . . .
C9 C7 N6 C3 107.3(7) . . . .
C9 C7 C1 O12 108.3(8) . . . .
C9 C7 C1 O13 -74.5(7) . . . .
C9 C7 C8 O10 114(5) . . . .
C9 C7 C8 C11 -11(3) . . . .
C4 C3 N6 C7 -179.6(3) . . . .
N5 Zn1 O13 C1 -84.8(3) 4_646 . . .
N5 Zn1 O13 C1 44.4(3) 3_566 . . .
C1 C7 N6 C3 -138.7(4) . . . .
C1 C7 C8 O10 56.8(14) . . . .
C1 C7 C8 C11 -68.3(13) . . . .
O13 Zn1 O13 C1 154.0(3) 2_765 . . .
C8 C7 N6 C3 89.2(9) . . . .
C8 C7 C1 O12 124.0(8) . . . .
C8 C7 C1 O13 -58.8(8) . . . .
