Side-chain control of porosity closure in single- and multiple-peptide-based porous materials by cooperative folding
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; Nature Chemistry 6 (2014) 343–351; doi:10.1038/nchem.1871

data_1552059
_publ_section_title
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 Side-chain control of porosity closure in single- and
 multiple-peptide-based porous materials by cooperative folding
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_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.
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_computing_publication_material
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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 \w-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 \l/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/[\s^2^(Fo^2^)+(0.0875P)^2^+0.6298P] where P=(Fo^2^+2Fc^2^)/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
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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)
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