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_1552058
_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(C20 H36 N8 O14 Zn2), 0.67(C O), 0.3(O)'
_chemical_formula_sum            'C10.67 H18 N4 O7.97 Zn'
_chemical_formula_weight         395.13
_chemical_name_systematic        'Zn[(GlyAla)0.5(GlySer)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                   13.8742(6)
_cell_length_b                   14.6060(7)
_cell_length_c                   4.7321(2)
_cell_measurement_temperature    100.15
_cell_volume                     958.94(7)
_computing_molecular_graphics
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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_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            17014
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         4.05
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction carried out using SADABS 2008/1 (Bruker, 2008).
wR2(int) was 0.0883 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.7111.
The \l/2 correction factor is 0.0015.
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_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    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             407
_exptl_crystal_recrystallization_method
'Crystallised directly from synthesis reaction in methanol.'
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       0.065(13)
_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   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1268P)^2^+0.1814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                2228
_reflns_number_total             2547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.1871-s3.cif
_cod_data_source_block           b00113
_cod_database_code               1552058
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H) groups, All N(H) groups, All N(H,H) groups,
  All O(H) groups
2. Restrained distances
 C7-C9 = C7-C8
 1.52 with sigma of 0.01
 C9-O11 = C8-O10
 1.43 with sigma of 0.01
 C8-H10A
 1.75 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O11) = Uanis(O10)
4. Others
 Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=1-FVAR(1)
 Sof(H11B)=Sof(O10)=Sof(H10A)=0.5*(1-FVAR(2))
 Sof(O11)=Sof(H11A)=Sof(H10B)=0.5*FVAR(2)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
 Fixed Sof: C17(0.33333) O16(0.33333) O15(0.15)
5.a Riding coordinates:
 O11(H11A), C9(H11B), O10(H10A), C8(H10B)
5.b Ternary CH refined with riding coordinates:
 C7(H7A), C7(H7B)
5.c Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), C4(H4A,H4B), C9(H9A,H9B), C8(H8A,H8B)
5.d Aromatic/amide H refined with riding coordinates:
 N6(H6)
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