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_1552057
_publ_section_title
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 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_compound_source        Synthesised.
_chemical_formula_moiety         '0.5(C20 H36 N8 O16 Zn2), 1.67(C H4 O), H2 O'
_chemical_formula_sum            'C11.67 H26.67 N4 O10.67 Zn'
_chemical_formula_weight         459.07
_chemical_name_common            'Zinc(GlySer)2 H2O MeOH'
_chemical_name_systematic        'Zinc(GlySer)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'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                   14.0129(10)
_cell_length_b                   14.6036(10)
_cell_length_c                   4.7205(3)
_cell_measurement_reflns_used    12270
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.747
_cell_measurement_theta_min      2.789
_cell_volume                     966.00(11)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b17 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b17 (Rigaku, 2011)
;
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann,
 in preparation (2013)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
	Number of images: 125
	           Slice: -110.0000 - 15.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -68.0000
	             Phi: 0.0000
	             XTD: 40.1030
	          2theta: -20.0806
scan:
	Number of images: 125
	           Slice: -110.0000 - 15.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -68.0000
	             Phi: 90.0000
	             XTD: 40.1030
	          2theta: -20.0806
scan:
	Number of images: 60
	           Slice: -110.0000 - -50.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -68.0000
	             Phi: 180.0000
	             XTD: 40.1030
	          2theta: -20.0806
scan:
	Number of images: 180
	           Slice: -90.0000 - 90.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 40.1030
	          2theta: -0.0806
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  Rigaku_AFC12K_724P_007HF_Mo
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 20um'
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.046734
_diffrn_orient_matrix_UB_12      -0.000649
_diffrn_orient_matrix_UB_13      -0.066803
_diffrn_orient_matrix_UB_21      -0.086489
_diffrn_orient_matrix_UB_22      0.064740
_diffrn_orient_matrix_UB_23      -0.006907
_diffrn_orient_matrix_UB_31      0.187600
_diffrn_orient_matrix_UB_32      0.030009
_diffrn_orient_matrix_UB_33      0.013457
_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  0.0690
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            12557
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.01
_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    1.332
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1232 before and 0.0852 after correction.
The Ratio of minimum to maximum transmission is 0.6570.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rect. Prism'
_exptl_crystal_F_000             480
_exptl_crystal_preparation
;
Crystals were isolated from the syntesis reaction as formed.
;
_exptl_crystal_recrystallization_method
;
Crystals were isolated from the synthesis reaction as formed.
;
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2575
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0771P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                2201
_reflns_number_total             2575
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.1871-s2.cif
_cod_data_source_block           sntb00014c1
_cod_database_code               1552057
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Shared sites
{O1A, C2B}
{C2A, O1B}
3. Rigid bond restraints
 C2A, O1A, O1C, C2C, O1W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C8 \\sim O9A \\sim C8 \\sim O9B \\sim C2C \\sim O1C \\sim C2A \\sim O1A: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C2A) = Uanis(O1B)
Uanis(O1A) = Uanis(C2B)
5. Others
 Sof(H8BC)=Sof(H8BD)=Sof(O9B)=Sof(H9B)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(O9A)=Sof(H9A)=FVAR(1)
 Fixed Sof: O1A(0.25) H1A(0.25) C2A(0.25) H2AA(0.25) H2AB(0.25) H2AC(0.25)
 O1B(0.25) H1B(0.25) C2B(0.25) H2BA(0.25) H2BB(0.25) H2BC(0.25) O1C(0.33333)
 H1C(0.33333) C2C(0.33333) H2CA(0.33333) H2CB(0.33333) H2CC(0.33333) O1W(0.5)
 H1WA(0.5) H1WB(0.5)
6.a Free rotating group:
 O1W(H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
 C7(H7)
6.c Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), C4(H4A,H4B), C8(H8AA,H8AB), C8(H8BC,H8BD)
6.d Me refined with riding coordinates:
 C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C2C(H2CA,H2CB,H2CC)
6.e Aromatic/amide H refined with riding coordinates:
 N6(H6)
6.f Tetrahedral OH refined with riding coordinates:
 O9B(H9B), O1A(H1A), O1B(H1B), O1C(H1C)
6.g Idealised tetrahedral OH refined as rotating group:
 O9A(H9A)
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