Peptide metal-organic frameworks under pressure: flexible linkers for cooperative compression.
Navarro-Sánchez, José; Mullor-Ruíz, Ismael; Popescu, Catalin; Santamaría-Pérez, David; Segura, Alfredo; Errandonea, Daniel; González-Platas, Javier; Martí-Gastaldo, Carlos; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10654–10659; doi:10.1039/c8dt01765d

data_7046342
_publ_section_title
;
 Peptide metal-organic frameworks under pressure: flexible linkers for
 cooperative compression.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10654
_journal_page_last               10659
_journal_paper_doi               10.1039/c8dt01765d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C22 H26 N4 O8 Zn'
_chemical_formula_sum            'C22 H26 N4 O8 Zn'
_chemical_formula_weight         539.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-12-01 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.31(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0813(19)
_cell_length_b                   5.2012(11)
_cell_length_c                   25.88(10)
_cell_measurement_reflns_used    157
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      10.9450
_cell_measurement_theta_min      2.1940
_cell_volume                     941(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_pressure         3950000(40000)
_diffrn_ambient_temperature      298(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.282
_diffrn_measured_fraction_theta_max 0.282
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -18.20  10.00   0.20    1.00   0.00   0.00   0.00    --   141
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0065878921
_diffrn_orient_matrix_UB_12      0.0011890616
_diffrn_orient_matrix_UB_13      0.0123976586
_diffrn_orient_matrix_UB_21      0.0390569421
_diffrn_orient_matrix_UB_22      -0.0308599604
_diffrn_orient_matrix_UB_23      0.0003461225
_diffrn_orient_matrix_UB_31      0.0226289873
_diffrn_orient_matrix_UB_32      0.0529090666
_diffrn_orient_matrix_UB_33      -0.0001272492
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3185
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.282
_diffrn_reflns_Laue_measured_fraction_max 0.282
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            387
_diffrn_reflns_point_group_measured_fraction_full 0.223
_diffrn_reflns_point_group_measured_fraction_max 0.223
_diffrn_reflns_theta_full        10.880
_diffrn_reflns_theta_max         10.880
_diffrn_reflns_theta_min         2.187
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 48 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.52(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         367
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1434P)^2^+1.2214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2420
_reflns_Friedel_coverage         0.406
_reflns_Friedel_fraction_full    0.147
_reflns_Friedel_fraction_max     0.147
_reflns_number_gt                230
_reflns_number_total             367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01765d2.cif
_cod_data_source_block           GlyTyr_395GPa
_cod_depositor_comments
'Adding full bibliography for 7046340--7046346.cif.'
_cod_database_code               7046342
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C22 H26 N4 O8 Zn1'
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.942
_reflns_odcompleteness_completeness 13.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     10.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C1-C3
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Zn1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C7) = Uiso(C8) = Uiso(C9) = Uiso(C4) = Uiso(C5) = Uiso(C6) = Uiso(C3) =
Uiso(C1) = Uiso(C2) = Uiso(C10) = Uiso(C11)
Uiso(O4) = Uiso(O3) = Uiso(O1) = Uiso(O2)
Uiso(N1) = Uiso(N2)
4.a Ternary CH refined with riding coordinates:
 C1(H1A)
4.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C11(H11A,H11B), C3(H3A,H3B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C8(H8), C9(H9), C5(H5), C6(H6)
4.d Fitted hexagon refined as free rotating group:
 C7(C8,C9,C4,C5,C6)
4.e Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.774
_oxdiff_exptl_absorpt_empirical_full_min 0.710