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_7046340
_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             2017-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-11-29 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.740(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4908(2)
_cell_length_b                   5.4877(2)
_cell_length_c                   26.5634(10)
_cell_measurement_reflns_used    2930
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      75.6050
_cell_measurement_theta_min      6.4140
_cell_volume                     1082.00(6)
_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         0.000(1)
_diffrn_ambient_temperature      298(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -98.00 -64.00   1.00    5.00    --  -41.61 -77.00-150.00   34
  2  \w    -97.00 -72.00   1.00    5.00    --  -41.61-133.00 126.00   25
  3  \w     53.00  99.00   1.00    5.00    --   41.61  38.00 -60.00   46
  4  \w      8.00  43.00   1.00    5.00    --   41.61 -99.00 -60.00   35
  5  \w     19.00  50.00   1.00    5.00    --   41.61  38.00 -60.00   31
  6  \w    -29.00  61.00   1.00    5.00    --   41.61 -61.00   1.00   90
  7  \w     18.00 112.00   1.00    5.00    --   41.61  61.00 139.00   94
  8  \w     99.00 167.00   1.00   30.00    --  112.00  30.00 -60.00   68
  9  \w     41.00  81.00   1.00   30.00    --  112.00 -30.00-180.00   40
 10  \w     40.00 116.00   1.00   30.00    --  112.00 -61.00   1.00   76
 11  \w    124.00 155.00   1.00   30.00    --  112.00 -15.00-120.00   31
 12  \w     84.00 115.00   1.00   30.00    --  112.00  61.00-120.00   31
 13  \w    128.00 175.00   1.00   30.00    --  112.00  61.00-120.00   47
 14  \w     39.00  89.00   1.00   30.00    --  112.00 -30.00 -30.00   50
 15  \w    108.00 177.00   1.00   30.00    --  112.00  45.00  60.00   69
 16  \w     86.00 118.00   1.00   30.00    --  112.00  45.00 -90.00   32
 17  \w     93.00 165.00   1.00   30.00    --  112.00  30.00  30.00   72
 18  \w     85.00 119.00   1.00   30.00    --  112.00  61.00-150.00   34
 19  \w     80.00 160.00   1.00   30.00    --  112.00  77.00-150.00   80
 20  \w    151.00 176.00   1.00   30.00    --  112.00  45.00 -90.00   25
 21  \w    113.00 140.00   1.00   30.00    --  112.00  45.00  90.00   27
 22  \w     35.00 112.00   1.00   30.00    --  112.00 -15.00-120.00   77
 23  \w     36.00  77.00   1.00   30.00    --  112.00-111.00-180.00   41
 24  \w     50.00  76.00   1.00   30.00    --  112.00 -30.00 150.00   26
 25  \w     79.00 105.00   1.00   30.00    --  112.00  15.00-120.00   26
 26  \w    142.00 178.00   1.00   30.00    --  112.00 111.00-120.00   36
 27  \w     79.00 106.00   1.00   30.00    --  112.00  77.00-120.00   27
 28  \w    117.00 172.00   1.00   30.00    --  112.00 111.00 -30.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0190212000
_diffrn_orient_matrix_UB_12      0.0682863000
_diffrn_orient_matrix_UB_13      0.0552725000
_diffrn_orient_matrix_UB_21      -0.1450109000
_diffrn_orient_matrix_UB_22      0.1895711000
_diffrn_orient_matrix_UB_23      -0.0191924000
_diffrn_orient_matrix_UB_31      -0.1472586000
_diffrn_orient_matrix_UB_32      -0.1955589000
_diffrn_orient_matrix_UB_33      0.0006922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            4430
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.408
_diffrn_reflns_theta_min         3.358
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.657
_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         0.268
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 954 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2206
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0437P)^2^+0.2281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                2173
_reflns_number_total             2206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01765d2.cif
_cod_data_source_block           GlyTyr_RT
_cod_depositor_comments
'Adding full bibliography for 7046340--7046346.cif.'
_cod_database_code               7046340
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Ternary CH refined with riding coordinates:
 C1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C11(H11A,H11B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C9(H9), C8(H8), C6(H6), C5(H5)
2.d 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 1.182
_oxdiff_exptl_absorpt_empirical_full_min 0.929