Guest-dependent mechanical anisotropy in pillared-layered soft porous crystals ‒ a nanoindentation study
Henke, Sebastian; Li, Wei; Cheetham, Anthony K.; Chemical Science 5 (2014) 2392–; doi:10.1039/c4sc00497c

data_1516570
_publ_section_title
;
 Guest-dependent mechanical anisotropy in pillared-layered soft porous
 crystals -- a nanoindentation study
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2392
_journal_paper_doi               10.1039/c4sc00497c
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C22 H18 N4 O12 Zn2'
_chemical_formula_sum            'C22 H18 N4 O12 Zn2'
_chemical_formula_weight         661.14
_chemical_name_common            NO2-DMOF_toluene
_space_group_crystal_system      tetragonal
_space_group_IT_number           123
_space_group_name_Hall           '-P 4 2'
_space_group_name_H-M_alt        'P 4/m m m'
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   10.90313(18)
_cell_length_b                   10.90313(18)
_cell_length_c                   9.6490(3)
_cell_measurement_reflns_used    2678
_cell_measurement_temperature    290
_cell_measurement_theta_max      69.9590
_cell_measurement_theta_min      6.1040
_cell_volume                     1147.06(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      290.0
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9942
_diffrn_measured_fraction_theta_max 0.9942
_diffrn_measurement_details
;
  1 omega    9.00   41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000    0.0000 32

  2 omega   36.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -120.0000 36

  3 omega   76.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  150.0000 51

  4 omega   73.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   90.0000 54

  5 omega   73.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   30.0000 54

  6 omega  117.00  172.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000   90.0000 55

  7 omega   39.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -60.0000 25

  8 omega   38.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000 -120.0000 30

  9 omega   40.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -90.0000 28

 10 omega   36.00   82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000 -120.0000 46

 11 omega   50.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000    0.0000 36

 12 omega   91.00  130.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000 -120.0000 39

 13 omega   52.00  118.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000  -30.0000 66

 14 omega  -71.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -180.0000 103

 15 omega -124.00  -33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -56.0000  -14.0000 91

 16 omega   23.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -120.0000 103

 17 omega   70.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000   30.0000 44

 18 omega   78.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -90.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0759923000
_diffrn_orient_matrix_UB_12      -0.1072220000
_diffrn_orient_matrix_UB_13      -0.0585766000
_diffrn_orient_matrix_UB_21      0.0736803000
_diffrn_orient_matrix_UB_22      0.0906454000
_diffrn_orient_matrix_UB_23      -0.0897954000
_diffrn_orient_matrix_UB_31      0.0935872000
_diffrn_orient_matrix_UB_32      0.0157739000
_diffrn_orient_matrix_UB_33      0.1183331000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4246
_diffrn_reflns_theta_full        70.13
_diffrn_reflns_theta_max         70.13
_diffrn_reflns_theta_min         6.12
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_platon_squeeze_details
;
;
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         689
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0544
_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^)+(0.1110P)^2^+0.7733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1615
_reflns_number_gt                678
_reflns_number_total             689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00497c2.cif
_cod_data_source_block           NO2-DMOF_toluene
_cod_database_code               1516570
_chemical_oxdiff_formula         'C11 H9 N2 O6 Zn'
_reflns_odcompleteness_completeness 92.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 N1-C3
 1.47 with sigma of 0.01
 N1-O2 = N1-O3
 1.22 with sigma of 0.01
 O3-O2
 2.1 with sigma of 0.01
 N2-C4 \\sim N2-C5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uiso(O3) = Uiso(O2)
4. Others
 Fixed Sof: C4(0.25) H4A(0.25) H4B(0.25) C3(0.5) C5(0.125) H5A(0.125)
 H5B(0.125) N1(0.125) O2(0.125) O3(0.125)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
;