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_1516567
_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
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2ab 2b'
_space_group_name_H-M_alt        'P b a n'
_symmetry_space_group_name_Hall  '-P 2ab 2b'
_symmetry_space_group_name_H-M   'P b a n :2'
_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            2
_cell_length_a                   16.2647(5)
_cell_length_b                   14.5206(5)
_cell_length_c                   9.6475(3)
_cell_measurement_reflns_used    2472
_cell_measurement_temperature    270
_cell_measurement_theta_max      70.2080
_cell_measurement_theta_min      4.5770
_cell_volume                     2278.48(13)
_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      270.0
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9948
_diffrn_measured_fraction_theta_max 0.9948
_diffrn_measurement_details
;
  1 omega  -68.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 30

  2 omega  -10.00   20.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 30

  3 omega   33.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 37

  4 omega  -76.00   -3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500   57.0000  -30.0000 73

  5 omega   90.00  120.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000 -120.0000 30

  6 omega   88.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   88.0000  122.0000 36

  7 omega -130.00 -104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -88.0000    6.0000 26

  8 omega -146.00 -109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -75.0000 -111.0000  -30.0000 37

  9 omega   35.00   71.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000    0.0000 36

 10 omega   37.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000 -120.0000 33

 11 omega   35.00   65.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 30

 12 omega   38.00   71.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   60.0000 33

 13 omega   39.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 29

 14 omega   38.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   90.0000 77

 15 omega   72.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000   90.0000 26

 16 omega  126.00  152.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000 -120.0000 26

 17 omega   40.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   60.0000 26

 18 omega   56.00  118.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000   30.0000 62

 19 omega   37.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 31

 20 omega  111.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000 -120.0000 26

 21 omega   46.00   71.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000 -120.0000 25

 22 omega   50.00   84.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000    0.0000 34
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0871799000
_diffrn_orient_matrix_UB_12      0.0415074000
_diffrn_orient_matrix_UB_13      0.0008430000
_diffrn_orient_matrix_UB_21      -0.0330513000
_diffrn_orient_matrix_UB_22      0.0863896000
_diffrn_orient_matrix_UB_23      0.0741185000
_diffrn_orient_matrix_UB_31      0.0168605000
_diffrn_orient_matrix_UB_32      -0.0454578000
_diffrn_orient_matrix_UB_33      0.1414128000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6716
_diffrn_reflns_theta_full        70.37
_diffrn_reflns_theta_max         70.37
_diffrn_reflns_theta_min         4.58
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90061
_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    0.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2178
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1211P)^2^+1.7605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2025
_refine_ls_wR_factor_ref         0.2116
_reflns_number_gt                1641
_reflns_number_total             2178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00497c2.cif
_cod_data_source_block           NO2-DMOF
_cod_original_cell_volume        2278.50(14)
_cod_database_code               1516567
_chemical_oxdiff_formula         'C22 H18 N4 O12 Zn2'
_reflns_odcompleteness_completeness 86.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N2-O4 = N2-O3
 1.22 with sigma of 0.01
 C3-N2
 1.47 with sigma of 0.01
 O3-O4
 2.1 with sigma of 0.01
 N1-C7 \\sim N1-C8 \\sim N1-C5 \\sim N1-C9 \\sim N1-C6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uiso(O4) = Uiso(O3)
4. Others
 Fixed Sof: C7(0.3) H7A(0.3) H7B(0.3) C8(0.3) H8A(0.3) H8B(0.3) C5(0.3)
 H5A(0.3) H5B(0.3) C9(0.3) H9A(0.3) H9B(0.3) C6(0.3) H6A(0.3) H6B(0.3) N2(0.5)
 O4(0.5) O3(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C5(H5A,H5B), C9(H9A,H9B), C6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4)
;