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_1516572
_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         'C30 H24 N2 O8 Zn2'
_chemical_formula_sum            'C30 H24 N2 O8 Zn2'
_chemical_formula_weight         671.26
_chemical_name_common            ndc-DMOF
_space_group_crystal_system      tetragonal
_space_group_IT_number           127
_space_group_name_Hall           '-P 4 2ab'
_space_group_name_H-M_alt        'P 4/m b m'
_symmetry_space_group_name_Hall  '-P 4 2ab'
_symmetry_space_group_name_H-M   'P 4/m b 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            2
_cell_length_a                   15.4195(4)
_cell_length_b                   15.4195(4)
_cell_length_c                   9.6416(4)
_cell_measurement_reflns_used    3018
_cell_measurement_temperature    290(1)
_cell_measurement_theta_max      29.3060
_cell_measurement_theta_min      3.7430
_cell_volume                     2292.40(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      290.0(10)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9953
_diffrn_measured_fraction_theta_max 0.9953
_diffrn_measurement_details
;
  1 omega  -43.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5080   77.0000    0.0000 89

  2 omega  -56.00  -26.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5080  -57.0000 -180.0000 30

  3 omega  -46.00    6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5080   57.0000  150.0000 52

  4 omega  -94.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5080  -57.0000    0.0000 91
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0349334000
_diffrn_orient_matrix_UB_12      -0.0129138000
_diffrn_orient_matrix_UB_13      0.0431154000
_diffrn_orient_matrix_UB_21      -0.0117308000
_diffrn_orient_matrix_UB_22      -0.0322429000
_diffrn_orient_matrix_UB_23      -0.0489203000
_diffrn_orient_matrix_UB_31      0.0275620000
_diffrn_orient_matrix_UB_32      -0.0301523000
_diffrn_orient_matrix_UB_33      0.0340192000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12583
_diffrn_reflns_theta_full        30.72
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85971
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
;
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1827
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0748P)^2^+1.6338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1704
_reflns_number_gt                1188
_reflns_number_total             1827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00497c2.cif
_cod_data_source_block           ndc-DMOF
_cod_original_cell_volume        2292.39(13)
_cod_database_code               1516572
_chemical_oxdiff_formula         'C15 H12 N O4 Zn'
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C4 \\sim C3 \\sim C5 \\sim C6: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: C7(0.25) H7A(0.25) H7B(0.25) C9(0.25) H9A(0.25) H9B(0.25) C4(0.5)
 C3(0.5) H3(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C8(0.25) H8A(0.25) H8B(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C8(H8A,H8B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
;