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_1516571
_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 H20 N2 O8 Zn2) 4(C3 H7 N O)'
_chemical_formula_sum            'C34 H48 N6 O12 Zn2'
_chemical_formula_weight         863.52
_chemical_name_common            DMOF
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_symmetry_space_group_name_Hall  '-I 4 2c'
_symmetry_space_group_name_H-M   'I 4/m c 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            4
_cell_length_a                   15.0609(8)
_cell_length_b                   15.0609(8)
_cell_length_c                   19.2433(13)
_cell_measurement_reflns_used    1150
_cell_measurement_temperature    270.00(14)
_cell_measurement_theta_max      26.8700
_cell_measurement_theta_min      4.2500
_cell_volume                     4365.0(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      270.00(14)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9847
_diffrn_measured_fraction_theta_max 0.9847
_diffrn_measurement_details
;
  1 omega  -80.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4634  -57.0000    0.0000 81

  2 omega  -63.00  -31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4634   19.0000  -90.0000 32

  3 omega  -62.00  -36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4634  -19.0000 -150.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0370018000
_diffrn_orient_matrix_UB_12      0.0255888000
_diffrn_orient_matrix_UB_13      0.0106219000
_diffrn_orient_matrix_UB_21      -0.0026182000
_diffrn_orient_matrix_UB_22      -0.0190900000
_diffrn_orient_matrix_UB_23      0.0336952000
_diffrn_orient_matrix_UB_31      0.0289105000
_diffrn_orient_matrix_UB_32      -0.0346624000
_diffrn_orient_matrix_UB_33      -0.0106112000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5404
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57880
_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    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1349
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0863P)^2^+8.3113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1811
_reflns_number_gt                882
_reflns_number_total             1349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00497c2.cif
_cod_data_source_block           DMOF
_cod_database_code               1516571
_chemical_oxdiff_formula         'C17 H24 N3 O6 Zn'
_reflns_odcompleteness_completeness 88.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.10
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-N2
 2.3 with sigma of 0.01
 O2-C6
 1.2 with sigma of 0.01
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
4. Others
 Fixed Sof: C4(0.375) H4A(0.375) H4B(0.375) C5(0.375) H5A(0.375) H5B(0.375)
 O2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;