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_1516573
_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 Br2 N2 O8 Zn2'
_chemical_formula_sum            'C22 H18 Br2 N2 O8 Zn2'
_chemical_formula_weight         728.94
_chemical_name_common            Br-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                   16.3684(4)
_cell_length_b                   14.4237(3)
_cell_length_c                   9.6406(2)
_cell_measurement_reflns_used    3251
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      70.2600
_cell_measurement_theta_min      4.5840
_cell_volume                     2276.08(9)
_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      270.15
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9940
_diffrn_measured_fraction_theta_max 0.9940
_diffrn_measurement_details
;
  1 omega   35.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   30.0000 42

  2 omega   -8.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -120.0000 33

  3 omega   32.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  150.0000 25

  4 omega   77.00  119.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   30.0000 42

  5 omega   41.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000  150.0000 71

  6 omega   77.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  120.0000 50

  7 omega -144.00 -103.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -91.0000 -180.0000 41

  8 omega   40.00   66.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000 -180.0000 26

  9 omega   38.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -60.0000 29

 10 omega   38.00   70.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  150.0000 32

 11 omega   61.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -61.0000  120.0000 50

 12 omega   39.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -30.0000 26

 13 omega   40.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -90.0000 25

 14 omega   36.00   80.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -12.0000 -120.0000 44

 15 omega  147.00  173.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -12.0000 -120.0000 26

 16 omega   92.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -12.0000 -120.0000 34

 17 omega   38.00   70.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   90.0000 32

 18 omega   50.00   76.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -30.0000 26

 19 omega  126.00  162.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000  -90.0000 36

 20 omega   89.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000 -180.0000 37

 21 omega  147.00  173.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000 -180.0000 26

 22 omega   39.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000  -90.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0663864000
_diffrn_orient_matrix_UB_12      0.0749045000
_diffrn_orient_matrix_UB_13      0.0170668000
_diffrn_orient_matrix_UB_21      0.0239293000
_diffrn_orient_matrix_UB_22      0.0116199000
_diffrn_orient_matrix_UB_23      0.1536183000
_diffrn_orient_matrix_UB_31      0.0622471000
_diffrn_orient_matrix_UB_32      0.0752477000
_diffrn_orient_matrix_UB_33      -0.0407064000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6928
_diffrn_reflns_theta_full        70.36
_diffrn_reflns_theta_max         70.36
_diffrn_reflns_theta_min         4.59
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71954
_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    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2175
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0833P)^2^+3.1623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                1903
_reflns_number_total             2175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00497c2.cif
_cod_data_source_block           Br-DMOF
_cod_original_cell_volume        2276.07(9)
_cod_database_code               1516573
_chemical_oxdiff_formula         'C11 H9 Br N O4 Zn'
_reflns_odcompleteness_completeness 86.55
_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
 N1-C9 \\sim N1-C5 \\sim N1-C7 \\sim N1-C10 \\sim N1-C8 \\sim N1-C6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(Br2)
Uanis(C9) = Uanis(C5) = Uanis(C7) = Uanis(C10) = Uanis(C8) = Uanis(C6)
4. Others
 0.5*[Sof(Br1)+Sof(Br2)]+1*[Sof(H3)]=1 with esd of 0
 1*[Sof(H3)]+1*[Sof(H4)]=1.5 with esd of 0
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=0.5*(1-FVAR(2))
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 0.5*FVAR(2)
 Sof(Br2)=0.5*(1-FVAR(3))
 Sof(Br1)=0.5*FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C5(H5A,H5B), C7(H7A,H7B), C10(H10A,H10B), C8(H8A,H8B), C6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;