#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/65/1516572.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1516572
loop_
_publ_author_name
'Henke, Sebastian'
'Li, Wei'
'Cheetham, Anthony K.'
_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       'ω 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/[σ²(Fo²)+(0.0748P)²+1.6338P] where P=(Fo²+2Fc²)/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
#BEGIN Tags that were not found in dictionaries:
_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)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x, z'
3 '-x, -y, z'
4 'y, -x, z'
5 'x+1/2, -y+1/2, -z'
6 '-x+1/2, y+1/2, -z'
7 'y+1/2, x+1/2, -z'
8 '-y+1/2, -x+1/2, -z'
9 '-x, -y, -z'
10 'y, -x, -z'
11 'x, y, -z'
12 '-y, x, -z'
13 '-x-1/2, y-1/2, z'
14 'x-1/2, -y-1/2, z'
15 '-y-1/2, -x-1/2, z'
16 'y-1/2, x-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn1 Zn 1.0000 0.0000 0.15301(5) 0.0232(2) Uani 1 4 d S .
O1 O 0.91201(15) 0.09446(15) 0.1142(3) 0.0559(7) Uani 1 1 d . .
N1 N 1.0000 0.0000 0.3657(4) 0.0267(8) Uani 1 4 d S .
C1 C 0.8889(2) 0.1224(2) 0.0000 0.0347(8) Uani 1 2 d S .
C2 C 0.8235(3) 0.1951(3) 0.0000 0.0395(10) Uani 1 2 d S .
C7 C 1.0847(9) 0.0363(13) 0.4210(11) 0.027(2) Uani 0.25 1 d PU 1
H7A H 1.0925 0.0951 0.3874 0.033 Uiso 0.25 1 calc PR 1
H7B H 1.1327 0.0015 0.3874 0.033 Uiso 0.25 1 calc PR 1
C9 C 1.0732(10) -0.0578(12) 0.4194(13) 0.028(3) Uani 0.25 1 d PU 2
H9A H 1.1284 -0.0365 0.3855 0.034 Uiso 0.25 1 calc PR 2
H9B H 1.0653 -0.1165 0.3855 0.034 Uiso 0.25 1 calc PR 2
C4 C 0.8370(4) 0.2725(4) -0.0751(9) 0.067(2) Uani 0.50 1 d PU .
C3 C 0.7512(5) 0.1866(5) 0.0822(8) 0.065(2) Uani 0.50 1 d P .
H3 H 0.7449 0.1379 0.1382 0.078 Uiso 0.50 1 calc PR .
C5 C 0.9142(6) 0.2880(6) -0.1531(11) 0.103(3) Uani 0.50 1 d PU .
H5 H 0.9595 0.2482 -0.1483 0.124 Uiso 0.50 1 calc PR .
C6 C 0.9233(6) 0.3623(6) -0.2375(13) 0.125(4) Uani 0.50 1 d PU .
H6 H 0.9722 0.3686 -0.2932 0.149 Uiso 0.50 1 calc PR .
C8 C 1.0898(8) -0.0122(15) 0.4197(12) 0.027(2) Uani 0.25 1 d PU 3
H8A H 1.1267 0.0342 0.3860 0.033 Uiso 0.25 1 calc PR 3
H8B H 1.1130 -0.0667 0.3860 0.033 Uiso 0.25 1 calc PR 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 -1 0.0689 -0.0008 0.0003 -0.9987 -0.0430 0.0489 -0.0340
-1 1 0 0.1186 -0.9994 0.9986 -0.0001 0.0220 -0.0205 -0.0577
1 1 0 0.0988 0.9997 0.9979 -0.0001 -0.0478 -0.0439 -0.0025
-1 -1 0 0.1718 -0.9997 -0.9979 0.0001 0.0478 0.0439 0.0025
1 -1 0 0.1496 0.9994 -0.9986 0.0001 -0.0220 0.0205 0.0577
0 0 1 0.0689 0.0008 -0.0003 0.9987 0.0430 -0.0489 0.0340
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Zn1 Zn1 79.35(7) 2_645 9_755
O1 Zn1 Zn1 79.35(7) 4_665 9_755
O1 Zn1 Zn1 79.35(7) . 9_755
O1 Zn1 Zn1 79.35(7) 3_755 9_755
O1 Zn1 O1 88.04(3) 2_645 3_755
O1 Zn1 O1 88.04(3) 4_665 .
O1 Zn1 O1 88.04(3) 2_645 .
O1 Zn1 O1 158.70(15) 3_755 .
O1 Zn1 O1 158.70(15) 4_665 2_645
O1 Zn1 O1 88.04(3) 4_665 3_755
O1 Zn1 N1 100.65(7) 3_755 .
O1 Zn1 N1 100.65(7) . .
O1 Zn1 N1 100.65(7) 2_645 .
O1 Zn1 N1 100.65(7) 4_665 .
N1 Zn1 Zn1 180.0 . 9_755
C1 O1 Zn1 127.5(2) . .
C7 N1 C7 82.9(3) 4_665 3_755
C7 N1 C7 82.9(3) 2_645 3_755
C7 N1 C7 138.8(8) . 3_755
C7 N1 C7 82.9(3) . 4_665
C7 N1 C7 82.9(3) . 2_645
C7 N1 C7 138.8(8) 2_645 4_665
C7 N1 C9 107.5(6) 3_755 .
C7 N1 C9 26.7(6) 4_665 .
C7 N1 C9 130.9(6) 4_665 3_755
C7 N1 C9 26.7(6) 2_645 3_755
C7 N1 C9 107.5(6) 2_645 4_665
C7 N1 C9 57.4(6) 4_665 4_665
C7 N1 C9 26.7(6) 3_755 4_665
C7 N1 C9 130.9(6) 2_645 .
C7 N1 C9 57.4(6) . .
C7 N1 C9 130.9(6) . 4_665
C7 N1 C9 57.4(6) 3_755 3_755
C7 N1 C9 130.9(6) 3_755 2_645
C7 N1 C9 107.5(6) . 3_755
C7 N1 C9 107.5(6) 4_665 2_645
C7 N1 C9 26.7(6) . 2_645
C7 N1 C9 57.4(6) 2_645 2_645
C9 N1 C9 83.4(3) 2_645 3_755
C9 N1 C9 83.4(3) 4_665 3_755
C9 N1 C9 140.3(9) 2_645 4_665
C9 N1 C9 83.4(3) 2_645 .
C9 N1 C9 83.4(3) 4_665 .
C9 N1 C9 140.3(9) 3_755 .
C8 N1 C7 129.0(6) . 3_755
C8 N1 C7 55.0(6) 4_665 3_755
C8 N1 C7 28.9(6) 2_645 2_645
C8 N1 C7 129.0(6) 3_755 .
C8 N1 C7 109.2(6) 3_755 4_665
C8 N1 C7 28.9(6) 4_665 4_665
C8 N1 C7 109.2(6) 2_645 3_755
C8 N1 C7 28.9(6) 3_755 3_755
C8 N1 C7 129.0(6) 2_645 4_665
C8 N1 C7 55.0(6) 3_755 2_645
C8 N1 C7 129.0(6) 4_665 2_645
C8 N1 C7 109.2(6) . 2_645
C8 N1 C7 109.2(6) 4_665 .
C8 N1 C7 28.9(6) . .
C8 N1 C7 55.0(6) . 4_665
C8 N1 C7 55.0(6) 2_645 .
C8 N1 C9 109.3(5) . 4_665
C8 N1 C9 109.3(5) 4_665 3_755
C8 N1 C9 28.7(5) 2_645 2_645
C8 N1 C9 55.5(5) . 2_645
C8 N1 C9 55.5(5) 3_755 4_665
C8 N1 C9 28.7(5) 4_665 4_665
C8 N1 C9 55.5(5) 2_645 3_755
C8 N1 C9 129.8(5) . 3_755
C8 N1 C9 109.3(5) 2_645 .
C8 N1 C9 28.7(5) . .
C8 N1 C9 55.5(5) 4_665 .
C8 N1 C9 129.8(5) 3_755 .
C8 N1 C9 129.8(5) 4_665 2_645
C8 N1 C9 109.3(5) 3_755 2_645
C8 N1 C9 28.7(5) 3_755 3_755
C8 N1 C9 129.8(5) 2_645 4_665
C8 N1 C8 83.0(3) 4_665 3_755
C8 N1 C8 139.1(9) . 3_755
C8 N1 C8 83.0(3) 2_645 3_755
C8 N1 C8 83.0(3) . 4_665
C8 N1 C8 139.1(9) 2_645 4_665
C8 N1 C8 83.0(3) 2_645 .
O1 C1 O1 126.1(4) 11 .
O1 C1 C2 116.93(18) 11 .
O1 C1 C2 116.93(18) . .
C4 C2 C1 122.0(4) . .
C4 C2 C1 122.0(4) 11 .
C4 C2 C4 61.7(7) 11 .
C3 C2 C1 118.1(4) . .
C3 C2 C1 118.1(4) 11 .
C3 C2 C4 84.5(5) 11 .
C3 C2 C4 119.8(5) . .
C3 C2 C4 84.5(5) . 11
C3 C2 C4 119.8(5) 11 11
C3 C2 C3 70.5(8) 11 .
N1 C7 C7 110.6(4) . 11_556
N1 C9 C9 109.8(5) . 11_556
C2 C4 C5 122.3(6) . .
C4 C4 C2 119.6(3) 16_655 .
C4 C4 C5 118.1(4) 16_655 .
C2 C3 C4 48.6(4) . 11
C2 C3 C3 120.4(3) . 16_655
C3 C3 C4 90.0(2) 16_655 11
C6 C5 C4 121.5(7) . .
C6 C6 C5 120.2(5) 16_655 .
N1 C8 C8 110.4(5) . 11_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 Zn1 2.9504(10) 9_755
Zn1 O1 2.025(2) 3_755
Zn1 O1 2.025(2) 2_645
Zn1 O1 2.025(2) .
Zn1 O1 2.025(2) 4_665
Zn1 N1 2.050(4) .
O1 C1 1.235(3) .
N1 C7 1.518(11) 4_665
N1 C7 1.518(11) 3_755
N1 C7 1.518(11) .
N1 C7 1.518(11) 2_645
N1 C9 1.528(12) 4_665
N1 C9 1.528(12) 2_645
N1 C9 1.528(12) .
N1 C9 1.528(12) 3_755
N1 C8 1.492(11) 4_665
N1 C8 1.492(11) 3_755
N1 C8 1.492(11) 2_645
N1 C8 1.492(11) .
C1 O1 1.235(3) 11
C1 C2 1.507(5) .
C2 C4 1.412(7) .
C2 C4 1.412(7) 11
C2 C3 1.374(7) 11
C2 C3 1.374(7) .
C7 C7 1.52(2) 11_556
C9 C9 1.55(2) 11_556
C4 C4 1.406(11) 16_655
C4 C5 1.428(10) .
C3 C4 1.874(11) 11
C3 C3 1.409(11) 16_655
C5 C6 1.412(11) .
C6 C6 1.332(16) 16_655
C8 C8 1.55(2) 11_556
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 57 3 N,N-dimethylformamide
2 0.500 1.000 0.000 57 3 N,N-dimethylformamide
3 0.085 0.412 0.500 554 52 N,N-dimethylformamide
