#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/96/4119690.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_4119690
loop_
_publ_author_name
'Ilne Grobler'
'Vincent J. Smith'
'Prashant M. Bhatt'
'Simon A. Herbert'
'Leonard J. Barbour'
_publ_section_title
;
 Tunable Anisotropic Thermal Expansion of a Porous Zinc(II) Metal-Organic
 Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6411
_journal_page_last               6414
_journal_paper_doi               10.1021/ja401671p
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C18 H11 N2 O3 Zn'
_chemical_formula_sum            'C18 H11 N2 O3 Zn'
_chemical_formula_weight         368.66
_chemical_name_common            MOF-150
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.5112(9)
_cell_length_b                   26.5112(9)
_cell_length_c                   5.2351(2)
_cell_measurement_reflns_used    7370
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      29.6255
_cell_measurement_theta_min      2.4295
_cell_volume                     3679.5(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'X-Seed (Barbour,2001; Atwood & Barbour,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker Apex DUO CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'Incoatec I\mS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            14425
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.7970
_exptl_absorpt_correction_T_min  0.3454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (SAINT(Bruker,2008))
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       Block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.034(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0439
_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/[σ²(Fo²)+(0.0911P)²+0.5584P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                4606
_reflns_number_total             5190
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja401671p_si_001_2.cif
_cod_data_source_block           C:1_apohost_190K
_cod_original_sg_symbol_Hall     I-4
_cod_database_code               4119690
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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_assembly
_atom_site_disorder_group
Zn1 Zn 0.273779(11) 0.214732(11) 0.91607(7) 0.04160(11) Uani 1 1 d . . .
O1 O 0.22249(9) 0.25240(10) 1.0897(6) 0.0583(6) Uani 1 1 d . . .
N1 N 0.25146(11) 0.14176(8) 0.8916(7) 0.0531(7) Uani 1 1 d . . .
C1 C 0.26853(14) 0.10434(11) 1.0290(8) 0.0590(10) Uani 1 1 d . . .
H1 H 0.2953 0.1076 1.1483 0.071 Uiso 1 1 calc R . .
N2 N 0.24380(11) 0.06007(9) 0.9834(7) 0.0553(8) Uani 1 1 d . A .
C2 C 0.21233(11) 0.12207(9) 0.7419(7) 0.0446(6) Uani 1 1 d . . .
O2 O 0.27749(11) -0.16567(10) 1.3732(7) 0.0731(9) Uani 1 1 d . . .
C3 C 0.18326(11) 0.14527(9) 0.5589(7) 0.0433(6) Uani 1 1 d . . .
H3 H 0.1876 0.1800 0.5192 0.052 Uiso 1 1 calc R . .
O3A O 0.3086(6) -0.1274(4) 1.684(2) 0.134(6) Uani 0.453(5) 1 d P A 2
O3B O 0.3531(2) -0.1349(2) 1.403(3) 0.132(5) Uani 0.547(5) 1 d P A 1
C4 C 0.14694(10) 0.11580(9) 0.4328(6) 0.0396(5) Uani 1 1 d . . .
C5 C 0.11743(12) 0.13650(12) 0.2301(7) 0.0511(7) Uani 1 1 d . . .
H5 H 0.1219 0.1707 0.1810 0.061 Uiso 1 1 calc R . .
C6 C 0.08272(13) 0.10727(14) 0.1065(8) 0.0591(8) Uani 1 1 d . . .
H6 H 0.0630 0.1214 -0.0271 0.071 Uiso 1 1 calc R . .
C7 C 0.07584(14) 0.05639(15) 0.1749(9) 0.0643(10) Uani 1 1 d . . .
H7 H 0.0513 0.0367 0.0878 0.077 Uiso 1 1 calc R . .
C8 C 0.10362(12) 0.03512(12) 0.3626(7) 0.0513(7) Uani 1 1 d . . .
H8 H 0.0982 0.0008 0.4064 0.062 Uiso 1 1 calc R . .
C9 C 0.14111(10) 0.06373(10) 0.4964(6) 0.0400(6) Uani 1 1 d . . .
C10 C 0.17152(11) 0.04054(10) 0.6812(6) 0.0421(6) Uani 1 1 d . . .
H10 H 0.1676 0.0059 0.7232 0.051 Uiso 1 1 calc R . .
C11 C 0.20714(12) 0.06993(9) 0.7990(7) 0.0451(7) Uani 1 1 d . . .
C12 C 0.25802(12) 0.01244(10) 1.0908(8) 0.0491(7) Uani 1 1 d . . .
C13A C 0.2711(4) 0.0113(3) 1.3393(19) 0.066(2) Uani 0.453(5) 1 d P A 2
H13A H 0.2714 0.0417 1.4352 0.080 Uiso 0.453(5) 1 calc PR A 2
C13B C 0.3073(3) 0.0048(3) 1.1426(18) 0.066(2) Uani 0.547(5) 1 d P A 1
H13B H 0.3307 0.0318 1.1268 0.079 Uiso 0.547(5) 1 calc PR A 1
C14A C 0.2847(5) -0.0355(4) 1.462(2) 0.076(3) Uani 0.453(5) 1 d P A 2
H14A H 0.2919 -0.0381 1.6390 0.092 Uiso 0.453(5) 1 calc PR A 2
C14B C 0.3239(3) -0.0432(3) 1.220(2) 0.075(3) Uani 0.547(5) 1 d P A 1
H14B H 0.3588 -0.0509 1.2322 0.090 Uiso 0.547(5) 1 calc PR A 1
C15 C 0.28613(15) -0.08009(12) 1.2805(11) 0.0702(13) Uani 1 1 d . . .
C16A C 0.2696(4) -0.0773(4) 1.067(2) 0.078(3) Uiso 0.453(5) 1 d P A 2
H16A H 0.2621 -0.1079 0.9799 0.093 Uiso 0.453(5) 1 calc PR A 2
C16B C 0.2379(2) -0.07040(18) 1.2436(10) 0.0399(11) Uani 0.547(5) 1 d P A 1
H16B H 0.2135 -0.0959 1.2752 0.048 Uiso 0.547(5) 1 calc PR A 1
C17A C 0.2606(5) -0.0309(3) 0.937(2) 0.095(5) Uani 0.453(5) 1 d P A 2
H17A H 0.2567 -0.0293 0.7565 0.114 Uiso 0.453(5) 1 calc PR A 2
C17B C 0.22234(19) -0.02271(19) 1.1581(11) 0.0421(12) Uani 0.547(5) 1 d P A 1
H17B H 0.1875 -0.0148 1.1468 0.050 Uiso 0.547(5) 1 calc PR A 1
C18 C 0.3009(3) -0.13090(19) 1.390(2) 0.135(4) Uani 1 1 d . A .
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_
_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 O1 102.84(7) . 7_554
O1 Zn1 O2 105.04(12) . 6_557
O1 Zn1 O2 114.27(14) 7_554 6_557
O1 Zn1 N1 108.68(13) . .
O1 Zn1 N1 113.07(14) 7_554 .
O2 Zn1 N1 112.04(11) 6_557 .
Zn1 O1 Zn1 128.46(13) . 7
C1 N1 C2 106.4(2) . .
C1 N1 Zn1 126.1(2) . .
C2 N1 Zn1 127.38(19) . .
N1 C1 N2 113.0(3) . .
N1 C1 H1 123.5 . .
N2 C1 H1 123.5 . .
C1 N2 C11 107.1(2) . .
C1 N2 C12 124.2(3) . .
C11 N2 C12 128.3(2) . .
C3 C2 N1 129.6(2) . .
C3 C2 C11 121.9(3) . .
N1 C2 C11 108.4(2) . .
C18 O2 Zn1 125.1(4) . 8_547
C2 C3 C4 117.6(2) . .
C2 C3 H3 121.2 . .
C4 C3 H3 121.2 . .
C3 C4 C9 120.1(3) . .
C3 C4 C5 120.7(3) . .
C9 C4 C5 119.0(3) . .
C6 C5 C4 120.2(3) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C7 120.7(3) . .
C5 C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C8 C7 C6 121.0(3) . .
C8 C7 H7 119.5 . .
C6 C7 H7 119.5 . .
C7 C8 C9 120.8(3) . .
C7 C8 H8 119.6 . .
C9 C8 H8 119.6 . .
C10 C9 C4 121.5(2) . .
C10 C9 C8 120.3(3) . .
C4 C9 C8 118.2(3) . .
C11 C10 C9 117.2(2) . .
C11 C10 H10 121.4 . .
C9 C10 H10 121.4 . .
C10 C11 N2 133.2(3) . .
C10 C11 C2 121.7(3) . .
N2 C11 C2 105.1(2) . .
C13A C12 C13B 63.4(6) . .
C13A C12 C17B 85.1(5) . .
C13B C12 C17B 120.9(4) . .
C13A C12 C17A 121.6(6) . .
C13B C12 C17A 86.9(6) . .
C17B C12 C17A 68.1(7) . .
C13A C12 N2 117.9(5) . .
C13B C12 N2 117.7(4) . .
C17B C12 N2 121.1(3) . .
C17A C12 N2 120.5(5) . .
C12 C13A C14A 120.9(8) . .
C12 C13A H13A 119.5 . .
C14A C13A H13A 119.5 . .
C12 C13B C14B 119.7(6) . .
C12 C13B H13B 120.2 . .
C14B C13B H13B 120.2 . .
C13A C14A C15 113.5(8) . .
C13A C14A H14A 123.3 . .
C15 C14A H14A 123.3 . .
C13B C14B C15 117.6(6) . .
C13B C14B H14B 121.2 . .
C15 C14B H14B 121.2 . .
C16A C15 C16B 59.9(6) . .
C16A C15 C14B 90.5(8) . .
C16B C15 C14B 120.8(4) . .
C16A C15 C18 120.0(8) . .
C16B C15 C18 118.7(4) . .
C14B C15 C18 120.6(5) . .
C16A C15 C14A 121.7(7) . .
C16B C15 C14A 85.1(6) . .
C14B C15 C14A 67.9(6) . .
C18 C15 C14A 117.6(6) . .
C15 C16A C17A 123.8(11) . .
C15 C16A H16A 118.1 . .
C17A C16A H16A 118.1 . .
C15 C16B C17B 120.5(4) . .
C15 C16B H16B 119.7 . .
C17B C16B H16B 119.7 . .
C12 C17A C16A 116.0(10) . .
C12 C17A H17A 122.0 . .
C16A C17A H17A 122.0 . .
C12 C17B C16B 119.4(4) . .
C12 C17B H17B 120.3 . .
C16B C17B H17B 120.3 . .
O2 C18 O3B 119.7(6) . .
O2 C18 C15 124.1(5) . .
O3B C18 C15 110.1(6) . .
O2 C18 O3A 101.5(9) . .
O3B C18 O3A 80.0(9) . .
C15 C18 O3A 110.8(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.916(3) .
Zn1 O1 1.920(3) 7_554
Zn1 O2 1.959(3) 6_557
Zn1 N1 2.027(2) .
O1 Zn1 1.920(3) 7
N1 C1 1.306(4) .
N1 C2 1.401(4) .
C1 N2 1.365(4) .
C1 H1 0.9500 .
N2 C11 1.394(4) .
N2 C12 1.433(3) .
C2 C3 1.375(4) .
C2 C11 1.421(3) .
O2 C18 1.115(6) .
O2 Zn1 1.959(3) 8_547
C3 C4 1.405(4) .
C3 H3 0.9500 .
O3A C18 1.556(15) .
O3B C18 1.388(9) .
C4 C9 1.429(4) .
C4 C5 1.428(4) .
C5 C6 1.366(5) .
C5 H5 0.9500 .
C6 C7 1.407(6) .
C6 H6 0.9500 .
C7 C8 1.352(5) .
C7 H7 0.9500 .
C8 C9 1.433(4) .
C8 H8 0.9500 .
C9 C10 1.401(4) .
C10 C11 1.371(4) .
C10 H10 0.9500 .
C12 C13A 1.347(11) .
C12 C13B 1.349(7) .
C12 C17B 1.374(6) .
C12 C17A 1.405(9) .
C13A C14A 1.442(11) .
C13A H13A 0.9500 .
C13B C14B 1.407(9) .
C13B H13B 0.9500 .
C14A C15 1.517(12) .
C14A H14A 0.9500 .
C14B C15 1.434(8) .
C14B H14B 0.9500 .
C15 C16A 1.203(14) .
C15 C16B 1.318(6) .
C15 C18 1.516(5) .
C16A C17A 1.429(14) .
C16A H16A 0.9500 .
C16B C17B 1.403(6) .
C16B H16B 0.9500 .
C17A H17A 0.9500 .
C17B H17B 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 Zn1 O1 Zn1 -125.6(3) 7_554 7
O2 Zn1 O1 Zn1 -5.8(2) 6_557 7
N1 Zn1 O1 Zn1 114.29(19) . 7
O1 Zn1 N1 C1 -104.5(4) . .
O1 Zn1 N1 C1 142.0(4) 7_554 .
O2 Zn1 N1 C1 11.1(4) 6_557 .
O1 Zn1 N1 C2 69.8(4) . .
O1 Zn1 N1 C2 -43.7(4) 7_554 .
O2 Zn1 N1 C2 -174.6(3) 6_557 .
C2 N1 C1 N2 0.2(5) . .
Zn1 N1 C1 N2 175.4(3) . .
N1 C1 N2 C11 -0.2(5) . .
N1 C1 N2 C12 174.0(4) . .
C1 N1 C2 C3 -177.5(4) . .
Zn1 N1 C2 C3 7.4(6) . .
C1 N1 C2 C11 -0.1(5) . .
Zn1 N1 C2 C11 -175.3(3) . .
N1 C2 C3 C4 178.6(4) . .
C11 C2 C3 C4 1.5(5) . .
C2 C3 C4 C9 0.1(5) . .
C2 C3 C4 C5 -176.3(3) . .
C3 C4 C5 C6 179.1(3) . .
C9 C4 C5 C6 2.6(5) . .
C4 C5 C6 C7 -0.6(6) . .
C5 C6 C7 C8 -0.6(6) . .
C6 C7 C8 C9 -0.4(6) . .
C3 C4 C9 C10 -1.0(5) . .
C5 C4 C9 C10 175.5(3) . .
C3 C4 C9 C8 -179.9(3) . .
C5 C4 C9 C8 -3.5(4) . .
C7 C8 C9 C10 -176.6(3) . .
C7 C8 C9 C4 2.4(5) . .
C4 C9 C10 C11 0.1(5) . .
C8 C9 C10 C11 179.0(3) . .
C9 C10 C11 N2 -178.6(4) . .
C9 C10 C11 C2 1.6(5) . .
C1 N2 C11 C10 -179.8(4) . .
C12 N2 C11 C10 6.4(7) . .
C1 N2 C11 C2 0.1(4) . .
C12 N2 C11 C2 -173.8(4) . .
C3 C2 C11 C10 -2.5(6) . .
N1 C2 C11 C10 179.9(3) . .
C3 C2 C11 N2 177.6(3) . .
N1 C2 C11 N2 0.0(4) . .
C1 N2 C12 C13A 42.9(8) . .
C11 N2 C12 C13A -144.2(6) . .
C1 N2 C12 C13B -30.1(7) . .
C11 N2 C12 C13B 142.8(6) . .
C1 N2 C12 C17B 144.8(5) . .
C11 N2 C12 C17B -42.3(7) . .
C1 N2 C12 C17A -133.9(8) . .
C11 N2 C12 C17A 39.1(9) . .
C13B C12 C13A C14A -72.6(11) . .
C17B C12 C13A C14A 55.7(10) . .
C17A C12 C13A C14A -4.9(15) . .
N2 C12 C13A C14A 178.5(9) . .
C13A C12 C13B C14B 78.2(10) . .
C17B C12 C13B C14B 12.5(12) . .
C17A C12 C13B C14B -49.6(10) . .
N2 C12 C13B C14B -172.7(7) . .
C12 C13A C14A C15 4.3(15) . .
C12 C13B C14B C15 -9.8(14) . .
C13B C14B C15 C16A 60.2(11) . .
C13B C14B C15 C16B 5.5(13) . .
C13B C14B C15 C18 -174.0(8) . .
C13B C14B C15 C14A -64.1(9) . .
C13A C14A C15 C16A -11.3(15) . .
C13A C14A C15 C16B -61.2(10) . .
C13A C14A C15 C14B 64.8(9) . .
C13A C14A C15 C18 178.9(8) . .
C16B C15 C16A C17A 80.4(12) . .
C14B C15 C16A C17A -45.5(12) . .
C18 C15 C16A C17A -171.8(10) . .
C14A C15 C16A C17A 18.6(16) . .
C16A C15 C16B C17B -74.1(8) . .
C14B C15 C16B C17B -3.6(10) . .
C18 C15 C16B C17B 175.9(7) . .
C14A C15 C16B C17B 57.1(7) . .
C13A C12 C17A C16A 10.2(15) . .
C13B C12 C17A C16A 66.2(11) . .
C17B C12 C17A C16A -59.0(10) . .
N2 C12 C17A C16A -173.2(8) . .
C15 C16A C17A C12 -17.8(18) . .
C13A C12 C17B C16B -65.3(7) . .
C13B C12 C17B C16B -10.4(9) . .
C17A C12 C17B C16B 61.6(6) . .
N2 C12 C17B C16B 175.0(4) . .
C15 C16B C17B C12 5.8(9) . .
Zn1 O2 C18 O3B 47.6(15) 8_547 .
Zn1 O2 C18 C15 -162.5(6) 8_547 .
Zn1 O2 C18 O3A -37.4(11) 8_547 .
C16A C15 C18 O2 -45.2(15) . .
C16B C15 C18 O2 24.7(15) . .
C14B C15 C18 O2 -155.7(10) . .
C14A C15 C18 O2 124.9(12) . .
C16A C15 C18 O3B 107.2(11) . .
C16B C15 C18 O3B 177.1(9) . .
C14B C15 C18 O3B -3.4(14) . .
C14A C15 C18 O3B -82.8(12) . .
C16A C15 C18 O3A -166.1(10) . .
C16B C15 C18 O3A -96.3(9) . .
C14B C15 C18 O3A 83.3(13) . .
C14A C15 C18 O3A 3.9(12) . .
