#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/59/4105917.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_4105917
loop_
_publ_author_name
'Chang Yeon Lee'
'Youn-Sang Bae'
'Nak Cheon Jeong'
'Omar K. Farha'
'Amy A. Sarjeant'
'Charlotte L. Stern'
'Peter Nickias'
'Randall Q. Snurr'
'Joseph T. Hupp'
'SonBinh T. Nguyen'
_publ_section_title
;
 Kinetic Separation of Propene and Propane in Metal-Organic Frameworks:
 Controlling Diffusion Rates in Plate-Shaped Crystals via Tuning of Pore
 Apertures and Crystallite Aspect Ratios
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5228
_journal_page_last               5231
_journal_paper_doi               10.1021/ja200553m
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C16.5 H10.5 Br0.5 N2 O3.5 Zn0.5'
_chemical_formula_weight         365.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           10
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 1'
_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                 101.594(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.106(2)
_cell_length_b                   15.916(2)
_cell_length_c                   16.224(3)
_cell_measurement_reflns_used    2328
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.61
_cell_measurement_theta_min      2.78
_cell_volume                     2809.3(8)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1327
_diffrn_reflns_av_sigmaI/netI    0.1717
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10968
_diffrn_reflns_theta_full        57.73
_diffrn_reflns_theta_max         57.73
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  0.9571
_exptl_absorpt_correction_T_min  0.6680
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.864
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3624
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0800
_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)+(0.1147P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1897
_refine_ls_wR_factor_ref         0.2098
_reflns_number_gt                1820
_reflns_number_total             3624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200553m_si_004.cif
_cod_data_source_block           n0081
_cod_original_formula_sum        'C16.50 H10.50 Br0.50 N2 O3.50 Zn0.50'
_cod_database_code               4105917
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'-x, -y, -z'
'x, -y, 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
Br1 Br 0.79289(12) 0.0000 0.49640(12) 0.0831(7) Uani 1 2 d SU
Zn1 Zn 0.97304(11) 0.5000 0.40740(8) 0.0260(4) Uani 1 2 d SU
O1 O 0.8523(5) 0.4096(3) 0.4261(4) 0.0514(15) Uani 1 1 d U
O2 O 0.8931(5) 0.4102(3) 0.5649(4) 0.0477(14) Uani 1 1 d U
N1 N 0.9478(16) 0.5000 0.2879(7) 0.092(4) Uani 1 2 d SU
C1 C 0.8448(7) 0.3833(4) 0.4957(5) 0.0311(17) Uani 1 1 d U
C2 C 0.7606(6) 0.3055(4) 0.4961(5) 0.0316(16) Uani 1 1 d U
C3 C 0.7091(8) 0.2671(5) 0.4222(5) 0.052(2) Uani 1 1 d U
H3 H 0.7207 0.2902 0.3703 0.062 Uiso 1 1 calc R
C4 C 0.6406(9) 0.1951(5) 0.4224(6) 0.059(2) Uani 1 1 d U
H4 H 0.5998 0.1708 0.3708 0.071 Uiso 1 1 calc R
C5 C 0.6312(6) 0.1581(3) 0.4986(5) 0.0314(17) Uani 1 1 d U
C6 C 0.6840(8) 0.1977(4) 0.5721(5) 0.049(2) Uani 1 1 d U
H6 H 0.6739 0.1742 0.6241 0.058 Uiso 1 1 calc R
C7 C 0.7498(8) 0.2687(5) 0.5726(5) 0.049(2) Uani 1 1 d U
H7 H 0.7886 0.2936 0.6244 0.059 Uiso 1 1 calc R
C8 C 0.5599(6) 0.0775(4) 0.4969(5) 0.0343(18) Uani 1 1 d U
C9 C 0.6219(10) 0.0000 0.4968(8) 0.044(3) Uani 1 2 d SU
C10 C 1.055(3) 0.5000 0.2523(11) 0.158(7) Uani 1 2 d SU
H10 H 1.1321 0.5000 0.2899 0.190 Uiso 1 2 calc SR
C11 C 1.054(2) 0.5000 0.1644(10) 0.175(8) Uani 1 2 d SDU
H11 H 1.1311 0.5000 0.1469 0.209 Uiso 1 2 calc SR
C12 C 0.9474(19) 0.5000 0.1034(10) 0.126(6) Uani 1 2 d SDU
C13 C 0.841(2) 0.5000 0.1370(9) 0.176(8) Uani 1 2 d SDU
C14 C 0.846(3) 0.5000 0.2246(9) 0.160(8) Uani 1 2 d SDU
H14 H 0.7688 0.5000 0.2418 0.192 Uiso 1 2 calc SR
C15 C 0.933(3) 0.5000 0.0156(11) 0.156(9) Uani 1 2 d SU
H15 H 0.8556 0.5000 -0.0219 0.188 Uiso 1 2 calc SR
C16 C 0.726(3) 0.5000 0.083(3) 0.218(15) Uani 0.50 2 d SPDU
C17 C 0.620(4) 0.5000 0.046(6) 0.42(4) Uani 0.50 2 d SPDU
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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
N1 Zn1 O1 100.7(4) . .
N1 Zn1 O1 100.7(4) . 4_565
O1 Zn1 O1 90.2(3) . 4_565
N1 Zn1 O2 100.1(4) . 3_766
O1 Zn1 O2 159.1(2) . 3_766
O1 Zn1 O2 86.8(2) 4_565 3_766
N1 Zn1 O2 100.1(4) . 2_756
O1 Zn1 O2 86.8(2) . 2_756
O1 Zn1 O2 159.1(2) 4_565 2_756
O2 Zn1 O2 88.6(3) 3_766 2_756
N1 Zn1 Zn1 176.8(5) . 3_766
O1 Zn1 Zn1 81.51(17) . 3_766
O1 Zn1 Zn1 81.51(17) 4_565 3_766
O2 Zn1 Zn1 77.62(16) 3_766 3_766
O2 Zn1 Zn1 77.62(16) 2_756 3_766
C1 O1 Zn1 123.3(5) . .
C1 O2 Zn1 127.8(5) . 3_766
C14 N1 C10 109.1(15) . .
C14 N1 Zn1 134.0(13) . .
C10 N1 Zn1 116.8(14) . .
O2 C1 O1 129.1(6) . .
O2 C1 C2 115.5(6) . .
O1 C1 C2 115.4(7) . .
C3 C2 C7 119.8(6) . .
C3 C2 C1 120.0(7) . .
C7 C2 C1 119.7(7) . .
C2 C3 C4 120.4(7) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C3 C4 C5 119.6(8) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
C6 C5 C4 118.8(6) . .
C6 C5 C8 122.6(6) . .
C4 C5 C8 118.5(7) . .
C7 C6 C5 121.9(7) . .
C7 C6 H6 119.0 . .
C5 C6 H6 119.0 . .
C6 C7 C2 119.3(7) . .
C6 C7 H7 120.4 . .
C2 C7 H7 120.4 . .
C8 C8 C9 119.1(5) 2_656 .
C8 C8 C5 121.3(3) 2_656 .
C9 C8 C5 119.3(6) . .
C8 C9 C8 121.7(9) 4 .
C8 C9 Br1 119.2(5) 4 .
C8 C9 Br1 119.2(5) . .
N1 C10 C11 125(2) . .
N1 C10 H10 117.4 . .
C11 C10 H10 117.4 . .
C12 C11 C10 123(2) . .
C12 C11 H11 118.6 . .
C10 C11 H11 118.6 . .
C11 C12 C15 129(2) . .
C11 C12 C13 113.2(16) . .
C15 C12 C13 117.6(18) . .
C16 C13 C12 120(2) . .
C16 C13 C14 119(3) . .
C12 C13 C14 121.8(19) . .
N1 C14 C13 128(2) . .
N1 C14 H14 116.0 . .
C13 C14 H14 116.0 . .
C12 C15 C15 113(3) . 3_765
C12 C15 H15 123.7 . .
C15 C15 H15 123.7 3_765 .
C17 C16 C13 172(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C9 1.900(11) .
Zn1 N1 1.902(12) .
Zn1 O1 2.031(5) .
Zn1 O1 2.031(5) 4_565
Zn1 O2 2.046(5) 3_766
Zn1 O2 2.046(5) 2_756
Zn1 Zn1 2.943(3) 3_766
O1 C1 1.223(8) .
O2 C1 1.219(9) .
O2 Zn1 2.046(5) 3_766
N1 C14 1.37(3) .
N1 C10 1.42(3) .
C1 C2 1.553(10) .
C2 C3 1.364(10) .
C2 C7 1.399(10) .
C3 C4 1.376(11) .
C3 H3 0.9500 .
C4 C5 1.391(11) .
C4 H4 0.9500 .
C5 C6 1.372(11) .
C5 C8 1.504(9) .
C6 C7 1.346(10) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 C8 1.355(13) 2_656
C8 C9 1.414(8) .
C9 C8 1.414(8) 4
C10 C11 1.43(2) .
C10 H10 0.9500 .
C11 C12 1.386(10) .
C11 H11 0.9500 .
C12 C15 1.40(2) .
C12 C13 1.402(10) .
C13 C16 1.396(9) .
C13 C14 1.412(9) .
C14 H14 0.9500 .
C15 C15 1.66(5) 3_765
C15 H15 0.9500 .
C16 C17 1.206(9) .
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
N1 Zn1 O1 C1 173.7(6) . .
O1 Zn1 O1 C1 -85.4(6) 4_565 .
O2 Zn1 O1 C1 -3.7(9) 3_766 .
O2 Zn1 O1 C1 74.0(6) 2_756 .
Zn1 Zn1 O1 C1 -4.0(5) 3_766 .
O1 Zn1 N1 C14 46.14(17) . .
O1 Zn1 N1 C14 -46.14(17) 4_565 .
O2 Zn1 N1 C14 -134.79(17) 3_766 .
O2 Zn1 N1 C14 134.79(17) 2_756 .
Zn1 Zn1 N1 C14 180.000(15) 3_766 .
O1 Zn1 N1 C10 -133.86(17) . .
O1 Zn1 N1 C10 133.86(17) 4_565 .
O2 Zn1 N1 C10 45.21(17) 3_766 .
O2 Zn1 N1 C10 -45.21(17) 2_756 .
Zn1 Zn1 N1 C10 0.000(17) 3_766 .
Zn1 O2 C1 O1 -9.9(11) 3_766 .
Zn1 O2 C1 C2 170.9(4) 3_766 .
Zn1 O1 C1 O2 9.4(10) . .
Zn1 O1 C1 C2 -171.4(4) . .
O2 C1 C2 C3 -175.4(7) . .
O1 C1 C2 C3 5.3(9) . .
O2 C1 C2 C7 -3.2(9) . .
O1 C1 C2 C7 177.5(7) . .
C7 C2 C3 C4 3.9(13) . .
C1 C2 C3 C4 176.0(8) . .
C2 C3 C4 C5 -4.6(13) . .
C3 C4 C5 C6 4.4(12) . .
C3 C4 C5 C8 -177.6(8) . .
C4 C5 C6 C7 -3.5(12) . .
C8 C5 C6 C7 178.5(8) . .
C5 C6 C7 C2 2.8(13) . .
C3 C2 C7 C6 -2.9(12) . .
C1 C2 C7 C6 -175.1(7) . .
C6 C5 C8 C8 82.9(12) . 2_656
C4 C5 C8 C8 -95.1(11) . 2_656
C6 C5 C8 C9 -91.1(10) . .
C4 C5 C8 C9 90.9(10) . .
C8 C8 C9 C8 4.6(19) 2_656 4
C5 C8 C9 C8 178.8(7) . 4
C8 C8 C9 Br1 -175.5(8) 2_656 .
C5 C8 C9 Br1 -1.3(12) . .
C14 N1 C10 C11 0.000(4) . .
Zn1 N1 C10 C11 180.000(3) . .
N1 C10 C11 C12 0.000(4) . .
C10 C11 C12 C15 180.000(3) . .
C10 C11 C12 C13 0.000(2) . .
C11 C12 C13 C16 180.000(1) . .
C15 C12 C13 C16 0.0 . .
C11 C12 C13 C14 0.000(2) . .
C15 C12 C13 C14 180.000(3) . .
C10 N1 C14 C13 0.000(3) . .
Zn1 N1 C14 C13 180.000(3) . .
C16 C13 C14 N1 180.000(2) . .
C12 C13 C14 N1 0.000(3) . .
C11 C12 C15 C15 0.000(1) . 3_765
C13 C12 C15 C15 180.000(1) . 3_765
C12 C13 C16 C17 180.000(7) . .
C14 C13 C16 C17 0.000(13) . .
