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#$Date: 2016-03-21 18:33:37 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178816 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/70/4107066.cif $
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#
# 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_4107066
loop_
_publ_author_name
'Subash Chandra Sahoo'
'Tanay Kundu'
'Rahul Banerjee'
_publ_contact_author_address
;Dr. Rahul Banerjee
Scientist
Physical/Materials Chemistry Division
National Chemical Laboratory
Dr. Homi Bhabha Road
Pune 411008, India
;
_publ_contact_author_email       r.banerjee@ncl.res.in
_publ_contact_author_fax         '91 020 2590 2636'
_publ_contact_author_name        'Dr. Rahul Banerjee'
_publ_contact_author_phone       '91 020 2590 2535'
_publ_section_title
;
 Helical Water Chain Mediated Proton Conductivity in Homochiral
 Metal-Organic Frameworks with Unprecedented Zeolitic unh-Topology
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17950
_journal_page_last               17958
_journal_paper_doi               10.1021/ja2078637
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C11 H15 Br N2 O2 Zn, 2(O)'
_chemical_formula_sum            'C11 H15 Br N2 O4 Zn'
_chemical_formula_weight         384.54
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      169
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.768(2)
_cell_length_b                   17.768(2)
_cell_length_c                   10.4796(11)
_cell_measurement_reflns_used    5864
_cell_measurement_temperature    195(2)
_cell_measurement_theta_max      20.90
_cell_measurement_theta_min      2.29
_cell_volume                     2865.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      195(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33184
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.385
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       rod
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.620
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.294
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         4567
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0618
_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)+(0.1700P)²+0.0500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1928
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                3827
_reflns_number_total             4567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2078637_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4107066
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/6'
'-y, x-y, z+1/3'
'-x, -y, z+1/2'
'-x+y, -x, z+2/3'
'y, -x+y, z+5/6'
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 0.67968(7) 0.13151(7) 0.25161(13) 0.0677(4) Uani 1 1 d .
Zn1 Zn 0.52779(5) 0.07072(4) 0.26285(6) 0.0206(2) Uani 1 1 d .
O1 O 0.5117(3) 0.0273(3) 0.4589(4) 0.0254(10) Uani 1 1 d .
O2 O 0.5207(4) 0.0927(3) 0.0677(4) 0.0418(14) Uani 1 1 d .
N1 N 0.4331(3) -0.0595(3) 0.2435(4) 0.0202(10) Uani 1 1 d .
H1 H 0.4451 -0.0796 0.1708 0.024 Uiso 1 1 calc R
N2 N 0.4815(4) 0.1548(3) 0.3028(5) 0.0277(12) Uani 1 1 d .
C5 C 0.4790(4) -0.0532(4) 0.4690(6) 0.0221(13) Uani 1 1 d .
C4 C 0.4356(5) -0.1133(4) 0.3529(6) 0.0234(13) Uani 1 1 d .
H2 H 0.3752 -0.1539 0.3767 0.028 Uiso 1 1 calc R
C2 C 0.4780(5) -0.1676(4) 0.3220(6) 0.0322(15) Uani 1 1 d .
H3 H 0.4792 -0.1958 0.4018 0.039 Uiso 1 1 calc R
C1 C 0.5713(6) -0.1119(5) 0.2800(10) 0.045(2) Uani 1 1 d .
H4A H 0.5915 -0.1480 0.2428 0.068 Uiso 1 1 calc R
H4B H 0.6067 -0.0817 0.3524 0.068 Uiso 1 1 calc R
H4C H 0.5750 -0.0704 0.2179 0.068 Uiso 1 1 calc R
C3 C 0.4246(7) -0.2408(5) 0.2261(8) 0.052(2) Uani 1 1 d .
H9A H 0.4318 -0.2167 0.1421 0.078 Uiso 1 1 calc R
H9B H 0.3643 -0.2693 0.2495 0.078 Uiso 1 1 calc R
H9C H 0.4444 -0.2822 0.2270 0.078 Uiso 1 1 calc R
C10 C 0.4401(5) 0.1488(4) 0.4099(7) 0.0299(14) Uani 1 1 d .
H10 H 0.4268 0.1027 0.4649 0.036 Uiso 1 1 calc R
C9 C 0.4983(6) 0.2192(5) 0.2205(7) 0.0379(18) Uani 1 1 d .
H11 H 0.5276 0.2232 0.1450 0.045 Uiso 1 1 calc R
C11 C 0.4153(5) 0.2103(4) 0.4434(7) 0.0332(15) Uani 1 1 d .
H13 H 0.3879 0.2062 0.5209 0.040 Uiso 1 1 calc R
C7 C 0.4323(5) 0.2762(4) 0.3599(7) 0.0308(14) Uani 1 1 d .
C8 C 0.4733(6) 0.2793(5) 0.2453(7) 0.044(2) Uani 1 1 d .
H15 H 0.4837 0.3222 0.1856 0.053 Uiso 1 1 calc R
C6 C 0.3462(4) -0.0670(4) 0.2266(7) 0.0327(15) Uani 1 1 d .
H16A H 0.3306 -0.0492 0.3051 0.039 Uiso 1 1 calc R
H16B H 0.3503 -0.0273 0.1599 0.039 Uiso 1 1 calc R
O3 O 0.3107(6) 0.2622(6) 0.6983(10) 0.084(3) Uani 1 1 d .
O4 O 0.190(2) 0.048(3) 0.649(5) 0.327(17) Uiso 1 1 d .
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'
Br Br -0.2901 2.4595 '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
N2 Zn1 N1 115.4(2) . .
N2 Zn1 O2 88.9(2) . .
N1 Zn1 O2 91.21(19) . .
N2 Zn1 O1 92.1(2) . .
N1 Zn1 O1 78.86(17) . .
O2 Zn1 O1 169.4(2) . .
N2 Zn1 Br1 117.08(17) . .
N1 Zn1 Br1 127.50(16) . .
O2 Zn1 Br1 91.57(19) . .
O1 Zn1 Br1 97.34(14) . .
C5 O1 Zn1 113.1(4) . .
C5 O2 Zn1 133.2(4) 4_654 .
C6 N1 C4 113.0(5) . .
C6 N1 Zn1 109.6(4) . .
C4 N1 Zn1 111.5(3) . .
C6 N1 H1 107.5 . .
C4 N1 H1 107.5 . .
Zn1 N1 H1 107.5 . .
C10 N2 C9 119.7(6) . .
C10 N2 Zn1 121.3(4) . .
C9 N2 Zn1 119.0(5) . .
O2 C5 O1 125.6(6) 4_655 .
O2 C5 C4 113.8(5) 4_655 .
O1 C5 C4 120.6(5) . .
N1 C4 C2 114.8(5) . .
N1 C4 C5 108.9(4) . .
C2 C4 C5 111.7(6) . .
N1 C4 H2 107.0 . .
C2 C4 H2 107.0 . .
C5 C4 H2 107.0 . .
C1 C2 C4 112.0(6) . .
C1 C2 C3 112.0(7) . .
C4 C2 C3 112.4(7) . .
C1 C2 H3 106.7 . .
C4 C2 H3 106.7 . .
C3 C2 H3 106.7 . .
C2 C1 H4A 109.5 . .
C2 C1 H4B 109.5 . .
H4A C1 H4B 109.5 . .
C2 C1 H4C 109.5 . .
H4A C1 H4C 109.5 . .
H4B C1 H4C 109.5 . .
C2 C3 H9A 109.5 . .
C2 C3 H9B 109.5 . .
H9A C3 H9B 109.5 . .
C2 C3 H9C 109.5 . .
H9A C3 H9C 109.5 . .
H9B C3 H9C 109.5 . .
N2 C10 C11 121.8(6) . .
N2 C10 H10 119.1 . .
C11 C10 H10 119.1 . .
N2 C9 C8 121.4(7) . .
N2 C9 H11 119.3 . .
C8 C9 H11 119.3 . .
C7 C11 C10 118.8(6) . .
C7 C11 H13 120.6 . .
C10 C11 H13 120.6 . .
C11 C7 C8 118.3(6) . .
C11 C7 C6 121.4(7) . 2
C8 C7 C6 120.2(6) . 2
C9 C8 C7 120.0(6) . .
C9 C8 H15 120.0 . .
C7 C8 H15 120.0 . .
C7 C6 N1 113.7(6) 6_554 .
C7 C6 H16A 108.8 6_554 .
N1 C6 H16A 108.8 . .
C7 C6 H16B 108.8 6_554 .
N1 C6 H16B 108.8 . .
H16A C6 H16B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Zn1 2.3556(14) .
Zn1 N2 2.077(6) .
Zn1 N1 2.081(5) .
Zn1 O2 2.098(5) .
Zn1 O1 2.163(4) .
O1 C5 1.249(7) .
O2 C5 1.251(8) 4_654
N1 C6 1.492(9) .
N1 C4 1.508(7) .
N1 H1 0.9100 .
N2 C10 1.317(9) .
N2 C9 1.341(9) .
C5 O2 1.251(8) 4_655
C5 C4 1.547(8) .
C4 C2 1.528(9) .
C4 H2 0.9800 .
C2 C1 1.511(12) .
C2 C3 1.539(10) .
C2 H3 0.9800 .
C1 H4A 0.9600 .
C1 H4B 0.9600 .
C1 H4C 0.9600 .
C3 H9A 0.9600 .
C3 H9B 0.9600 .
C3 H9C 0.9600 .
C10 C11 1.412(9) .
C10 H10 0.9300 .
C9 C8 1.373(10) .
C9 H11 0.9300 .
C11 C7 1.369(10) .
C11 H13 0.9300 .
C7 C8 1.391(11) .
C7 C6 1.486(9) 2
C8 H15 0.9300 .
C6 C7 1.486(9) 6_554
C6 H16A 0.9700 .
C6 H16B 0.9700 .
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
N2 Zn1 O1 C5 136.4(5) . .
N1 Zn1 O1 C5 21.0(5) . .
O2 Zn1 O1 C5 41.3(14) . .
Br1 Zn1 O1 C5 -105.9(5) . .
N2 Zn1 O2 C5 -163.1(8) . 4_654
N1 Zn1 O2 C5 -47.7(8) . 4_654
O1 Zn1 O2 C5 -67.6(16) . 4_654
Br1 Zn1 O2 C5 79.9(7) . 4_654
N2 Zn1 N1 C6 15.4(5) . .
O2 Zn1 N1 C6 -73.9(4) . .
O1 Zn1 N1 C6 102.4(4) . .
Br1 Zn1 N1 C6 -166.8(3) . .
N2 Zn1 N1 C4 -110.4(4) . .
O2 Zn1 N1 C4 160.2(4) . .
O1 Zn1 N1 C4 -23.4(4) . .
Br1 Zn1 N1 C4 67.3(4) . .
N1 Zn1 N2 C10 64.0(6) . .
O2 Zn1 N2 C10 154.8(6) . .
O1 Zn1 N2 C10 -14.6(6) . .
Br1 Zn1 N2 C10 -114.0(5) . .
N1 Zn1 N2 C9 -119.5(6) . .
O2 Zn1 N2 C9 -28.7(6) . .
O1 Zn1 N2 C9 161.8(6) . .
Br1 Zn1 N2 C9 62.5(6) . .
Zn1 O1 C5 O2 164.3(6) . 4_655
Zn1 O1 C5 C4 -13.7(8) . .
C6 N1 C4 C2 133.1(6) . .
Zn1 N1 C4 C2 -103.0(5) . .
C6 N1 C4 C5 -100.9(6) . .
Zn1 N1 C4 C5 23.1(6) . .
O2 C5 C4 N1 175.8(6) 4_655 .
O1 C5 C4 N1 -6.0(9) . .
O2 C5 C4 C2 -56.4(8) 4_655 .
O1 C5 C4 C2 121.8(7) . .
N1 C4 C2 C1 59.7(8) . .
C5 C4 C2 C1 -64.8(7) . .
N1 C4 C2 C3 -67.4(8) . .
C5 C4 C2 C3 168.0(6) . .
C9 N2 C10 C11 -2.3(11) . .
Zn1 N2 C10 C11 174.1(6) . .
C10 N2 C9 C8 0.0(13) . .
Zn1 N2 C9 C8 -176.6(7) . .
N2 C10 C11 C7 2.3(12) . .
C10 C11 C7 C8 0.0(12) . .
C10 C11 C7 C6 -175.8(7) . 2
N2 C9 C8 C7 2.4(14) . .
C11 C7 C8 C9 -2.3(13) . .
C6 C7 C8 C9 173.6(8) 2 .
C4 N1 C6 C7 -63.4(7) . 6_554
Zn1 N1 C6 C7 171.6(5) . 6_554
