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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/4/10/70/4107069.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_4107069
loop_
_publ_author_name
'Subash Chandra Sahoo'
'Tanay Kundu'
'Rahul Banerjee'
_publ_contact_author_address
;Dr. Rahul Banerjee
Physical Chemistry Division
National Chemical Laboratory, Pune
Dr. Homi Bhabha Road
Maharashtra, 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 Cl N2 O2 Zn'
_chemical_formula_sum            'C11 H15 Cl N2 O2 Zn'
_chemical_formula_weight         308.09
_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                   17.7661(15)
_cell_length_b                   17.7661(15)
_cell_length_c                   10.5104(16)
_cell_measurement_reflns_used    4216
_cell_measurement_temperature    353(2)
_cell_measurement_theta_max      22.14
_cell_measurement_theta_min      2.29
_cell_volume                     2873.0(6)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      353(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.1086
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11671
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.32
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              X-ray
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       rod
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.264
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         4331
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0642
_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)+(0.0740P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1665
_reflns_number_gt                3241
_reflns_number_total             4331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2078637_si_002_5.cif
_cod_data_source_block           1'
_cod_database_code               4107069
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
Zn1 Zn 0.54374(5) 0.47053(5) 0.36838(8) 0.0341(2) Uani 1 1 d .
Cl1 Cl 0.46003(19) 0.32803(15) 0.3602(3) 0.0897(8) Uani 1 1 d .
O1 O 0.5749(4) 0.4848(4) 0.1726(5) 0.0509(14) Uani 1 1 d .
O2 O 0.5168(3) 0.4891(3) 0.5651(4) 0.0389(11) Uani 1 1 d .
N1 N 0.6740(4) 0.5187(4) 0.4086(5) 0.0425(15) Uani 1 1 d .
N2 N 0.5064(3) 0.5652(3) 0.3497(5) 0.0313(12) Uani 1 1 d .
H1A H 0.4747 0.5539 0.2770 0.038 Uiso 1 1 calc R
C1 C 0.7220(5) 0.5051(6) 0.3250(8) 0.060(2) Uani 1 1 d .
H1 H 0.6977 0.4792 0.2474 0.072 Uiso 1 1 calc R
C5 C 0.7083(4) 0.5561(5) 0.5177(7) 0.0460(17) Uani 1 1 d .
H2 H 0.6747 0.5668 0.5746 0.055 Uiso 1 1 calc R
C4 C 0.7922(5) 0.5799(5) 0.5508(8) 0.054(2) Uani 1 1 d .
H3 H 0.8139 0.6051 0.6297 0.065 Uiso 1 1 calc R
C7 C 0.4501(4) 0.5612(5) 0.4591(7) 0.0360(15) Uani 1 1 d .
H4 H 0.4696 0.6214 0.4834 0.043 Uiso 1 1 calc R
C11 C 0.5333(4) 0.4817(4) 0.0751(6) 0.0325(15) Uani 1 1 d .
C8 C 0.3547(5) 0.5202(5) 0.4263(7) 0.0487(19) Uani 1 1 d .
H7 H 0.3248 0.5182 0.5057 0.058 Uiso 1 1 calc R
C10 C 0.3183(6) 0.4275(7) 0.3847(10) 0.077(3) Uani 1 1 d .
H8A H 0.3474 0.4259 0.3087 0.115 Uiso 1 1 calc R
H8B H 0.2573 0.4022 0.3680 0.115 Uiso 1 1 calc R
H8C H 0.3271 0.3954 0.4507 0.115 Uiso 1 1 calc R
C3 C 0.8451(5) 0.5665(5) 0.4667(7) 0.0448(18) Uani 1 1 d .
C6 C 0.5865(5) 0.6506(4) 0.3348(7) 0.0425(17) Uani 1 1 d .
H10A H 0.6225 0.6463 0.2689 0.051 Uiso 1 1 calc R
H10B H 0.6191 0.6658 0.4138 0.051 Uiso 1 1 calc R
C9 C 0.3353(6) 0.5752(7) 0.3323(9) 0.073(3) Uani 1 1 d .
H38A H 0.3647 0.6347 0.3598 0.109 Uiso 1 1 calc R
H38B H 0.2738 0.5536 0.3297 0.109 Uiso 1 1 calc R
H38C H 0.3553 0.5716 0.2490 0.109 Uiso 1 1 calc R
C2 C 0.8067(5) 0.5284(7) 0.3509(8) 0.066(3) Uani 1 1 d .
H41 H 0.8389 0.5186 0.2902 0.079 Uiso 1 1 calc R
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'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 '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 N2 115.0(2) . .
N1 Zn1 O1 88.7(2) . .
N2 Zn1 O1 88.99(19) . .
N1 Zn1 O2 91.6(2) . .
N2 Zn1 O2 77.68(18) . .
O1 Zn1 O2 165.43(18) . .
N1 Zn1 Cl1 117.11(19) . .
N2 Zn1 Cl1 127.80(17) . .
O1 Zn1 Cl1 94.90(17) . .
O2 Zn1 Cl1 97.90(15) . .
C11 O1 Zn1 132.8(4) . .
C11 O2 Zn1 113.7(4) 4_665 .
C5 N1 C1 119.4(6) . .
C5 N1 Zn1 121.9(5) . .
C1 N1 Zn1 118.4(5) . .
C6 N2 C7 114.0(5) . .
C6 N2 Zn1 107.6(4) . .
C7 N2 Zn1 111.1(4) . .
C6 N2 H1A 108.0 . .
C7 N2 H1A 108.0 . .
Zn1 N2 H1A 108.0 . .
N1 C1 C2 121.4(7) . .
N1 C1 H1 119.3 . .
C2 C1 H1 119.3 . .
N1 C5 C4 122.3(7) . .
N1 C5 H2 118.8 . .
C4 C5 H2 118.8 . .
C5 C4 C3 120.4(7) . .
C5 C4 H3 119.8 . .
C3 C4 H3 119.8 . .
N2 C7 C8 114.1(6) . .
N2 C7 C11 109.9(5) . 4_665
C8 C7 C11 112.8(6) . 4_665
N2 C7 H4 106.5 . .
C8 C7 H4 106.5 . .
C11 C7 H4 106.5 4_665 .
O2 C11 O1 125.9(6) 4_664 .
O2 C11 C7 119.7(6) 4_664 4_664
O1 C11 C7 114.4(5) . 4_664
C10 C8 C7 111.0(6) . .
C10 C8 C9 113.4(7) . .
C7 C8 C9 113.1(7) . .
C10 C8 H7 106.3 . .
C7 C8 H7 106.3 . .
C9 C8 H7 106.3 . .
C8 C10 H8A 109.5 . .
C8 C10 H8B 109.5 . .
H8A C10 H8B 109.5 . .
C8 C10 H8C 109.5 . .
H8A C10 H8C 109.5 . .
H8B C10 H8C 109.5 . .
C2 C3 C4 115.4(6) . .
C2 C3 C6 122.0(6) . 2_655
C4 C3 C6 122.5(7) . 2_655
N2 C6 C3 111.8(5) . 6_564
N2 C6 H10A 109.3 . .
C3 C6 H10A 109.3 6_564 .
N2 C6 H10B 109.3 . .
C3 C6 H10B 109.3 6_564 .
H10A C6 H10B 107.9 . .
C8 C9 H38A 109.5 . .
C8 C9 H38B 109.5 . .
H38A C9 H38B 109.5 . .
C8 C9 H38C 109.5 . .
H38A C9 H38C 109.5 . .
H38B C9 H38C 109.5 . .
C1 C2 C3 121.0(7) . .
C1 C2 H41 119.5 . .
C3 C2 H41 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.070(5) .
Zn1 N2 2.104(4) .
Zn1 O1 2.113(5) .
Zn1 O2 2.184(4) .
Zn1 Cl1 2.205(3) .
O1 C11 1.249(8) .
O2 C11 1.237(7) 4_665
N1 C5 1.312(10) .
N1 C1 1.328(9) .
N2 C6 1.481(9) .
N2 C7 1.502(8) .
N2 H1A 0.9100 .
C1 C2 1.374(11) .
C1 H1 0.9300 .
C5 C4 1.376(10) .
C5 H2 0.9300 .
C4 C3 1.394(10) .
C4 H3 0.9300 .
C7 C8 1.513(9) .
C7 C11 1.543(9) 4_665
C7 H4 0.9800 .
C11 O2 1.237(7) 4_664
C11 C7 1.543(9) 4_664
C8 C10 1.502(12) .
C8 C9 1.545(10) .
C8 H7 0.9800 .
C10 H8A 0.9600 .
C10 H8B 0.9600 .
C10 H8C 0.9600 .
C3 C2 1.394(11) .
C3 C6 1.514(9) 2_655
C6 C3 1.514(9) 6_564
C6 H10A 0.9700 .
C6 H10B 0.9700 .
C9 H38A 0.9600 .
C9 H38B 0.9600 .
C9 H38C 0.9600 .
C2 H41 0.9300 .
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 C11 -167.5(6) . .
N2 Zn1 O1 C11 -52.5(6) . .
O2 Zn1 O1 C11 -76.1(11) . .
Cl1 Zn1 O1 C11 75.4(6) . .
N1 Zn1 O2 C11 138.6(5) . 4_665
N2 Zn1 O2 C11 23.4(4) . 4_665
O1 Zn1 O2 C11 47.5(10) . 4_665
Cl1 Zn1 O2 C11 -103.7(4) . 4_665
N2 Zn1 N1 C5 67.6(7) . .
O1 Zn1 N1 C5 155.9(6) . .
O2 Zn1 N1 C5 -9.6(6) . .
Cl1 Zn1 N1 C5 -109.3(6) . .
N2 Zn1 N1 C1 -117.8(6) . .
O1 Zn1 N1 C1 -29.5(6) . .
O2 Zn1 N1 C1 165.1(6) . .
Cl1 Zn1 N1 C1 65.3(6) . .
N1 Zn1 N2 C6 15.2(5) . .
O1 Zn1 N2 C6 -72.9(4) . .
O2 Zn1 N2 C6 101.2(4) . .
Cl1 Zn1 N2 C6 -168.3(4) . .
N1 Zn1 N2 C7 -110.2(4) . .
O1 Zn1 N2 C7 161.7(4) . .
O2 Zn1 N2 C7 -24.2(4) . .
Cl1 Zn1 N2 C7 66.3(5) . .
C5 N1 C1 C2 0.7(13) . .
Zn1 N1 C1 C2 -174.1(7) . .
C1 N1 C5 C4 -1.7(12) . .
Zn1 N1 C5 C4 172.9(6) . .
N1 C5 C4 C3 1.3(12) . .
C6 N2 C7 C8 133.6(6) . .
Zn1 N2 C7 C8 -104.7(5) . .
C6 N2 C7 C11 -98.5(6) . 4_665
Zn1 N2 C7 C11 23.2(7) . 4_665
Zn1 O1 C11 O2 38.5(10) . 4_664
Zn1 O1 C11 C7 -142.9(5) . 4_664
N2 C7 C8 C10 61.6(9) . .
C11 C7 C8 C10 -64.8(8) 4_665 .
N2 C7 C8 C9 -67.1(8) . .
C11 C7 C8 C9 166.5(6) 4_665 .
C5 C4 C3 C2 0.1(12) . .
C5 C4 C3 C6 -176.2(8) . 2_655
C7 N2 C6 C3 -65.3(7) . 6_564
Zn1 N2 C6 C3 171.1(5) . 6_564
N1 C1 C2 C3 0.7(14) . .
C4 C3 C2 C1 -1.0(13) . .
C6 C3 C2 C1 175.3(8) 2_655 .
