#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:00:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180367 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/36/7203634.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_7203634
loop_
_publ_author_name
'Kumar, D. Krishna'
'Das, Amitava'
'Dastidar, Parthasarathi'
_publ_section_title
;
 Hydrogen-bonded microporous network, helix and 1-D zigzag chains in
 MOFs of Zn(ii): studying the effects of ligating topologies, hydrogen
 bonding backbone and counter-anions
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              805
_journal_paper_doi               10.1039/b612163m
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C13 H20 Cl2 N4 O3 Zn'
_chemical_formula_weight         416.62
_chemical_name_systematic
;
?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   19.1929(13)
_cell_length_b                   7.1978(5)
_cell_length_c                   24.4277(17)
_cell_measurement_temperature    100(2)
_cell_volume                     3374.6(4)
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_collection       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_molecular_graphics    'BRUKER SHELXLTL'
_computing_publication_material  'MERCURY 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'BRUKER SMART CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18871
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  0.8701
_exptl_absorpt_correction_T_min  0.5202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   BRUKER-SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0477
_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)+(0.0509P)²+5.0479P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                3302
_reflns_number_total             4036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b612163m.txt
_cod_data_source_block           kkb482i
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'ORTHORHOMBIC' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7203634
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-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_assembly
_atom_site_disorder_group
Zn1 Zn 0.110954(17) 1.08231(5) 0.113250(13) 0.02123(12) Uani 1 1 d . . .
Cl1 Cl 0.00155(4) 1.01305(17) 0.08740(3) 0.0439(3) Uani 1 1 d . . .
Cl2 Cl 0.12343(4) 1.37593(12) 0.14162(3) 0.02676(19) Uani 1 1 d . . .
N1 N 0.13319(13) 0.9271(4) 0.18021(10) 0.0239(6) Uani 1 1 d . . .
C2 C 0.08718(16) 0.8021(5) 0.19924(13) 0.0257(7) Uani 1 1 d . . .
H2 H 0.0487 0.7734 0.1777 0.031 Uiso 1 1 calc R . .
C3 C 0.09395(16) 0.7150(5) 0.24853(13) 0.0279(7) Uani 1 1 d . . .
H3 H 0.0603 0.6305 0.2599 0.033 Uiso 1 1 calc R . .
C4 C 0.15120(15) 0.7522(5) 0.28193(12) 0.0238(7) Uani 1 1 d . . .
C5 C 0.20071(17) 0.8770(5) 0.26208(13) 0.0309(8) Uani 1 1 d . . .
H5 H 0.2406 0.9037 0.2822 0.037 Uiso 1 1 calc R . .
C6 C 0.18936(17) 0.9597(6) 0.21218(13) 0.0317(8) Uani 1 1 d . . .
H6 H 0.2225 1.0436 0.1996 0.038 Uiso 1 1 calc R . .
N7 N 0.15362(13) 0.6665(4) 0.33290(11) 0.0284(6) Uani 1 1 d . . .
H7 H 0.1176 0.6038 0.3427 0.034 Uiso 1 1 calc R . .
C8 C 0.20877(15) 0.6729(5) 0.36927(12) 0.0213(6) Uani 1 1 d . . .
O9 O 0.26508(11) 0.7386(3) 0.35818(8) 0.0244(5) Uani 1 1 d . . .
N10 N 0.19187(13) 0.5966(4) 0.41927(11) 0.0256(6) Uani 1 1 d . . .
H10 H 0.1489 0.5691 0.4249 0.031 Uiso 1 1 calc R . .
C11 C 0.23874(15) 0.5607(4) 0.46129(12) 0.0203(6) Uani 1 1 d . . .
C12 C 0.21182(15) 0.5124(5) 0.51265(12) 0.0221(6) Uani 1 1 d . . .
H12 H 0.1639 0.5066 0.5179 0.026 Uiso 1 1 calc R . .
C13 C 0.25602(15) 0.4741(4) 0.55496(11) 0.0187(6) Uani 1 1 d . . .
H13 H 0.2370 0.4421 0.5887 0.022 Uiso 1 1 calc R . .
N14 N 0.32600(12) 0.4804(3) 0.55022(10) 0.0168(5) Uani 1 1 d . . .
C15 C 0.35206(15) 0.5263(4) 0.50081(12) 0.0190(6) Uani 1 1 d . . .
H15 H 0.4002 0.5307 0.4969 0.023 Uiso 1 1 calc R . .
C16 C 0.31145(15) 0.5672(4) 0.45568(12) 0.0202(6) Uani 1 1 d . . .
H16 H 0.3318 0.5982 0.4224 0.024 Uiso 1 1 calc R . .
C17 C 0.0751(3) 0.2458(8) 0.3001(2) 0.0544(13) Uani 1 1 d . . .
O18 O 0.04545(16) 0.3977(5) 0.32842(15) 0.0556(9) Uani 1 1 d . . .
C19A C -0.0061(3) 0.4203(10) 0.5285(3) 0.0261(14) Uiso 0.50 1 d P . .
C19B C 0.0164(3) 0.4596(10) 0.4701(3) 0.0255(14) Uiso 0.50 1 d P . .
O20A O 0.0577(2) 0.6231(6) 0.46642(18) 0.0236(9) Uiso 0.50 1 d P . .
O20B O -0.0560(2) 0.5567(6) 0.54732(18) 0.0259(10) Uiso 0.50 1 d P . .
H17A H 0.042(4) 0.162(9) 0.285(3) 0.11(2) Uiso 1 1 d . . .
H17B H 0.106(3) 0.174(9) 0.326(3) 0.10(2) Uiso 1 1 d . . .
H17C H 0.107(3) 0.259(9) 0.275(3) 0.10(2) Uiso 1 1 d . . .
H18 H 0.009(3) 0.378(8) 0.341(2) 0.070(18) 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'
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N14 Zn1 N1 111.59(10) 2_564 . ?
N14 Zn1 Cl2 112.64(8) 2_564 . ?
N1 Zn1 Cl2 104.37(8) . . ?
N14 Zn1 Cl1 107.30(7) 2_564 . ?
N1 Zn1 Cl1 107.53(8) . . ?
Cl2 Zn1 Cl1 113.35(4) . . ?
C2 N1 C6 116.1(3) . . ?
C2 N1 Zn1 120.7(2) . . ?
C6 N1 Zn1 122.6(2) . . ?
N1 C2 C3 123.4(3) . . ?
N1 C2 H2 118.3 . . ?
C3 C2 H2 118.3 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
N7 C4 C5 125.1(3) . . ?
N7 C4 C3 117.7(3) . . ?
C5 C4 C3 117.2(3) . . ?
C6 C5 C4 118.7(3) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
N1 C6 C5 124.3(3) . . ?
N1 C6 H6 117.8 . . ?
C5 C6 H6 117.8 . . ?
C8 N7 C4 125.9(3) . . ?
C8 N7 H7 117.1 . . ?
C4 N7 H7 117.1 . . ?
O9 C8 N10 124.3(3) . . ?
O9 C8 N7 123.6(3) . . ?
N10 C8 N7 112.1(3) . . ?
C8 N10 C11 125.2(3) . . ?
C8 N10 H10 117.4 . . ?
C11 N10 H10 117.4 . . ?
N10 C11 C12 118.0(3) . . ?
N10 C11 C16 124.4(3) . . ?
C12 C11 C16 117.6(3) . . ?
C13 C12 C11 119.9(3) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
N14 C13 C12 123.1(3) . . ?
N14 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
C15 N14 C13 117.0(2) . . ?
C15 N14 Zn1 121.19(19) . 2_565 ?
C13 N14 Zn1 121.75(19) . 2_565 ?
N14 C15 C16 123.9(3) . . ?
N14 C15 H15 118.1 . . ?
C16 C15 H15 118.1 . . ?
C15 C16 C11 118.4(3) . . ?
C15 C16 H16 120.8 . . ?
C11 C16 H16 120.8 . . ?
O18 C17 H17A 115(4) 1 . ?
O18 C17 H17A 115(4) . . ?
O18 C17 H17B 109(4) 1 . ?
O18 C17 H17B 109(4) . . ?
H17A C17 H17B 108(5) . . ?
O18 C17 H17C 123(4) 1 . ?
O18 C17 H17C 123(4) . . ?
H17A C17 H17C 106(5) . . ?
H17B C17 H17C 94(5) . . ?
C17 O18 H18 114(4) . . ?
C19B C19A O20A 94.3(8) 5_566 5_566 ?
C19B C19A O20B 34.8(5) 5_566 . ?
O20A C19A O20B 62.5(4) 5_566 . ?
C19B C19A C19B 85.4(8) 5_566 . ?
O20A C19A C19B 115.9(6) 5_566 . ?
O20B C19A C19B 111.2(6) . . ?
C19B C19A C19A 56.3(6) 5_566 5_566 ?
O20A C19A C19A 113.7(7) 5_566 5_566 ?
O20B C19A C19A 84.3(5) . 5_566 ?
C19B C19A C19A 29.1(3) . 5_566 ?
O20B C19B C19A 110.0(9) 5_566 5_566 ?
O20B C19B O20A 66.2(6) 5_566 . ?
C19A C19B O20A 47.2(6) 5_566 . ?
O20B C19B O20A 66.2(6) 5_566 1 ?
C19A C19B O20A 47.2(6) 5_566 1 ?
O20B C19B C19A 132.5(8) 5_566 . ?
C19A C19B C19A 94.6(8) 5_566 . ?
O20A C19B C19A 111.8(6) . . ?
O20A C19B C19A 111.8(6) 1 . ?
O20B C19B C19B 141.6(9) 5_566 5_566 ?
C19A C19B C19B 63.1(7) 5_566 5_566 ?
O20A C19B C19B 88.7(6) . 5_566 ?
O20A C19B C19B 88.7(6) 1 5_566 ?
C19A C19B C19B 31.4(3) . 5_566 ?
C19A O20A O20B 73.6(5) 5_566 5_566 ?
C19A O20A C19B 38.5(4) 5_566 . ?
O20B O20A C19B 37.0(3) 5_566 . ?
C19B O20B O20A 76.8(6) 5_566 5_566 ?
C19B O20B C19A 35.2(5) 5_566 . ?
O20A O20B C19A 43.9(3) 5_566 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N14 2.010(2) 2_564 ?
Zn1 N1 2.026(3) . ?
Zn1 Cl2 2.2370(9) . ?
Zn1 Cl1 2.2486(8) . ?
N1 C2 1.344(4) . ?
N1 C6 1.352(4) . ?
C2 C3 1.363(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(4) . ?
C3 H3 0.9300 . ?
C4 N7 1.390(4) . ?
C4 C5 1.395(4) . ?
C5 C6 1.374(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
N7 C8 1.383(4) . ?
N7 H7 0.8600 . ?
C8 O9 1.210(4) . ?
C8 N10 1.378(4) . ?
N10 C11 1.389(4) . ?
N10 H10 0.8600 . ?
C11 C12 1.401(4) . ?
C11 C16 1.403(4) . ?
C12 C13 1.365(4) . ?
C12 H12 0.9300 . ?
C13 N14 1.349(4) . ?
C13 H13 0.9300 . ?
N14 C15 1.348(4) . ?
N14 Zn1 2.010(2) 2_565 ?
C15 C16 1.382(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 O18 1.413(7) 1 ?
C17 O18 1.413(7) . ?
C17 H17A 0.95(7) . ?
C17 H17B 1.00(7) . ?
C17 H17C 0.87(7) . ?
O18 H18 0.77(5) . ?
C19A C19B 0.887(8) 5_566 ?
C19A O20A 1.046(7) 5_566 ?
C19A O20B 1.446(8) . ?
C19A C19B 1.517(9) . ?
C19A C19A 1.818(14) 5_566 ?
C19B O20B 0.879(7) 5_566 ?
C19B C19A 0.887(8) 5_566 ?
C19B O20A 1.422(8) . ?
C19B O20A 1.422(8) 1 ?
C19B C19B 1.696(13) 5_566 ?
O20A C19A 1.046(7) 5_566 ?
O20A O20B 1.337(6) 5_566 ?
O20B C19B 0.879(7) 5_566 ?
O20B O20A 1.337(6) 5_566 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O18 0.86 2.06 2.840(4) 150.7 1
N10 H10 O20A 0.86 2.06 2.827(5) 148.3 1
N10 H10 O20B 0.86 2.11 2.947(5) 163.9 5_566
O18 H18 Cl2 0.77(5) 2.58(5) 3.327(3) 163(5) 3_545
C3 H3 O18 0.93 2.39 3.145(4) 138.8 1
C12 H12 O20A 0.93 2.54 3.265(5) 135.3 1
