#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:22:12 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179627 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/91/4509139.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4509139
loop_
_publ_author_name
'Mondal, Raju'
'Basu, Tannistha'
'Sadhukhan, Dipali'
'Chattopadhyay, Tanmay'
'Bhunia, Manas kumar'
_publ_contact_author
;
Dr. Raju Mondal 
;
_publ_section_title
;
 Influence of Anion on the Coordination Mode of a Flexible Neutral Ligand
 in Zn(II) Complexes: From Discrete Zero-Dimensional to Infinite 1D
 Helical Chains, 2D Nanoporous Bilayer Networks, and 3D Interpenetrated
 Metal−Organic Frameworks
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1095
_journal_paper_doi               10.1021/cg800923g
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C22 H32 N10 O6 Zn'
_chemical_formula_weight         597.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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                   13.4139(7)
_cell_length_b                   13.4139(7)
_cell_length_c                   31.309(3)
_cell_measurement_reflns_used    8870
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.5
_cell_volume                     5633.5(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0113
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            35322
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0297
_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)+(0.0420P)²+8.9639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                1197
_reflns_number_total             1407
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cg800923gsup1.cif
_cod_data_source_block           08rmd023_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      I4(1)/acd
_cod_database_code               4509139
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'
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 0.5000 0.2500 0.1250 0.01507(15) Uani 1 4 d S
N2 N 0.38699(11) 0.27937(12) 0.08600(4) 0.0192(3) Uani 1 1 d .
C6 C 0.37978(14) 0.35178(14) 0.05650(6) 0.0198(4) Uani 1 1 d .
N3 N 0.29912(13) 0.23034(14) 0.08482(6) 0.0286(4) Uani 1 1 d .
C5 C 0.46376(17) 0.42210(18) 0.04867(7) 0.0317(5) Uani 1 1 d .
C4 C 0.28730(14) 0.34820(14) 0.03653(6) 0.0241(4) Uani 1 1 d .
C3 C 0.2500 0.4112(2) 0.0000 0.0285(6) Uani 1 2 d S
C2 C 0.23749(16) 0.26975(17) 0.05576(7) 0.0339(5) Uani 1 1 d .
C1 C 0.1333(3) 0.2326(3) 0.05010(14) 0.0718(12) Uani 1 1 d .
N1 N 0.75976(15) 0.00976(15) 0.1250 0.0323(6) Uani 1 2 d S
O2 O 0.74454(14) 0.08666(12) 0.14529(5) 0.0486(5) Uani 1 1 d .
O1 O 0.69446(16) -0.05554(16) 0.1250 0.0825(12) Uani 1 2 d S
H3 H 0.3046(17) 0.4568(18) -0.0101(7) 0.035(7) Uiso 1 1 d .
H333 H 0.291(2) 0.177(2) 0.0980(9) 0.047(8) Uiso 1 1 d .
H5C H 0.440(3) 0.488(3) 0.0526(12) 0.093(12) Uiso 1 1 d .
H5B H 0.517(2) 0.414(2) 0.0680(10) 0.061(9) Uiso 1 1 d .
H5A H 0.488(3) 0.419(3) 0.0182(12) 0.099(13) Uiso 1 1 d .
H1C H 0.118(3) 0.182(3) 0.0696(12) 0.081(11) Uiso 1 1 d .
H1B H 0.143(3) 0.193(3) 0.0227(13) 0.094(13) Uiso 1 1 d .
H1A H 0.086(4) 0.277(4) 0.0434(15) 0.137(19) Uiso 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.01703(18) 0.01703(18) 0.0112(2) 0.000 0.000 0.000
N2 0.0181(8) 0.0218(8) 0.0178(7) 0.0021(6) -0.0025(6) -0.0036(6)
C6 0.0225(9) 0.0215(9) 0.0154(8) -0.0003(7) -0.0036(7) -0.0011(7)
N3 0.0244(9) 0.0298(10) 0.0317(9) 0.0109(8) -0.0078(7) -0.0104(7)
C5 0.0304(11) 0.0333(12) 0.0314(11) 0.0130(9) -0.0113(9) -0.0116(9)
C4 0.0253(10) 0.0245(10) 0.0226(9) -0.0004(7) -0.0075(8) -0.0015(8)
C3 0.0353(16) 0.0233(14) 0.0267(14) 0.000 -0.0159(12) 0.000
C2 0.0256(11) 0.0397(12) 0.0364(11) 0.0084(9) -0.0125(9) -0.0095(9)
C1 0.0393(17) 0.090(3) 0.087(3) 0.047(2) -0.0339(17) -0.0367(17)
N1 0.0365(10) 0.0365(10) 0.0237(12) -0.0002(7) 0.0002(7) 0.0125(13)
O2 0.0693(12) 0.0352(9) 0.0414(9) -0.0082(7) 0.0066(9) 0.0259(9)
O1 0.0986(18) 0.0986(18) 0.0504(17) -0.0281(13) 0.0281(13) -0.065(2)
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
N2 Zn1 N2 112.21(4) 20_656 .
N2 Zn1 N2 104.11(9) 20_656 27_565
N2 Zn1 N2 112.21(4) . 27_565
N2 Zn1 N2 112.21(4) 20_656 10_554
N2 Zn1 N2 104.11(9) . 10_554
N2 Zn1 N2 112.21(4) 27_565 10_554
C6 N2 N3 105.69(15) . .
C6 N2 Zn1 128.38(12) . .
N3 N2 Zn1 125.91(12) . .
N2 C6 C4 110.39(16) . .
N2 C6 C5 121.09(17) . .
C4 C6 C5 128.52(17) . .
C2 N3 N2 111.44(17) . .
C2 N3 H333 126.4(19) . .
N2 N3 H333 121.4(19) . .
C6 C5 H5C 109(2) . .
C6 C5 H5B 113.5(19) . .
H5C C5 H5B 106(3) . .
C6 C5 H5A 112(2) . .
H5C C5 H5A 106(3) . .
H5B C5 H5A 111(3) . .
C2 C4 C6 105.16(17) . .
C2 C4 C3 126.57(17) . .
C6 C4 C3 128.18(17) . .
C4 C3 C4 111.8(2) 5 .
C4 C3 H3 110.1(13) 5 .
C4 C3 H3 109.8(14) . .
N3 C2 C4 107.32(18) . .
N3 C2 C1 121.8(2) . .
C4 C2 C1 130.8(2) . .
C2 C1 H1C 112(2) . .
C2 C1 H1B 99(2) . .
H1C C1 H1B 102(3) . .
C2 C1 H1A 118(3) . .
H1C C1 H1A 119(4) . .
H1B C1 H1A 104(3) . .
O2 N1 O2 123.1(3) . 15_534
O2 N1 O1 118.44(15) . .
O2 N1 O1 118.44(15) 15_534 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N2 1.9860(15) 20_656
Zn1 N2 1.9860(15) .
Zn1 N2 1.9860(15) 27_565
Zn1 N2 1.9860(15) 10_554
N2 C6 1.344(2) .
N2 N3 1.350(2) .
C6 C4 1.390(3) .
C6 C5 1.490(3) .
N3 C2 1.338(3) .
N3 H333 0.83(3) .
C5 H5C 0.95(4) .
C5 H5B 0.95(3) .
C5 H5A 1.01(4) .
C4 C2 1.384(3) .
C4 C3 1.507(2) .
C3 C4 1.507(2) 5
C3 H3 1.01(2) .
C2 C1 1.494(3) .
C1 H1C 0.93(4) .
C1 H1B 1.02(4) .
C1 H1A 0.90(5) .
N1 O2 1.229(2) .
N1 O2 1.229(2) 15_534
N1 O1 1.239(4) .
