#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:44:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179153 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/14/4311494.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_4311494
loop_
_publ_author_name
'Sujit K. Ghosh'
'G. Savitha'
'Parimal K. Bharadwaj'
_publ_section_title
;
 Reactivity of Pyridine-2,4,6-tricarboxylic Acid toward Zn(II) Salts under
 Different Reaction Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5495
_journal_page_last               5497
_journal_paper_doi               10.1021/ic049490c
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C12 H12 N2 O5 Zn'
_chemical_formula_sum            'C12 H12 N2 O5 Zn'
_chemical_formula_weight         329.61
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 91.806(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   9.444(2)
_cell_length_b                   8.827(2)
_cell_length_c                   15.397(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.04
_cell_volume                     1282.9(5)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45  (Bruker, 2003)'
_computing_molecular_graphics    'Diamond 2.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8324
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        <0.05
_exptl_absorpt_coefficient_mu    1.935
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular parallelopipeds'
_exptl_crystal_F_000             672
_exptl_crystal_size_max          o.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.483
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.105
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0707P)²+2.4253P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                2683
_reflns_number_total             3144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049490csi20040709_100307_2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '100K' was changed to '100' -
the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '100K' was changed
to '100' - the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1282.9(11)
_cod_database_code               4311494
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.75438(4) 0.08271(4) 0.07703(3) 0.01546(14) Uani 1 1 d . . .
O1 O 0.9379(2) 0.1785(3) 0.03002(16) 0.0176(5) Uani 1 1 d . . .
O2 O 0.6419(3) 0.0968(3) -0.04521(16) 0.0179(5) Uani 1 1 d . . .
O3 O 0.5668(2) -0.0306(3) 0.10587(15) 0.0165(5) Uani 1 1 d . . .
O4 O 0.8605(3) -0.1150(3) 0.03335(17) 0.0182(5) Uani 1 1 d . . .
OW1 O 0.804(3) 0.482(2) 0.3194(13) 0.385(11) Uani 1 1 d . . .
N1 N 0.8250(3) 0.0350(3) 0.2073(2) 0.0183(6) Uani 1 1 d . . .
N2 N 0.6779(3) 0.3052(3) 0.10619(19) 0.0173(6) Uani 1 1 d . . .
C1 C 0.8865(6) 0.1350(5) 0.2590(3) 0.0439(13) Uani 1 1 d . . .
H1 H 0.8985 0.2331 0.2385 0.053 Uiso 1 1 calc R . .
C2 C 0.9346(9) 0.1010(6) 0.3430(3) 0.067(2) Uani 1 1 d . . .
H2 H 0.9795 0.1749 0.3769 0.080 Uiso 1 1 calc R . .
C3 C 0.9158(5) -0.0402(5) 0.3753(3) 0.0381(11) Uani 1 1 d . . .
H3 H 0.9468 -0.0651 0.4314 0.046 Uiso 1 1 calc R . .
C4 C 0.8491(5) -0.1456(6) 0.3222(4) 0.0496(14) Uani 1 1 d . . .
H4 H 0.8333 -0.2436 0.3419 0.060 Uiso 1 1 calc R . .
C5 C 0.8063(6) -0.1033(6) 0.2395(4) 0.0515(16) Uani 1 1 d . . .
H5 H 0.7617 -0.1753 0.2041 0.062 Uiso 1 1 calc R . .
C6 C 0.5994(6) 0.3355(5) 0.1739(3) 0.0539(16) Uani 1 1 d . . .
H6 H 0.5806 0.2576 0.2125 0.065 Uiso 1 1 calc R . .
C7 C 0.5440(7) 0.4777(6) 0.1898(3) 0.0582(18) Uani 1 1 d . . .
H7 H 0.4899 0.4942 0.2383 0.070 Uiso 1 1 calc R . .
C8 C 0.5694(4) 0.5937(4) 0.1334(3) 0.0243(8) Uani 1 1 d . . .
H8 H 0.5320 0.6898 0.1420 0.029 Uiso 1 1 calc R . .
C9 C 0.6517(5) 0.5634(4) 0.0640(3) 0.0315(9) Uani 1 1 d . . .
H9 H 0.6733 0.6399 0.0251 0.038 Uiso 1 1 calc R . .
C10 C 0.7026(5) 0.4187(4) 0.0521(3) 0.0287(9) Uani 1 1 d . . .
H10 H 0.7568 0.3997 0.0039 0.034 Uiso 1 1 calc R . .
C11 C 0.4778(3) -0.0366(4) 0.0437(2) 0.0140(6) Uani 1 1 d . . .
C12 C 0.9776(4) -0.0849(4) 0.0007(2) 0.0158(6) Uani 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'
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
O1 Zn1 O3 171.20(9) . . ?
O1 Zn1 O4 79.51(10) . . ?
O3 Zn1 O4 94.88(10) . . ?
O1 Zn1 O2 93.81(10) . . ?
O3 Zn1 O2 79.29(9) . . ?
O4 Zn1 O2 89.73(10) . . ?
O1 Zn1 N1 99.68(11) . . ?
O3 Zn1 N1 87.01(10) . . ?
O4 Zn1 N1 89.94(11) . . ?
O2 Zn1 N1 166.21(10) . . ?
O1 Zn1 N2 89.45(11) . . ?
O3 Zn1 N2 95.74(11) . . ?
O4 Zn1 N2 168.63(10) . . ?
O2 Zn1 N2 88.26(10) . . ?
N1 Zn1 N2 94.66(11) . . ?
C12 O1 Zn1 114.3(2) 3_755 . ?
C11 O2 Zn1 112.6(2) 3_655 . ?
C11 O3 Zn1 114.2(2) . . ?
C12 O4 Zn1 112.4(2) . . ?
C1 N1 C5 117.0(4) . . ?
C1 N1 Zn1 123.8(3) . . ?
C5 N1 Zn1 119.3(3) . . ?
C6 N2 C10 117.1(3) . . ?
C6 N2 Zn1 123.4(3) . . ?
C10 N2 Zn1 119.5(2) . . ?
N1 C1 C2 122.9(4) . . ?
C3 C2 C1 119.8(5) . . ?
C2 C3 C4 117.7(4) . . ?
C5 C4 C3 118.8(5) . . ?
N1 C5 C4 123.7(5) . . ?
N2 C6 C7 123.1(4) . . ?
C8 C7 C6 119.4(4) . . ?
C9 C8 C7 117.7(4) . . ?
C8 C9 C10 119.7(4) . . ?
N2 C10 C9 123.1(4) . . ?
O2 C11 O3 126.1(3) 3_655 . ?
O2 C11 C11 117.3(4) 3_655 3_655 ?
O3 C11 C11 116.7(3) . 3_655 ?
O1 C12 O4 126.2(3) 3_755 . ?
O1 C12 C12 116.9(4) 3_755 3_755 ?
O4 C12 C12 116.9(4) . 3_755 ?
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 O1 2.079(2) . ?
Zn1 O3 2.094(3) . ?
Zn1 O4 2.131(3) . ?
Zn1 O2 2.135(3) . ?
Zn1 N1 2.136(3) . ?
Zn1 N2 2.145(3) . ?
O1 C12 1.253(4) 3_755 ?
O2 C11 1.250(4) 3_655 ?
O3 C11 1.254(4) . ?
O4 C12 1.258(4) . ?
N1 C1 1.312(5) . ?
N1 C5 1.331(5) . ?
N2 C6 1.325(5) . ?
N2 C10 1.329(5) . ?
C1 C2 1.390(7) . ?
C2 C3 1.356(7) . ?
C3 C4 1.378(7) . ?
C4 C5 1.375(7) . ?
C6 C7 1.385(6) . ?
C7 C8 1.368(6) . ?
C8 C9 1.367(6) . ?
C9 C10 1.379(5) . ?
C11 O2 1.250(4) 3_655 ?
C11 C11 1.563(6) 3_655 ?
C12 O1 1.253(4) 3_755 ?
C12 C12 1.557(6) 3_755 ?
