#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:44:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179153 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/14/4311493.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_4311493
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 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.724(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   9.444(3)
_cell_length_b                   9.162(3)
_cell_length_c                   14.979(2)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.04
_cell_volume                     1291.7(6)
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8473
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        <0.05
_exptl_absorpt_coefficient_mu    1.922
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular parallelopiped'
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.770
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.810
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0756P)²+4.8980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                2681
_reflns_number_total             3172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049490csi20040709_100307_1.cif
_cod_data_source_block           Compound1
_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        1291.7(11)
_cod_database_code               4311493
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.24998(3) 0.15236(3) -0.004751(19) 0.01017(13) Uani 1 1 d . . .
O1 O -0.0699(2) -0.1420(2) -0.06856(13) 0.0131(4) Uani 1 1 d . . .
O2 O 0.1320(2) -0.0166(2) -0.07486(13) 0.0134(4) Uani 1 1 d . . .
O3 O 0.3637(2) -0.0123(2) 0.07210(13) 0.0130(4) Uani 1 1 d . . .
O4 O 0.5689(2) -0.1338(2) 0.07443(13) 0.0127(4) Uani 1 1 d . . .
OW1 O 0.6921(12) 0.2851(14) 0.0795(8) 0.254(5) Uani 1 1 d . . .
N1 N 0.3290(2) 0.3148(3) 0.08958(16) 0.0132(5) Uani 1 1 d . . .
N2 N 0.1639(2) 0.3078(3) -0.10158(15) 0.0128(5) Uani 1 1 d . . .
C1 C 0.2239(3) 0.3348(3) -0.17824(19) 0.0173(6) Uani 1 1 d . . .
H1 H 0.3051 0.2829 -0.1896 0.021 Uiso 1 1 calc R . .
C2 C 0.1709(3) 0.4355(4) -0.2410(2) 0.0207(6) Uani 1 1 d . . .
H2 H 0.2150 0.4503 -0.2935 0.025 Uiso 1 1 calc R . .
C3 C 0.0505(3) 0.5142(3) -0.22406(19) 0.0181(6) Uani 1 1 d . . .
H3 H 0.0124 0.5832 -0.2648 0.022 Uiso 1 1 calc R . .
C4 C -0.0120(3) 0.4876(3) -0.14499(19) 0.0194(6) Uani 1 1 d . . .
H4 H -0.0925 0.5390 -0.1317 0.023 Uiso 1 1 calc R . .
C5 C 0.0471(3) 0.3836(3) -0.08609(18) 0.0153(5) Uani 1 1 d . . .
H5 H 0.0039 0.3656 -0.0336 0.018 Uiso 1 1 calc R . .
C6 C 0.3634(3) 0.4515(3) 0.06676(19) 0.0173(6) Uani 1 1 d . . .
H6 H 0.3579 0.4758 0.0063 0.021 Uiso 1 1 calc R . .
C7 C 0.4063(3) 0.5572(4) 0.1286(2) 0.0226(6) Uani 1 1 d . . .
H7 H 0.4290 0.6506 0.1101 0.027 Uiso 1 1 calc R . .
C8 C 0.4149(3) 0.5220(4) 0.2187(2) 0.0217(6) Uani 1 1 d . . .
H8 H 0.4439 0.5912 0.2618 0.026 Uiso 1 1 calc R . .
C9 C 0.3794(3) 0.3814(4) 0.2434(2) 0.0213(6) Uani 1 1 d . . .
H9 H 0.3835 0.3550 0.3035 0.026 Uiso 1 1 calc R . .
C10 C 0.3378(3) 0.2811(3) 0.17723(18) 0.0166(6) Uani 1 1 d . . .
H10 H 0.3150 0.1869 0.1941 0.020 Uiso 1 1 calc R . .
C11 C 0.4799(3) -0.0420(3) 0.04234(17) 0.0111(5) Uani 1 1 d . . .
C12 C 0.0181(3) -0.0462(3) -0.04154(16) 0.0113(5) 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
O4 Zn1 O1 172.61(8) 3_655 3 ?
O4 Zn1 O2 96.40(8) 3_655 . ?
O1 Zn1 O2 79.16(8) 3 . ?
O4 Zn1 O3 79.35(8) 3_655 . ?
O1 Zn1 O3 94.54(8) 3 . ?
O2 Zn1 O3 88.37(9) . . ?
O4 Zn1 N1 97.53(9) 3_655 . ?
O1 Zn1 N1 86.56(8) 3 . ?
O2 Zn1 N1 165.48(8) . . ?
O3 Zn1 N1 90.16(9) . . ?
O4 Zn1 N2 89.80(8) 3_655 . ?
O1 Zn1 N2 96.04(9) 3 . ?
O2 Zn1 N2 89.74(9) . . ?
O3 Zn1 N2 168.70(8) . . ?
N1 Zn1 N2 94.40(10) . . ?
C12 O1 Zn1 114.01(17) . 3 ?
C12 O2 Zn1 113.10(17) . . ?
C11 O3 Zn1 112.30(17) . . ?
C11 O4 Zn1 114.46(17) . 3_655 ?
C10 N1 C6 117.7(3) . . ?
C10 N1 Zn1 118.3(2) . . ?
C6 N1 Zn1 123.85(19) . . ?
C5 N2 C1 117.6(2) . . ?
C5 N2 Zn1 119.92(19) . . ?
C1 N2 Zn1 122.45(19) . . ?
N2 C1 C2 123.3(3) . . ?
C1 C2 C3 118.6(3) . . ?
C2 C3 C4 118.5(3) . . ?
C5 C4 C3 119.2(3) . . ?
N2 C5 C4 122.7(3) . . ?
N1 C6 C7 123.2(3) . . ?
C6 C7 C8 118.9(3) . . ?
C7 C8 C9 118.7(3) . . ?
C10 C9 C8 119.0(3) . . ?
N1 C10 C9 122.5(3) . . ?
O3 C11 O4 126.1(2) . . ?
O3 C11 C11 117.7(3) . 3_655 ?
O4 C11 C11 116.2(3) . 3_655 ?
O2 C12 O1 126.3(2) . . ?
O2 C12 C12 116.8(3) . 3 ?
O1 C12 C12 116.9(3) . 3 ?
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 O4 2.083(2) 3_655 ?
Zn1 O1 2.101(2) 3 ?
Zn1 O2 2.132(2) . ?
Zn1 O3 2.133(2) . ?
Zn1 N1 2.144(2) . ?
Zn1 N2 2.145(2) . ?
O1 C12 1.253(3) . ?
O1 Zn1 2.101(2) 3 ?
O2 C12 1.252(3) . ?
O3 C11 1.248(3) . ?
O4 C11 1.257(3) . ?
O4 Zn1 2.083(2) 3_655 ?
N1 C10 1.345(4) . ?
N1 C6 1.345(4) . ?
N2 C5 1.340(4) . ?
N2 C1 1.344(4) . ?
C1 C2 1.382(4) . ?
C2 C3 1.387(4) . ?
C3 C4 1.387(4) . ?
C4 C5 1.384(4) . ?
C6 C7 1.378(4) . ?
C7 C8 1.382(4) . ?
C8 C9 1.389(5) . ?
C9 C10 1.384(4) . ?
C11 C11 1.557(5) 3_655 ?
C12 C12 1.566(5) 3 ?
