#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/64/2236465.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2236465
loop_
_publ_author_name
'Sen, Rupam'
'Mal, Dasarath'
'Brandao, Paula'
'Lin, Zhi'
_publ_section_title
;
 Tetraaquabis[2-(pyridin-4-yl-κN)pyrimidine-5-carboxylato]zinc
;
_journal_coeditor_code           LH5541
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1429
_journal_paper_doi               10.1107/S160053681204411X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Zn (C10 H6 N3 O2)2 (H2 O)4]'
_chemical_formula_moiety         'C20 H20 N6 O8 Zn'
_chemical_formula_sum            'C20 H20 N6 O8 Zn'
_chemical_formula_weight         537.79
_chemical_name_systematic
;
Tetraaquabis[2-(pyridin-4-yl-κN)pyrimidine-5-carboxylato]zinc
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.676(7)
_cell_angle_beta                 92.638(7)
_cell_angle_gamma                112.639(5)
_cell_formula_units_Z            1
_cell_length_a                   6.2764(7)
_cell_length_b                   6.9208(7)
_cell_length_c                   12.7810(17)
_cell_measurement_reflns_used    246
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.56
_cell_volume                     501.36(10)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'SMART (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'fine-focus sealed tube'
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8143
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.38
_diffrn_reflns_theta_min         3.26
_diffrn_standards_interval_count 0.5
_diffrn_standards_interval_time  10
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.9501
_exptl_absorpt_correction_T_min  0.7299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.607
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2184
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0325
_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)+(0.0522P)²+0.1478P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                2030
_reflns_number_total             2184
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh5541.cif
_cod_data_source_block           I
_cod_database_code               2236465
_cod_database_fobs_code          2236465
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Zn Zn 0.0000 0.0000 0.0000 0.01467(13) Uani d S 1
O O1 0.1899(3) -0.1897(2) -0.03156(12) 0.0170(3) Uani d D 1
H H1A 0.129(5) -0.303(3) -0.0767(17) 0.028(7) Uiso d D 1
H H1B 0.238(6) -0.227(6) 0.0190(19) 0.051(10) Uiso d D 1
O O2 0.2499(3) 0.2665(3) -0.05357(13) 0.0196(3) Uani d D 1
H H2A 0.184(5) 0.334(5) -0.080(2) 0.044(9) Uiso d D 1
H H2B 0.365(4) 0.265(5) -0.082(2) 0.046(10) Uiso d D 1
N N3 0.1681(3) 0.1214(3) 0.16096(14) 0.0152(4) Uani d . 1
C C4 0.0418(4) 0.1047(3) 0.24398(17) 0.0165(4) Uani d . 1
H H4 -0.1216 0.0610 0.2296 0.020 Uiso calc R 1
C C5 0.1386(4) 0.1481(3) 0.34911(16) 0.0159(4) Uani d . 1
H H5 0.0430 0.1334 0.4053 0.019 Uiso calc R 1
C C6 0.3782(4) 0.2137(3) 0.37137(16) 0.0138(4) Uani d . 1
C C7 0.5107(4) 0.2394(3) 0.28616(17) 0.0167(4) Uani d . 1
H H7 0.6751 0.2890 0.2985 0.020 Uiso calc R 1
C C8 0.3995(4) 0.1916(3) 0.18334(17) 0.0173(4) Uani d . 1
H H8 0.4914 0.2094 0.1259 0.021 Uiso calc R 1
C C9 0.4895(4) 0.2521(3) 0.48227(16) 0.0148(4) Uani d . 1
N N10 0.3511(3) 0.2432(3) 0.56043(14) 0.0167(4) Uani d . 1
C C11 0.4536(4) 0.2753(3) 0.65945(17) 0.0169(4) Uani d . 1
H H11 0.3620 0.2685 0.7169 0.020 Uiso calc R 1
C C12 0.6871(4) 0.3180(3) 0.68231(16) 0.0146(4) Uani d . 1
C C13 0.8139(4) 0.3264(4) 0.59538(17) 0.0179(4) Uani d . 1
H H13 0.9751 0.3571 0.6078 0.022 Uiso calc R 1
N N14 0.7165(3) 0.2928(3) 0.49487(14) 0.0179(4) Uani d . 1
C C15 0.7950(4) 0.3495(3) 0.79525(16) 0.0166(4) Uani d . 1
O O16 1.0133(3) 0.4300(3) 0.81382(12) 0.0203(3) Uani d . 1
O O17 0.6557(3) 0.2901(3) 0.86250(12) 0.0214(3) Uani d . 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Zn O1 . 2 180.0
O1 Zn N3 . 2 88.59(6)
O1 Zn N3 2 2 91.41(6)
O1 Zn N3 . . 91.41(6)
O1 Zn N3 2 . 88.59(6)
N3 Zn N3 2 . 180.0
O1 Zn O2 . 2 86.31(6)
O1 Zn O2 2 2 93.69(6)
N3 Zn O2 2 2 91.45(6)
N3 Zn O2 . 2 88.55(6)
O1 Zn O2 . . 93.69(6)
O1 Zn O2 2 . 86.31(6)
N3 Zn O2 2 . 88.55(6)
N3 Zn O2 . . 91.45(6)
O2 Zn O2 2 . 180.0
Zn O1 H1A . . 118(2)
Zn O1 H1B . . 118(2)
H1A O1 H1B . . 103(3)
Zn O2 H2A . . 110(2)
Zn O2 H2B . . 125(2)
H2A O2 H2B . . 114(3)
C8 N3 C4 . . 117.43(18)
C8 N3 Zn . . 121.52(14)
C4 N3 Zn . . 120.54(14)
N3 C4 C5 . . 123.19(19)
N3 C4 H4 . . 118.4
C5 C4 H4 . . 118.4
C4 C5 C6 . . 118.99(19)
C4 C5 H5 . . 120.5
C6 C5 H5 . . 120.5
C5 C6 C7 . . 118.01(19)
C5 C6 C9 . . 121.15(18)
C7 C6 C9 . . 120.83(19)
C8 C7 C6 . . 119.2(2)
C8 C7 H7 . . 120.4
C6 C7 H7 . . 120.4
N3 C8 C7 . . 123.13(19)
N3 C8 H8 . . 118.4
C7 C8 H8 . . 118.4
N14 C9 N10 . . 126.45(19)
N14 C9 C6 . . 117.08(18)
N10 C9 C6 . . 116.48(19)
C11 N10 C9 . . 115.59(19)
N10 C11 C12 . . 123.16(19)
N10 C11 H11 . . 118.4
C12 C11 H11 . . 118.4
C11 C12 C13 . . 116.22(19)
C11 C12 C15 . . 121.41(18)
C13 C12 C15 . . 122.36(19)
N14 C13 C12 . . 122.3(2)
N14 C13 H13 . . 118.8
C12 C13 H13 . . 118.8
C9 N14 C13 . . 116.28(18)
O16 C15 O17 . . 125.88(19)
O16 C15 C12 . . 117.94(18)
O17 C15 C12 . . 116.18(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Zn O1 . 2.0923(15)
Zn O1 2 2.0923(15)
Zn N3 2 2.1419(17)
Zn N3 . 2.1420(17)
Zn O2 2 2.1512(15)
Zn O2 . 2.1512(15)
O1 H1A . 0.830(10)
O1 H1B . 0.822(10)
O2 H2A . 0.833(10)
O2 H2B . 0.827(10)
N3 C8 . 1.341(3)
N3 C4 . 1.347(3)
C4 C5 . 1.383(3)
C4 H4 . 0.9500
C5 C6 . 1.393(3)
C5 H5 . 0.9500
C6 C7 . 1.394(3)
C6 C9 . 1.486(3)
C7 C8 . 1.384(3)
C7 H7 . 0.9500
C8 H8 . 0.9500
C9 N14 . 1.338(3)
C9 N10 . 1.348(3)
N10 C11 . 1.336(3)
C11 C12 . 1.385(3)
C11 H11 . 0.9500
C12 C13 . 1.392(3)
C12 C15 . 1.510(3)
C13 N14 . 1.340(3)
C13 H13 . 0.9500
C15 O16 . 1.257(3)
C15 O17 . 1.258(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1A O16 1_444 0.83(2) 1.98(2) 2.805(3) 175(3) yes
O1 H1B O17 2_656 0.82(3) 1.81(3) 2.631(3) 175(4) yes
O2 H2A O16 1_454 0.83(4) 2.04(4) 2.840(3) 162(4) yes
O2 H2B O17 1_554 0.83(3) 1.94(3) 2.767(3) 173(3) yes
