#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:25:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180434 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/03/7210320.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_7210320
loop_
_publ_author_name
'Eshtiagh-Hosseini, Hossein'
'Mirzaei, Masoud'
'Biabani, Marzieh'
'Lippolis, Vito'
'Chahkandi, Mohammad'
'Bazzicalupi, Carla'
_publ_section_title
;
 Insight into the connecting roles of interaction synthons and water
 clusters within different transition metal coordination compounds of
 pyridine-2,5-dicarboxylic acid: experimental and theoretical studies
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              6752
_journal_paper_doi               10.1039/c3ce40743h
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C40 H40 N6 Ni O14'
_chemical_formula_weight         887.49
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 116.268(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.580(2)
_cell_length_b                   8.0664(3)
_cell_length_c                   16.7188(9)
_cell_measurement_reflns_used    7349
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.1062
_cell_measurement_theta_min      2.9451
_cell_volume                     3698.2(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_molecular_graphics    'Mercury, CCDC'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19837
_diffrn_reflns_theta_full        71.24
_diffrn_reflns_theta_max         71.24
_diffrn_reflns_theta_min         3.22
_diffrn_standards_interval_count infinity
_diffrn_standards_interval_time  infinity
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.393
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3532
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0442
_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)+(0.0624P)²+9.0673P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                2861
_reflns_number_total             3532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40743h.txt
_cod_data_source_block           MB89
_cod_original_cell_volume        3698.2(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7210320
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ni Ni 0.0000 0.40359(8) -0.2500 0.02024(18) Uani 1 2 d S
O1 O -0.04732(6) 0.2199(2) -0.32599(12) 0.0214(4) Uani 1 1 d .
O2 O -0.06685(6) 0.0652(2) -0.44784(12) 0.0242(4) Uani 1 1 d .
C1 C -0.04194(9) 0.1747(3) -0.39407(16) 0.0203(5) Uani 1 1 d .
C2 C -0.00247(9) 0.2612(3) -0.40945(17) 0.0194(5) Uani 1 1 d .
C3 C 0.00806(10) 0.2187(3) -0.47915(18) 0.0239(6) Uani 1 1 d .
H3A H -0.0099 0.1370 -0.5196 0.029 Uiso 1 1 calc R
C4 C 0.04557(10) 0.2988(3) -0.48800(18) 0.0244(6) Uani 1 1 d .
H4A H 0.0536 0.2692 -0.5336 0.029 Uiso 1 1 calc R
C5 C 0.07126(9) 0.4236(3) -0.42850(17) 0.0207(5) Uani 1 1 d .
C6 C 0.05797(9) 0.4609(3) -0.36052(17) 0.0204(5) Uani 1 1 d .
H6A H 0.0747 0.5450 -0.3205 0.024 Uiso 1 1 calc R
N1 N 0.02228(7) 0.3811(3) -0.35042(14) 0.0197(5) Uani 1 1 d .
C7 C 0.11261(9) 0.5145(3) -0.43694(17) 0.0214(5) Uani 1 1 d .
O3 O 0.13718(7) 0.6166(2) -0.37787(12) 0.0259(4) Uani 1 1 d .
O4 O 0.11910(7) 0.4762(2) -0.50451(12) 0.0267(4) Uani 1 1 d .
OW1 O 0.05193(7) 0.5852(3) -0.18421(13) 0.0283(4) Uani 1 1 d D
N2 N 0.33181(8) 0.3785(3) -0.03814(15) 0.0227(5) Uani 1 1 d D
C8 C 0.29086(9) 0.4188(3) -0.03427(16) 0.0195(5) Uani 1 1 d .
C9 C 0.24472(9) 0.3546(3) -0.09827(17) 0.0191(5) Uani 1 1 d .
C10 C 0.23972(10) 0.2557(3) -0.17190(17) 0.0227(6) Uani 1 1 d .
H10A H 0.2671 0.2310 -0.1802 0.027 Uiso 1 1 calc R
C11 C 0.19514(10) 0.1961(3) -0.23097(17) 0.0249(6) Uani 1 1 d .
H11 H 0.1925 0.1321 -0.2792 0.030 Uiso 1 1 calc R
C12 C 0.15340(10) 0.2313(3) -0.21895(18) 0.0242(6) Uani 1 1 d .
H12 H 0.1233 0.1895 -0.2591 0.029 Uiso 1 1 calc R
C13 C 0.15666(9) 0.3266(3) -0.14874(17) 0.0212(5) Uani 1 1 d .
H13 H 0.1289 0.3498 -0.1414 0.025 Uiso 1 1 calc R
C14 C 0.20249(9) 0.3896(3) -0.08744(16) 0.0177(5) Uani 1 1 d .
N3 N 0.20558(8) 0.4831(3) -0.01699(14) 0.0182(4) Uani 1 1 d .
C15 C 0.24778(9) 0.5566(3) 0.04119(16) 0.0183(5) Uani 1 1 d .
C16 C 0.24757(10) 0.6612(3) 0.10900(17) 0.0216(5) Uani 1 1 d .
H16 H 0.2190 0.6764 0.1150 0.026 Uiso 1 1 calc R
C17 C 0.28953(10) 0.7399(3) 0.16558(17) 0.0236(6) Uani 1 1 d .
H17 H 0.2892 0.8105 0.2093 0.028 Uiso 1 1 calc R
C18 C 0.33333(10) 0.7153(3) 0.15838(17) 0.0234(6) Uani 1 1 d .
H18 H 0.3616 0.7700 0.1970 0.028 Uiso 1 1 calc R
C19 C 0.33428(10) 0.6110(3) 0.09467(17) 0.0222(5) Uani 1 1 d .
H19 H 0.3635 0.5936 0.0912 0.027 Uiso 1 1 calc R
C20 C 0.29145(9) 0.5291(3) 0.03396(16) 0.0187(5) Uani 1 1 d .
OW2 O 0.09899(8) -0.0737(3) -0.36204(15) 0.0380(5) Uani 1 1 d D
OW3 O 0.04624(8) -0.1046(3) -0.26029(16) 0.0359(5) Uani 1 1 d D
H2 H 0.3597(8) 0.422(4) 0.0003(17) 0.026(5) Uiso 1 1 d D
H3 H 0.1815(12) 0.498(4) -0.010(2) 0.026(5) Uiso 1 1 d .
H1 H 0.3317(11) 0.304(3) -0.0753(17) 0.026(5) Uiso 1 1 d D
H4 H 0.0480(15) 0.696(3) -0.197(3) 0.067(9) Uiso 1 1 d D
H5 H 0.0737(13) 0.575(5) -0.1263(15) 0.067(9) Uiso 1 1 d D
H8 H 0.0630(15) -0.081(5) -0.291(3) 0.076(15) Uiso 1 1 d D
H7 H 0.1121(18) -0.180(4) -0.361(4) 0.099(18) Uiso 1 1 d D
H9 H 0.0476(16) -0.011(4) -0.232(3) 0.072(14) Uiso 1 1 d D
H10 H 0.0835(17) -0.052(6) -0.4225(15) 0.090(17) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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
O1 Ni O1 88.47(10) . 2_554
O1 Ni N1 92.47(8) . 2_554
O1 Ni N1 80.31(8) 2_554 2_554
O1 Ni N1 80.31(8) . .
O1 Ni N1 92.47(8) 2_554 .
N1 Ni N1 169.99(12) 2_554 .
O1 Ni OW1 172.67(7) . .
O1 Ni OW1 90.96(8) 2_554 .
N1 Ni OW1 94.64(8) 2_554 .
N1 Ni OW1 92.41(8) . .
O1 Ni OW1 90.96(8) . 2_554
O1 Ni OW1 172.67(7) 2_554 2_554
N1 Ni OW1 92.41(8) 2_554 2_554
N1 Ni OW1 94.64(8) . 2_554
OW1 Ni OW1 90.53(12) . 2_554
C1 O1 Ni 114.99(16) . .
O2 C1 O1 124.5(2) . .
O2 C1 C2 118.8(2) . .
O1 C1 C2 116.6(2) . .
N1 C2 C3 122.0(2) . .
N1 C2 C1 116.0(2) . .
C3 C2 C1 122.0(2) . .
C4 C3 C2 119.3(3) . .
C3 C4 C5 119.7(2) . .
C4 C5 C6 117.5(2) . .
C4 C5 C7 120.8(2) . .
C6 C5 C7 121.6(2) . .
N1 C6 C5 123.0(2) . .
C6 N1 C2 118.5(2) . .
C6 N1 Ni 129.44(18) . .
C2 N1 Ni 112.01(16) . .
O3 C7 O4 126.0(2) . .
O3 C7 C5 118.6(2) . .
O4 C7 C5 115.4(2) . .
N2 C8 C9 120.9(2) . .
N2 C8 C20 120.7(2) . .
C9 C8 C20 118.4(2) . .
C14 C9 C10 118.1(2) . .
C14 C9 C8 119.0(2) . .
C10 C9 C8 122.8(2) . .
C11 C10 C9 121.0(2) . .
C10 C11 C12 120.2(2) . .
C13 C12 C11 120.6(2) . .
C12 C13 C14 119.7(2) . .
N3 C14 C9 120.2(2) . .
N3 C14 C13 119.4(2) . .
C9 C14 C13 120.3(2) . .
C15 N3 C14 122.6(2) . .
N3 C15 C20 120.3(2) . .
N3 C15 C16 119.5(2) . .
C20 C15 C16 120.1(2) . .
C17 C16 C15 119.7(2) . .
C16 C17 C18 120.7(2) . .
C19 C18 C17 120.1(2) . .
C18 C19 C20 120.9(2) . .
C15 C20 C19 118.4(2) . .
C15 C20 C8 119.0(2) . .
C19 C20 C8 122.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni O1 2.0679(18) .
Ni O1 2.0679(18) 2_554
Ni N1 2.080(2) 2_554
Ni N1 2.080(2) .
Ni OW1 2.081(2) .
Ni OW1 2.081(2) 2_554
O1 C1 1.273(3) .
O2 C1 1.250(3) .
C1 C2 1.512(3) .
C2 N1 1.349(3) .
C2 C3 1.383(4) .
C3 C4 1.380(4) .
C4 C5 1.389(4) .
C5 C6 1.398(4) .
C5 C7 1.521(3) .
C6 N1 1.341(3) .
C7 O3 1.250(3) .
C7 O4 1.269(3) .
N2 C8 1.323(3) .
C8 C9 1.438(4) .
C8 C20 1.441(3) .
C9 C14 1.410(3) .
C9 C10 1.417(4) .
C10 C11 1.369(4) .
C11 C12 1.406(4) .
C12 C13 1.369(4) .
C13 C14 1.414(4) .
C14 N3 1.366(3) .
N3 C15 1.361(3) .
C15 C20 1.410(3) .
C15 C16 1.416(4) .
C16 C17 1.367(4) .
C17 C18 1.411(4) .
C18 C19 1.368(4) .
C19 C20 1.416(4) .
