#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:29:14 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179581 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/46/4504661.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_4504661
loop_
_publ_author_name
'Prasad, T. K.'
'Rajasekharan, M. V.'
_publ_section_title
;
 A Novel Water Octamer in Ce(dipic)2(H2O)3·4H2O: 
 Crystallographic, Thermal, and Theoretical Studies
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              488
_journal_paper_doi               10.1021/cg050417m
_journal_volume                  6
_journal_year                    2006
_chemical_formula_moiety         'C14 H12 Ce N2 O11, 4(H2 O)'
_chemical_formula_sum            'C14 H20 Ce N2 O15'
_chemical_formula_weight         596.44
_chemical_name_systematic
;
 Triaquabis{pyridine-2,6-dicarboxylato}cerium(IV)tertahydrate 
;
_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                93.8160(10)
_cell_angle_beta                 107.8430(10)
_cell_angle_gamma                93.6880(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0048(8)
_cell_length_b                   10.4951(8)
_cell_length_c                   10.6453(8)
_cell_measurement_reflns_used    5296
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.45
_cell_volume                     1057.42(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury v. 1.3 (CCDC)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10880
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.232
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS absorption correction - V2.10'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4140
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0238P)²+0.6403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                4105
_reflns_number_total             4140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050417msi20050814_110540.cif
_cod_data_source_block           mvr27_m
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4504661
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ce Ce 0.194192(10) 0.318527(9) 0.902769(10) 0.00745(5) Uani 1 1 d .
C11 C 0.2072(2) 0.00991(19) 0.9813(2) 0.0105(4) Uani 1 1 d .
C12 C 0.2571(2) -0.1012(2) 1.0345(2) 0.0133(4) Uani 1 1 d .
H12 H 0.2003 -0.1804 1.0108 0.016 Uiso 1 1 calc R
C13 C 0.3928(2) -0.0935(2) 1.1234(2) 0.0151(4) Uani 1 1 d .
H13 H 0.4293 -0.1678 1.1628 0.018 Uiso 1 1 calc R
C14 C 0.4747(2) 0.0228(2) 1.1544(2) 0.0145(4) Uani 1 1 d .
H14 H 0.5675 0.0298 1.2151 0.017 Uiso 1 1 calc R
C15 C 0.4175(2) 0.1286(2) 1.0944(2) 0.0109(4) Uani 1 1 d .
C16 C 0.4955(2) 0.2590(2) 1.1076(2) 0.0114(4) Uani 1 1 d .
C17 C 0.0629(2) 0.0184(2) 0.8845(2) 0.0104(4) Uani 1 1 d .
C21 C -0.0515(2) 0.36649(19) 0.6119(2) 0.0115(4) Uani 1 1 d .
C22 C -0.1276(2) 0.3595(2) 0.4782(2) 0.0153(4) Uani 1 1 d .
H22 H -0.2074 0.4067 0.4473 0.018 Uiso 1 1 calc R
C23 C -0.0833(2) 0.2810(2) 0.3908(2) 0.0176(5) Uani 1 1 d .
H23 H -0.1341 0.2723 0.2988 0.021 Uiso 1 1 calc R
C24 C 0.0360(2) 0.2154(2) 0.4393(2) 0.0162(4) Uani 1 1 d .
H24 H 0.0685 0.1621 0.3811 0.019 Uiso 1 1 calc R
C25 C 0.1061(2) 0.2297(2) 0.5741(2) 0.0113(4) Uani 1 1 d .
C26 C 0.2407(2) 0.1705(2) 0.6399(2) 0.0119(4) Uani 1 1 d .
C27 C -0.0843(2) 0.4467(2) 0.7191(2) 0.0110(4) Uani 1 1 d .
N11 N 0.28614(18) 0.12205(16) 1.01096(16) 0.0095(3) Uani 1 1 d .
N12 N 0.06141(17) 0.30219(16) 0.65830(17) 0.0094(3) Uani 1 1 d .
O11 O 0.41920(15) 0.34285(14) 1.04351(14) 0.0120(3) Uani 1 1 d .
O12 O 0.62108(15) 0.27786(14) 1.17071(15) 0.0156(3) Uani 1 1 d .
O13 O 0.03735(15) 0.13167(13) 0.84920(14) 0.0114(3) Uani 1 1 d .
O14 O -0.02146(16) -0.07734(14) 0.84396(15) 0.0132(3) Uani 1 1 d .
O21 O 0.29186(15) 0.20014(14) 0.76535(14) 0.0116(3) Uani 1 1 d .
O22 O 0.29412(16) 0.10242(16) 0.57325(16) 0.0186(3) Uani 1 1 d .
O23 O -0.01670(15) 0.42214(14) 0.83808(14) 0.0120(3) Uani 1 1 d .
O24 O -0.16750(16) 0.52972(14) 0.69215(15) 0.0150(3) Uani 1 1 d .
O31 O 0.30446(16) 0.46916(14) 0.79997(15) 0.0122(3) Uani 1 1 d D
O32 O 0.22554(16) 0.53034(14) 1.02962(15) 0.0125(3) Uani 1 1 d D
O33 O 0.10426(16) 0.30107(14) 1.08652(15) 0.0130(3) Uani 1 1 d D
O1W O 0.78480(18) 0.10271(17) 0.62093(18) 0.0228(4) Uani 1 1 d D
O2W O 0.58284(19) 0.65353(18) 0.64754(18) 0.0248(4) Uani 1 1 d D
O3W O 0.54474(17) 0.42716(16) 0.74748(16) 0.0164(3) Uani 1 1 d D
O4W O 0.55089(18) 0.22424(16) 0.57598(17) 0.0199(3) Uani 1 1 d D
H31A H 0.322(4) 0.5482(19) 0.823(3) 0.045(10) Uiso 1 1 d D
H31B H 0.373(3) 0.444(3) 0.782(3) 0.032(9) Uiso 1 1 d D
H32A H 0.295(3) 0.545(3) 1.099(2) 0.036(9) Uiso 1 1 d D
H32B H 0.156(2) 0.549(3) 1.053(3) 0.027(8) Uiso 1 1 d D
H33A H 0.125(3) 0.353(2) 1.153(2) 0.019(7) Uiso 1 1 d D
H33B H 0.068(3) 0.232(2) 1.100(3) 0.037(9) Uiso 1 1 d D
H1A H 0.774(3) 0.035(2) 0.572(3) 0.030(8) Uiso 1 1 d D
H1B H 0.848(3) 0.095(4) 0.689(3) 0.052(11) Uiso 1 1 d D
H2A H 0.655(3) 0.640(3) 0.628(3) 0.040(10) Uiso 1 1 d D
H2B H 0.531(3) 0.692(3) 0.585(3) 0.051(11) Uiso 1 1 d D
H3A H 0.555(3) 0.496(2) 0.716(3) 0.034(9) Uiso 1 1 d D
H3B H 0.549(3) 0.367(2) 0.693(3) 0.027(8) Uiso 1 1 d D
H4A H 0.625(3) 0.187(3) 0.594(3) 0.044(10) Uiso 1 1 d D
H4B H 0.485(3) 0.171(3) 0.574(3) 0.041(10) 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 0.0033 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'
Ce Ce -0.2486 2.6331 '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'
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
O11 Ce O21 83.90(5) . . y
O11 Ce O13 127.44(5) . . y
O21 Ce O13 79.87(5) . . y
O11 Ce O23 142.49(5) . . y
O21 Ce O23 127.14(5) . . y
O13 Ce O23 83.14(5) . . y
O11 Ce O31 78.18(5) . . y
O21 Ce O31 73.34(5) . . y
O13 Ce O31 140.57(5) . . y
O23 Ce O31 90.41(5) . . y
O11 Ce O33 90.54(5) . . y
O21 Ce O33 142.11(5) . . y
O13 Ce O33 74.04(5) . . y
O23 Ce O33 76.65(5) . . y
O31 Ce O33 141.93(5) . . y
O11 Ce O32 72.97(5) . . y
O21 Ce O32 141.06(5) . . y
O13 Ce O32 139.00(5) . . y
O23 Ce O32 69.53(5) . . y
O31 Ce O32 71.55(5) . . y
O33 Ce O32 70.38(5) . . y
O11 Ce N11 63.89(5) . . y
O21 Ce N11 70.67(5) . . y
O13 Ce N11 63.56(5) . . y
O23 Ce N11 139.87(5) . . y
O31 Ce N11 129.45(5) . . y
O33 Ce N11 73.25(5) . . y
O32 Ce N11 122.09(5) . . y
O11 Ce N12 140.33(5) . . y
O21 Ce N12 63.97(5) . . y
O13 Ce N12 71.43(5) . . y
O23 Ce N12 63.18(5) . . y
O31 Ce N12 70.99(5) . . y
O33 Ce N12 129.08(5) . . y
O32 Ce N12 117.91(5) . . y
N11 Ce N12 120.00(5) . . y
N11 C11 C12 122.03(19) . . ?
N11 C11 C17 113.05(17) . . ?
C12 C11 C17 124.92(19) . . ?
C11 C12 C13 118.19(19) . . ?
C14 C13 C12 119.8(2) . . ?
C15 C14 C13 118.2(2) . . ?
N11 C15 C14 122.10(19) . . ?
N11 C15 C16 112.66(18) . . ?
C14 C15 C16 125.14(19) . . ?
O12 C16 O11 125.32(19) . . ?
O12 C16 C15 120.87(19) . . ?
O11 C16 C15 113.76(18) . . ?
O14 C17 O13 124.10(19) . . ?
O14 C17 C11 121.22(18) . . ?
O13 C17 C11 114.69(17) . . ?
N12 C21 C22 122.55(19) . . ?
N12 C21 C27 112.71(18) . . ?
C22 C21 C27 124.74(19) . . ?
C21 C22 C23 117.9(2) . . ?
C22 C23 C24 119.5(2) . . ?
C25 C24 C23 118.4(2) . . ?
N12 C25 C24 122.02(19) . . ?
N12 C25 C26 113.51(18) . . ?
C24 C25 C26 124.43(19) . . ?
O22 C26 O21 125.32(19) . . ?
O22 C26 C25 120.11(19) . . ?
O21 C26 C25 114.54(18) . . ?
O24 C27 O23 124.39(19) . . ?
O24 C27 C21 121.14(19) . . ?
O23 C27 C21 114.46(17) . . ?
C15 N11 C11 119.65(18) . . ?
C15 N11 Ce 119.62(13) . . ?
C11 N11 Ce 120.66(13) . . ?
C21 N12 C25 119.59(18) . . ?
C21 N12 Ce 120.89(13) . . ?
C25 N12 Ce 119.52(13) . . ?
C16 O11 Ce 129.88(13) . . ?
C17 O13 Ce 127.76(13) . . ?
C26 O21 Ce 128.18(13) . . ?
C26 O22 O4W 109.20(14) . . ?
C27 O23 Ce 126.11(13) . . ?
Ce O31 O3W 121.89(7) . . ?
O4W O1W O22 102.94(7) . 2_656 y
O4W O1W O13 129.60(8) . 1_655 y
O22 O1W O13 125.91(7) 2_656 1_655 y
O3W O2W O4W 137.09(9) . 2_666 y
O3W O2W O24 71.74(6) . 1_655 y
O4W O2W O24 126.67(8) 2_666 1_655 y
O31 O3W O2W 97.98(7) . . y
O31 O3W O4W 119.98(8) . . y
O2W O3W O4W 111.19(8) . . y
O31 O3W O32 111.80(7) . 2_667 y
O2W O3W O32 96.34(7) . 2_667 y
O4W O3W O32 115.34(7) . 2_667 y
O1W O4W O3W 118.99(8) . . y
O1W O4W O22 122.37(8) . . y
O3W O4W O22 95.10(7) . . y
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
Ce O11 2.2773(14) . y
Ce O21 2.3300(14) . y
Ce O13 2.3538(14) . y
Ce O23 2.3692(14) . y
Ce O31 2.3790(15) . y
Ce O33 2.4030(15) . y
Ce O32 2.4728(15) . y
Ce N11 2.5171(17) . y
Ce N12 2.5218(17) . y
C11 N11 1.337(3) . ?
C11 C12 1.385(3) . ?
C11 C17 1.506(3) . ?
C12 C13 1.390(3) . ?
C13 C14 1.387(3) . ?
C14 C15 1.386(3) . ?
C15 N11 1.336(3) . ?
C15 C16 1.507(3) . ?
C16 O12 1.225(3) . ?
C16 O11 1.292(3) . ?
C17 O14 1.232(3) . ?
C17 O13 1.289(3) . ?
C21 N12 1.333(3) . ?
C21 C22 1.388(3) . ?
C21 C27 1.502(3) . ?
C22 C23 1.392(3) . ?
C23 C24 1.393(3) . ?
C24 C25 1.384(3) . ?
C25 N12 1.334(3) . ?
C25 C26 1.509(3) . ?
C26 O22 1.230(3) . ?
C26 O21 1.283(3) . ?
C27 O24 1.230(3) . ?
C27 O23 1.292(3) . ?
O22 O4W 2.786(2) . y
O31 O3W 2.686(2) . y
O1W O4W 2.667(2) . y
O1W O22 2.778(2) 2_656 y
O1W O13 2.902(2) 1_655 y
O2W O3W 2.718(2) . y
O2W O4W 2.788(2) 2_666 y
O2W O24 2.815(2) 1_655 y
O3W O4W 2.728(2) . y
O3W O32 2.738(2) 2_667 y
