#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308566.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_4308566
loop_
_publ_author_name
'Zheng He'
'En-Qing Gao'
'Zhe-Ming Wang'
'Chun-Hua Yan'
'Mohamedally Kurmoo'
_publ_contact_author_address
;
State Key Lab of Rare Earth Materials Chemistry and Applications & 
PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, 
College of Chemistry and Molecular Engineering, 
Peking University, 
Beijing 100871, 
China
;
_publ_contact_author_email       chyan@chem.pku.edu.cn
_publ_contact_author_fax         86-(10)-62754179
_publ_contact_author_name        'Prof. Chun-Hua Yan'
_publ_contact_author_phone       86-(10)-62754179
_publ_section_title
;
Coordination Polymers Based on Inorganic Lanthanide(III) Sulfate Skeletons
and an Organic Isonicotinate N-oxide Connector: Segregation into Three
Structural Types by the Lanthanide Contraction Effect
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              862
_journal_page_last               874
_journal_paper_doi               10.1021/ic0487575
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C6 H6 Ce N O8 S'
_chemical_formula_weight         392.30
_chemical_name_systematic
; 
 ? 
;
_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                77.3540(10)
_cell_angle_beta                 87.4134(11)
_cell_angle_gamma                89.8783(14)
_cell_formula_units_Z            2
_cell_length_a                   6.6459(2)
_cell_length_b                   7.3040(2)
_cell_length_c                   10.3885(3)
_cell_measurement_reflns_used    6729
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     491.53(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9506
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.876
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.104
_refine_diff_density_min         -1.565
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.0134(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0370P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                2099
_reflns_number_total             2266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0487575si20040906_123354_02.cif
_cod_data_source_block           2
_cod_database_code               4308566
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.32701(3) 0.73737(2) 0.016512(18) 0.01253(11) Uani 1 1 d . . .
C1 C 0.2830(5) 0.5373(5) -0.3840(4) 0.0169(7) Uani 1 1 d . . .
C2 C 0.2628(6) 0.7241(5) -0.4466(4) 0.0217(8) Uani 1 1 d . . .
H2A H 0.2760 0.8175 -0.3994 0.026 Uiso 1 1 calc R . .
C3 C 0.2233(6) 0.7716(5) -0.5789(4) 0.0239(8) Uani 1 1 d . . .
H3A H 0.2149 0.8972 -0.6216 0.029 Uiso 1 1 calc R . .
C4 C 0.2181(5) 0.4539(5) -0.5880(4) 0.0206(8) Uani 1 1 d . . .
H4A H 0.2017 0.3622 -0.6363 0.025 Uiso 1 1 calc R . .
C5 C 0.2634(5) 0.4029(5) -0.4581(4) 0.0179(7) Uani 1 1 d . . .
H5A H 0.2812 0.2769 -0.4191 0.021 Uiso 1 1 calc R . .
C6 C 0.3284(5) 0.4907(5) -0.2391(3) 0.0150(7) Uani 1 1 d . . .
N1 N 0.1969(5) 0.6364(4) -0.6464(3) 0.0192(7) Uani 1 1 d . . .
O1 O 0.2730(4) 0.6078(4) -0.1749(3) 0.0221(6) Uani 1 1 d . . .
O2 O 0.4245(4) 0.3412(4) -0.1961(2) 0.0187(5) Uani 1 1 d . . .
O3 O 0.1412(4) 0.6841(4) -0.7703(2) 0.0240(6) Uani 1 1 d . . .
O4 O 0.6548(4) 0.9343(3) -0.0658(3) 0.0179(5) Uani 1 1 d . . .
O5 O 0.6669(4) 0.6186(3) -0.0845(3) 0.0180(5) Uani 1 1 d . . .
O6 O 0.9569(4) 0.7574(4) -0.0072(3) 0.0218(6) Uani 1 1 d . . .
O7 O 0.8753(4) 0.8487(4) -0.2356(2) 0.0191(5) Uani 1 1 d . . .
O8 O 0.2602(5) 0.9896(4) -0.1958(3) 0.0272(7) Uani 1 1 d . . .
S1 S 0.79663(13) 0.78961(12) -0.10064(8) 0.01375(19) Uani 1 1 d . . .
HW1 H 0.287(9) 1.090(9) -0.183(6) 0.06(2) Uiso 1 1 d . . .
HW2 H 0.156(10) 0.993(9) -0.211(7) 0.06(2) Uiso 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'
S S 0.1246 0.1234 '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'
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 Ce1 O3 130.04(9) . 1_556 ?
O1 Ce1 O6 76.04(9) . 1_455 ?
O3 Ce1 O6 67.75(9) 1_556 1_455 ?
O1 Ce1 O2 131.95(8) . 2_665 ?
O3 Ce1 O2 71.59(8) 1_556 2_665 ?
O6 Ce1 O2 139.21(9) 1_455 2_665 ?
O1 Ce1 O5 70.91(9) . 2_665 ?
O3 Ce1 O5 79.06(8) 1_556 2_665 ?
O6 Ce1 O5 95.06(8) 1_455 2_665 ?
O2 Ce1 O5 73.90(8) 2_665 2_665 ?
O1 Ce1 O4 136.46(9) . 2_675 ?
O3 Ce1 O4 79.43(9) 1_556 2_675 ?
O6 Ce1 O4 92.30(8) 1_455 2_675 ?
O2 Ce1 O4 83.34(8) 2_665 2_675 ?
O5 Ce1 O4 152.61(9) 2_665 2_675 ?
O1 Ce1 O8 66.31(10) . . ?
O3 Ce1 O8 127.89(10) 1_556 . ?
O6 Ce1 O8 72.19(10) 1_455 . ?
O2 Ce1 O8 140.75(10) 2_665 . ?
O5 Ce1 O8 137.11(10) 2_665 . ?
O4 Ce1 O8 70.18(10) 2_675 . ?
O1 Ce1 O4 99.80(8) . . ?
O3 Ce1 O4 130.06(9) 1_556 . ?
O6 Ce1 O4 139.97(9) 1_455 . ?
O2 Ce1 O4 72.40(8) 2_665 . ?
O5 Ce1 O4 121.64(8) 2_665 . ?
O4 Ce1 O4 63.03(9) 2_675 . ?
O8 Ce1 O4 69.93(10) . . ?
O1 Ce1 O5 67.24(8) . . ?
O3 Ce1 O5 137.70(9) 1_556 . ?
O6 Ce1 O5 143.24(9) 1_455 . ?
O2 Ce1 O5 71.33(8) 2_665 . ?
O5 Ce1 O5 71.74(9) 2_665 . ?
O4 Ce1 O5 115.39(8) 2_675 . ?
O8 Ce1 O5 94.01(9) . . ?
O4 Ce1 O5 52.92(7) . . ?
O1 Ce1 S1 84.55(6) . . ?
O3 Ce1 S1 138.68(7) 1_556 . ?
O6 Ce1 S1 152.99(7) 1_455 . ?
O2 Ce1 S1 67.72(6) 2_665 . ?
O5 Ce1 S1 96.13(6) 2_665 . ?
O4 Ce1 S1 88.96(6) 2_675 . ?
O8 Ce1 S1 82.94(8) . . ?
O4 Ce1 S1 26.54(5) . . ?
O5 Ce1 S1 26.51(5) . . ?
C5 C1 C2 118.1(3) . . ?
C5 C1 C6 123.3(3) . . ?
C2 C1 C6 118.6(3) . . ?
C3 C2 C1 120.1(4) . . ?
N1 C3 C2 120.1(4) . . ?
N1 C4 C5 120.3(3) . . ?
C4 C5 C1 120.5(4) . . ?
O1 C6 O2 126.4(3) . . ?
O1 C6 C1 115.9(3) . . ?
O2 C6 C1 117.7(3) . . ?
O3 N1 C3 119.2(3) . . ?
O3 N1 C4 120.0(3) . . ?
C3 N1 C4 120.8(3) . . ?
C6 O1 Ce1 146.0(2) . . ?
C6 O2 Ce1 131.0(2) . 2_665 ?
N1 O3 Ce1 133.2(2) . 1_554 ?
S1 O4 Ce1 138.46(14) . 2_675 ?
S1 O4 Ce1 102.49(12) . . ?
Ce1 O4 Ce1 116.97(9) 2_675 . ?
S1 O5 Ce1 142.69(15) . 2_665 ?
S1 O5 Ce1 100.55(11) . . ?
Ce1 O5 Ce1 108.26(9) 2_665 . ?
S1 O6 Ce1 145.05(16) . 1_655 ?
O7 S1 O6 111.86(16) . . ?
O7 S1 O5 110.82(15) . . ?
O6 S1 O5 110.66(16) . . ?
O7 S1 O4 110.58(15) . . ?
O6 S1 O4 109.03(15) . . ?
O5 S1 O4 103.57(14) . . ?
O7 S1 Ce1 129.79(11) . . ?
O6 S1 Ce1 118.31(11) . . ?
O5 S1 Ce1 52.94(9) . . ?
O4 S1 Ce1 50.97(10) . . ?
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
Ce1 O1 2.423(2) . ?
Ce1 O3 2.441(2) 1_556 ?
Ce1 O6 2.484(3) 1_455 ?
Ce1 O2 2.519(3) 2_665 ?
Ce1 O5 2.541(2) 2_665 ?
Ce1 O4 2.564(2) 2_675 ?
Ce1 O8 2.600(3) . ?
Ce1 O4 2.618(2) . ?
Ce1 O5 2.671(2) . ?
Ce1 S1 3.2904(8) . ?
C1 C5 1.383(5) . ?
C1 C2 1.386(5) . ?
C1 C6 1.513(5) . ?
C2 C3 1.379(6) . ?
C3 N1 1.346(5) . ?
C4 N1 1.349(5) . ?
C4 C5 1.366(5) . ?
C6 O1 1.240(4) . ?
C6 O2 1.268(4) . ?
N1 O3 1.326(4) . ?
O2 Ce1 2.519(2) 2_665 ?
O3 Ce1 2.441(2) 1_554 ?
O4 S1 1.506(2) . ?
O4 Ce1 2.564(2) 2_675 ?
O5 S1 1.494(2) . ?
O5 Ce1 2.541(2) 2_665 ?
O6 S1 1.457(3) . ?
O6 Ce1 2.484(3) 1_655 ?
O7 S1 1.448(3) . ?
