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#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308565.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_4308565
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 La N O8 S'
_chemical_formula_weight         391.09
_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                77.323(2)
_cell_angle_beta                 87.664(2)
_cell_angle_gamma                89.533(3)
_cell_formula_units_Z            2
_cell_length_a                   6.6774(3)
_cell_length_b                   7.3389(4)
_cell_length_c                   10.4329(6)
_cell_measurement_reflns_used    12470
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.58
_cell_volume                     498.38(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0837
_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            9648
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.58
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.528
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.734
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       0.0066(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0327
_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)+(0.0141P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0515
_reflns_number_gt                1776
_reflns_number_total             2287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0487575si20040906_123354_01.cif
_cod_data_source_block           1
_cod_database_code               4308565
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
La1 La 0.32568(4) 0.73853(4) 0.01605(3) 0.01854(11) Uani 1 1 d . . .
C1 C 0.2820(6) 0.5389(6) -0.3843(4) 0.0207(10) Uani 1 1 d . . .
C2 C 0.2593(7) 0.7234(6) -0.4473(4) 0.0282(11) Uani 1 1 d . . .
H2A H 0.2717 0.8160 -0.3999 0.034 Uiso 1 1 calc R . .
C3 C 0.2188(7) 0.7734(7) -0.5782(5) 0.0298(11) Uani 1 1 d . . .
H3A H 0.2085 0.8987 -0.6198 0.036 Uiso 1 1 calc R . .
C4 C 0.2180(6) 0.4565(6) -0.5893(4) 0.0233(10) Uani 1 1 d . . .
H4A H 0.2028 0.3658 -0.6380 0.028 Uiso 1 1 calc R . .
C5 C 0.2651(6) 0.4052(6) -0.4593(4) 0.0230(10) Uani 1 1 d . . .
H5A H 0.2860 0.2800 -0.4212 0.028 Uiso 1 1 calc R . .
C6 C 0.3285(6) 0.4923(6) -0.2423(4) 0.0221(10) Uani 1 1 d . . .
N1 N 0.1939(5) 0.6385(5) -0.6459(3) 0.0235(9) Uani 1 1 d . . .
O1 O 0.2741(4) 0.6091(4) -0.1774(3) 0.0285(7) Uani 1 1 d . . .
O2 O 0.4246(4) 0.3421(4) -0.1976(3) 0.0237(7) Uani 1 1 d . . .
O3 O 0.1385(4) 0.6869(4) -0.7697(3) 0.0292(7) Uani 1 1 d . . .
O4 O 0.6541(4) 0.9327(4) -0.0669(3) 0.0220(7) Uani 1 1 d . . .
O5 O 0.6670(4) 0.6184(4) -0.0841(3) 0.0247(7) Uani 1 1 d . . .
O6 O 0.9568(4) 0.7573(4) -0.0087(3) 0.0282(7) Uani 1 1 d . . .
O7 O 0.8716(4) 0.8463(4) -0.2363(3) 0.0271(7) Uani 1 1 d . . .
O8 O 0.2524(6) 0.9928(6) -0.1953(4) 0.0316(9) Uani 1 1 d . . .
S1 S 0.79419(15) 0.78863(15) -0.10096(10) 0.0212(3) Uani 1 1 d . . .
HW1 H 0.263(8) 1.082(7) -0.193(5) 0.028(19) Uiso 1 1 d . . .
HW2 H 0.131(9) 0.968(8) -0.204(6) 0.07(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'
La La -0.2871 2.4523 '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 La1 O3 130.56(10) . 1_556 ?
O1 La1 O6 76.17(10) . 1_455 ?
O3 La1 O6 67.68(9) 1_556 1_455 ?
O1 La1 O2 131.69(10) . 2_665 ?
O3 La1 O2 71.63(9) 1_556 2_665 ?
O6 La1 O2 139.11(10) 1_455 2_665 ?
O1 La1 O5 70.98(10) . 2_665 ?
O3 La1 O5 79.35(10) 1_556 2_665 ?
O6 La1 O5 94.62(9) 1_455 2_665 ?
O2 La1 O5 73.85(9) 2_665 2_665 ?
O1 La1 O4 136.74(10) . 2_675 ?
O3 La1 O4 79.16(9) 1_556 2_675 ?
O6 La1 O4 93.22(9) 1_455 2_675 ?
O2 La1 O4 82.88(9) 2_665 2_675 ?
O5 La1 O4 152.28(9) 2_665 2_675 ?
O1 La1 O8 66.57(11) . . ?
O3 La1 O8 126.79(11) 1_556 . ?
O6 La1 O8 71.68(11) 1_455 . ?
O2 La1 O8 141.28(11) 2_665 . ?
O5 La1 O8 137.34(11) 2_665 . ?
O4 La1 O8 70.27(11) 2_675 . ?
O1 La1 O4 98.94(9) . . ?
O3 La1 O4 130.40(9) 1_556 . ?
O6 La1 O4 140.43(9) 1_455 . ?
O2 La1 O4 72.64(9) 2_665 . ?
O5 La1 O4 121.32(9) 2_665 . ?
O4 La1 O4 63.22(10) 2_675 . ?
O8 La1 O4 70.53(11) . . ?
O1 La1 O5 66.94(9) . . ?
O3 La1 O5 137.88(9) 1_556 . ?
O6 La1 O5 143.04(9) 1_455 . ?
O2 La1 O5 71.30(9) 2_665 . ?
O5 La1 O5 71.76(9) 2_665 . ?
O4 La1 O5 114.99(8) 2_675 . ?
O8 La1 O5 94.91(11) . . ?
O4 La1 O5 52.43(8) . . ?
O1 La1 S1 83.88(7) . . ?
O3 La1 S1 138.97(7) 1_556 . ?
O6 La1 S1 152.85(7) 1_455 . ?
O2 La1 S1 68.01(7) 2_665 . ?
O5 La1 S1 96.09(6) 2_665 . ?
O4 La1 S1 88.78(6) 2_675 . ?
O8 La1 S1 83.63(9) . . ?
O4 La1 S1 26.23(6) . . ?
O5 La1 S1 26.32(6) . . ?
C2 C1 C5 117.3(4) . . ?
C2 C1 C6 119.4(4) . . ?
C5 C1 C6 123.3(4) . . ?
C3 C2 C1 121.5(4) . . ?
N1 C3 C2 119.2(4) . . ?
N1 C4 C5 119.8(4) . . ?
C4 C5 C1 120.6(4) . . ?
O1 C6 O2 125.3(4) . . ?
O1 C6 C1 116.0(4) . . ?
O2 C6 C1 118.7(4) . . ?
O3 N1 C4 119.6(3) . . ?
O3 N1 C3 119.0(4) . . ?
C4 N1 C3 121.4(4) . . ?
C6 O1 La1 146.8(3) . . ?
C6 O2 La1 131.4(3) . 2_665 ?
N1 O3 La1 133.2(2) . 1_554 ?
S1 O4 La1 138.24(15) . 2_675 ?
S1 O4 La1 102.72(13) . . ?
La1 O4 La1 116.78(10) 2_675 . ?
S1 O5 La1 143.16(17) . 2_665 ?
S1 O5 La1 100.49(14) . . ?
La1 O5 La1 108.24(9) 2_665 . ?
S1 O6 La1 145.91(18) . 1_655 ?
O7 S1 O6 111.30(17) . . ?
O7 S1 O5 110.71(17) . . ?
O6 S1 O5 110.76(18) . . ?
O7 S1 O4 110.67(17) . . ?
O6 S1 O4 109.21(17) . . ?
O5 S1 O4 103.94(16) . . ?
O7 S1 La1 129.70(12) . . ?
O6 S1 La1 118.96(13) . . ?
O5 S1 La1 53.19(11) . . ?
O4 S1 La1 51.06(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
La1 O1 2.449(3) . ?
La1 O3 2.472(3) 1_556 ?
La1 O6 2.487(3) 1_455 ?
La1 O2 2.543(3) 2_665 ?
La1 O5 2.560(3) 2_665 ?
La1 O4 2.587(3) 2_675 ?
La1 O8 2.617(4) . ?
La1 O4 2.635(3) . ?
La1 O5 2.691(3) . ?
La1 S1 3.3050(10) . ?
C1 C2 1.379(6) . ?
C1 C5 1.391(6) . ?
C1 C6 1.490(6) . ?
C2 C3 1.372(6) . ?
C3 N1 1.352(5) . ?
C4 N1 1.348(6) . ?
C4 C5 1.374(6) . ?
C6 O1 1.247(5) . ?
C6 O2 1.277(5) . ?
N1 O3 1.329(4) . ?
O2 La1 2.543(3) 2_665 ?
O3 La1 2.472(3) 1_554 ?
O4 S1 1.497(3) . ?
O4 La1 2.587(3) 2_675 ?
O5 S1 1.490(3) . ?
O5 La1 2.560(3) 2_665 ?
O6 S1 1.464(3) . ?
O6 La1 2.487(3) 1_655 ?
O7 S1 1.457(3) . ?
