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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/4/30/85/4308567.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_4308567
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 N O8 Pr S'
_chemical_formula_weight         393.09
_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                77.3539(13)
_cell_angle_beta                 87.3002(12)
_cell_angle_gamma                90.0259(15)
_cell_formula_units_Z            2
_cell_length_a                   6.6182(2)
_cell_length_b                   7.2788(2)
_cell_length_c                   10.3611(3)
_cell_measurement_reflns_used    5738
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.60
_cell_volume                     486.44(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 0.997
_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  0.0816
_diffrn_reflns_av_sigmaI/netI    0.0652
_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            9677
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.256
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    2.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.576
_refine_diff_density_min         -2.300
_refine_diff_density_rms         0.267
_refine_ls_extinction_coef       0.065(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0369
_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)+(0.0439P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                1939
_reflns_number_total             2231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0487575si20040906_123354_03.cif
_cod_data_source_block           3
_cod_database_code               4308567
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
Pr1 Pr 0.32819(4) 0.73704(4) 0.01653(3) 0.01442(16) Uani 1 1 d . . .
C1 C 0.2840(8) 0.5375(8) -0.3836(5) 0.0178(11) Uani 1 1 d . . .
C2 C 0.2647(9) 0.7246(8) -0.4469(6) 0.0239(12) Uani 1 1 d . . .
H2A H 0.2772 0.8185 -0.3996 0.029 Uiso 1 1 calc R . .
C3 C 0.2274(9) 0.7719(8) -0.5789(6) 0.0244(13) Uani 1 1 d . . .
H3A H 0.2227 0.8980 -0.6220 0.029 Uiso 1 1 calc R . .
C4 C 0.2173(8) 0.4532(8) -0.5889(6) 0.0225(12) Uani 1 1 d . . .
H4A H 0.2002 0.3614 -0.6374 0.027 Uiso 1 1 calc R . .
C5 C 0.2633(8) 0.4017(8) -0.4578(6) 0.0205(12) Uani 1 1 d . . .
H5A H 0.2807 0.2753 -0.4187 0.025 Uiso 1 1 calc R . .
C6 C 0.3285(8) 0.4911(8) -0.2380(6) 0.0176(11) Uani 1 1 d . . .
N1 N 0.1972(7) 0.6356(7) -0.6469(5) 0.0200(10) Uani 1 1 d . . .
O1 O 0.2723(6) 0.6086(5) -0.1745(4) 0.0211(8) Uani 1 1 d . . .
O2 O 0.4253(5) 0.3408(5) -0.1951(4) 0.0191(8) Uani 1 1 d . . .
O3 O 0.1425(6) 0.6826(6) -0.7711(4) 0.0244(9) Uani 1 1 d . . .
O4 O 0.6560(5) 0.9344(5) -0.0654(4) 0.0193(8) Uani 1 1 d . . .
O5 O 0.6663(5) 0.6180(5) -0.0843(4) 0.0190(8) Uani 1 1 d . . .
O6 O 0.9591(5) 0.7565(6) -0.0072(4) 0.0222(8) Uani 1 1 d . . .
O7 O 0.8780(5) 0.8488(5) -0.2352(4) 0.0196(8) Uani 1 1 d . . .
O8 O 0.2647(8) 0.9871(7) -0.1955(5) 0.0269(11) Uani 1 1 d . . .
S1 S 0.79795(18) 0.78952(18) -0.09991(13) 0.0149(3) Uani 1 1 d . . .
HW1 H 0.276(12) 1.069(12) -0.171(8) 0.05(3) Uiso 1 1 d . . .
HW2 H 0.183(11) 0.983(11) -0.220(7) 0.02(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'
Pr Pr -0.2180 2.8214 '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 Pr1 O3 129.74(13) . 1_556 ?
O1 Pr1 O6 75.60(12) . 1_455 ?
O3 Pr1 O6 67.86(13) 1_556 1_455 ?
O1 Pr1 O2 132.35(12) . 2_665 ?
O3 Pr1 O2 71.50(12) 1_556 2_665 ?
O6 Pr1 O2 139.24(13) 1_455 2_665 ?
O1 Pr1 O5 71.09(13) . 2_665 ?
O3 Pr1 O5 78.89(13) 1_556 2_665 ?
O6 Pr1 O5 95.07(12) 1_455 2_665 ?
O2 Pr1 O5 73.90(12) 2_665 2_665 ?
O1 Pr1 O4 136.10(13) . 2_675 ?
O3 Pr1 O4 79.49(13) 1_556 2_675 ?
O6 Pr1 O4 91.93(12) 1_455 2_675 ?
O2 Pr1 O4 83.65(12) 2_665 2_675 ?
O5 Pr1 O4 152.76(13) 2_665 2_675 ?
O1 Pr1 O8 65.88(15) . . ?
O3 Pr1 O8 128.46(14) 1_556 . ?
O6 Pr1 O8 72.46(16) 1_455 . ?
O2 Pr1 O8 140.63(16) 2_665 . ?
O5 Pr1 O8 136.90(16) 2_665 . ?
O4 Pr1 O8 70.23(15) 2_675 . ?
O1 Pr1 O4 100.11(12) . . ?
O3 Pr1 O4 130.07(12) 1_556 . ?
O6 Pr1 O4 139.92(13) 1_455 . ?
O2 Pr1 O4 72.40(12) 2_665 . ?
O5 Pr1 O4 121.69(11) 2_665 . ?
O4 Pr1 O4 63.25(12) 2_675 . ?
O8 Pr1 O4 69.70(15) . . ?
O1 Pr1 O5 67.45(12) . . ?
O3 Pr1 O5 137.55(13) 1_556 . ?
O6 Pr1 O5 143.00(12) 1_455 . ?
O2 Pr1 O5 71.47(12) 2_665 . ?
O5 Pr1 O5 71.54(13) 2_665 . ?
O4 Pr1 O5 115.96(11) 2_675 . ?
O8 Pr1 O5 93.64(14) . . ?
O4 Pr1 O5 53.23(11) . . ?
O1 Pr1 S1 84.95(9) . . ?
O3 Pr1 S1 138.55(10) 1_556 . ?
O6 Pr1 S1 153.04(10) 1_455 . ?
O2 Pr1 S1 67.65(9) 2_665 . ?
O5 Pr1 S1 96.07(8) 2_665 . ?
O4 Pr1 S1 89.29(8) 2_675 . ?
O8 Pr1 S1 82.68(12) . . ?
O4 Pr1 S1 26.65(8) . . ?
O5 Pr1 S1 26.73(8) . . ?
C2 C1 C5 118.0(5) . . ?
C2 C1 C6 118.7(5) . . ?
C5 C1 C6 123.3(5) . . ?
C3 C2 C1 120.3(5) . . ?
N1 C3 C2 120.3(6) . . ?
N1 C4 C5 120.2(5) . . ?
C4 C5 C1 120.3(5) . . ?
O1 C6 O2 126.9(5) . . ?
O1 C6 C1 115.7(5) . . ?
O2 C6 C1 117.4(4) . . ?
O3 N1 C4 119.5(5) . . ?
O3 N1 C3 119.7(5) . . ?
C4 N1 C3 120.7(5) . . ?
C6 O1 Pr1 145.2(4) . . ?
C6 O2 Pr1 130.9(3) . 2_665 ?
N1 O3 Pr1 133.5(3) . 1_554 ?
S1 O4 Pr1 138.9(2) . 2_675 ?
S1 O4 Pr1 102.34(18) . . ?
Pr1 O4 Pr1 116.75(12) 2_675 . ?
S1 O5 Pr1 142.4(2) . 2_665 ?
S1 O5 Pr1 100.49(17) . . ?
Pr1 O5 Pr1 108.46(13) 2_665 . ?
S1 O6 Pr1 145.5(2) . 1_655 ?
O7 S1 O6 111.4(2) . . ?
O7 S1 O5 110.7(2) . . ?
O6 S1 O5 110.9(2) . . ?
O7 S1 O4 110.5(2) . . ?
O6 S1 O4 109.6(2) . . ?
O5 S1 O4 103.4(2) . . ?
O7 S1 Pr1 129.83(17) . . ?
O6 S1 Pr1 118.76(17) . . ?
O5 S1 Pr1 52.78(14) . . ?
O4 S1 Pr1 51.01(14) . . ?
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
Pr1 O1 2.410(4) . ?
Pr1 O3 2.423(4) 1_556 ?
Pr1 O6 2.468(4) 1_455 ?
Pr1 O2 2.496(4) 2_665 ?
Pr1 O5 2.526(4) 2_665 ?
Pr1 O4 2.553(3) 2_675 ?
Pr1 O8 2.579(5) . ?
Pr1 O4 2.604(4) . ?
Pr1 O5 2.651(3) . ?
Pr1 S1 3.2727(12) . ?
C1 C2 1.385(8) . ?
C1 C5 1.388(7) . ?
C1 C6 1.515(8) . ?
C2 C3 1.369(9) . ?
C3 N1 1.357(7) . ?
C4 N1 1.342(7) . ?
C4 C5 1.377(8) . ?
C6 O1 1.235(6) . ?
C6 O2 1.273(6) . ?
N1 O3 1.324(6) . ?
O2 Pr1 2.496(4) 2_665 ?
O3 Pr1 2.423(4) 1_554 ?
O4 S1 1.503(3) . ?
O4 Pr1 2.553(3) 2_675 ?
O5 S1 1.497(4) . ?
O5 Pr1 2.526(4) 2_665 ?
O6 S1 1.453(4) . ?
O6 Pr1 2.468(4) 1_655 ?
O7 S1 1.448(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O8 HW1 O2 0.70(8) 2.17(8) 2.786(6) 147(8) 1_565
O8 HW2 O7 0.61(7) 2.27(7) 2.831(7) 154(9) 1_455
C3 H3A O7 0.93 2.22 3.102(7) 157.9 2_674
C4 H4A O7 0.93 2.30 3.227(7) 173.2 2_664
