#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:07:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179094 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/56/4305653.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_4305653
loop_
_publ_author_name
'Na Xu'
'Wei Shi'
'Dai-Zheng Liao'
'Shi-Ping Yan'
'Peng Cheng'
_publ_contact_author_address
;Department of Chemistry
Nankai University
Tianjin 300071, P. R. China
;
_publ_contact_author_email       liaodz@nankai.edu.cn
_publ_contact_author_fax         +86-22-23502458
_publ_contact_author_name        'Dai-Zheng Liao'
_publ_contact_author_phone       +86-22-23505063
_publ_section_title
;
Template Synthesis of Lanthanide (Pr, Nd, Gd) Coordination Polymers with
2-Hydroxynicotinic Acid Exhibiting Ferro-/Antiferromagnetic Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8748
_journal_page_last               8756
_journal_paper_doi               10.1021/ic800623v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C6 H8 N O9 Pr S'
_chemical_formula_sum            'C6 H8 N O9 Pr S'
_chemical_formula_weight         411.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.036(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0390(11)
_cell_length_b                   18.706(3)
_cell_length_c                   8.9548(14)
_cell_measurement_reflns_used    3790
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.55
_cell_volume                     1161.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6414
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    4.416
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.603641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    2.352
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2372
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0237
_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)+(0.0192P)²+0.3451P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                2090
_reflns_number_total             2372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800623v_si_001_2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1161.0(3)
_cod_database_code               4305653
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.22650(3) 0.451360(9) 0.40102(2) 0.01092(7) Uani 1 1 d . . .
O1 O 0.3352(3) 0.33028(13) 0.4010(3) 0.0232(6) Uani 1 1 d . . .
O2 O 0.5935(3) 0.43912(12) 0.4863(3) 0.0159(5) Uani 1 1 d . . .
O3 O 0.8878(3) 0.42671(13) 0.4381(3) 0.0160(5) Uani 1 1 d . . .
O4 O 0.3969(4) 0.47250(19) 0.1886(3) 0.0327(7) Uani 1 1 d D . .
O5 O 0.0344(4) 0.39465(15) 0.1628(3) 0.0221(6) Uani 1 1 d D . .
N1 N 0.4655(5) 0.22727(16) 0.3413(4) 0.0291(9) Uani 1 1 d . . .
H1 H 0.3550 0.2077 0.3414 0.035 Uiso 1 1 calc R . .
C1 C 0.4834(5) 0.29808(19) 0.3785(4) 0.0185(8) Uani 1 1 d . . .
C2 C 0.6742(5) 0.32712(18) 0.3846(4) 0.0166(8) Uani 1 1 d . . .
C3 C 0.8175(6) 0.2837(2) 0.3468(5) 0.0269(10) Uani 1 1 d . . .
H3 H 0.9404 0.3026 0.3498 0.032 Uiso 1 1 calc R . .
C4 C 0.7841(6) 0.2127(2) 0.3044(6) 0.0374(12) Uani 1 1 d . . .
H4 H 0.8817 0.1849 0.2767 0.045 Uiso 1 1 calc R . .
C5 C 0.6070(6) 0.1852(2) 0.3042(5) 0.0351(11) Uani 1 1 d . . .
H5 H 0.5820 0.1375 0.2787 0.042 Uiso 1 1 calc R . .
C6 C 0.7218(5) 0.40162(18) 0.4375(4) 0.0122(7) Uani 1 1 d . . .
S1 S -0.15793(12) 0.56353(5) 0.19881(10) 0.01445(19) Uani 1 1 d . . .
O6 O 0.0493(3) 0.54797(12) 0.2468(3) 0.0176(6) Uani 1 1 d . . .
O7 O -0.2516(3) 0.50157(14) 0.1136(3) 0.0207(6) Uani 1 1 d . . .
O8 O -0.2504(4) 0.57597(14) 0.3326(3) 0.0205(6) Uani 1 1 d . . .
O9 O -0.1820(4) 0.62770(14) 0.1027(3) 0.0213(6) Uani 1 1 d . . .
H4A H 0.516(2) 0.480(2) 0.192(5) 0.041(13) Uiso 1 1 d D . .
H4B H 0.328(5) 0.471(4) 0.100(3) 0.11(3) Uiso 1 1 d D . .
H5A H 0.079(6) 0.378(2) 0.088(3) 0.050(15) Uiso 1 1 d D . .
H5B H -0.052(5) 0.4269(19) 0.141(4) 0.048(16) 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'
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 O8 80.36(9) . 3_566 ?
O1 Pr1 O4 87.29(11) . . ?
O8 Pr1 O4 147.22(9) 3_566 . ?
O1 Pr1 O6 145.24(9) . . ?
O8 Pr1 O6 130.31(8) 3_566 . ?
O4 Pr1 O6 73.52(10) . . ?
O1 Pr1 O3 97.90(8) . 1_455 ?
O8 Pr1 O3 74.61(8) 3_566 1_455 ?
O4 Pr1 O3 137.54(9) . 1_455 ?
O6 Pr1 O3 79.04(8) . 1_455 ?
O1 Pr1 O2 129.09(8) . 3_666 ?
O8 Pr1 O2 80.41(9) 3_566 3_666 ?
O4 Pr1 O2 84.26(10) . 3_666 ?
O6 Pr1 O2 78.44(8) . 3_666 ?
O3 Pr1 O2 121.26(8) 1_455 3_666 ?
O1 Pr1 O5 74.25(9) . . ?
O8 Pr1 O5 132.33(9) 3_566 . ?
O4 Pr1 O5 71.20(9) . . ?
O6 Pr1 O5 72.23(8) . . ?
O3 Pr1 O5 69.89(8) 1_455 . ?
O2 Pr1 O5 145.91(8) 3_666 . ?
O1 Pr1 O2 67.11(8) . . ?
O8 Pr1 O2 78.15(8) 3_566 . ?
O4 Pr1 O2 69.08(9) . . ?
O6 Pr1 O2 127.78(8) . . ?
O3 Pr1 O2 150.84(8) 1_455 . ?
O2 Pr1 O2 62.98(9) 3_666 . ?
O5 Pr1 O2 124.74(8) . . ?
O1 Pr1 O3 149.98(8) . 3_666 ?
O8 Pr1 O3 69.63(8) 3_566 3_666 ?
O4 Pr1 O3 118.46(10) . 3_666 ?
O6 Pr1 O3 62.90(7) . 3_666 ?
O3 Pr1 O3 74.04(8) 1_455 3_666 ?
O2 Pr1 O3 47.41(7) 3_666 3_666 ?
O5 Pr1 O3 126.39(8) . 3_666 ?
O2 Pr1 O3 105.96(7) . 3_666 ?
C1 O1 Pr1 137.1(2) . . ?
C6 O2 Pr1 104.3(2) . 3_666 ?
C6 O2 Pr1 132.8(2) . . ?
Pr1 O2 Pr1 117.02(9) 3_666 . ?
C6 O3 Pr1 166.4(2) . 1_655 ?
C6 O3 Pr1 87.6(2) . 3_666 ?
Pr1 O3 Pr1 105.96(8) 1_655 3_666 ?
Pr1 O4 H4A 128(3) . . ?
Pr1 O4 H4B 116(3) . . ?
H4A O4 H4B 116.2(19) . . ?
Pr1 O5 H5A 127(3) . . ?
Pr1 O5 H5B 99(3) . . ?
H5A O5 H5B 115.4(18) . . ?
C5 N1 C1 125.6(3) . . ?
C5 N1 H1 117.2 . . ?
C1 N1 H1 117.2 . . ?
O1 C1 N1 117.5(3) . . ?
O1 C1 C2 127.6(3) . . ?
N1 C1 C2 114.8(3) . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 C6 119.6(3) . . ?
C1 C2 C6 121.4(3) . . ?
C2 C3 C4 122.2(4) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 118.6(4) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 N1 119.7(4) . . ?
C4 C5 H5 120.1 . . ?
N1 C5 H5 120.1 . . ?
O3 C6 O2 120.3(3) . . ?
O3 C6 C2 120.5(3) . . ?
O2 C6 C2 119.2(3) . . ?
O9 S1 O6 109.80(14) . . ?
O9 S1 O7 110.03(15) . . ?
O6 S1 O7 108.97(14) . . ?
O9 S1 O8 108.90(15) . . ?
O6 S1 O8 110.35(15) . . ?
O7 S1 O8 108.78(15) . . ?
S1 O6 Pr1 133.04(14) . . ?
S1 O8 Pr1 143.32(15) . 3_566 ?
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 2.391(2) . ?
Pr1 O8 2.417(3) 3_566 ?
Pr1 O4 2.451(3) . ?
Pr1 O6 2.475(2) . ?
Pr1 O3 2.507(2) 1_455 ?
Pr1 O2 2.525(2) 3_666 ?
Pr1 O5 2.549(3) . ?
Pr1 O2 2.573(2) . ?
Pr1 O3 2.886(2) 3_666 ?
O1 C1 1.251(4) . ?
O2 C6 1.279(4) . ?
O2 Pr1 2.525(2) 3_666 ?
O3 C6 1.258(4) . ?
O3 Pr1 2.507(2) 1_655 ?
O3 Pr1 2.886(2) 3_666 ?
O4 H4A 0.849(10) . ?
O4 H4B 0.853(10) . ?
O5 H5A 0.854(10) . ?
O5 H5B 0.853(10) . ?
N1 C5 1.355(5) . ?
N1 C1 1.366(4) . ?
N1 H1 0.8600 . ?
C1 C2 1.441(5) . ?
C2 C3 1.382(5) . ?
C2 C6 1.491(5) . ?
C3 C4 1.389(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.349(6) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
S1 O9 1.470(3) . ?
S1 O6 1.476(3) . ?
S1 O7 1.478(3) . ?
S1 O8 1.478(3) . ?
O8 Pr1 2.417(3) 3_566 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 Pr1 O1 C1 -113.0(4) 3_566 . . . ?
O4 Pr1 O1 C1 36.5(4) . . . . ?
O6 Pr1 O1 C1 92.0(4) . . . . ?
O3 Pr1 O1 C1 174.2(4) 1_455 . . . ?
O2 Pr1 O1 C1 -43.9(4) 3_666 . . . ?
O5 Pr1 O1 C1 107.7(4) . . . . ?
O2 Pr1 O1 C1 -31.9(4) . . . . ?
O3 Pr1 O1 C1 -114.2(4) 3_666 . . . ?
O1 Pr1 O2 C6 42.3(3) . . . . ?
O8 Pr1 O2 C6 126.7(3) 3_566 . . . ?
O4 Pr1 O2 C6 -53.9(3) . . . . ?
O6 Pr1 O2 C6 -101.0(3) . . . . ?
O3 Pr1 O2 C6 105.5(3) 1_455 . . . ?
O2 Pr1 O2 C6 -148.1(4) 3_666 . . . ?
O5 Pr1 O2 C6 -7.1(3) . . . . ?
O3 Pr1 O2 C6 -168.8(3) 3_666 . . . ?
O1 Pr1 O2 Pr1 -169.60(14) . . . 3_666 ?
O8 Pr1 O2 Pr1 -85.18(11) 3_566 . . 3_666 ?
O4 Pr1 O2 Pr1 94.28(13) . . . 3_666 ?
O6 Pr1 O2 Pr1 47.17(15) . . . 3_666 ?
O3 Pr1 O2 Pr1 -106.36(15) 1_455 . . 3_666 ?
O2 Pr1 O2 Pr1 0.0 3_666 . . 3_666 ?
O5 Pr1 O2 Pr1 141.04(10) . . . 3_666 ?
O3 Pr1 O2 Pr1 -20.64(12) 3_666 . . 3_666 ?
Pr1 O1 C1 N1 -159.1(3) . . . . ?
Pr1 O1 C1 C2 19.7(6) . . . . ?
C5 N1 C1 O1 175.8(4) . . . . ?
C5 N1 C1 C2 -3.2(6) . . . . ?
O1 C1 C2 C3 -176.0(4) . . . . ?
N1 C1 C2 C3 2.9(6) . . . . ?
O1 C1 C2 C6 6.9(6) . . . . ?
N1 C1 C2 C6 -174.2(3) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
C6 C2 C3 C4 176.6(4) . . . . ?
C2 C3 C4 C5 -1.8(8) . . . . ?
C3 C4 C5 N1 1.6(7) . . . . ?
C1 N1 C5 C4 1.0(7) . . . . ?
Pr1 O3 C6 O2 -168.2(7) 1_655 . . . ?
Pr1 O3 C6 O2 6.4(3) 3_666 . . . ?
Pr1 O3 C6 C2 13.8(12) 1_655 . . . ?
Pr1 O3 C6 C2 -171.6(3) 3_666 . . . ?
Pr1 O2 C6 O3 -7.5(4) 3_666 . . . ?
Pr1 O2 C6 O3 143.4(2) . . . . ?
Pr1 O2 C6 C2 170.5(2) 3_666 . . . ?
Pr1 O2 C6 C2 -38.5(5) . . . . ?
C3 C2 C6 O3 4.9(5) . . . . ?
C1 C2 C6 O3 -178.1(3) . . . . ?
C3 C2 C6 O2 -173.2(4) . . . . ?
C1 C2 C6 O2 3.9(5) . . . . ?
O9 S1 O6 Pr1 -178.20(17) . . . . ?
O7 S1 O6 Pr1 -57.6(2) . . . . ?
O8 S1 O6 Pr1 61.7(2) . . . . ?
O1 Pr1 O6 S1 79.8(2) . . . . ?
O8 Pr1 O6 S1 -67.1(2) 3_566 . . . ?
O4 Pr1 O6 S1 138.9(2) . . . . ?
O3 Pr1 O6 S1 -8.30(19) 1_455 . . . ?
O2 Pr1 O6 S1 -133.7(2) 3_666 . . . ?
O5 Pr1 O6 S1 63.90(19) . . . . ?
O2 Pr1 O6 S1 -175.52(16) . . . . ?
O3 Pr1 O6 S1 -85.9(2) 3_666 . . . ?
O9 S1 O8 Pr1 -146.7(2) . . . 3_566 ?
O6 S1 O8 Pr1 -26.1(3) . . . 3_566 ?
O7 S1 O8 Pr1 93.4(3) . . . 3_566 ?
