#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:38:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179254 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/74/4317420.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_4317420
loop_
_publ_author_name
'Xian-He Bu'
'Wei Weng'
'Jian-Rong Li'
'Wei Chen'
'Ruo-Hua Zhang'
_publ_section_title
;
 Novel Five-Connected Lanthanide(III)-Bis(sulfinyl) Coordination Polymers
 Forming a Unique Two-Dimensional (3/4,5) Network
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              413
_journal_page_last               415
_journal_paper_doi               10.1021/ic010605b
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C23 H45 N3 O5 S8 Yb'
_chemical_formula_weight         873.14
_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                97.0230(10)
_cell_angle_beta                 95.5590(10)
_cell_angle_gamma                96.9410(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9752(6)
_cell_length_b                   12.4973(8)
_cell_length_c                   17.1536(10)
_cell_measurement_temperature    298(2)
_cell_volume                     1883.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7910
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    2.960
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.602
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0563P)²+0.3891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                5835
_reflns_number_total             6605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010605b_2.cif
_cod_data_source_block           complex2(yb)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317420
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
Yb1 Yb 0.67232(2) 0.975518(16) 0.755252(10) 0.03277(8) Uani 1 1 d . . .
C1 C 0.4553(6) 1.1717(4) 0.8357(3) 0.0469(12) Uani 1 1 d . . .
N1 N 0.5270(5) 1.1143(4) 0.8017(3) 0.0514(11) Uani 1 1 d . . .
O1 O 0.5343(4) 0.9004(3) 0.84552(18) 0.0454(8) Uani 1 1 d . . .
S1 S 0.56248(14) 0.86177(11) 0.92532(7) 0.0418(3) Uani 1 1 d . . .
C2 C 0.7653(6) 0.8147(5) 0.5860(3) 0.0538(14) Uani 1 1 d . . .
N2 N 0.7247(5) 0.8628(4) 0.6394(3) 0.0538(11) Uani 1 1 d . . .
O2 O 0.4341(3) 0.9007(3) 0.68766(18) 0.0427(8) Uani 1 1 d . . .
S2 S 0.29698(14) 0.84405(11) 0.71842(7) 0.0451(3) Uani 1 1 d . . .
C3 C 0.8923(6) 0.7731(4) 0.8092(3) 0.0460(12) Uani 1 1 d . . .
N3 N 0.8153(5) 0.8391(4) 0.7990(3) 0.0545(11) Uani 1 1 d . . .
O3 O 0.6419(4) 1.0833(3) 0.65330(18) 0.0429(8) Uani 1 1 d . . .
S3 S 0.51145(13) 1.11867(11) 0.60553(7) 0.0426(3) Uani 1 1 d . . .
C4 C 0.4575(6) 0.9438(4) 0.9881(3) 0.0478(12) Uani 1 1 d . . .
H4A H 0.3598 0.9485 0.9602 0.057 Uiso 1 1 calc R . .
H4B H 0.4409 0.9098 1.0350 0.057 Uiso 1 1 calc R . .
O4 O 0.9064(4) 1.0589(3) 0.73372(19) 0.0450(8) Uani 1 1 d . . .
S4 S 0.97948(14) 1.07641(12) 0.65942(8) 0.0489(3) Uani 1 1 d . . .
C5 C 0.4386(7) 0.7359(5) 0.9159(3) 0.0613(15) Uani 1 1 d . . .
H5A H 0.4290 0.7149 0.9680 0.074 Uiso 1 1 calc R . .
H5B H 0.3391 0.7460 0.8928 0.074 Uiso 1 1 calc R . .
O5 O 0.7979(4) 1.0567(3) 0.88093(19) 0.0489(9) Uani 1 1 d . . .
S5 S 0.96243(15) 1.10056(14) 0.90673(8) 0.0604(4) Uani 1 1 d . . .
C6 C 0.4961(12) 0.6469(6) 0.8653(5) 0.100(3) Uani 1 1 d . . .
H6A H 0.4523 0.6482 0.8115 0.120 Uiso 1 1 calc R . .
H6B H 0.6040 0.6680 0.8665 0.120 Uiso 1 1 calc R . .
S6 S 0.3537(2) 1.24827(18) 0.88517(11) 0.0895(6) Uani 1 1 d . . .
C7 C 0.480(4) 0.5587(13) 0.8760(11) 0.46(3) Uani 1 1 d . . .
H7A H 0.5277 0.5159 0.8379 0.683 Uiso 1 1 calc R . .
H7B H 0.3740 0.5324 0.8709 0.683 Uiso 1 1 calc R . .
H7C H 0.5245 0.5532 0.9283 0.683 Uiso 1 1 calc R . .
S7 S 0.8233(3) 0.7488(3) 0.50980(13) 0.1234(11) Uani 1 1 d . . .
C8 C 0.1646(6) 0.9420(5) 0.7244(4) 0.0606(15) Uani 1 1 d . . .
H8A H 0.0770 0.9105 0.7468 0.073 Uiso 1 1 calc R . .
H8B H 0.2113 1.0054 0.7607 0.073 Uiso 1 1 calc R . .
S8 S 1.0053(2) 0.68428(15) 0.82391(12) 0.0814(5) Uani 1 1 d . . .
C9 C 0.2074(7) 0.7475(5) 0.6367(4) 0.0730(18) Uani 1 1 d . . .
H9A H 0.1073 0.7194 0.6478 0.088 Uiso 1 1 calc R . .
H9B H 0.1964 0.7834 0.5899 0.088 Uiso 1 1 calc R . .
C10 C 0.2955(11) 0.6567(6) 0.6215(5) 0.101(3) Uani 1 1 d . . .
H10A H 0.3083 0.6216 0.6687 0.121 Uiso 1 1 calc R . .
H10B H 0.3949 0.6846 0.6092 0.121 Uiso 1 1 calc R . .
C11 C 0.2163(13) 0.5732(7) 0.5525(6) 0.128(4) Uani 1 1 d . . .
H11A H 0.2757 0.5148 0.5438 0.192 Uiso 1 1 calc R . .
H11B H 0.2050 0.6076 0.5057 0.192 Uiso 1 1 calc R . .
H11C H 0.1185 0.5447 0.5650 0.192 Uiso 1 1 calc R . .
C12 C 0.5265(7) 1.0610(4) 0.5057(3) 0.0526(13) Uani 1 1 d . . .
H12A H 0.4653 1.0956 0.4691 0.063 Uiso 1 1 calc R . .
H12B H 0.6307 1.0740 0.4947 0.063 Uiso 1 1 calc R . .
C13 C 0.5734(7) 1.2586(4) 0.5950(3) 0.0579(14) Uani 1 1 d . . .
H13A H 0.6736 1.2646 0.5779 0.069 Uiso 1 1 calc R . .
H13B H 0.5055 1.2819 0.5548 0.069 Uiso 1 1 calc R . .
C14 C 0.5766(9) 1.3323(5) 0.6732(4) 0.0777(19) Uani 1 1 d . . .
H14A H 0.6414 1.3073 0.7138 0.093 Uiso 1 1 calc R . .
H14B H 0.4756 1.3284 0.6893 0.093 Uiso 1 1 calc R . .
C15 C 0.6348(13) 1.4502(6) 0.6653(6) 0.119(3) Uani 1 1 d . . .
H15A H 0.6355 1.4951 0.7149 0.178 Uiso 1 1 calc R . .
H15B H 0.5699 1.4753 0.6255 0.178 Uiso 1 1 calc R . .
H15C H 0.7355 1.4543 0.6504 0.178 Uiso 1 1 calc R . .
C16 C 1.1114(7) 0.9787(5) 0.6471(4) 0.0624(16) Uani 1 1 d . . .
H16A H 1.0634 0.9160 0.6105 0.075 Uiso 1 1 calc R . .
H16B H 1.1980 1.0112 0.6245 0.075 Uiso 1 1 calc R . .
C17 C 1.1035(6) 1.2013(5) 0.6876(4) 0.0613(15) Uani 1 1 d . . .
H17A H 1.1513 1.2034 0.7411 0.074 Uiso 1 1 calc R . .
H17B H 1.1821 1.2057 0.6527 0.074 Uiso 1 1 calc R . .
C18 C 1.0170(9) 1.2963(6) 0.6834(5) 0.081(2) Uani 1 1 d . . .
H18A H 0.9328 1.2880 0.7147 0.097 Uiso 1 1 calc R . .
H18B H 0.9762 1.2971 0.6291 0.097 Uiso 1 1 calc R . .
C19 C 1.1149(13) 1.4026(7) 0.7134(7) 0.133(4) Uani 1 1 d . . .
H19A H 1.0559 1.4613 0.7100 0.199 Uiso 1 1 calc R . .
H19B H 1.1971 1.4117 0.6820 0.199 Uiso 1 1 calc R . .
H19C H 1.1540 1.4025 0.7675 0.199 Uiso 1 1 calc R . .
C20 C 1.0010(7) 1.0596(5) 1.0035(4) 0.0715(19) Uani 1 1 d . . .
H20A H 1.0991 1.0955 1.0281 0.086 Uiso 1 1 calc R . .
H20B H 0.9254 1.0813 1.0367 0.086 Uiso 1 1 calc R . .
C21 C 0.9580(13) 1.2412(8) 0.9425(7) 0.129(4) Uani 1 1 d . . .
H21A H 0.9100 1.2443 0.9909 0.154 Uiso 1 1 calc R . .
H21B H 1.0615 1.2757 0.9564 0.154 Uiso 1 1 calc R . .
C22 C 0.890(2) 1.2992(11) 0.8956(12) 0.261(11) Uani 1 1 d . . .
H22A H 0.7934 1.2565 0.8751 0.313 Uiso 1 1 calc R . .
H22B H 0.9482 1.3028 0.8510 0.313 Uiso 1 1 calc R . .
C23 C 0.858(2) 1.4098(11) 0.9189(10) 0.229(8) Uani 1 1 d . . .
H23A H 0.8189 1.4389 0.8731 0.344 Uiso 1 1 calc R . .
H23B H 0.9493 1.4545 0.9429 0.344 Uiso 1 1 calc R . .
H23C H 0.7846 1.4085 0.9561 0.344 Uiso 1 1 calc R . .
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'
Yb Yb -0.3850 5.5486 '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'
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 Yb1 O4 145.23(11) . . ?
O1 Yb1 O3 139.36(12) . . ?
O4 Yb1 O3 70.67(11) . . ?
O1 Yb1 O2 73.07(11) . . ?
O4 Yb1 O2 141.45(11) . . ?
O3 Yb1 O2 76.78(11) . . ?
O1 Yb1 O5 74.99(12) . . ?
O4 Yb1 O5 73.08(12) . . ?
O3 Yb1 O5 119.46(12) . . ?
O2 Yb1 O5 143.38(11) . . ?
O1 Yb1 N1 75.38(14) . . ?
O4 Yb1 N1 108.22(15) . . ?
O3 Yb1 N1 73.44(13) . . ?
O2 Yb1 N1 80.85(14) . . ?
O5 Yb1 N1 74.12(13) . . ?
O1 Yb1 N3 75.63(14) . . ?
O4 Yb1 N3 83.45(14) . . ?
O3 Yb1 N3 142.43(13) . . ?
O2 Yb1 N3 112.53(15) . . ?
O5 Yb1 N3 75.69(15) . . ?
N1 Yb1 N3 142.43(15) . . ?
O1 Yb1 N2 120.03(15) . . ?
O4 Yb1 N2 77.95(14) . . ?
O3 Yb1 N2 75.87(14) . . ?
O2 Yb1 N2 74.50(13) . . ?
O5 Yb1 N2 138.74(14) . . ?
N1 Yb1 N2 144.18(15) . . ?
N3 Yb1 N2 72.34(15) . . ?
N1 C1 S6 177.8(5) . . ?
C1 N1 Yb1 167.9(4) . . ?
S1 O1 Yb1 138.2(2) . . ?
O1 S1 C5 103.7(2) . . ?
O1 S1 C4 103.6(2) . . ?
C5 S1 C4 98.0(3) . . ?
N2 C2 S7 178.9(6) . . ?
C2 N2 Yb1 172.6(5) . . ?
S2 O2 Yb1 129.81(18) . . ?
O2 S2 C9 104.6(3) . . ?
O2 S2 C8 105.5(2) . . ?
C9 S2 C8 101.6(3) . . ?
N3 C3 S8 177.9(5) . . ?
C3 N3 Yb1 169.8(4) . . ?
S3 O3 Yb1 136.4(2) . . ?
O3 S3 C12 103.9(2) . . ?
O3 S3 C13 104.9(2) . . ?
C12 S3 C13 97.3(3) . . ?
C4 C4 S1 110.5(5) 2_677 . ?
S4 O4 Yb1 133.0(2) . . ?
O4 S4 C17 103.6(2) . . ?
O4 S4 C16 107.4(2) . . ?
C17 S4 C16 101.9(3) . . ?
C6 C5 S1 111.6(5) . . ?
S5 O5 Yb1 130.9(2) . . ?
O5 S5 C21 103.7(4) . . ?
O5 S5 C20 104.7(3) . . ?
C21 S5 C20 95.3(4) . . ?
C7 C6 C5 123.1(11) . . ?
C16 C8 S2 115.5(4) 1_455 . ?
C10 C9 S2 111.3(5) . . ?
C9 C10 C11 111.0(8) . . ?
C12 C12 S3 110.1(5) 2_676 . ?
C14 C13 S3 110.7(4) . . ?
C13 C14 C15 110.9(6) . . ?
C8 C16 S4 112.1(4) 1_655 . ?
C18 C17 S4 110.2(5) . . ?
C17 C18 C19 111.8(7) . . ?
C20 C20 S5 110.1(5) 2_777 . ?
C22 C21 S5 117.7(10) . . ?
C21 C22 C23 124.7(18) . . ?
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
Yb1 O1 2.293(3) . ?
Yb1 O4 2.313(3) . ?
Yb1 O3 2.349(3) . ?
Yb1 O2 2.358(3) . ?
Yb1 O5 2.380(3) . ?
Yb1 N1 2.398(4) . ?
Yb1 N3 2.403(5) . ?
Yb1 N2 2.411(4) . ?
C1 N1 1.163(6) . ?
C1 S6 1.621(5) . ?
O1 S1 1.515(3) . ?
S1 C5 1.794(6) . ?
S1 C4 1.805(5) . ?
C2 N2 1.147(7) . ?
C2 S7 1.621(6) . ?
O2 S2 1.517(3) . ?
S2 C9 1.789(6) . ?
S2 C8 1.807(6) . ?
C3 N3 1.156(6) . ?
C3 S8 1.617(6) . ?
O3 S3 1.506(3) . ?
S3 C12 1.799(5) . ?
S3 C13 1.806(6) . ?
C4 C4 1.504(10) 2_677 ?
O4 S4 1.516(3) . ?
S4 C17 1.789(6) . ?
S4 C16 1.809(6) . ?
C5 C6 1.499(9) . ?
O5 S5 1.515(3) . ?
S5 C21 1.795(11) . ?
S5 C20 1.810(6) . ?
C6 C7 1.134(15) . ?
C8 C16 1.509(8) 1_455 ?
C9 C10 1.471(10) . ?
C10 C11 1.534(11) . ?
C12 C12 1.523(11) 2_676 ?
C13 C14 1.528(9) . ?
C14 C15 1.530(10) . ?
C16 C8 1.509(8) 1_655 ?
C17 C18 1.500(9) . ?
C18 C19 1.505(11) . ?
C20 C20 1.477(13) 2_777 ?
C21 C22 1.305(18) . ?
C22 C23 1.461(17) . ?
