#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/09/2210932.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2210932
loop_
_publ_author_name
'Zhang, Shu-Hua'
_publ_section_title
Poly[[μ₃-2-[(2-pyridylmethylene)amino]ethanesulfonato-κ⁵N,N':O:O':O'']sodium(I)]
_journal_coeditor_code           CI2187
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3062
_journal_page_last               m3064
_journal_paper_doi               10.1107/S1600536806043352
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Na (C8 H9 N2 O3 S)]'
_chemical_formula_moiety         'C8 H9 N2 Na O3 S'
_chemical_formula_sum            'C8 H9 N2 Na O3 S'
_chemical_formula_weight         236.23
_chemical_name_systematic
;
Poly[[μ₃-2-[(2-Pyridylmethylene)amino]ethanesulfonato-
κ⁵N,N':O:O':O'']sodium(I)]
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.198(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3001(14)
_cell_length_b                   10.1413(14)
_cell_length_c                   9.6613(13)
_cell_measurement_reflns_used    2068
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.00
_cell_volume                     998.9(2)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.1005
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5474
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.540
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0434
_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)+(0.0653P)²+0.2404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                1921
_reflns_number_total             2062
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ci2187.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2210932
_cod_database_fobs_code          2210932
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.4797(2) 0.4958(2) 0.6908(2) 0.0426(5) Uani d . 1
H H1 0.4471 0.5504 0.6165 0.051 Uiso calc R 1
C C2 0.6110(2) 0.4629(2) 0.7069(2) 0.0461(5) Uani d . 1
H H2 0.6648 0.4937 0.6444 0.055 Uiso calc R 1
C C3 0.66075(19) 0.3837(2) 0.8172(2) 0.0473(5) Uani d . 1
H H3 0.7489 0.3600 0.8306 0.057 Uiso calc R 1
C C4 0.57776(19) 0.3399(2) 0.9080(2) 0.0405(5) Uani d . 1
H H4 0.6093 0.2874 0.9843 0.049 Uiso calc R 1
C C5 0.44642(16) 0.37564(17) 0.88291(18) 0.0321(4) Uani d . 1
C C6 0.35470(19) 0.32853(18) 0.9772(2) 0.0365(4) Uani d . 1
H H6 0.3864 0.2745 1.0522 0.044 Uiso calc R 1
C C7 0.15162(19) 0.3073(2) 1.05561(19) 0.0385(4) Uani d . 1
H H7A 0.1118 0.3790 1.1009 0.046 Uiso calc R 1
H H7B 0.2033 0.2546 1.1271 0.046 Uiso calc R 1
C C8 0.04581(17) 0.22261(18) 0.97251(17) 0.0318(4) Uani d . 1
H H8A 0.0864 0.1438 0.9412 0.038 Uiso calc R 1
H H8B 0.0078 0.2711 0.8901 0.038 Uiso calc R 1
N N1 0.39663(15) 0.45371(17) 0.77558(16) 0.0360(4) Uani d . 1
N N2 0.23508(15) 0.35954(16) 0.95851(16) 0.0344(3) Uani d . 1
Na Na1 0.16606(6) 0.52184(7) 0.75924(6) 0.0299(2) Uani d . 1
O O1 -0.02427(12) 0.09104(13) 1.18190(12) 0.0346(3) Uani d . 1
O O2 -0.13476(14) 0.29554(14) 1.11748(14) 0.0387(3) Uani d . 1
O O3 -0.17606(12) 0.10502(13) 0.96751(12) 0.0338(3) Uani d . 1
S S1 -0.08189(3) 0.17499(4) 1.06755(4) 0.02468(17) Uani d . 1
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'
Na Na 0.0362 0.0249 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 123.80(19) ?
N1 C1 H1 . . 118.1 ?
C2 C1 H1 . . 118.1 ?
C3 C2 C1 . . 118.68(19) ?
C3 C2 H2 . . 120.7 ?
C1 C2 H2 . . 120.7 ?
C2 C3 C4 . . 118.98(18) ?
C2 C3 H3 . . 120.5 ?
C4 C3 H3 . . 120.5 ?
C3 C4 C5 . . 118.71(19) ?
C3 C4 H4 . . 120.6 ?
C5 C4 H4 . . 120.6 ?
N1 C5 C4 . . 122.87(17) ?
N1 C5 C6 . . 117.17(15) ?
C4 C5 C6 . . 119.96(17) ?
N2 C6 C5 . . 121.87(16) ?
N2 C6 H6 . . 119.1 ?
C5 C6 H6 . . 119.1 ?
N2 C7 C8 . . 107.97(14) ?
N2 C7 H7A . . 110.1 ?
C8 C7 H7A . . 110.1 ?
N2 C7 H7B . . 110.1 ?
C8 C7 H7B . . 110.1 ?
H7A C7 H7B . . 108.4 ?
C7 C8 S1 . . 114.07(12) ?
C7 C8 H8A . . 108.7 ?
S1 C8 H8A . . 108.7 ?
C7 C8 H8B . . 108.7 ?
S1 C8 H8B . . 108.7 ?
H8A C8 H8B . . 107.6 ?
C1 N1 C5 . . 116.95(16) ?
C1 N1 Na1 . . 124.64(13) ?
C5 N1 Na1 . . 118.25(11) ?
C6 N2 C7 . . 118.11(16) ?
C6 N2 Na1 . . 115.47(13) ?
C7 N2 Na1 . . 126.31(12) ?
O2 Na1 O1 3_567 4_565 113.68(6) yes
O2 Na1 O3 3_567 2_556 103.03(6) yes
O1 Na1 O3 4_565 2_556 91.39(5) yes
O2 Na1 N1 3_567 . 114.06(6) yes
O1 Na1 N1 4_565 . 130.69(6) yes
O3 Na1 N1 2_556 . 89.45(5) yes
O2 Na1 N2 3_567 . 100.18(6) yes
O1 Na1 N2 4_565 . 93.26(5) yes
O3 Na1 N2 2_556 . 152.13(6) yes
N1 Na1 N2 . . 66.92(5) yes
S1 O1 Na1 . 4_566 140.83(8) yes
S1 O2 Na1 . 3_567 163.73(9) yes
S1 O3 Na1 . 2_546 132.67(8) yes
O2 S1 O1 . . 111.93(8) ?
O2 S1 O3 . . 112.75(8) ?
O1 S1 O3 . . 112.41(8) ?
O2 S1 C8 . . 106.50(9) ?
O1 S1 C8 . . 107.48(8) ?
O3 S1 C8 . . 105.21(8) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.336(3) ?
C1 C2 . 1.381(3) ?
C1 H1 . 0.93 ?
C2 C3 . 1.373(3) ?
C2 H2 . 0.93 ?
C3 C4 . 1.383(3) ?
C3 H3 . 0.93 ?
C4 C5 . 1.388(2) ?
C4 H4 . 0.93 ?
C5 N1 . 1.347(2) ?
C5 C6 . 1.482(3) ?
C6 N2 . 1.259(3) yes
C6 H6 . 0.93 ?
C7 N2 . 1.460(2) yes
C7 C8 . 1.523(2) ?
C7 H7A . 0.97 ?
C7 H7B . 0.97 ?
C8 S1 . 1.7751(17) ?
C8 H8A . 0.97 ?
C8 H8B . 0.97 ?
N1 Na1 . 2.4568(16) yes
N2 Na1 . 2.5555(17) yes
Na1 O2 3_567 2.2498(15) yes
Na1 O1 4_565 2.3010(14) yes
Na1 O3 2_556 2.3634(13) yes
O1 S1 . 1.4528(12) yes
O1 Na1 4_566 2.3010(14) ?
O2 S1 . 1.4488(14) yes
O2 Na1 3_567 2.2498(15) ?
O3 S1 . 1.4530(12) yes
O3 Na1 2_546 2.3634(13) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C8 H8B O1 4_565 0.97 2.43 3.376(2) 164
