#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:26:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179141 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/02/4310277.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_4310277
loop_
_publ_author_name
'Zhong-Ming Sun'
'Jiang-Gao Mao'
'Yan-Qiong Sun'
'Hui-Yi Zeng'
'Abraham Clearfield'
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structures of Three New Divalent
 Metal Carboxylate-Sulfonates with a Layered and One-Dimensional Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              336
_journal_page_last               341
_journal_paper_doi               10.1021/ic0343307
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C18 H18 N2 O10 S Zn'
_chemical_formula_weight         519.77
_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                96.608(2)
_cell_angle_beta                 94.816(2)
_cell_angle_gamma                117.269(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7273(3)
_cell_length_b                   9.5184(4)
_cell_length_c                   13.7818(6)
_cell_measurement_temperature    293(2)
_cell_volume                     998.68(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'narrow frame method'
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5144
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    1.397
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0701
_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)+(0.0978P)²+7.3607P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                2618
_reflns_number_total             3473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0343307si20030516_112750.cif
_cod_data_source_block           1
_cod_original_cell_volume        998.67(7)
_cod_database_code               4310277
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
Zn1 Zn 0.90520(10) 0.66454(10) 0.01262(6) 0.0282(3) Uani 1 1 d . . .
S1 S 1.7458(2) 0.9819(2) 0.33208(13) 0.0303(5) Uani 1 1 d . . .
N1 N 0.7517(7) 0.6486(7) -0.1136(4) 0.0258(13) Uani 1 1 d . . .
N2 N 0.2291(9) 0.5694(10) -0.5529(5) 0.0485(19) Uani 1 1 d . . .
H0A H 0.1664 0.5615 -0.6069 0.058 Uiso 1 1 calc R . .
C1 C 0.8108(9) 0.7541(9) -0.1757(5) 0.0315(16) Uani 1 1 d . . .
H1A H 0.9229 0.8400 -0.1587 0.038 Uiso 1 1 calc R . .
C2 C 0.7133(9) 0.7410(9) -0.2634(6) 0.0324(17) Uani 1 1 d . . .
H2A H 0.7597 0.8161 -0.3046 0.039 Uiso 1 1 calc R . .
C3 C 0.5448(9) 0.6145(8) -0.2897(5) 0.0278(15) Uani 1 1 d . . .
C4 C 0.4836(9) 0.5044(9) -0.2258(5) 0.0306(16) Uani 1 1 d . . .
H4A H 0.3718 0.4177 -0.2405 0.037 Uiso 1 1 calc R . .
C5 C 0.5905(9) 0.5260(9) -0.1418(6) 0.0336(17) Uani 1 1 d . . .
H5A H 0.5485 0.4500 -0.1007 0.040 Uiso 1 1 calc R . .
C6 C 0.4331(10) 0.5966(9) -0.3824(6) 0.0340(17) Uani 1 1 d . . .
C7 C 0.3039(11) 0.4491(10) -0.4308(6) 0.047(2) Uani 1 1 d . . .
H7A H 0.2869 0.3571 -0.4059 0.057 Uiso 1 1 calc R . .
C8 C 0.1993(12) 0.4360(12) -0.5159(7) 0.055(2) Uani 1 1 d . . .
H8A H 0.1095 0.3366 -0.5471 0.066 Uiso 1 1 calc R . .
C9 C 0.3538(11) 0.7136(12) -0.5077(6) 0.047(2) Uani 1 1 d . . .
H9A H 0.3698 0.8038 -0.5346 0.056 Uiso 1 1 calc R . .
C10 C 0.4579(10) 0.7314(10) -0.4233(6) 0.0397(19) Uani 1 1 d . . .
H10A H 0.5450 0.8328 -0.3930 0.048 Uiso 1 1 calc R . .
C11 C 1.4765(9) 0.9560(8) 0.1983(5) 0.0283(16) Uani 1 1 d . . .
H11A H 1.4071 0.8608 0.2197 0.034 Uiso 1 1 calc R . .
C12 C 1.4065(9) 1.0091(8) 0.1253(5) 0.0249(15) Uani 1 1 d . . .
C13 C 1.5110(9) 1.1477(8) 0.0916(5) 0.0257(15) Uani 1 1 d . . .
H13A H 1.4637 1.1821 0.0424 0.031 Uiso 1 1 calc R . .
C14 C 1.6889(8) 1.2370(8) 0.1312(5) 0.0221(14) Uani 1 1 d . . .
C15 C 1.7570(9) 1.1846(8) 0.2054(5) 0.0288(16) Uani 1 1 d . . .
H15A H 1.8744 1.2429 0.2324 0.035 Uiso 1 1 calc R . .
C16 C 1.6509(9) 1.0472(8) 0.2385(5) 0.0273(15) Uani 1 1 d . . .
C17 C 1.2200(8) 0.9101(8) 0.0767(5) 0.0267(15) Uani 1 1 d . . .
C18 C 1.8084(9) 1.3822(8) 0.0910(5) 0.0260(15) Uani 1 1 d . . .
O1 O 1.1298(6) 0.7784(6) 0.1067(4) 0.0336(12) Uani 1 1 d . . .
O2 O 1.1578(6) 0.9515(6) 0.0076(4) 0.0315(12) Uani 1 1 d . . .
O3 O 1.7431(6) 1.4611(6) 0.0535(4) 0.0308(12) Uani 1 1 d . . .
O4 O 1.9677(6) 1.4174(5) 0.0973(4) 0.0284(11) Uani 1 1 d . . .
O11 O 1.6063(8) 0.8527(9) 0.3634(6) 0.070(2) Uani 1 1 d . . .
O12 O 1.8462(9) 1.1180(7) 0.4083(5) 0.0606(19) Uani 1 1 d . . .
O13 O 1.8578(9) 0.9319(9) 0.2846(5) 0.0624(19) Uani 1 1 d . . .
O1W O 0.7882(6) 0.7965(6) 0.0850(4) 0.0341(12) Uani 1 1 d . . .
O2W O 2.1392(9) 0.9136(9) 0.3849(5) 0.0602(18) Uani 1 1 d . . .
O3W O 2.0706(10) 0.6098(9) 0.2888(5) 0.067(2) Uani 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'
Zn Zn 0.2839 1.4301 '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
O3 Zn1 O1 110.9(2) 1_445 . ?
O3 Zn1 N1 98.5(2) 1_445 . ?
O1 Zn1 N1 150.6(2) . . ?
O3 Zn1 O1W 92.8(2) 1_445 . ?
O1 Zn1 O1W 94.4(2) . . ?
N1 Zn1 O1W 85.2(2) . . ?
O3 Zn1 O4 102.48(19) 1_445 2_875 ?
O1 Zn1 O4 90.7(2) . 2_875 ?
N1 Zn1 O4 81.5(2) . 2_875 ?
O1W Zn1 O4 161.01(18) . 2_875 ?
O11 S1 O12 114.1(5) . . ?
O11 S1 O13 112.2(5) . . ?
O12 S1 O13 110.5(4) . . ?
O11 S1 C16 107.1(4) . . ?
O12 S1 C16 107.0(3) . . ?
O13 S1 C16 105.4(3) . . ?
C5 N1 C1 116.3(6) . . ?
C5 N1 Zn1 121.5(5) . . ?
C1 N1 Zn1 122.1(5) . . ?
C9 N2 C8 121.4(7) . . ?
C9 N2 O3W 107.7(6) . 1_354 ?
C8 N2 O3W 130.9(6) . 1_354 ?
C9 N2 H0A 119.3 . . ?
C8 N2 H0A 119.3 . . ?
O3W N2 H0A 11.7 1_354 . ?
N1 C1 C2 123.1(7) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C1 C2 C3 119.4(6) . . ?
C1 C2 H2A 120.3 . . ?
C3 C2 H2A 120.3 . . ?
C2 C3 C4 117.7(6) . . ?
C2 C3 C6 121.6(6) . . ?
C4 C3 C6 120.8(6) . . ?
C5 C4 C3 118.7(7) . . ?
C5 C4 H4A 120.7 . . ?
C3 C4 H4A 120.7 . . ?
N1 C5 C4 124.9(7) . . ?
N1 C5 H5A 117.6 . . ?
C4 C5 H5A 117.6 . . ?
C7 C6 C10 118.0(7) . . ?
C7 C6 C3 122.0(7) . . ?
C10 C6 C3 120.0(7) . . ?
C6 C7 C8 120.8(8) . . ?
C6 C7 H7A 119.6 . . ?
C8 C7 H7A 119.6 . . ?
N2 C8 C7 119.0(8) . . ?
N2 C8 H8A 120.5 . . ?
C7 C8 H8A 120.5 . . ?
N2 C9 C10 121.3(8) . . ?
N2 C9 H9A 119.4 . . ?
C10 C9 H9A 119.4 . . ?
C9 C10 C6 119.5(8) . . ?
C9 C10 H10A 120.3 . . ?
C6 C10 H10A 120.3 . . ?
C16 C11 C12 119.0(6) . . ?
C16 C11 H11A 120.5 . . ?
C12 C11 H11A 120.5 . . ?
C13 C12 C11 120.3(6) . . ?
C13 C12 C17 118.9(6) . . ?
C11 C12 C17 120.6(6) . . ?
C12 C13 C14 120.1(6) . . ?
C12 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
C15 C14 C13 119.1(6) . . ?
C15 C14 C18 119.5(6) . . ?
C13 C14 C18 121.3(6) . . ?
C16 C15 C14 119.9(6) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C15 C16 C11 121.4(6) . . ?
C15 C16 S1 118.3(5) . . ?
C11 C16 S1 120.2(5) . . ?
O2 C17 O1 121.4(6) . . ?
O2 C17 C12 121.5(6) . . ?
O1 C17 C12 117.0(6) . . ?
O3 C18 O4 124.3(6) . . ?
O3 C18 C14 117.7(6) . . ?
O4 C18 C14 118.0(6) . . ?
C17 O1 Zn1 105.8(4) . . ?
C18 O3 Zn1 117.5(4) . 1_665 ?
C18 O4 Zn1 127.5(4) . 2_875 ?
S1 O13 O2W 124.4(4) . . ?
Zn1 O1W O13 127.1(2) . 1_455 ?
O13 O2W O3W 98.7(3) . . ?
O13 O2W O12 120.8(3) . 2_976 ?
O3W O2W O12 103.0(3) . 2_976 ?
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
Zn1 O3 1.986(4) 1_445 ?
Zn1 O1 2.000(5) . ?
Zn1 N1 2.051(6) . ?
Zn1 O1W 2.162(5) . ?
Zn1 O4 2.222(5) 2_875 ?
S1 O11 1.421(6) . ?
S1 O12 1.429(6) . ?
S1 O13 1.439(7) . ?
S1 C16 1.793(7) . ?
N1 C5 1.338(9) . ?
N1 C1 1.343(9) . ?
N2 C9 1.333(12) . ?
N2 C8 1.345(11) . ?
N2 O3W 2.644(9) 1_354 ?
N2 H0A 0.8600 . ?
C1 C2 1.377(10) . ?
C1 H1A 0.9300 . ?
C2 C3 1.389(10) . ?
C2 H2A 0.9300 . ?
C3 C4 1.392(10) . ?
C3 C6 1.483(10) . ?
C4 C5 1.357(10) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.377(11) . ?
C6 C10 1.395(11) . ?
C7 C8 1.381(12) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.358(11) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C16 1.384(10) . ?
C11 C12 1.390(10) . ?
C11 H11A 0.9300 . ?
C12 C13 1.378(9) . ?
C12 C17 1.501(9) . ?
C13 C14 1.404(9) . ?
C13 H13A 0.9300 . ?
C14 C15 1.391(10) . ?
C14 C18 1.502(9) . ?
C15 C16 1.369(10) . ?
C15 H15A 0.9300 . ?
C17 O2 1.246(8) . ?
C17 O1 1.278(8) . ?
C18 O3 1.261(8) . ?
C18 O4 1.264(8) . ?
O3 Zn1 1.986(4) 1_665 ?
O4 Zn1 2.222(5) 2_875 ?
O13 O2W 2.801(8) . ?
O1W O13 2.790(8) 1_455 ?
O2W O3W 2.806(10) . ?
O2W O12 2.898(9) 2_976 ?
