#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:19:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179407 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/04/4330416.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_4330416
loop_
_publ_author_name
'Kamal Kumar Bisht'
'Eringathodi Suresh'
_publ_section_title
;
 Spontaneous Resolution of a Mixed-Ligand Nickel(II) Coordination Polymer
 with Achiral Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9577
_journal_page_last               9579
_journal_paper_doi               10.1021/ic301636z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C21 H15 N2 O6 S Zn'
_chemical_formula_weight         488.78
_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                110.01(2)
_cell_angle_beta                 101.593(19)
_cell_angle_gamma                92.468(19)
_cell_formula_units_Z            2
_cell_length_a                   7.220(7)
_cell_length_b                   12.829(12)
_cell_length_c                   13.163(13)
_cell_measurement_reflns_used    886
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.84
_cell_volume                     1113.9(19)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4223
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  0.9639
_exptl_absorpt_correction_T_min  0.8269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plates
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0731
_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)+(0.1008P)²+0.1821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1790
_reflns_number_gt                2784
_reflns_number_total             3518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301636z_si_002_4.cif
_cod_data_source_block           kl112mComp3Zn
_cod_database_code               4330416
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
Zn1 Zn 0.69394(9) 0.03332(5) 0.58147(6) 0.0217(3) Uani 1 1 d .
S3 S 0.8512(3) 0.38480(13) 0.13092(15) 0.0349(5) Uani 1 1 d .
O1 O 0.7359(6) 0.1091(4) 0.4710(4) 0.0342(11) Uani 1 1 d .
O2 O 0.4459(6) 0.0698(4) 0.3590(4) 0.0387(12) Uani 1 1 d .
O5 O 0.7758(6) 0.8889(3) 0.4838(4) 0.0343(11) Uani 1 1 d .
O6 O 0.4864(6) 0.8496(4) 0.3679(4) 0.0370(12) Uani 1 1 d .
O4 O 1.0532(7) 0.3874(4) 0.1420(5) 0.0455(13) Uani 1 1 d .
O3 O 0.7251(8) 0.3457(4) 0.0216(4) 0.0467(14) Uani 1 1 d .
N1 N 0.9114(7) 0.1012(4) 0.7147(4) 0.0243(12) Uani 1 1 d .
N2 N 1.1973(7) 0.1380(4) 0.8242(4) 0.0252(12) Uani 1 1 d .
C15 C 1.0862(8) 0.0733(5) 0.7237(5) 0.0245(14) Uani 1 1 d .
H15 H 1.1272 0.0176 0.6692 0.029 Uiso 1 1 calc R
C16 C 0.9134(9) 0.1855(5) 0.8132(6) 0.0304(16) Uani 1 1 d .
H16 H 0.8088 0.2216 0.8308 0.037 Uiso 1 1 calc R
C17 C 1.0888(9) 0.2087(5) 0.8807(6) 0.0328(16) Uani 1 1 d .
H17 H 1.1273 0.2625 0.9517 0.039 Uiso 1 1 calc R
C18 C 1.4023(8) 0.1337(6) 0.8616(6) 0.0325(16) Uani 1 1 d .
H18A H 1.4642 0.2092 0.9033 0.039 Uiso 1 1 calc R
H18B H 1.4553 0.1041 0.7967 0.039 Uiso 1 1 calc R
C5 C 0.7824(10) 0.3056(5) 0.2054(6) 0.0321(16) Uani 1 1 d .
C4 C 0.9196(9) 0.2769(5) 0.2788(6) 0.0343(17) Uani 1 1 d .
H4 H 1.0479 0.2989 0.2873 0.041 Uiso 1 1 calc R
C1 C 0.6136(8) 0.1151(5) 0.3912(6) 0.0261(15) Uani 1 1 d .
C7 C 0.5381(9) 0.2115(6) 0.2527(6) 0.0342(16) Uani 1 1 d .
H7 H 0.4096 0.1895 0.2438 0.041 Uiso 1 1 calc R
C3 C 0.8664(9) 0.2160(5) 0.3393(6) 0.0348(17) Uani 1 1 d .
H3 H 0.9586 0.1976 0.3886 0.042 Uiso 1 1 calc R
C2 C 0.6737(9) 0.1821(5) 0.3262(5) 0.0268(15) Uani 1 1 d .
C6 C 0.5906(10) 0.2720(6) 0.1935(6) 0.0364(17) Uani 1 1 d .
H6 H 0.4978 0.2910 0.1450 0.044 Uiso 1 1 calc R
C12 C 0.5717(9) 0.6472(5) 0.2398(6) 0.0365(17) Uani 1 1 d .
H12 H 0.4497 0.6663 0.2225 0.044 Uiso 1 1 calc R
C11 C 0.7069(9) 0.7204(5) 0.3284(5) 0.0264(14) Uani 1 1 d .
C19 C 1.4482(8) 0.0635(5) 0.9329(5) 0.0267(15) Uani 1 1 d .
C14 C 0.6511(10) 0.8295(5) 0.3987(6) 0.0278(15) Uani 1 1 d .
C20 C 1.3130(9) 0.0119(6) 0.9671(6) 0.0326(16) Uani 1 1 d .
H20 H 1.1851 0.0192 0.9448 0.039 Uiso 1 1 calc R
C10 C 0.8912(8) 0.6940(5) 0.3525(5) 0.0257(14) Uani 1 1 d .
H10 H 0.9830 0.7452 0.4101 0.031 Uiso 1 1 calc R
C21 C 1.6351(9) 0.0504(6) 0.9661(6) 0.0339(16) Uani 1 1 d .
H21 H 1.7284 0.0836 0.9436 0.041 Uiso 1 1 calc R
C8 C 0.7993(9) 0.5198(5) 0.2039(5) 0.0259(14) Uani 1 1 d .
C13 C 0.6178(10) 0.5459(5) 0.1770(6) 0.0374(18) Uani 1 1 d .
H13 H 0.5276 0.4960 0.1173 0.045 Uiso 1 1 calc R
C9 C 0.9384(9) 0.5923(5) 0.2912(6) 0.0338(16) Uani 1 1 d .
H9 H 1.0603 0.5728 0.3080 0.041 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'
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'
H H 0.0000 0.0000 '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
N1 Zn1 O5 106.1(2) . 1_545
N1 Zn1 O6 96.5(2) . 2_666
O5 Zn1 O6 157.11(18) 1_545 2_666
N1 Zn1 O1 105.4(2) . .
O5 Zn1 O1 90.0(2) 1_545 .
O6 Zn1 O1 86.8(2) 2_666 .
N1 Zn1 O2 97.8(2) . 2_656
O5 Zn1 O2 85.1(2) 1_545 2_656
O6 Zn1 O2 88.9(2) 2_666 2_656
O1 Zn1 O2 156.68(19) . 2_656
N1 Zn1 Zn1 165.42(15) . 2_656
O5 Zn1 Zn1 87.44(14) 1_545 2_656
O6 Zn1 Zn1 69.69(15) 2_666 2_656
O1 Zn1 Zn1 79.31(14) . 2_656
O2 Zn1 Zn1 77.71(15) 2_656 2_656
O4 S3 O3 119.8(3) . .
O4 S3 C5 108.2(3) . .
O3 S3 C5 108.3(3) . .
O4 S3 C8 109.0(3) . .
O3 S3 C8 107.4(3) . .
C5 S3 C8 102.8(3) . .
C1 O1 Zn1 127.1(4) . .
C1 O2 Zn1 129.4(5) . 2_656
C14 O5 Zn1 115.6(4) . 1_565
C14 O6 Zn1 139.9(4) . 2_666
C15 N1 C16 105.6(5) . .
C15 N1 Zn1 125.8(4) . .
C16 N1 Zn1 128.5(4) . .
C17 N2 C15 108.1(5) . .
C17 N2 C18 126.6(5) . .
C15 N2 C18 125.2(5) . .
N1 C15 N2 110.0(5) . .
C17 C16 N1 110.2(6) . .
C16 C17 N2 106.0(6) . .
N2 C18 C19 114.4(5) . .
C4 C5 C6 119.1(7) . .
C4 C5 S3 120.1(5) . .
C6 C5 S3 120.8(6) . .
C3 C4 C5 120.5(6) . .
O2 C1 O1 126.2(7) . .
O2 C1 C2 116.0(6) . .
O1 C1 C2 117.8(5) . .
C6 C7 C2 121.1(6) . .
C4 C3 C2 119.9(7) . .
C7 C2 C3 119.0(7) . .
C7 C2 C1 120.5(6) . .
C3 C2 C1 120.5(6) . .
C7 C6 C5 120.4(7) . .
C13 C12 C11 120.0(6) . .
C12 C11 C10 120.4(6) . .
C12 C11 C14 119.0(6) . .
C10 C11 C14 120.6(6) . .
C21 C19 C20 117.9(6) . .
C21 C19 C18 118.0(6) . .
C20 C19 C18 124.1(6) . .
O6 C14 O5 127.3(6) . .
O6 C14 C11 116.5(6) . .
O5 C14 C11 116.2(6) . .
C19 C20 C21 121.2(6) . 2_857
C9 C10 C11 120.2(6) . .
C19 C21 C20 120.8(6) . 2_857
C13 C8 C9 122.4(6) . .
C13 C8 S3 118.5(5) . .
C9 C8 S3 118.9(5) . .
C8 C13 C12 118.9(6) . .
C10 C9 C8 118.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.007(5) .
Zn1 O5 2.050(4) 1_545
Zn1 O6 2.056(4) 2_666
Zn1 O1 2.067(5) .
Zn1 O2 2.072(5) 2_656
Zn1 Zn1 3.049(3) 2_656
S3 O4 1.434(5) .
S3 O3 1.446(5) .
S3 C5 1.753(7) .
S3 C8 1.768(6) .
O1 C1 1.256(8) .
O2 C1 1.245(7) .
O2 Zn1 2.072(5) 2_656
O5 C14 1.264(8) .
O5 Zn1 2.050(4) 1_565
O6 C14 1.244(8) .
O6 Zn1 2.056(4) 2_666
N1 C15 1.320(7) .
N1 C16 1.372(8) .
N2 C17 1.350(8) .
N2 C15 1.360(8) .
N2 C18 1.472(7) .
C16 C17 1.348(9) .
C18 C19 1.510(9) .
C5 C4 1.394(10) .
C5 C6 1.395(9) .
C4 C3 1.384(10) .
C1 C2 1.509(9) .
C7 C6 1.364(10) .
C7 C2 1.392(9) .
C3 C2 1.397(9) .
C12 C13 1.376(9) .
C12 C11 1.382(9) .
C11 C10 1.388(8) .
C11 C14 1.514(8) .
C19 C21 1.369(9) .
C19 C20 1.385(9) .
C20 C21 1.389(9) 2_857
C10 C9 1.378(8) .
C21 C20 1.389(9) 2_857
C8 C13 1.373(9) .
C8 C9 1.385(9) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.048 0.500 0.500 150.0 13.2
2 0.111 0.067 0.183 7.3 -0.1
3 0.889 0.933 0.817 7.3 -0.1
