#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:26:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179631 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/95/4509580.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4509580
loop_
_publ_author_name
'Kanoo, Prakash'
'K. L., Gurunatha'
'Maji, Tapas Kumar'
_publ_section_title
;
 Temperature-Controlled Synthesis of Metal-Organic Coordination Polymers:
 Crystal Structure, Supramolecular Isomerism, and Porous Property
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4147
_journal_paper_doi               10.1021/cg900386q
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C20 H22 N2 Ni O10 S2'
_chemical_formula_weight         573.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.613(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6515(3)
_cell_length_b                   11.2360(3)
_cell_length_c                   15.9913(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2324.58(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker,2000)'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_molecular_graphics    'Mercury 1.4.1'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14104
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    1.074
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.7525
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0397
_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)+(0.0347P)²+1.6881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                1982
_reflns_number_total             2682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900386qsup1.cif
_cod_data_source_block           complex4
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4509580
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
C1 C 0.9320(2) -0.1137(2) 0.77697(18) 0.0260(6) Uani 1 1 d .
C2 C 0.9289(2) 0.0086(2) 0.77716(17) 0.0253(6) Uani 1 1 d .
C3 C 1.0000 0.0731(3) 0.7500 0.0232(8) Uani 1 2 d S
C4 C 0.9189(2) -0.6076(2) 0.7549(2) 0.0333(7) Uani 1 1 d .
C5 C 0.9150(2) -0.7298(2) 0.7534(2) 0.0351(7) Uani 1 1 d .
C6 C 1.0000 -0.7950(3) 0.7500 0.0260(8) Uani 1 2 d S
C7 C 1.1046(2) -0.0913(2) 0.97916(17) 0.0291(6) Uani 1 1 d .
C8 C 1.1646(2) -0.0040(2) 0.96189(17) 0.0272(6) Uani 1 1 d .
C9 C 1.1383(2) 0.1178(2) 0.96445(19) 0.0321(7) Uani 1 1 d .
C10 C 1.0515(2) 0.1493(2) 0.98299(18) 0.0321(6) Uani 1 1 d .
C11 C 0.9866(2) 0.0605(2) 1.00060(17) 0.0259(6) Uani 1 1 d .
N1 N 1.0000 -0.5450(2) 0.7500 0.0268(7) Uani 1 2 d S
N2 N 1.0000 -0.1761(2) 0.7500 0.0243(7) Uani 1 2 d S
O1 O 1.15849(16) -0.3612(2) 0.82473(14) 0.0316(5) Uani 1 1 d .
O2 O 0.96642(18) -0.35882(16) 0.86717(13) 0.0277(4) Uani 1 1 d .
O3 O 1.26895(17) -0.16037(17) 0.90487(16) 0.0485(6) Uani 1 1 d .
O4 O 1.36127(16) -0.02857(19) 1.02287(13) 0.0459(5) Uani 1 1 d .
O5 O 1.28854(15) 0.04825(17) 0.87541(13) 0.0410(5) Uani 1 1 d .
S1 S 1.27924(5) -0.04021(6) 0.93848(4) 0.02853(18) Uani 1 1 d .
Ni1 Ni 1.0000 -0.35982(3) 0.7500 0.02104(14) Uani 1 2 d S
H1 H 0.883(2) -0.156(2) 0.7973(16) 0.022(7) Uiso 1 1 d .
H1A H 1.171(3) -0.398(3) 0.868(2) 0.065(13) Uiso 1 1 d .
H1B H 1.189(3) -0.293(3) 0.840(2) 0.063(11) Uiso 1 1 d .
H2 H 0.880(2) 0.045(2) 0.7976(17) 0.032(8) Uiso 1 1 d .
H2A H 1.012(3) -0.394(3) 0.905(2) 0.055(11) Uiso 1 1 d .
H2B H 0.913(2) -0.385(2) 0.8672(18) 0.024(8) Uiso 1 1 d .
H4 H 0.858(2) -0.565(2) 0.7546(18) 0.035(8) Uiso 1 1 d .
H5 H 0.851(2) -0.768(2) 0.7525(17) 0.037(8) Uiso 1 1 d .
H7 H 1.1251(18) -0.1687(19) 0.9817(14) 0.010(6) Uiso 1 1 d .
H9 H 1.183(2) 0.175(2) 0.9512(17) 0.030(7) Uiso 1 1 d .
H10 H 1.030(2) 0.230(3) 0.9815(17) 0.040(8) Uiso 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'
Ni Ni 0.3393 1.1124 '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
N2 C1 C2 123.3(3) . .
C1 C2 C3 119.8(3) . .
C2 C3 C2 117.0(3) . 2_756
C2 C3 C6 121.50(15) . 1_565
C2 C3 C6 121.50(15) 2_756 1_565
N1 C4 C5 123.6(3) . .
C4 C5 C6 120.0(3) . .
C5 C6 C5 116.4(3) 2_756 .
C5 C6 C3 121.82(16) 2_756 1_545
C5 C6 C3 121.82(16) . 1_545
C8 C7 C11 119.8(2) . 5_757
C7 C8 C9 121.0(3) . .
C7 C8 S1 120.5(2) . .
C9 C8 S1 118.5(2) . .
C10 C9 C8 120.3(3) . .
C9 C10 C11 120.2(3) . .
C11 C11 C10 119.6(3) 5_757 .
C11 C11 C7 119.0(3) 5_757 5_757
C10 C11 C7 121.3(2) . 5_757
C4 N1 C4 116.4(3) . 2_756
C4 N1 Ni1 121.78(15) . .
C4 N1 Ni1 121.78(15) 2_756 .
C1 N2 C1 116.8(3) 2_756 .
C1 N2 Ni1 121.58(15) 2_756 .
C1 N2 Ni1 121.58(15) . .
O3 S1 O5 113.70(13) . .
O3 S1 O4 112.53(13) . .
O5 S1 O4 111.73(12) . .
O3 S1 C8 107.85(12) . .
O5 S1 C8 105.62(12) . .
O4 S1 C8 104.68(12) . .
N2 Ni1 O2 89.69(5) . .
N2 Ni1 O2 89.69(5) . 2_756
O2 Ni1 O2 179.37(10) . 2_756
N2 Ni1 N1 180.000(1) . .
O2 Ni1 N1 90.31(5) . .
O2 Ni1 N1 90.31(5) 2_756 .
N2 Ni1 O1 90.41(6) . 2_756
O2 Ni1 O1 91.69(9) . 2_756
O2 Ni1 O1 88.32(9) 2_756 2_756
N1 Ni1 O1 89.59(6) . 2_756
N2 Ni1 O1 90.41(6) . .
O2 Ni1 O1 88.32(9) . .
O2 Ni1 O1 91.69(9) 2_756 .
N1 Ni1 O1 89.59(6) . .
O1 Ni1 O1 179.19(12) 2_756 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.340(3) .
C1 C2 1.375(3) .
C2 C3 1.387(3) .
C3 C2 1.387(3) 2_756
C3 C6 1.482(4) 1_565
C4 N1 1.335(3) .
C4 C5 1.375(4) .
C5 C6 1.388(3) .
C6 C5 1.388(3) 2_756
C6 C3 1.482(4) 1_545
C7 C8 1.362(4) .
C7 C11 1.426(4) 5_757
C8 C9 1.419(4) .
C8 S1 1.768(3) .
C9 C10 1.358(4) .
C10 C11 1.420(4) .
C11 C11 1.410(5) 5_757
C11 C7 1.426(4) 5_757
N1 C4 1.335(3) 2_756
N1 Ni1 2.081(3) .
N2 C1 1.340(3) 2_756
N2 Ni1 2.064(3) .
O1 Ni1 2.112(2) .
O2 Ni1 2.0663(19) .
O3 S1 1.4433(19) .
O4 S1 1.459(2) .
O5 S1 1.4501(19) .
Ni1 O2 2.0663(19) 2_756
Ni1 O1 2.112(2) 2_756
