#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:26:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179631 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/95/4509579.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_4509579
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           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                101.3480(10)
_cell_angle_beta                 90.2660(10)
_cell_angle_gamma                117.0750(10)
_cell_formula_units_Z            1
_cell_length_a                   8.4893(2)
_cell_length_b                   8.6526(2)
_cell_length_c                   9.1010(2)
_cell_measurement_temperature    293(2)
_cell_volume                     580.20(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4853
_diffrn_reflns_theta_full        23.92
_diffrn_reflns_theta_max         23.92
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_correction_T_min  0.8174
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0272
_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)+(0.0350P)²+0.3649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                1612
_reflns_number_total             1794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900386qsup1.cif
_cod_data_source_block           complex3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4509579
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
C1 C -0.0500(3) 0.3062(3) 1.1693(3) 0.0264(6) Uani 1 1 d .
C2 C -0.0487(3) 0.4326(3) 1.2881(3) 0.0268(6) Uani 1 1 d .
C3 C -0.0037(3) 0.4314(3) 1.4344(3) 0.0223(5) Uani 1 1 d .
C4 C 0.0350(4) 0.2956(3) 1.4508(3) 0.0307(6) Uani 1 1 d .
C5 C 0.0323(4) 0.1757(3) 1.3265(3) 0.0297(6) Uani 1 1 d .
C6 C 0.4275(3) 0.6437(3) 1.3149(3) 0.0253(6) Uani 1 1 d .
C7 C 0.4319(3) 0.7437(3) 1.4591(3) 0.0305(6) Uani 1 1 d .
C8 C 0.4693(4) 0.6977(3) 1.5847(3) 0.0302(6) Uani 1 1 d .
C9 C 0.5022(3) 0.5506(3) 1.5722(3) 0.0248(5) Uani 1 1 d .
C10 C 0.4597(3) 0.5012(3) 1.2980(3) 0.0282(6) Uani 1 1 d .
N1 N -0.0092(3) 0.1784(2) 1.1853(2) 0.0229(5) Uani 1 1 d .
O1 O -0.2413(2) -0.0433(2) 0.9032(2) 0.0273(4) Uani 1 1 d .
O2 O 0.1418(3) 0.2046(2) 0.8866(2) 0.0301(4) Uani 1 1 d .
O3 O 0.2582(3) 0.7784(3) 1.1952(2) 0.0412(5) Uani 1 1 d .
O4 O 0.3210(3) 0.5638(2) 1.0281(2) 0.0464(5) Uani 1 1 d .
O5 O 0.5573(2) 0.8571(2) 1.1367(2) 0.0409(5) Uani 1 1 d .
S1 S 0.38579(8) 0.71369(8) 1.15512(7) 0.02620(18) Uani 1 1 d .
Ni1 Ni 0.0000 0.0000 1.0000 0.01933(15) Uani 1 2 d S
H1 H -0.310(4) -0.069(3) 0.958(3) 0.023 Uiso 1 1 d .
H2 H -0.243(4) 0.028(4) 0.871(3) 0.023 Uiso 1 1 d .
H3 H 0.176(4) 0.296(4) 0.932(3) 0.023 Uiso 1 1 d .
H4 H 0.231(4) 0.194(3) 0.863(3) 0.023 Uiso 1 1 d .
H5 H -0.081(3) 0.309(3) 1.070(3) 0.024(6) Uiso 1 1 d .
H6 H -0.077(4) 0.513(4) 1.270(3) 0.035(8) Uiso 1 1 d .
H7 H 0.065(4) 0.284(3) 1.546(3) 0.037(7) Uiso 1 1 d .
H8 H 0.060(3) 0.089(3) 1.337(3) 0.024(7) Uiso 1 1 d .
H9 H 0.405(4) 0.840(4) 1.465(3) 0.036(7) Uiso 1 1 d .
H10 H 0.468(3) 0.758(3) 1.682(3) 0.032(7) Uiso 1 1 d .
H11 H 0.463(4) 0.440(4) 1.201(3) 0.039 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
N1 C1 C2 123.6(2) . .
C1 C2 C3 120.1(2) . .
C2 C3 C4 116.1(2) . .
C2 C3 C3 121.8(3) . 2_568
C4 C3 C3 122.1(3) . 2_568
C5 C4 C3 120.2(2) . .
N1 C5 C4 123.5(2) . .
C10 C6 C7 121.4(2) . .
C10 C6 S1 120.6(2) . .
C7 C6 S1 117.98(19) . .
C8 C7 C6 119.8(2) . .
C7 C8 C9 120.6(2) . .
C8 C9 C9 120.0(3) . 2_668
C8 C9 C10 121.7(2) . 2_668
C9 C9 C10 118.3(3) 2_668 2_668
C6 C10 C9 119.9(2) . 2_668
C1 N1 C5 116.4(2) . .
C1 N1 Ni1 121.63(16) . .
C5 N1 Ni1 121.89(16) . .
O4 S1 O3 113.61(13) . .
O4 S1 O5 112.37(13) . .
O3 S1 O5 111.59(12) . .
O4 S1 C6 108.10(11) . .
O3 S1 C6 105.65(11) . .
O5 S1 C6 104.83(11) . .
O1 Ni1 O1 180.0 . 2_557
O1 Ni1 N1 90.94(7) . .
O1 Ni1 N1 89.06(7) 2_557 .
O1 Ni1 N1 89.06(7) . 2_557
O1 Ni1 N1 90.94(7) 2_557 2_557
N1 Ni1 N1 180.000(1) . 2_557
O1 Ni1 O2 88.19(8) . 2_557
O1 Ni1 O2 91.81(8) 2_557 2_557
N1 Ni1 O2 87.80(7) . 2_557
N1 Ni1 O2 92.20(8) 2_557 2_557
O1 Ni1 O2 91.81(8) . .
O1 Ni1 O2 88.19(8) 2_557 .
N1 Ni1 O2 92.20(8) . .
N1 Ni1 O2 87.80(7) 2_557 .
O2 Ni1 O2 180.000(1) 2_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.332(3) .
C1 C2 1.375(3) .
C2 C3 1.386(3) .
C3 C4 1.391(4) .
C3 C3 1.487(4) 2_568
C4 C5 1.369(3) .
C5 N1 1.339(3) .
C6 C10 1.360(4) .
C6 C7 1.413(4) .
C6 S1 1.773(2) .
C7 C8 1.363(4) .
C8 C9 1.406(4) .
C9 C9 1.418(5) 2_668
C9 C10 1.428(3) 2_668
C10 C9 1.428(3) 2_668
N1 Ni1 2.0781(18) .
O1 Ni1 2.0659(18) .
O2 Ni1 2.1073(18) .
O3 S1 1.4477(19) .
O4 S1 1.4411(19) .
O5 S1 1.4582(19) .
Ni1 O1 2.0659(18) 2_557
Ni1 N1 2.0781(18) 2_557
Ni1 O2 2.1073(18) 2_557
