#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:19:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179407 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/04/4330414.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_4330414
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            'C28 H22 N4 Ni O6 S'
_chemical_formula_weight         601.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           22
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 2'
_symmetry_space_group_name_H-M   'F 2 2 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.252(4)
_cell_length_b                   22.160(9)
_cell_length_c                   23.571(9)
_cell_measurement_reflns_used    4150
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.52
_cell_volume                     6400(4)
_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 0.935
_diffrn_measured_fraction_theta_max 0.935
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8192
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.8883
_exptl_absorpt_correction_T_min  0.8251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            Aquamarine
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.139(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0517P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                3367
_reflns_number_total             3665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301636z_si_002_2.cif
_cod_data_source_block           kl107fComp1MNi
_cod_original_cell_volume        6399(4)
_cod_database_code               4330414
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -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
Ni1 Ni 0.7500 0.976311(13) 0.7500 0.03753(11) Uani 1 2 d S
O1 O 0.77045(13) 0.90930(7) 0.68844(7) 0.0507(4) Uani 1 1 d .
O2 O 0.61036(12) 0.94991(7) 0.70220(6) 0.0453(3) Uani 1 1 d .
O3 O 0.5910(2) 0.71038(8) 0.47670(8) 0.0879(8) Uani 1 1 d .
S1 S 0.5000 0.74296(4) 0.5000 0.0650(3) Uani 1 2 d S
N1 N 0.68966(15) 1.04031(8) 0.80234(7) 0.0436(4) Uani 1 1 d .
N2 N 0.58689(15) 1.11390(8) 0.83371(8) 0.0437(4) Uani 1 1 d .
C1 C 0.67124(18) 0.91253(9) 0.67756(9) 0.0425(5) Uani 1 1 d .
C2 C 0.62577(19) 0.87074(9) 0.63340(9) 0.0446(5) Uani 1 1 d .
C3 C 0.6946(2) 0.85063(11) 0.59083(10) 0.0584(6) Uani 1 1 d .
H3 H 0.7671 0.8630 0.5900 0.070 Uiso 1 1 calc R
C4 C 0.6550(2) 0.81202(12) 0.54956(11) 0.0605(7) Uani 1 1 d .
H4 H 0.6998 0.7995 0.5200 0.073 Uiso 1 1 calc R
C5 C 0.5484(2) 0.79239(10) 0.55282(10) 0.0501(6) Uani 1 1 d .
C6 C 0.4810(2) 0.81198(11) 0.59444(10) 0.0582(6) Uani 1 1 d .
H6 H 0.4092 0.7985 0.5959 0.070 Uiso 1 1 calc R
C7 C 0.5191(2) 0.85220(11) 0.63486(11) 0.0529(6) Uani 1 1 d .
H7 H 0.4725 0.8666 0.6629 0.063 Uiso 1 1 calc R
C8 C 0.59791(19) 1.06996(9) 0.79532(9) 0.0436(5) Uani 1 1 d .
H8 H 0.5470 1.0614 0.7672 0.052 Uiso 1 1 calc R
C9 C 0.7396(3) 1.06698(10) 0.84771(10) 0.0598(6) Uani 1 1 d .
H9 H 0.8065 1.0554 0.8628 0.072 Uiso 1 1 calc R
C10 C 0.6772(2) 1.11275(12) 0.86731(12) 0.0624(7) Uani 1 1 d .
H10 H 0.6928 1.1383 0.8976 0.075 Uiso 1 1 calc R
C11 C 0.49682(19) 1.15699(10) 0.83701(10) 0.0497(5) Uani 1 1 d .
H11A H 0.4985 1.1767 0.8738 0.060 Uiso 1 1 calc R
H11B H 0.4283 1.1352 0.8341 0.060 Uiso 1 1 calc R
C12 C 0.50086(19) 1.20422(9) 0.79147(10) 0.0440(5) Uani 1 1 d .
C13 C 0.5973(2) 1.22770(10) 0.77035(10) 0.0563(6) Uani 1 1 d .
H13 H 0.6635 1.2131 0.7839 0.068 Uiso 1 1 calc R
C14 C 0.4040(2) 1.22717(10) 0.77002(10) 0.0545(6) Uani 1 1 d .
H14 H 0.3379 1.2116 0.7828 0.065 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'
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 Ni1 N1 90.80(11) 11_656 .
N1 Ni1 O1 91.77(7) 11_656 .
N1 Ni1 O1 165.06(6) . .
N1 Ni1 O1 165.06(6) 11_656 11_656
N1 Ni1 O1 91.77(7) . 11_656
O1 Ni1 O1 89.52(10) . 11_656
N1 Ni1 O2 99.42(7) 11_656 .
N1 Ni1 O2 102.82(7) . .
O1 Ni1 O2 62.24(6) . .
O1 Ni1 O2 94.34(6) 11_656 .
N1 Ni1 O2 102.82(7) 11_656 11_656
N1 Ni1 O2 99.42(7) . 11_656
O1 Ni1 O2 94.34(6) . 11_656
O1 Ni1 O2 62.24(6) 11_656 11_656
O2 Ni1 O2 148.12(8) . 11_656
N1 Ni1 C1 134.09(8) 11_656 11_656
N1 Ni1 C1 97.19(8) . 11_656
O1 Ni1 C1 91.55(7) . 11_656
O1 Ni1 C1 30.97(7) 11_656 11_656
O2 Ni1 C1 122.24(7) . 11_656
O2 Ni1 C1 31.28(6) 11_656 11_656
C1 O1 Ni1 89.15(13) . .
C1 O2 Ni1 87.06(13) . .
O3 S1 O3 119.7(2) . 3_656
O3 S1 C5 107.66(12) . 3_656
O3 S1 C5 108.74(12) 3_656 3_656
O3 S1 C5 108.74(12) . .
O3 S1 C5 107.66(12) 3_656 .
C5 S1 C5 103.08(15) 3_656 .
C8 N1 C9 105.39(19) . .
C8 N1 Ni1 126.01(15) . .
C9 N1 Ni1 128.17(17) . .
C8 N2 C10 107.36(19) . .
C8 N2 C11 126.05(19) . .
C10 N2 C11 126.5(2) . .
O1 C1 O2 121.5(2) . .
O1 C1 C2 118.0(2) . .
O2 C1 C2 120.5(2) . .
C7 C2 C3 120.2(2) . .
C7 C2 C1 121.5(2) . .
C3 C2 C1 118.4(2) . .
C4 C3 C2 119.7(3) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C5 C4 C3 119.2(2) . .
C5 C4 H4 120.4 . .
C3 C4 H4 120.4 . .
C6 C5 C4 121.1(2) . .
C6 C5 S1 120.5(2) . .
C4 C5 S1 118.41(19) . .
C5 C6 C7 120.0(3) . .
C5 C6 H6 120.0 . .
C7 C6 H6 120.0 . .
C2 C7 C6 119.8(2) . .
C2 C7 H7 120.1 . .
C6 C7 H7 120.1 . .
N1 C8 N2 111.47(19) . .
N1 C8 H8 124.3 . .
N2 C8 H8 124.3 . .
C10 C9 N1 109.8(2) . .
C10 C9 H9 125.1 . .
N1 C9 H9 125.1 . .
C9 C10 N2 106.0(2) . .
C9 C10 H10 127.0 . .
N2 C10 H10 127.0 . .
N2 C11 C12 113.13(19) . .
N2 C11 H11A 109.0 . .
C12 C11 H11A 109.0 . .
N2 C11 H11B 109.0 . .
C12 C11 H11B 109.0 . .
H11A C11 H11B 107.8 . .
C13 C12 C14 117.5(2) . .
C13 C12 C11 123.2(2) . .
C14 C12 C11 119.3(2) . .
C13 C13 C12 121.36(14) 8_576 .
C13 C13 H13 119.3 8_576 .
C12 C13 H13 119.3 . .
C14 C14 C12 121.13(14) 8_576 .
C14 C14 H14 119.4 8_576 .
C12 C14 H14 119.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.0196(18) 11_656
Ni1 N1 2.0198(18) .
Ni1 O1 2.0913(15) .
Ni1 O1 2.0914(15) 11_656
Ni1 O2 2.1304(15) .
Ni1 O2 2.1305(15) 11_656
Ni1 C1 2.418(2) 11_656
O1 C1 1.244(3) .
O2 C1 1.257(3) .
O3 S1 1.438(2) .
S1 O3 1.438(2) 3_656
S1 C5 1.761(2) 3_656
S1 C5 1.761(2) .
N1 C8 1.313(3) .
N1 C9 1.366(3) .
N2 C8 1.336(3) .
N2 C10 1.361(3) .
N2 C11 1.461(3) .
C1 C2 1.500(3) .
C2 C7 1.370(4) .
C2 C3 1.385(3) .
C3 C4 1.383(3) .
C3 H3 0.9300 .
C4 C5 1.379(4) .
C4 H4 0.9300 .
C5 C6 1.353(4) .
C6 C7 1.386(3) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 C10 1.351(4) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.500(3) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.384(3) .
C12 C14 1.386(4) .
C13 C13 1.377(5) 8_576
C13 H13 0.9300 .
C14 C14 1.384(5) 8_576
C14 H14 0.9300 .
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 -0.014 0.000 0.000 360.9 71.8
2 -0.022 0.000 0.500 360.9 71.8
3 -0.026 0.500 0.000 360.9 71.8
4 -0.025 0.500 0.500 360.9 71.8
