#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/17/4321781.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_4321781
loop_
_publ_author_name
'Sudeep Bhattacharyya'
'Timothy J. R. Weakley'
'Muktimoy Chaudhury'
_publ_section_title
;
 Nickel(II) in an N4S Donor Environment: An Unprecedented Alcoholysis
 Reaction through the Activation of a Carbon-Nitrogen Single Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              633
_journal_page_last               638
_journal_paper_doi               10.1021/ic9703888
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C17 H27 Cl N4 Ni O5 S2'
_chemical_formula_weight         525.70
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue May  7 13:23:45 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                108.784(8)
_cell_angle_beta                 108.887(6)
_cell_angle_gamma                95.139(6)
_cell_formula_units_Z            2
_cell_length_a                   10.4886(5)
_cell_length_b                   10.706(1)
_cell_length_c                   11.487(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      30.0
_cell_volume                     1128.07(18)
_computing_cell_refinement       'Enraf-Nonius CAD-4 software v.5 '
_computing_data_collection       'Enraf-Nonius CAD-4 software v.5 '
_computing_data_reduction        'MSC TEXSAN v.5.0 (1989) '
_computing_publication_material  'MSC TEXSAN v.5.0 (1989) '
_computing_structure_refinement  'MSC TEXSAN v.5.0 (1989) '
_computing_structure_solution    'MSC TEXSAN v.5.0 (1989) '
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.08250
_diffrn_orient_matrix_UB_12      -0.01035
_diffrn_orient_matrix_UB_13      0.06746
_diffrn_orient_matrix_UB_21      0.06007
_diffrn_orient_matrix_UB_22      0.02692
_diffrn_orient_matrix_UB_23      -0.04384
_diffrn_orient_matrix_UB_31      0.01543
_diffrn_orient_matrix_UB_32      0.09685
_diffrn_orient_matrix_UB_33      0.05793
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.91
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4206
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        1.63
_diffrn_standards_interval_count 60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  1.210
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Walker&Stuart_DIFABS
_exptl_crystal_colour            yellow-gretablet
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       tablet
_exptl_crystal_F_000             548.00
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.120
_refine_diff_density_max         -0.50
_refine_diff_density_min         0.69
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.688
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3225
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0418
_refine_ls_shift/esd_max         0.0747
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0541
_reflns_number_observed          3225
_reflns_number_total             4206
_reflns_observed_criterion       3.00
_cod_data_source_file            ic9703888_1.cif
_cod_data_source_block           C17H27ClN4NiO5S2
_cod_original_cell_volume        1128.0(4)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C17 H27 Cl N4 O5 Ni S2 '
_cod_database_code               4321781
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Ni() 0.53053(5) 0.65696(5) 0.23997(5) 0.0364(1) Uij ? ?
Cl() 0.9158(1) 0.2386(2) 0.2585(1) 0.0749(4) Uij ? ?
S(1) 0.3739(1) 0.76527(10) 0.1920(1) 0.0482(3) Uij ? ?
S(2) 0.3152(2) 1.0406(1) 0.2663(1) 0.0716(4) Uij ? ?
O(1) 0.6492(4) 0.5975(3) 0.4670(3) 0.076(1) Uij ? ?
O(2) 0.7747(5) 0.1851(5) 0.2187(6) 0.137(2) Uij ? ?
O(3) 0.9232(8) 0.3114(9) 0.1835(7) 0.224(4) Uij ? ?
O(4) 0.9607(5) 0.3290(6) 0.3913(5) 0.148(2) Uij ? ?
O(5) 0.9868(9) 0.1492(8) 0.2570(9) 0.273(5) Uij ? ?
N(1) 0.6780(3) 0.8050(3) 0.3344(3) 0.0431(9) Uij ? ?
N(2) 0.6666(3) 0.5422(3) 0.2619(3) 0.0411(9) Uij ? ?
N(3) 0.4674(3) 0.3835(3) 0.1088(3) 0.0457(9) Uij ? ?
N(4) 0.4011(3) 0.4866(3) 0.1432(3) 0.0433(9) Uij ? ?
C(1) 0.4343(5) 0.9359(4) 0.2809(4) 0.050(1) Uij ? ?
C(2) 0.5659(5) 0.9979(4) 0.3630(4) 0.047(1) Uij ? ?
C(3) 0.6150(6) 1.1493(4) 0.4377(5) 0.068(2) Uij ? ?
C(4) 0.7642(6) 1.1687(5) 0.5277(5) 0.075(2) Uij ? ?
C(5) 0.8110(5) 1.0391(4) 0.4728(5) 0.063(1) Uij ? ?
C(6) 0.6800(4) 0.9343(4) 0.3844(4) 0.046(1) Uij ? ?
C(7) 0.8128(4) 0.7655(4) 0.3682(5) 0.059(1) Uij ? ?
C(8) 0.7959(4) 0.6255(4) 0.2749(5) 0.056(1) Uij ? ?
C(9) 0.6134(4) 0.4211(4) 0.1386(4) 0.048(1) Uij ? ?
C(10) 0.4275(6) 0.1331(4) 0.0078(5) 0.073(2) Uij ? ?
C(11) 0.3809(5) 0.2619(4) 0.0527(4) 0.054(1) Uij ? ?
C(12) 0.2552(5) 0.2867(4) 0.0503(5) 0.060(1) Uij ? ?
C(13) 0.2694(4) 0.4256(4) 0.1068(4) 0.052(1) Uij ? ?
C(14) 0.1600(5) 0.4991(5) 0.1283(6) 0.075(2) Uij ? ?
C(15) 0.1576(6) 0.9336(7) 0.1431(6) 0.102(2) Uij ? ?
C(16) 0.6828(5) 0.5009(5) 0.3773(4) 0.064(1) Uij ? ?
C(17) 0.6820(7) 0.5789(6) 0.5886(5) 0.090(2) Uij ? ?
H(1) 0.6099 1.1945 0.3780 0.0821 Uij ? ?
H(2) 0.5612 1.1825 0.4886 0.0821 Uij ? ?
H(3) 0.8202 1.2432 0.5273 0.0902 Uij ? ?
H(4) 0.7701 1.1841 0.6157 0.0902 Uij ? ?
H(5) 0.8652 1.0506 0.4233 0.0757 Uij ? ?
H(6) 0.8631 1.0136 0.5427 0.0757 Uij ? ?
H(7) 0.8787 0.8259 0.3603 0.0702 Uij ? ?
H(8) 0.8434 0.7683 0.4566 0.0702 Uij ? ?
H(9) 0.8726 0.5891 0.3088 0.0672 Uij ? ?
H(10) 0.7894 0.6266 0.1908 0.0672 Uij ? ?
H(11) 0.6285 0.4413 0.0687 0.0578 Uij ? ?
H(12) 0.6574 0.3501 0.1513 0.0578 Uij ? ?
H(13) 0.3511 0.0588 -0.0293 0.0874 Uij ? ?
H(14) 0.4648 0.1334 -0.0573 0.0874 Uij ? ?
H(15) 0.4961 0.1251 0.0813 0.0874 Uij ? ?
H(16) 0.1722 0.2205 0.0159 0.0721 Uij ? ?
H(17) 0.1848 0.5479 0.2204 0.0905 Uij ? ?
H(18) 0.1504 0.5601 0.0831 0.0905 Uij ? ?
H(19) 0.0749 0.4360 0.0949 0.0905 Uij ? ?
H(20) 0.0889 0.9854 0.1303 0.1230 Uij ? ?
H(21) 0.1705 0.8932 0.0622 0.1230 Uij ? ?
H(22) 0.1290 0.8651 0.1708 0.1230 Uij ? ?
H(23) 0.7755 0.4945 0.4165 0.0767 Uij ? ?
H(24) 0.6229 0.4159 0.3490 0.0767 Uij ? ?
H(25) 0.6310 0.4938 0.5744 0.1078 Uij ? ?
H(26) 0.7780 0.5816 0.6245 0.1078 Uij ? ?
H(27) 0.6591 0.6488 0.6488 0.1078 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 34 0.002 0.002 'International Tables'
H 0 54 0.000 0.000 'International Tables'
Cl 0 2 0.132 0.159 'International Tables'
N 0 8 0.004 0.003 'International Tables'
Ni 0 2 0.285 1.113 'International Tables'
O 0 10 0.008 0.006 'International Tables'
S 0 4 0.110 0.124 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 NI N1 97.3(1) ? ? ? yes
S1 NI N2 173.13(10) ? ? ? yes
S1 NI N4 91.99(10) ? ? ? yes
N1 NI N2 87.3(1) ? ? ? yes
N1 NI N4 170.5(1) ? ? ? yes
N2 NI N4 83.3(1) ? ? ? yes
O2 CL O3 105.5(4) ? ? ? yes
O2 CL O4 106.8(4) ? ? ? yes
O2 CL O5 112.4(5) ? ? ? yes
O3 CL O4 107.9(5) ? ? ? yes
O3 CL O5 116.9(6) ? ? ? yes
O4 CL O5 106.8(5) ? ? ? yes
NI S1 C1 111.1(2) ? ? ? yes
C1 S2 C15 105.7(2) ? ? ? yes
C16 O1 C17 111.9(4) ? ? ? yes
NI N1 C6 130.5(3) ? ? ? yes
NI N1 C7 112.6(2) ? ? ? yes
C6 N1 C7 116.6(3) ? ? ? yes
NI N2 C8 104.1(2) ? ? ? yes
NI N2 C9 105.7(2) ? ? ? yes
NI N2 C16 112.5(2) ? ? ? yes
C8 N2 C9 111.5(3) ? ? ? yes
C8 N2 C16 113.2(3) ? ? ? yes
C9 N2 C16 109.5(3) ? ? ? yes
N4 N3 C9 117.1(3) ? ? ? yes
N4 N3 C11 111.8(3) ? ? ? yes
C9 N3 C11 131.1(3) ? ? ? yes
NI N4 N3 110.8(2) ? ? ? yes
NI N4 C13 143.5(3) ? ? ? yes
N3 N4 C13 105.2(3) ? ? ? yes
S1 C1 S2 117.7(3) ? ? ? yes
S1 C1 C2 126.0(3) ? ? ? yes
S2 C1 C2 116.3(3) ? ? ? yes
C1 C2 C3 124.1(4) ? ? ? yes
C1 C2 C6 125.8(4) ? ? ? yes
C3 C2 C6 109.9(4) ? ? ? yes
C2 C3 C4 104.7(4) ? ? ? yes
C3 C4 C5 106.9(4) ? ? ? yes
C4 C5 C6 105.2(4) ? ? ? yes
N1 C6 C2 127.4(4) ? ? ? yes
N1 C6 C5 122.8(4) ? ? ? yes
C2 C6 C5 109.8(4) ? ? ? yes
N1 C7 C8 108.6(3) ? ? ? yes
N2 C8 C7 107.9(3) ? ? ? yes
N2 C9 N3 105.6(3) ? ? ? yes
N3 C11 C10 122.5(4) ? ? ? yes
N3 C11 C12 105.8(4) ? ? ? yes
C10 C11 C12 131.7(4) ? ? ? yes
C11 C12 C13 108.1(4) ? ? ? yes
N4 C13 C12 109.1(4) ? ? ? yes
N4 C13 C14 123.8(4) ? ? ? yes
C12 C13 C14 127.1(4) ? ? ? yes
O1 C16 N2 107.7(3) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
NI S1 2.125(1) ? ? yes
NI N1 1.857(3) ? ? yes
NI N2 1.973(3) ? ? yes
NI N4 1.918(3) ? ? yes
CL O2 1.403(5) ? ? yes
CL O3 1.349(6) ? ? yes
CL O4 1.410(5) ? ? yes
CL O5 1.264(6) ? ? yes
S1 C1 1.719(4) ? ? yes
S2 C1 1.756(4) ? ? yes
S2 C15 1.775(7) ? ? yes
O1 C16 1.367(5) ? ? yes
O1 C17 1.410(6) ? ? yes
N1 C6 1.312(5) ? ? yes
N1 C7 1.479(5) ? ? yes
N2 C8 1.491(5) ? ? yes
N2 C9 1.474(5) ? ? yes
N2 C16 1.493(5) ? ? yes
N3 N4 1.376(4) ? ? yes
N3 C9 1.445(5) ? ? yes
N3 C11 1.342(5) ? ? yes
N4 C13 1.341(5) ? ? yes
C1 C2 1.351(6) ? ? yes
C2 C3 1.516(6) ? ? yes
C2 C6 1.420(6) ? ? yes
C3 C4 1.521(8) ? ? yes
C4 C5 1.524(7) ? ? yes
C5 C6 1.505(6) ? ? yes
C7 C8 1.490(6) ? ? yes
C10 C11 1.495(6) ? ? yes
C11 C12 1.361(6) ? ? yes
C12 C13 1.390(6) ? ? yes
C13 C14 1.489(6) ? ? yes
