#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/17/2011768.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2011768
loop_
_publ_author_name
'Hao, Qingli'
'Jian, Fangfang'
'Wang, Xin'
'Razak, Ibrahim Abdul'
'Shanmuga Sundara Raj, S.'
'Fun, Hoong-Kun'
_publ_section_title
;
 trans-Bis(2-aminopyridine-N)bis(O,O'-diisopropyl
 dithiophosphato-S,S')nickel(II)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              160
_journal_page_last               161
_journal_paper_doi               10.1107/S0108270100016073
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Ni(C6 H14 O2 PS2 )2 (C5 H6 N2 )2 ]'
_chemical_formula_moiety         'C22 H40 N4 Ni O4 P2 S4'
_chemical_formula_sum            'C22 H40 N4 Ni O4 P2 S4'
_chemical_formula_weight         673.47
_chemical_name_systematic
;
Trans-bis(aminopyridine)-bis(O,O'-diisopropyl dithiophosphato-S,S')nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.9380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.62960(10)
_cell_length_b                   16.3605(2)
_cell_length_c                   14.6386(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.49
_cell_volume                     1563.93(4)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL and  PARST (Nardelli, 1995)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measurement_device_type
;
Siemens SMART CCD area detector diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .058
_diffrn_reflns_av_sigmaI/netI    .059
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10833
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        negligible
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  .870
_exptl_absorpt_correction_T_min  .685
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             708
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .24
_exptl_crystal_size_min          .14
_refine_diff_density_max         .43
_refine_diff_density_min         -.71
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .97
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .97
_refine_ls_R_factor_all          .041
_refine_ls_R_factor_gt           .035
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0410P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .087
_reflns_number_gt                3246
_reflns_number_total             3823
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ln1110.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2011768
_cod_database_fobs_code          2011768
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 1.0000 .5000 .0000 .02178(9) Uani d S 1 . . Ni
P1 .91563(7) .37889(3) .14719(3) .02491(11) Uani d . 1 . . P
S1 1.19032(6) .40239(3) .11659(3) .02979(11) Uani d . 1 . . S
S2 .70622(6) .44565(3) .06641(3) .02791(11) Uani d . 1 . . S
O1 .9068(2) .38744(7) .25437(9) .0345(3) Uani d . 1 . . O
O2 .8653(2) .28386(7) .14268(9) .0338(3) Uani d . 1 . . O
N1 1.0261(2) .60077(8) .10370(10) .0263(3) Uani d . 1 . . N
N2 1.3746(2) .59021(11) .16186(12) .0438(4) Uani d . 1 . . N
H2A 1.3795 .5464 .1299 .053 Uiso calc R 1 . . H
H2B 1.4838 .6084 .1962 .053 Uiso calc R 1 . . H
C1 1.1957(3) .63046(11) .15812(12) .0309(4) Uani d . 1 . . C
C2 1.1896(3) .70225(13) .21090(15) .0454(5) Uani d . 1 . . C
H2C 1.3093 .7229 .2458 .055 Uiso calc R 1 . . H
C3 1.0081(4) .74135(14) .21067(17) .0534(6) Uani d . 1 . . C
H3A 1.0024 .7883 .2459 .064 Uiso calc R 1 . . H
C4 .8315(3) .71005(13) .15704(15) .0433(5) Uani d . 1 . . C
H4A .7052 .7350 .1565 .052 Uiso calc R 1 . . H
C5 .8482(3) .64201(10) .10541(13) .0310(4) Uani d . 1 . . C
H5A .7298 .6222 .0686 .037 Uiso calc R 1 . . H
C6 .9090(4) .46761(12) .29897(14) .0422(5) Uani d . 1 . . C
H6A .8738 .5099 .2515 .051 Uiso calc R 1 . . H
C7 .7457(5) .4639(2) .3587(2) .0786(9) Uani d . 1 . . C
H7A .6155 .4533 .3205 .118 Uiso calc R 1 . . H
H7B .7403 .5152 .3901 .118 Uiso calc R 1 . . H
H7C .7772 .4209 .4035 .118 Uiso calc R 1 . . H
C8 1.1183(5) .48395(18) .3529(2) .0699(8) Uani d . 1 . . C
H8A 1.2154 .4857 .3113 .105 Uiso calc R 1 . . H
H8B 1.1552 .4412 .3976 .105 Uiso calc R 1 . . H
H8C 1.1184 .5355 .3843 .105 Uiso calc R 1 . . H
C9 .8272(4) .24303(11) .05237(14) .0432(5) Uani d . 1 . . C
H9A .8422 .2827 .0038 .052 Uiso calc R 1 . . H
C10 .6097(4) .21280(18) .0378(2) .0836(10) Uani d . 1 . . C
H10A .5185 .2583 .0379 .125 Uiso calc R 1 . . H
H10B .5929 .1758 .0868 .125 Uiso calc R 1 . . H
H10C .5790 .1849 -.0207 .125 Uiso calc R 1 . . H
C11 .9838(4) .17673(15) .0533(2) .0648(7) Uani d . 1 . . C
H11A 1.1183 .2004 .0628 .097 Uiso calc R 1 . . H
H11B .9596 .1483 -.0049 .097 Uiso calc R 1 . . H
H11C .9737 .1391 .1026 .097 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N1 . 3_765 180.0 yes
N1 Ni1 S2 . 3_765 91.59(4) ?
N1 Ni1 S2 . . 88.41(4) yes
S2 Ni1 S2 3_765 . 180.0 ?
N1 Ni1 S1 . 3_765 87.90(4) ?
S2 Ni1 S1 . 3_765 99.060(14) ?
N1 Ni1 S1 . . 92.10(4) yes
S2 Ni1 S1 . . 80.940(14) yes
S1 Ni1 S1 3_765 . 180.0 yes
O1 P1 O2 . . 94.82(7) ?
O1 P1 S1 . . 113.44(6) ?
O2 P1 S1 . . 111.97(6) ?
O1 P1 S2 . . 113.49(6) ?
O2 P1 S2 . . 113.12(6) ?
S1 P1 S2 . . 109.44(3) yes
P1 S1 Ni1 . . 84.476(19) yes
P1 S2 Ni1 . . 85.142(19) yes
C6 O1 P1 . . 121.39(11) ?
C9 O2 P1 . . 119.09(11) ?
C1 N1 C5 . . 116.48(15) ?
C1 N1 Ni1 . . 128.81(12) ?
C5 N1 Ni1 . . 114.42(11) ?
N2 C1 N1 . . 118.99(16) ?
N2 C1 C2 . . 119.47(17) ?
N1 C1 C2 . . 121.54(18) ?
C3 C2 C1 . . 119.89(19) ?
C2 C3 C4 . . 119.08(19) ?
C5 C4 C3 . . 118.26(19) ?
C4 C5 N1 . . 124.69(18) ?
O1 C6 C8 . . 109.39(19) ?
O1 C6 C7 . . 105.67(19) ?
C8 C6 C7 . . 113.3(2) ?
O2 C9 C11 . . 108.08(19) ?
O2 C9 C10 . . 106.85(19) ?
C11 C9 C10 . . 114.11(19) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 . 2.2275(14) yes
Ni1 S2 . 2.4865(4) yes
Ni1 S1 . 2.5123(4) yes
P1 O1 . 1.5863(14) yes
P1 O2 . 1.5892(12) yes
P1 S1 . 1.9866(6) yes
P1 S2 . 1.9879(6) yes
O1 C6 . 1.464(2) yes
O2 C9 . 1.464(2) yes
N1 C1 . 1.351(2) ?
N1 C5 . 1.362(2) ?
N2 C1 . 1.350(2) ?
C1 C2 . 1.410(3) ?
C2 C3 . 1.362(3) ?
C3 C4 . 1.390(3) ?
C4 C5 . 1.361(3) ?
C6 C8 . 1.497(4) ?
C6 C7 . 1.505(4) ?
C9 C11 . 1.500(3) ?
C9 C10 . 1.504(3) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
O1 P1 S1 Ni1 . -127.36(5)
O2 P1 S1 Ni1 . 126.76(6)
S2 P1 S1 Ni1 . .50(3)
N1 Ni1 S1 P1 . 87.67(4)
N1 Ni1 S1 P1 3_765 -92.33(4)
S2 Ni1 S1 P1 3_765 179.617(19)
S2 Ni1 S1 P1 . -.383(19)
O1 P1 S2 Ni1 . 127.33(6)
O2 P1 S2 Ni1 . -126.11(6)
S1 P1 S2 Ni1 . -.51(3)
N1 Ni1 S2 P1 . -92.00(4)
N1 Ni1 S2 P1 3_765 88.00(4)
S1 Ni1 S2 P1 3_765 -179.618(19)
S1 Ni1 S2 P1 . .382(19)
O2 P1 O1 C6 . -169.77(15)
S1 P1 O1 C6 . 73.75(15)
S2 P1 O1 C6 . -51.98(16)
O1 P1 O2 C9 . 172.19(14)
S1 P1 O2 C9 . -70.14(15)
S2 P1 O2 C9 . 54.09(15)
S2 Ni1 N1 C1 3_765 -45.73(14)
S2 Ni1 N1 C1 . 134.27(14)
S1 Ni1 N1 C1 3_765 -126.60(14)
S1 Ni1 N1 C1 . 53.40(14)
S2 Ni1 N1 C5 3_765 127.76(11)
S2 Ni1 N1 C5 . -52.24(11)
S1 Ni1 N1 C5 3_765 46.89(11)
S1 Ni1 N1 C5 . -133.11(11)
C5 N1 C1 N2 . 177.49(17)
Ni1 N1 C1 N2 . -9.1(2)
C5 N1 C1 C2 . -2.5(3)
Ni1 N1 C1 C2 . 170.90(14)
N2 C1 C2 C3 . -177.2(2)
N1 C1 C2 C3 . 2.8(3)
C1 C2 C3 C4 . -.8(4)
C2 C3 C4 C5 . -1.1(4)
C3 C4 C5 N1 . 1.4(3)
C1 N1 C5 C4 . .4(3)
Ni1 N1 C5 C4 . -173.95(16)
P1 O1 C6 C8 . -102.5(2)
P1 O1 C6 C7 . 135.20(18)
P1 O2 C9 C11 . 120.07(17)
P1 O2 C9 C10 . -116.72(18)
