#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2011768.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_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 '\w 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/[\s^2^(Fo^2^)+(0.0410P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .087
_reflns_number_gt 3246
_reflns_number_total 3823
_reflns_threshold_expression I>2\s(I)
_[local]_cod_data_source_file ln1110.cif
_[local]_cod_data_source_block I
_[local]_cod_cif_authors_sg_H-M 'P 21/n'
_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_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_database_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_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_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni1 .01822(16) .02211(16) .02495(17) .00007(10) .00359(11) .00248(10)
P1 .0262(2) .0222(2) .0264(2) -.00074(15) .00482(17) .00325(15)
S1 .0225(2) .0320(2) .0342(2) .00169(16) .00279(17) .00615(17)
S2 .0206(2) .0295(2) .0336(2) .00070(15) .00472(16) .00493(16)
O1 .0483(8) .0293(6) .0266(7) .0005(5) .0088(6) .0033(5)
O2 .0429(8) .0236(6) .0350(7) -.0053(5) .0072(6) .0032(5)
N1 .0244(7) .0269(7) .0281(8) -.0041(5) .0057(6) -.0013(5)
N2 .0255(8) .0526(10) .0500(11) -.0044(7) -.0026(7) -.0106(8)
C1 .0305(9) .0341(9) .0275(9) -.0063(7) .0030(7) .0006(7)
C2 .0466(12) .0447(12) .0412(12) -.0102(9) -.0031(9) -.0123(9)
C3 .0673(16) .0417(12) .0504(14) -.0003(11) .0081(11) -.0198(10)
C4 .0431(11) .0404(11) .0474(12) .0076(9) .0108(9) -.0086(9)
C5 .0292(9) .0302(9) .0338(10) .0007(7) .0063(7) -.0015(7)
C6 .0638(14) .0300(9) .0324(10) .0041(9) .0067(9) .0002(8)
C7 .080(2) .081(2) .081(2) .0141(17) .0339(17) -.0246(17)
C8 .080(2) .0699(17) .0564(17) -.0188(15) .0014(14) -.0150(13)
C9 .0611(14) .0277(9) .0388(12) -.0070(9) .0030(10) -.0025(8)
C10 .0525(16) .0640(18) .122(3) -.0019(13) -.0197(17) -.0339(17)
C11 .0645(17) .0536(14) .0784(19) -.0002(12) .0185(14) -.0247(13)
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_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)