#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2200224.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_2200224
loop_
_publ_author_name
'Esterhuysen, Catharine'
'Kruger, Gert J.'
'Olivier, Denise K.'
'Raubenheimer, Helgard G.'
'Retief, Lizette'
'Cronje, Stephanie'
_publ_section_title
;
Tricarbonylbis(4-methyl-1,3-thiazole-2(3H)-thionato-N,S^2^)tungsten(II)
;
_journal_issue 2
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first m72
_journal_page_last m74
_journal_volume 57
_journal_year 2001
_chemical_formula_iupac '[W (C4 H4 N1 S2)2 (C O)3]'
_chemical_formula_moiety 'C11 H8 N2 O3 S4 W1'
_chemical_formula_sum 'C11 H8 N2 O3 S4 W'
_chemical_formula_weight 528.28
_chemical_name_systematic
;
Tricarbonylbis(4-methyl-1,3-thiazole-2(3H)-thionato-N,S^2^)tungsten(II)
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 97.672(11)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.6233(9)
_cell_length_b 10.2686(8)
_cell_length_c 16.272(2)
_cell_measurement_reflns_used 46
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 17.7
_cell_measurement_theta_min 4.5
_cell_volume 1593.6(3)
_computing_cell_refinement PWPC
_computing_data_collection 'PWPC (Gomm, 1998)'
_computing_data_reduction 'Xtal3.4 (Hall et al., 1995)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material SHELXL97
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full .939
_diffrn_measured_fraction_theta_max .939
_diffrn_measurement_device_type 'Philips PW1100'
_diffrn_measurement_method \w--2\q
_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 .069
_diffrn_reflns_av_sigmaI/netI .026
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 2993
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.0
_diffrn_reflns_theta_min 3.1
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 50
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 7.781
_exptl_absorpt_correction_T_max .459
_exptl_absorpt_correction_T_min .160
_exptl_absorpt_correction_type '\y scan'
_exptl_absorpt_process_details '(North et al., 1968)'
_exptl_crystal_colour orange-red
_exptl_crystal_density_diffrn 2.202
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1000
_exptl_crystal_size_max .25
_exptl_crystal_size_mid .23
_exptl_crystal_size_min .10
_refine_diff_density_max 1.20
_refine_diff_density_min -2.28
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.07
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 192
_refine_ls_number_reflns 2817
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.07
_refine_ls_R_factor_all .048
_refine_ls_R_factor_gt .036
_refine_ls_shift/su_max <0.001
_refine_ls_shift/su_mean .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0809P)^2^+1.9916P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .119
_reflns_number_gt 2259
_reflns_number_total 2817
_reflns_threshold_expression I>2\s(I)
_[local]_cod_data_source_file tk6003.cif
_[local]_cod_data_source_block I
_[local]_cod_cif_authors_sg_H-M 'P 21/c'
_[local]_cod_chemical_formula_sum_orig 'C11 H8 N2 O3 S4 W1'
_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_original_cell_volume 1593.5(3)
_cod_database_code 2200224
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
W1 .77064(3) .49051(3) .251981(18) .03869(17) Uani d . 1 W
S1 .9670(2) .5556(2) .16984(16) .0556(6) Uani d . 1 S
S2 .9807(3) .3314(3) .04536(14) .0596(6) Uani d . 1 S
S3 .5427(2) .3713(3) .25474(15) .0573(6) Uani d . 1 S
S4 .3383(3) .5057(3) .11324(19) .0667(8) Uani d . 1 S
O1 .7009(13) .5300(10) .4311(5) .109(4) Uani d . 1 O
O2 1.0234(7) .3820(7) .3731(5) .072(2) Uani d . 1 O
O3 .7901(8) .7905(7) .2826(5) .083(2) Uani d . 1 O
N1 .8226(7) .3411(6) .1584(4) .0387(14) Uani d . 1 N
N2 .5983(7) .5501(7) .1540(4) .0390(14) Uani d . 1 N
C1 .7224(14) .5151(11) .3636(6) .069(3) Uani d . 1 C
C2 .9311(9) .4205(9) .3271(6) .050(2) Uani d . 1 C
C3 .7821(9) .6805(10) .2734(6) .056(2) Uani d . 1 C
C4 .9179(9) .4073(8) .1255(5) .0448(19) Uani d . 1 C
C5 .8752(10) .2031(9) .0599(5) .055(2) Uani d . 1 C
H5 .8720 .1278 .0281 .065 Uiso calc R 1 H
C6 .7975(9) .2199(8) .1210(5) .0438(18) Uani d . 1 C
C7 .6995(12) .1248(9) .1508(7) .077(3) Uani d . 1 C
H7A .7284 .1066 .2084 .115 Uiso calc R 1 H
H7B .7003 .0456 .1195 .115 Uiso calc R 1 H
H7C .6065 .1604 .1438 .115 Uiso calc R 1 H
C8 .4967(10) .4719(9) .1732(6) .047(2) Uani d . 1 C
C9 .4191(10) .6244(11) .0629(6) .061(3) Uani d . 1 C
H9 .3731 .6749 .0203 .074 Uiso calc R 1 H
C10 .5558(9) .6370(8) .0914(5) .0426(18) Uani d . 1 C
C11 .6554(11) .7337(11) .0649(7) .071(3) Uani d . 1 C
H11A .7327 .6891 .0457 .106 Uiso calc R 1 H
H11B .6898 .7885 .1110 .106 Uiso calc R 1 H
H11C .6084 .7861 .0209 .106 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
W1 .0334(2) .0424(2) .0399(2) .00635(13) .00322(14) -.00361(13)
S1 .0446(13) .0429(12) .0818(17) -.0065(10) .0172(11) -.0041(11)
S2 .0550(14) .0776(17) .0488(13) .0063(12) .0161(10) -.0084(12)
S3 .0423(12) .0674(15) .0643(14) -.0018(11) .0147(10) .0191(12)
S4 .0353(13) .093(2) .0693(16) -.0069(12) -.0028(11) .0131(13)
O1 .135(10) .143(8) .054(5) .058(7) .025(5) -.002(5)
O2 .059(4) .065(4) .085(5) .020(4) -.015(4) .002(4)
O3 .080(5) .047(4) .114(6) .021(4) -.015(4) -.021(4)
N1 .033(3) .041(4) .043(3) -.002(3) .007(3) .000(3)
N2 .034(4) .037(3) .045(4) -.002(3) .003(3) -.005(3)
C1 .078(8) .085(8) .043(5) .037(6) .009(5) .002(5)
C2 .042(5) .049(5) .058(5) .016(4) .004(4) -.002(4)
C3 .041(5) .056(6) .064(5) .026(4) -.015(4) .005(4)
C4 .038(4) .051(5) .047(4) .006(4) .010(4) .000(4)
C5 .063(6) .044(5) .054(5) .000(4) .000(4) -.020(4)
C6 .049(5) .033(4) .047(4) -.002(4) -.001(4) -.006(3)
C7 .087(8) .035(5) .109(9) -.019(5) .010(7) -.017(5)
C8 .034(5) .057(5) .052(5) .004(4) .011(4) .007(4)
C9 .049(6) .075(7) .058(6) -.005(5) -.003(4) .011(5)
C10 .044(5) .037(4) .046(4) .003(4) .004(3) .009(3)
C11 .070(7) .073(7) .069(6) -.009(6) .008(5) .021(5)
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'
O O .0106 .0060 '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'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -.8490 6.8722 '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_publ_flag
C1 W1 C3 74.0(4) yes
C1 W1 C2 74.6(4) yes
C3 W1 C2 103.3(4) yes
C1 W1 N2 112.6(4) ?
C3 W1 N2 82.8(3) ?
C2 W1 N2 171.9(3) ?
C1 W1 N1 144.6(4) ?
C3 W1 N1 140.6(3) ?
C2 W1 N1 86.8(3) ?
N2 W1 N1 85.1(2) yes
C1 W1 S3 74.3(4) ?
C3 W1 S3 120.2(3) ?
C2 W1 S3 115.1(3) ?
N2 W1 S3 65.09(18) yes
N1 W1 S3 87.35(17) yes
C1 W1 S1 137.8(4) ?
C3 W1 S1 78.8(3) ?
C2 W1 S1 81.2(3) ?
N2 W1 S1 94.95(18) yes
N1 W1 S1 65.07(16) yes
S3 W1 S1 147.86(8) yes
C4 S1 W1 78.8(3) ?
C4 S2 C5 88.1(4) ?
C8 S3 W1 80.0(3) ?
C9 S4 C8 89.5(4) ?
C4 N1 C6 112.0(7) ?
C4 N1 W1 98.8(5) ?
C6 N1 W1 149.2(5) ?
C8 N2 C10 114.2(7) ?
C8 N2 W1 99.5(5) ?
C10 N2 W1 145.9(5) ?
O1 C1 W1 176.6(12) ?
O2 C2 W1 177.7(8) ?
O3 C3 W1 177.2(9) ?
N1 C4 S2 114.6(7) ?
N1 C4 S1 117.0(6) ?
S2 C4 S1 128.4(5) ?
C6 C5 S2 114.2(6) ?
C6 C5 H5 122.9 ?
S2 C5 H5 122.9 ?
C5 C6 N1 111.1(7) ?
C5 C6 C7 127.1(8) ?
N1 C6 C7 121.8(8) ?
C6 C7 H7A 109.5 ?
C6 C7 H7B 109.5 ?
H7A C7 H7B 109.5 ?
C6 C7 H7C 109.5 ?
H7A C7 H7C 109.5 ?
H7B C7 H7C 109.5 ?
N2 C8 S3 115.3(7) ?
N2 C8 S4 111.3(6) ?
S3 C8 S4 133.1(6) ?
C10 C9 S4 113.0(7) ?
C10 C9 H9 123.5 ?
S4 C9 H9 123.5 ?
C9 C10 N2 112.0(8) ?
C9 C10 C11 127.3(8) ?
N2 C10 C11 120.7(7) ?
C10 C11 H11A 109.5 ?
C10 C11 H11B 109.5 ?
H11A C11 H11B 109.5 ?
C10 C11 H11C 109.5 ?
H11A C11 H11C 109.5 ?
H11B C11 H11C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
W1 C1 1.950(10) yes
W1 C3 1.982(10) yes
W1 C2 1.973(9) yes
W1 N2 2.227(7) yes
W1 N1 2.264(6) yes
W1 S3 2.517(2) yes
W1 S1 2.545(2) yes
S1 C4 1.724(9) ?
S2 C4 1.698(8) ?
S2 C5 1.699(10) ?
S3 C8 1.692(9) ?
S4 C9 1.712(10) ?
S4 C8 1.732(10) ?
O1 C1 1.154(12) ?
O2 C2 1.152(10) ?
O3 C3 1.140(12) ?
N1 C4 1.311(10) ?
N1 C6 1.392(10) ?
N2 C8 1.334(11) ?
N2 C10 1.374(10) ?
C5 C6 1.332(12) ?
C5 H5 .9300 ?
C6 C7 1.484(12) ?
C7 H7A .9600 ?
C7 H7B .9600 ?
C7 H7C .9600 ?
C9 C10 1.341(12) ?
C9 H9 .9300 ?
C10 C11 1.484(12) ?
C11 H11A .9600 ?
C11 H11B .9600 ?
C11 H11C .9600 ?