#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/83/4308338.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_4308338
loop_
_publ_author_name
'Patrick J. Lim'
'Damian A. Slizys'
'Edward R. T. Tiekink'
'Charles G. Young'
_publ_section_title
;
Formation of Mono(dithiolene)-Thiocarboxamido Complexes in Reactions of
Thio(dithiocarbamato)-Mo/W Complexes and Dimethyl Acetylenedicarboxylate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              114
_journal_page_last               121
_journal_paper_doi               10.1021/ic048882g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C26 H38 B N7 O4 S3 W '
_chemical_formula_sum            'C26 H38 B N7 O4 S3 W'
_chemical_formula_weight         803.47
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                102.23(1)
_cell_angle_beta                 108.84(1)
_cell_angle_gamma                91.56(1)
_cell_formula_units_Z            2
_cell_length_a                   12.219(2)
_cell_length_b                   13.088(2)
_cell_length_c                   11.403(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      20.9
_cell_volume                     1677.7(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et. al. 1993)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Rigaku AFC6R'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      -0.02899
_diffrn_orient_matrix_UB_12      -0.04016
_diffrn_orient_matrix_UB_13      0.05141
_diffrn_orient_matrix_UB_21      -0.05537
_diffrn_orient_matrix_UB_22      0.05342
_diffrn_orient_matrix_UB_23      0.00968
_diffrn_orient_matrix_UB_31      -0.06043
_diffrn_orient_matrix_UB_32      -0.04136
_diffrn_orient_matrix_UB_33      -0.07964
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.065
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8096
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.6
_diffrn_reflns_theta_max         27.6
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -11.0
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.671
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type
;
\DF (DIFABS; Walker & Stuart, 1983)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.99
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.070
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0459P)²+1.5791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.099
_reflns_number_gt                6077
_reflns_number_total             7733
_reflns_threshold_expression     I>2.00σ(I)
_cod_data_source_file            ic048882gsi20040817_084428_2.cif
_cod_data_source_block           Tp*W{S2C2(CO2Me)2}(SCNEt2-?2S,C)
_cod_original_cell_volume        1677.8(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H38 B N7 O4 S3 W '
_cod_database_code               4308338
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -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
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.216587(19) 0.243923(17) 0.00899(2) 0.03292(7) Uani 1 1 d . . .
S1 S 0.05161(12) 0.21001(11) -0.17098(13) 0.0404(3) Uani 1 1 d . . .
S2 S 0.31019(12) 0.28302(12) -0.13835(13) 0.0403(3) Uani 1 1 d . . .
S3 S 0.14497(14) 0.36128(12) 0.14950(15) 0.0464(3) Uani 1 1 d . . .
O1 O 0.2614(5) 0.4339(4) -0.3497(5) 0.0790(16) Uani 1 1 d . . .
O2 O 0.2405(8) 0.2690(5) -0.4523(6) 0.121(3) Uani 1 1 d . . .
O3 O -0.1069(5) 0.2243(5) -0.4323(5) 0.0887(19) Uani 1 1 d . . .
O4 O 0.0074(6) 0.3425(7) -0.4573(8) 0.151(4) Uani 1 1 d . . .
N1 N 0.2093(5) 0.5038(4) 0.0415(5) 0.0543(13) Uani 1 1 d . . .
N11 N 0.2805(4) 0.0844(3) -0.0506(4) 0.0372(10) Uani 1 1 d . . .
N12 N 0.3363(4) 0.0350(4) 0.0435(4) 0.0390(10) Uani 1 1 d . . .
N21 N 0.1465(4) 0.1358(3) 0.1016(4) 0.0364(10) Uani 1 1 d . . .
N22 N 0.2229(4) 0.0881(4) 0.1865(4) 0.0414(11) Uani 1 1 d . . .
N31 N 0.3890(4) 0.2616(4) 0.1614(4) 0.0425(11) Uani 1 1 d . . .
N32 N 0.4184(4) 0.1859(4) 0.2317(4) 0.0434(11) Uani 1 1 d . . .
C1 C 0.0828(5) 0.2715(4) -0.2815(6) 0.0440(13) Uani 1 1 d . . .
C2 C 0.1944(5) 0.3001(5) -0.2667(5) 0.0431(13) Uani 1 1 d . . .
C3 C 0.2347(6) 0.3428(5) -0.3600(6) 0.0492(14) Uani 1 1 d . . .
C4 C 0.2837(16) 0.3081(11) -0.5434(12) 0.187(8) Uani 1 1 d . . .
H4A H 0.2209 0.3326 -0.6030 0.280 Uiso 1 1 calc R . .
H4B H 0.3145 0.2523 -0.5885 0.280 Uiso 1 1 calc R . .
H4C H 0.3437 0.3649 -0.4979 0.280 Uiso 1 1 calc R . .
C5 C -0.0155(6) 0.2758(6) -0.3957(6) 0.0572(17) Uani 1 1 d . . .
C6 C -0.0800(10) 0.3453(13) -0.5780(12) 0.198(9) Uani 1 1 d . . .
H6A H -0.1136 0.2751 -0.6234 0.297 Uiso 1 1 calc R . .
H6B H -0.0445 0.3761 -0.6279 0.297 Uiso 1 1 calc R . .
H6C H -0.1398 0.3867 -0.5624 0.297 Uiso 1 1 calc R . .
C11 C 0.2156(6) 0.0362(5) -0.2936(6) 0.0518(15) Uani 1 1 d . . .
H11A H 0.1439 0.0663 -0.2984 0.078 Uiso 1 1 calc R . .
H11B H 0.2001 -0.0295 -0.3556 0.078 Uiso 1 1 calc R . .
H11C H 0.2670 0.0835 -0.3105 0.078 Uiso 1 1 calc R . .
C12 C 0.2713(5) 0.0179(5) -0.1631(5) 0.0423(12) Uani 1 1 d . . .
C13 C 0.3231(6) -0.0717(5) -0.1384(6) 0.0490(14) Uani 1 1 d . . .
H13 H 0.3295 -0.1292 -0.1988 0.059 Uiso 1 1 calc R . .
C14 C 0.3627(5) -0.0604(4) -0.0104(6) 0.0424(13) Uani 1 1 d . . .
C15 C 0.4236(7) -0.1337(5) 0.0670(8) 0.0654(19) Uani 1 1 d . . .
H15A H 0.4384 -0.1940 0.0119 0.098 Uiso 1 1 calc R . .
H15B H 0.3757 -0.1557 0.1111 0.098 Uiso 1 1 calc R . .
H15C H 0.4960 -0.0985 0.1278 0.098 Uiso 1 1 calc R . .
C21 C -0.0683(5) 0.1542(5) 0.0383(6) 0.0509(15) Uani 1 1 d . . .
H21A H -0.0583 0.2283 0.0441 0.076 Uiso 1 1 calc R . .
H21B H -0.1296 0.1390 0.0694 0.076 Uiso 1 1 calc R . .
H21C H -0.0878 0.1167 -0.0490 0.076 Uiso 1 1 calc R . .
C22 C 0.0420(5) 0.1207(4) 0.1164(6) 0.0426(13) Uani 1 1 d . . .
C23 C 0.0533(6) 0.0651(5) 0.2099(6) 0.0511(15) Uani 1 1 d . . .
H23 H -0.0053 0.0448 0.2383 0.061 Uiso 1 1 calc R . .
C24 C 0.1674(6) 0.0456(5) 0.2525(6) 0.0493(14) Uani 1 1 d . . .
C25 C 0.2264(7) -0.0125(7) 0.3515(7) 0.073(2) Uani 1 1 d . . .
H25A H 0.2686 -0.0648 0.3173 0.109 Uiso 1 1 calc R . .
H25B H 0.1692 -0.0459 0.3762 0.109 Uiso 1 1 calc R . .
H25C H 0.2794 0.0360 0.4246 0.109 Uiso 1 1 calc R . .
C31 C 0.4799(6) 0.4384(5) 0.1685(7) 0.0637(19) Uani 1 1 d . . .
H31A H 0.4526 0.4206 0.0770 0.096 Uiso 1 1 calc R . .
H31B H 0.5588 0.4701 0.1996 0.096 Uiso 1 1 calc R . .
H31C H 0.4319 0.4871 0.1982 0.096 Uiso 1 1 calc R . .
C32 C 0.4744(5) 0.3408(5) 0.2163(6) 0.0448(13) Uani 1 1 d . . .
C33 C 0.5558(6) 0.3176(6) 0.3210(6) 0.0588(17) Uani 1 1 d . . .
H33 H 0.6224 0.3603 0.3759 0.071 Uiso 1 1 calc R . .
C34 C 0.5196(5) 0.2185(5) 0.3289(6) 0.0505(15) Uani 1 1 d . . .
C35 C 0.5739(7) 0.1550(7) 0.4230(7) 0.071(2) Uani 1 1 d . . .
H35A H 0.5300 0.1552 0.4793 0.106 Uiso 1 1 calc R . .
H35B H 0.6523 0.1848 0.4716 0.106 Uiso 1 1 calc R . .
H35C H 0.5745 0.0840 0.3786 0.106 Uiso 1 1 calc R . .
C41 C 0.2060(5) 0.4058(4) 0.0527(5) 0.0411(12) Uani 1 1 d . . .
C42 C 0.1659(8) 0.5862(5) 0.1206(8) 0.078(2) Uani 1 1 d . . .
H42A H 0.1015 0.5553 0.1379 0.093 Uiso 1 1 calc R . .
H42B H 0.1373 0.6393 0.0737 0.093 Uiso 1 1 calc R . .
C43 C 0.2580(11) 0.6368(9) 0.2433(10) 0.137(5) Uani 1 1 d . . .
H43A H 0.2265 0.6897 0.2918 0.205 Uiso 1 1 calc R . .
H43B H 0.3213 0.6687 0.2266 0.205 Uiso 1 1 calc R . .
H43C H 0.2855 0.5848 0.2908 0.205 Uiso 1 1 calc R . .
C44 C 0.2683(7) 0.5406(6) -0.0393(8) 0.069(2) Uani 1 1 d . . .
H44A H 0.3294 0.5960 0.0133 0.083 Uiso 1 1 calc R . .
H44B H 0.3041 0.4829 -0.0764 0.083 Uiso 1 1 calc R . .
C45 C 0.1869(11) 0.5804(8) -0.1421(10) 0.114(4) Uani 1 1 d . . .
H45A H 0.2281 0.6031 -0.1924 0.171 Uiso 1 1 calc R . .
H45B H 0.1527 0.6385 -0.1058 0.171 Uiso 1 1 calc R . .
H45C H 0.1269 0.5254 -0.1951 0.171 Uiso 1 1 calc R . .
B1 B 0.3464(6) 0.0792(5) 0.1816(7) 0.0434(15) Uani 1 1 d . . .
H1 H 0.3844 0.0308 0.2332 0.052 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'
B B 0.0013 0.0007 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-3 -1 0
-1 -3 0
-1 -3 1
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
_geom_angle_publ_flag
C41 W N31 91.3(2) . . ?
C41 W N21 121.78(19) . . ?
N31 W N21 89.73(17) . . ?
C41 W N11 161.5(2) . . ?
N31 W N11 79.59(17) . . ?
N21 W N11 74.65(16) . . ?
C41 W S1 94.51(16) . . ?
N31 W S1 170.72(13) . . ?
N21 W S1 93.29(12) . . ?
N11 W S1 92.74(12) . . ?
C41 W S3 44.28(16) . . ?
N31 W S3 90.31(13) . . ?
N21 W S3 77.51(12) . . ?
N11 W S3 150.34(12) . . ?
S1 W S3 98.91(6) . . ?
C41 W S2 84.59(16) . . ?
N31 W S2 90.36(13) . . ?
N21 W S2 153.62(12) . . ?
N11 W S2 79.43(12) . . ?
S1 W S2 83.04(5) . . ?
S3 W S2 128.86(5) . . ?
C1 S1 W 106.7(2) . . ?
C2 S2 W 103.3(2) . . ?
C41 S3 W 58.97(19) . . ?
C3 O2 C4 113.3(7) . . ?
C5 O4 C6 117.2(7) . . ?
C41 N1 C42 121.4(6) . . ?
C41 N1 C44 122.3(6) . . ?
C42 N1 C44 115.9(5) . . ?
C12 N11 N12 106.6(4) . . ?
C12 N11 W 135.4(4) . . ?
N12 N11 W 117.8(3) . . ?
C14 N12 N11 109.3(5) . . ?
C14 N12 B1 128.7(5) . . ?
N11 N12 B1 121.4(4) . . ?
C22 N21 N22 105.8(4) . . ?
C22 N21 W 133.2(4) . . ?
N22 N21 W 119.3(3) . . ?
C24 N22 N21 110.2(5) . . ?
C24 N22 B1 130.6(5) . . ?
N21 N22 B1 118.7(4) . . ?
C32 N31 N32 106.2(4) . . ?
C32 N31 W 133.0(4) . . ?
N32 N31 W 120.2(3) . . ?
C34 N32 N31 110.3(5) . . ?
C34 N32 B1 130.6(5) . . ?
N31 N32 B1 118.5(4) . . ?
C2 C1 C5 123.2(6) . . ?
C2 C1 S1 119.7(5) . . ?
C5 C1 S1 116.6(5) . . ?
C1 C2 C3 125.5(5) . . ?
C1 C2 S2 122.4(5) . . ?
C3 C2 S2 111.9(4) . . ?
O1 C3 O2 123.1(6) . . ?
O1 C3 C2 124.9(6) . . ?
O2 C3 C2 112.0(6) . . ?
O3 C5 O4 121.6(6) . . ?
O3 C5 C1 125.4(6) . . ?
O4 C5 C1 112.9(6) . . ?
N11 C12 C13 108.7(5) . . ?
N11 C12 C11 126.8(5) . . ?
C13 C12 C11 124.5(5) . . ?
C14 C13 C12 107.6(5) . . ?
C13 C14 N12 107.6(5) . . ?
C13 C14 C15 129.9(6) . . ?
N12 C14 C15 122.4(6) . . ?
N21 C22 C23 109.5(5) . . ?
N21 C22 C21 124.5(5) . . ?
C23 C22 C21 126.0(5) . . ?
C24 C23 C22 107.0(5) . . ?
N22 C24 C23 107.5(5) . . ?
N22 C24 C25 123.2(6) . . ?
C23 C24 C25 129.3(6) . . ?
N31 C32 C33 109.7(5) . . ?
N31 C32 C31 124.4(5) . . ?
C33 C32 C31 125.9(6) . . ?
C32 C33 C34 107.3(6) . . ?
N32 C34 C33 106.5(5) . . ?
N32 C34 C35 123.3(6) . . ?
C33 C34 C35 130.2(6) . . ?
N1 C41 S3 124.0(5) . . ?
N1 C41 W 158.6(5) . . ?
S3 C41 W 76.8(2) . . ?
N1 C42 C43 112.0(8) . . ?
C45 C44 N1 111.9(8) . . ?
N12 B1 N32 110.1(5) . . ?
N12 B1 N22 107.7(5) . . ?
N32 B1 N22 111.2(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W C41 2.088(5) . ?
W N31 2.225(5) . ?
W N21 2.237(4) . ?
W N11 2.294(4) . ?
W S1 2.3165(15) . ?
W S3 2.3723(15) . ?
W S2 2.4425(14) . ?
S1 C1 1.762(6) . ?
S2 C2 1.736(6) . ?
S3 C41 1.701(6) . ?
O1 C3 1.198(8) . ?
O2 C3 1.292(8) . ?
O2 C4 1.478(11) . ?
O3 C5 1.188(8) . ?
O4 C5 1.306(8) . ?
O4 C6 1.453(10) . ?
N1 C41 1.317(7) . ?
N1 C42 1.479(8) . ?
N1 C44 1.483(9) . ?
N11 C12 1.358(7) . ?
N11 N12 1.371(6) . ?
N12 C14 1.366(7) . ?
N12 B1 1.521(8) . ?
N21 C22 1.355(7) . ?
N21 N22 1.379(6) . ?
N22 C24 1.349(7) . ?
N22 B1 1.535(8) . ?
N31 C32 1.342(7) . ?
N31 N32 1.387(6) . ?
N32 C34 1.352(7) . ?
N32 B1 1.523(8) . ?
C1 C2 1.350(8) . ?
C1 C5 1.472(8) . ?
C2 C3 1.504(8) . ?
C11 C12 1.497(8) . ?
C12 C13 1.387(8) . ?
C13 C14 1.355(9) . ?
C14 C15 1.492(8) . ?
C21 C22 1.492(8) . ?
C22 C23 1.387(8) . ?
C23 C24 1.370(9) . ?
C24 C25 1.497(9) . ?
C31 C32 1.500(9) . ?
C32 C33 1.382(8) . ?
C33 C34 1.389(10) . ?
C34 C35 1.493(9) . ?
C42 C43 1.488(13) . ?
C44 C45 1.472(11) . ?
